HYDROTHERMAL PROCESS FOR MANUFACTURING SILVER NANOFILS FILTERS

专利摘要:
The invention relates to a method for producing filtered silver nanowires having a high aspect ratio, wherein the total glycol concentration is <0.001% by weight at any time.
公开号:FR3037266A1
申请号:FR1655244
申请日:2016-06-08
公开日:2016-12-16
发明作者:George L Athens；Raymond M Collins；William R Bauer；Patrick T Mcgough；Janet M Goss；George J Frycek；Wei Wang；Jonathan D Lunn；Robin P Ziebarth；Richard A Patyk
申请人:Dow Global Technologies LLC；
IPC主号:

专利说明:

[0001] The present invention relates generally to the field of manufacturing silver nanowires. In particular, the present invention relates to a method for producing filtered silver nanowires having a high aspect ratio for use in a variety of applications. [0002] High conductivity films with high transparency are of great value for use as electrodes or coatings in a wide range of electronic applications, including, for example, touchscreen displays and cells. PV. Current technology for these applications involves the use of films containing tin-doped indium oxide (ITO) that are deposited by physical vapor deposition processes. The high capital cost of physical vapor deposition processes has led to the desire to find other transparent conductive materials and other coating approaches. The use of dispersed silver nanowires in the form of a percolation network has emerged as a promising alternative to films containing ITO. The use of silver nanowires has the potential advantage that they can be implemented using roll-to-roll techniques. Thus, silver nanowires have the advantage of low cost manufacturing with the potential to provide higher transparency and conductivity than conventional ITO containing films. [73] The "polyol process" has been described for the manufacture of silver-based nanostructures. The polyol process utilizes ethylene glycol (or other glycol) both as a solvent and as a reducing agent in the production of silver nanowires. The use of glycols, however, has several inherent disadvantages. Specifically, the use of a glycol as both a reducing agent and a solvent leads to a decrease in control of the reaction because the main species of reducing agent (glycolaldehyde) is produced in situ and its presence and concentration are dependent on the extent of exposure to oxygen. Also, the use of a glycol introduces the possibility of formation of combustible glycol / air mixtures in the free space of the reactor used to produce the silver nanowires. Finally, the use of large volumes of glycol creates rejection problems, which increases the cost of marketing such operations. [An approach constituting an alternative to the polyol process for making silver nanowires has been described by Miyagishima, et al. In US Patent Application Publication No. 20100078197. Miyagishima, et al. disclose a method for producing metal nanowires, comprising: adding a solution of a metal complex to an aqueous solvent containing at least one halide as a reducing agent, and heating the resulting mixture to 150 ° C or less, wherein the metal nanowires comprise metal nanowires having a diameter of 50 nm or less and a major axis length of 5 μm or more in an amount of 50% by mass or more in terms of the amount of metal relative to the total metal particles . [0005] An alternative approach to the polyol process for making silver nanowires has been disclosed by Lunn, et al. in U.S. Patent Application Publication No. 20130283974. Lunn, et al. disclose a method for making silver nanowires having a high aspect ratio, wherein the recovered silver nanowires have an average diameter of 25 to 80 nm and an average length of 10 to 100 μm; and where the total glycol concentration is <0.001% wt at any time during the process. However, while producing silver nanowires having a desirable high aspect ratio, the manufacturing method described by Lunn, et al. Also leads to the formation of silver nanowire populations having an extended diameter distribution which can lead to a lack of uniformity in the electrical properties of the produced films. [0007] Thus, there remains a need for other methods of manufacturing silver nanowires; in particular, processes for manufacturing filtered silver nanowires which do not involve the use of glycol, wherein the filtered silver nanowires produced have a low content of silver nanoparticles. [0008] The present invention provides a method for making filtered silver nanowires having a high aspect ratio comprising: providing a container; the supply of an initial volume of water; the supply of an initial reducing sugar; providing an initial polyvinylpyrrolidone (PVP), wherein the initial polyvinylpyrrolidone (PVP) provided can be divided into a first portion of the initial polyvinylpyrrolidone (PVP) and a second portion of the initial polyvinylpyrrolidone (PVP); providing an initial copper (II) ion source; providing an initial halide ion source; providing an initial silver ion source, wherein the initial silver ion source provided can be divided into a first portion of the initial silver ion source and a second portion of the original silver ion source; adding the initial water volume, the initial reducing sugar, the initial copper (II) ion source and the initial halide ion source to the vessel to form a combination; heating the combination at a temperature between 110 and 160 ° C (including end values); mixing the first portion of the initial polyvinylpyrrolidone (PVP) with the first portion of the original silver ion source to form a polyvinylpyrrolidone / mixed silver ion source; adding the polyvinylpyrrolidone / silver ion source mixed with the combination into the vessel to form a creation mixture; then, following a delay period, adding to the vessel the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the initial silver ion source to form a growth mixture ; maintaining the growth mixture at a temperature between 110 and 160 ° C (including end values) for a hold period of 2 to 30 hours to produce a raw feed where the total glycol concentration in the vessel is < 0.001% by weight; where the raw feed produced comprises mother liquor and silver solids; where the mother liquor comprises the initial volume of water; and wherein the silver solids in the raw feed include silver nanowires having a high aspect ratio and silver particles having a low aspect ratio; Providing a dynamic filtration device, wherein the dynamic filtration device comprises: a housing, comprising: a cavity having a first side and a second side; wherein there is at least one inlet in the first side of the cavity, at least one product outlet from the first side of the cavity and at least one permeate outlet from the second side of the cavity; and a porous member disposed in the cavity; a turbulence inducing element disposed in the cavity; and a source of pressure; wherein the porous member is interposed between the first side of the cavity and the second side of the cavity; wherein the porous member has a plurality of passages therethrough from the first side of the cavity to the second side of the cavity; wherein the passages of this plurality of passages are sufficiently large to allow transfer of the mother liquor and silver particles having a low aspect ratio and sufficiently small to block the transfer of silver nanowires having an aspect ratio. high; wherein the porous element and the turbulence-inducing element cooperate to form a filtration gap, F6; and wherein at least one of the porous element and the turbulence inducing element is movable; providing a transport fluid, wherein the transport fluid comprises an additional volume of water and an additional polyvinylpyrrolidone (PVP); transferring the raw feed to the dynamic filtration device through the at least one inlet in the first side of the cavity; transferring a volume of the transport fluid to the dynamic filtration device through the at least one inlet in the first side of the cavity; where the filtration interval, FG, is filled with water; wherein the porous element and the turbulence-inducing element disposed in the cavity are both in contact with water; pressurizing the first side of the cavity by means of the pressure source which leads to a first-side pressure, FSp, in the first side of the cavity; where the first side pressure, FSp, is higher than a second side pressure, SSp, in the second side of the cavity, so that a pressure drop (PEA) is created through the porous element from the first side of the cavity to the second side of the cavity; wherein the source of pressure provides a primary driving force for inducing a current from the first side of the cavity through the porous member to the second side of the cavity, thereby producing a permeate; moving at least one of the porous element and the turbulence-inducing element such that a shear stress is produced in the water in the filtration range, FG; where the shear stress produced in water in the filtration range, FG, acts to reduce fouling of the porous member; removing the permeate from the at least one permeate outlet from the second side of the cavity, where the permeate comprises a second cut of the mother liquor and a second fraction of the silver solids; where the second fraction of the silver solids is rich in silver particles having a low aspect ratio; and removing a product from the at least one product outlet from the first side of the cavity, wherein the product comprises a first cut of the mother liquor and a first fraction of the silver solids; where the first fraction of the silver solids is depleted of silver particles having a low aspect ratio; and where the shear stress produced in the water in the filtration gap, FG, and the pressure drop (PEA) through the porous element from the first side of the cavity to the second side of the cavity are decoupled. According to alternative embodiments of the process of the invention, to be considered independently or in combination: the transporting fluid further comprises a source of additional halide ions; the transport fluid further comprises an additional reducing sugar; the process further comprises: removing (preferably by centrifugation) silver solids from the permeate to provide a purified permeate; and recycling the purified permeate into the dynamic filtration device through the at least one inlet in the first side of the cavity; the transport fluid then preferably comprising the purified permeate; the first part of the initial polyvinylpyrrolidone (PVP) represents 10 to 40% by weight of the polyvinylpyrrolidone (PVP) supplied; and the first portion of the initial silver ion source is 10 to 40% by weight of the silver ion source supplied; The method further comprises providing a pH adjusting agent; adding the pH adjusting agent to the combination prior to adding the polyvinylpyrrolidone / mixed silver ion source, wherein the combination has a pH of 2.0 to 4.0 before the addition of the Polyvinylpyrrolidone / silver ion source mixed with the container; the method further comprises: providing a reducing agent; adding the reducing agent to the creation mixture. the method further comprises: purging a gas space of the container in contact with the combination in the container to provide a reduced oxygen gas concentration in the container gas space; bubbling into the initial silver ion source provided with an inert gas to drive the oxygen gas from the source of the initial silver ion supplied and to give a low concentration of oxygen gas in an ion gas space silver in contact with the original silver ion source provided; purging a polyvinylpyrrolidone (PVP) gas space in contact with the initial polyvinylpyrrolidone (PVP) provided to give a dilute oxygen gas concentration in the polyvinylpyrrolidone (PVP) gas space; maintaining the low oxygen gas concentration in the silver ion gas space and the oxygen gas concentration diluted in the polyvinylpyrrolidone (PVP) gas space; and maintaining the reduced oxygen gas concentration in the container gas space during the addition of the polyvinylpyrrolidone / mixed silver ion source, during formation of the growth mixture, and during the holding period.
[0002] BRIEF DESCRIPTION OF THE DRAWINGS [0010] Figure 1 shows a dynamic filtration device of the present invention. [0011] Fig. 2 is a cross-sectional view taken along the line in Fig. 1. [0012] Fig. 3 shows a perspective view of a porous member disposed in a dynamic filtration device of the present invention. Figure 4 shows a dynamic filtration device 30 of the present invention with an associated permeate container.
[0003] DETAILED DESCRIPTION [0014] A method has been found for making filtered silver nanowires having a high aspect ratio which surprisingly allows the efficient separation of silver particles having a low aspect ratio from one another. with the silver solids present in a raw feed without significant loss of silver nanowires having a desired high aspect ratio or significant reduction in the average length of silver nanowires recovered in the product. It has been found that the composition of the transport fluid used in the separation process is critical to provide a product consisting of silver nanowires having a high aspect ratio having a high purity of the silver nanowires having a ratio high aspect ratio, where the fraction of nanowires, is 0.9. It has also been observed that the total flow rate of transporting fluid entering the filtering device can be minimized by the judicious choice of the content of transport fluid components. Finally, it has been observed that the judicious choice of the component content of the transport fluid imparts stability to the product consisting of silver nanowires having a high aspect ratio recovered. For example, the product consisting of silver nanowires having a high aspect ratio recovered in the method of the invention facilitates the formation of optical films having improved optical quality with less entanglement of wires and visible defects. The term "total glycol concentration" as used herein means the combined total of the concentration of all glycols (eg, ethylene glycol, propylene glycol, butylene glycol, poly (ethylene glycol), poly (propylene glycol)) present in the container. The term "silver nanowires having a high aspect ratio" as used herein refers to silver solids having an aspect ratio of> 3. The term "particles having a high aspect ratio" as used herein refers to silver solids having an aspect ratio of> 3. silver having a low aspect ratio "as used herein means silver solids having an aspect ratio of 3. The term" fraction by gross weight "or" Ir.kuten such that it is used herein means the weight of silver nanowires having a high aspect ratio in the raw feed divided by the total weight of the silver solids contained in the raw feed. [0019] The term " fraction by weight of permeate "or" WFpermeat "as used herein means the weight of silver nanowires having a high aspect ratio in the permeate divided by the total weight of the silver solids contained in the permeate The term "fraction by weight of product" or "WFproduct as used herein means the weight of silver nanowires having a ratio of in the product divided by the total weight of the silver solids contained in the product. The term "first side pressure" or "np" as used herein means the pressure measured in the first side (35) of the cavity (30) relative to the atmospheric pressure on the outer side of the housing (20). The term "second side pressure" or "Sn" as used herein means the pressure measured in the second side (17) of the cavity (30) relative to atmospheric pressure on the side outside the housing (20). The term "pressure drop across the porous member" or "PEN" as used herein means the difference between the first side pressure, FS, and the second side pressure, SSp, c. The term "substantially constant" as used herein with reference to the cross-sectional area, Xire, of a passageway (55) through a porous member (50). ) means that the largest cross-sectional area, the L-oirer presented by the passage given perpendicularly to the permeate stream through the thickness, T, of the porous member (55) may be greater than at 20% at the smallest cross-sectional area, as shown by the passage. The term "substantially perpendicular" as used herein with reference to an axisymmetry axis, axisym, of a passageway (55) through a porous member (50) means that the axis of symmetry, axesym, meets the upper surface (E2) of the porous element (50) at an angle, y, of 85 to 95 °. The term "fraction of silver nanowires having a high aspect ratio" or "NWF" used herein is the fraction of silver nanowires of a sample of silver nanowires determined according to the following equation : fK / F = TA where TA is the total surface area of a substrate which is occluded by a sample of given deposited silver nanowires; and k-LIA is the portion of the total occluded surface area that can be attributed to silver nanowires having a high aspect ratio in the deposited silver solids sample by the method described herein in the examples . [0027] Preferably, the method for producing filtered silver nanowires having a high aspect ratio according to the present invention comprises: providing a container; the supply of an initial volume of water; the supply of an initial reducing sugar; providing an initial polyvinylpyrrolidone (PVP), wherein the initial polyvinylpyrrolidone (PVP) provided can be divided into a first portion of the initial polyvinylpyrrolidone (PVP) and a second portion of the initial polyvinylpyrrolidone (PVP); providing an initial copper (II) ion source; providing an initial halide ion source; providing an initial silver ion source, wherein the initial silver ion source provided can be divided into a first portion of the initial silver ion source and a second portion of the original silver ion source; adding the initial water volume, the initial reducing sugar, the initial copper (II) ion source and the initial halide ion source to the vessel to form a combination; heating the combination at a temperature between 110 and 160 ° C (including end values); mixing the first portion of the initial polyvinylpyrrolidone (PVP) with the first portion of the original silver ion source to form a polyvinylpyrrolidone / mixed silver ion source; adding the polyvinylpyrrolidone / silver ion source mixed with the combination into the vessel to form a creation mixture; then, following a delay period, adding to the vessel the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the original silver ion source to form a growth mixture; maintaining the growth mixture at a temperature between 110 and 160 ° C (including end values) for a holding period of 2 to 15 hours to produce a raw feed (5) where the total glycol concentration in the container is <0.001% by weight; where the raw feed produced comprises mother liquor and silver solids; where the mother liquor comprises the initial volume of water; and where the silver solids in the raw feed (5) include silver nanowires having a high aspect ratio and silver particles having a low aspect ratio (preferably, where the feed crude has a fraction by gross weight, Li Brute); providing a dynamic filtration device (10), wherein the dynamic filtration device (10) comprises: a housing (20), comprising: a cavity (30) having a first side (35) and a second side (30); where there is at least one inlet (32) in the first side (35) of the cavity (30), at least one product outlet (37) from the first side (35) of the cavity (30), and minus one permeate outlet (47) from the second side (45) of the cavity (), and a porous member (51) disposed in the cavity (30), a turbulence-inducing member (60) disposed in the cavity ( 30) and a pressure source (; C), wherein the porous member 30 (50) is interposed between the first side (35) of the cavity (30) and the second side (45) of the cavity (30). wherein the porous member (50) has a plurality of passages (55) therethrough from the first side (35) of the cavity (30) to the second side (45) of the cavity (30); passages 5 (55) of this plurality of passages (55) are large enough to allow transfer of the mother liquor and silver particles having a low aspect ratio and sufficiently small to block the transfer of silver nanowires having a high aspect ratio ; wherein the porous member (50) and the turbulence-inducing member (60) cooperate to form a filtration gap, FG; and wherein at least one of the porous member (50) and the turbulence inducing member (60) is movable; providing a transport fluid, wherein the transport fluid comprises an additional volume of water and an additional polyvinylpyrrolidone (PVP); (Preferably, where the raw feed comprises the entire contents of the container, preferably, wherein the raw feed has a fraction by gross weight, 1: the transfer of the raw feed (5) - .rutei to the feed device. dynamic filtration (10) through the at least one inlet (32) in the first side (35) of the cavity (30), transferring a volume (150) of the transport fluid to the dynamic filtration device (10) by The at least one inlet (32) in the first side (35) of the cavity (30) (it should be noted here incidentally that, obviously, the raw supply and the volume of transport fluid in question are not necessarily transferred to the dynamic filtering device by the same inlet in the first side of the cavity (the advantageous variant of the transfers by the same inlet 32 being shown in FIGS. 1 and 4)), where the filtration interval, FG, is filled by water, where the porous element (30) and the turbulence inducing element (60) disposed in the cavity (30) are both in contact with the water; pressurizing the first side (35) of the cavity (30) by means of the pressure source (70) which leads to a first side pressure F5p in the first side (35) of the cavity 3037266 13 (30); where the first side pressure, F.Sp, is greater than a second side pressure, 5.5p, in the second side (45) of the cavity (30), so that there is creation of a pressure drop (PEA) through the porous member (50) from the first side (35) of the cavity (30) to the second side (47) of the cavity (30); wherein the pressure source (70) provides a primary driving force for inducing a current from the first side (35) of the cavity (30) through the porous member (50) to the second side (45) of the cavity (30), which produces a permeate; initiating (preferably continuously moving) at least one of the porous member (50) and the turbulence inducing member (60) such that a shear stress is produced in water in the filtration range, F6; wherein the shear stress produced in water in the filtration range, FG, acts to reduce fouling of the porous member (50); removing the permeate from the at least one permeate outlet (47) from the second side (45) of the cavity (30), where the permeate comprises a second cut of the mother liquor and a second fraction of the silver solids ; wherein the second fraction of the silver solids is rich in silver particles having a low aspect ratio (preferably where the permeate has a weight fraction of permeate, preferably, where > WFPermeat, more preferably, where vifF .- - .rute> WFPermeat 0.05, more preferably, where IVA - - ..rute> WFPermeat 0,01; particularly preferably, where HIA - - .rute> WFPermeat 0, 001); and removing a product from the at least one product outlet (37) from the first side (35) of the cavity (30), wherein the product comprises a first cut of the mother liquor and a first fraction of the solids money; wherein the first fraction of silver solids is depleted of silver particles having a low aspect ratio (preferably, where the product has a weight fraction of product, preferably produced, where rute <WFProduct; more preferably, where 14 / F. - - .rute <WFProduct 0.8; more preferably still, where WFt. - - <WFProduct 0.85; particularly preferably, where wF. urute <:: fFProduct 0.9); and where the shear stress produced in water in the filtration gap, FG ', and the pressure drop (PEA) through the porous member (50) from the first (35) side of the cavity ( 30) to the second side (45) of the cavity (30) are decoupled (i.e. they can be controlled independently).  (See Figure 1)  [7. 777] Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the initial polyvinylpyrrolidone (PVP) supplied is divided into a first portion of the initial polyvinylpyrrolidone (PVP) and a second part of the initial polyvinylpyrrolidone (PVP); and the supplied initial silver ion source is divided into a first portion of the initial silver ion source and a second portion of the original silver ion source; wherein the first portion of the initial polyvinylpyrrolidone (PVP) is mixed with the first portion of the initial silver ion source to form the polyvinylpyrrolidone / mixed silver ion source; where the remaining initial polyvinylpyrrolidone (PVP) is the second part of the initial polyvinylpyrrolidone (PVP); and where the remaining initial silver ion source is the second part of the original silver ion source.  Preferably, the first part of the initial polyvinylpyrrolidone (PVP) is 10 to 40% by weight (preferably 10 to 30% by weight, more preferably 15 to 25% by weight, particularly preferably % by weight) of the initial polyvinylpyrrolidone (PVP) provided; and the first part of the initial silver ion source is 10 to 40% by weight (preferably 10 to 30% by weight, more preferably 15 to 25% by weight, particularly preferably 20% by weight ) of the initial silver ion source provided.  Preferably, the polyvinylpyrrolidone / mixed silver ion source is added to the combination in the container for a charging time of 10 seconds to 10 minutes (more preferably 30 seconds to 5 minutes; , from 30 to 90 seconds).  Preferably, the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the original silver ion source are added to the container for a feed time of 1 to 60 minutes (more preferably 1 to 30 minutes). minutes, particularly preferably from 1 to 15 minutes).  [0029] Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the initial polyvinylpyrrolidone (PVP) supplied is divided into a first portion and a second portion and the source the initial silver ion supplied is divided into a first part and a second part; wherein the first portion of the initial polyvinylpyrrolidone (PVP) and the first portion of the original silver ion source are mixed to form the polyvinylpyrrolidone / mixed silver ion source.  Preferably, the first part of the initial polyvinylpyrrolidone (PVP) and the first part of the initial silver ion source are mixed during a pre-mixing period of 0.5 seconds to 4 hours (preferably 0.5 second at 1 hour, more preferably 1 minute to 1 hour, particularly preferably 5 minutes to 1 hour) to form the polyvinylpyrrolidone / mixed silver ion source.  The first part of the initial polyvinylpyrrolidone (PVP) and the first part of the initial silver ion source are mixed during the pre-mixing period with any method known to those skilled in the art.  Preferably, the first part of the initial polyvinylpyrrolidone (PVP) and the first part of the original silver ion source are mixed by mixing the first part of the initial polyvinylpyrrolidone (PVP) and the first part of the source of the initial polyvinylpyrrolidone (PVP). initial silver ions in a closed container (preferably under an inert atmosphere such as nitrogen); and simultaneously transferring the first portion of the initial polyvinylpyrrolidone (PVP) and the first portion of the original silver ion source through a conduit common to the combination in the container.  When the residence time in the common conduit for the first part of the initial polyvinylpyrrolidone (PVP) and the first part of the initial silver ion source is equal to the pre-mixing period, the premixing period is preferably from 2 to 30 seconds; more preferably, from 2 to 15 seconds; particularly preferably from 2 to 10 seconds.  [Cm21] Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the ion source initial silver can be added to the contents of the container successively, simultaneously as separate feeds, simultaneously in the form of a mixed feed or according to a certain combination of these variants (for example, some successively, some simultaneously as feeds). separated and some simultaneously as a mixed feed).  Preferably, at least one of the second part of the initial polyvinylpyrrolidone (PVP) and the second part of the initial silver ion source is added to the container at a point below the surface of the combination in the container.  More preferably, at least the second portion of the initial silver ion source is added to the container at a point beneath a surface of the combination in the container.  Preferably, the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the original silver ion source are added to the container simultaneously as separate feeds, simultaneously as a mixed feed or as a certain combination of these variants (for example, some simultaneously as separate feeds and some simultaneously as a mixed feed).  Particularly preferably, the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the original silver ion source are added to the container as a mixed feed.  Preferably, the mixed feed is added to the combination at a point below the surface of the combination in the container.  The mixed feed can be formed in the same manner as described for the formation of polyvinylpyrrolidone / mixed silver ion source, where the second part of the initial polyvinylpyrrolidone (PVP) and the second part of the initial silver ion source used are mixed for a mixing time of 0.5 seconds to 4 hours (preferably 0.5 seconds to 2 hours, more preferably 5 minutes to 1.5 hours, particularly preferably minutes to 1 hour) to form the mixed feed.  Preferably, the mixing time is the pre-mixing period.  [0031] Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, the raw feed (5) comprises: mother liquor and silver solids; where the mother liquor comprises the initial volume of water; and wherein the silver solids in the raw feed (5) include silver nanowires having a high aspect ratio and silver particles having a low aspect ratio.  Preferably, the raw feed comprises the entire contents of the container after the holding period.  Preferably, the silver solids are suspended in the mother liquor.  Preferably, the raw feed contains 5.  2% by weight of silver solids.  More preferably, the raw feed contains 0.01 to 1% by weight (more preferably 0.05 to 0.75% by weight, particularly preferably 0.1 to 0.5% by weight). ) silver solids.  [0032] Preferably, in the process for making filtered silver nanowires having a high aspect ratio of the present invention, the silver solids contained in the raw feed include silver nanowires having a ratio of high aspect ratio and silver particles having a low aspect ratio.  Preferably, the raw feed has a crude weight fraction, WFBrute, of silver nanowires having a high aspect ratio to silver particles having a low aspect ratio.  Preferably, the crude weight fraction, WFBrute, is maximized by the method used to synthesize silver nanowires having a high aspect ratio.  Nevertheless, the synthesis of silver nanowires having a high aspect ratio invariably gives a certain amount of undesirable silver particles having a low aspect ratio which desirably are removed in such a way that product weight, wF. . .  - produced> L Brute.  [0033] Preferably, in the process for making filtered silver nanowires having a high aspect ratio of the present invention, the supplied transport fluid comprises: an additional water volume and an additional polyvinylpyrrolidone (PVP).  More preferably, the supplied transport fluid comprises: an additional volume of water; additional polyvinylpyrrolidone (PVP); and at least one of an additional reducing sugar, an additional halide ion source, an additional copper (II) ion source and an additional silver ion source.  More preferably, the transport fluid provided comprises: a purified permeate, wherein the silver solids have been removed from the permeate.  Those skilled in the art will be able to choose a suitable method for removing silver solids from the permeate to provide a purified permeate.  Preferably, the silver solids are removed from the permeate by at least one method selected from filtration and centrifugation to provide a purified permeate.  Particularly preferably, the transport fluid provided comprises: an additional water volume, an additional polyvinylpyrrolidone (PVP) and an additional halide ion source.  Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, the transport fluid provided has a pH of 2 to 5 (more preferably 2.5 at 4.5, particularly preferably from 3 to 4).  [0035] Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, the supplied transport fluid is transferred to the dynamic filtration device by the at least one input into the filter. first side of the cavity.  Preferably, the volume of transport fluid can be transferred to the dynamic filtration device in a manner selected from at least one of the transfer of a single charge, the transfer of a plurality of charges (where the charges can contain the same quantity or different amounts of the transport fluid) and transfer continuously.  More preferably, the method for producing high aspect ratio filtered silver nanowires of the present invention comprises: transferring a volume of the transport fluid to the dynamic filtration device by the at least one input into the the first side of the cavity; where the concentration of the silver solids in the first side of the cavity is controlled by adjusting the volume of the transport fluid transferred to the first side of the cavity.  Most preferably, the method for producing high aspect ratio filtered silver nanowires of the present invention comprises: transferring a volume of the transport fluid to the dynamic filtration device through the at least one inlet in the first side of the cavity; where the concentration of the silver solids in the first side of the cavity is maintained at 2% by weight.  More preferably, the volume of transport fluid transferred to the dynamic filtration device is controlled such that the concentration of the silver solids in the first side of the cavity is maintained at 0.01 to 1% by weight ( more preferably, 0.05 to 0.75% by weight, particularly preferably 0.1 to 0.5% by weight).  Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, the raw feed (5) is transferred to the dynamic filtration device by means of a fluid moving device (80).  Those of ordinary skill in the art will be able to choose a fluid setting device (80) suitable for use with the raw feed.  Preferably, in the method for producing high aspect ratio filtered silver nanowires of the present invention, the fluid moving device (80) used to transfer the raw feed (5) to the device dynamic filtration system (10) is decoupled from the driving force used to induce a pressure drop (PEA) through the porous element (50) from the first side (35) of the cavity (30) in the dynamic filtration device (10) to the second side (45) of the cavity (30).  More preferably, the raw feed is transferred to the dynamic filtration device (10) by means of a low shear fluid (FO) setting device, such as a peristaltic pump or system head pressure ( for example, the gravity or the pressure of an inert gas).  Preferably, when a system head pressure is used as a fluid moving device (LI) to facilitate the transfer of the raw feed (5) to the dynamic filtration device (10), the delivery device fluid movement (80) further comprises a fluid valve () (preferably a fluid control valve) for regulating the rate at which the raw feed (5) is transferred to the dynamic filtration device (10).  (See Figure 1)  3.  Preferably, the method for producing high aspect ratio filtered silver nanowires of the present invention further comprises: providing a liquid level detector (90) and a control circuit ( 95), wherein the liquid level detector (90) and the control circuit (SZ) are integrated with the dynamic filtration device (10) and the fluid actuator (80) (preferably a peristaltic pump or system head pressure coupled with a control valve (85) for maintaining a stable liquid level (100) in the housing (20) such that the filtration gap (FG) remains filled with water.  (See Figure 1)  Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, the volume (. -. . 50) of transport fluid is transferred to the dynamic filtration device (10) by means of a liquid moving device (140).  Those skilled in the art will be able to select a liquid moving device (140) suitable for use with the transport fluid.  Preferably, in the method for producing silver nanowires having a high aspect ratio of the present invention, the liquid moving device (14r) used to transfer the volume (150) of transport fluid to the dynamic filtration device (10) is decoupled from the driving force used to induce a pressure drop (PEA) through the porous member (50) from the first side (35) of the cavity (30) in the filtration device dynamic (10) to the second side (45) of the cavity (30).  More preferably, the volume (150) of transport fluid is transferred to the dynamic filtration device (10) by means of a pump or pressure at the head of the system (for example, the gravity or pressure of the an inert gas).  Preferably, the dynamic filtration device (10) further comprises a liquid valve (145) (preferably a liquid control valve (1 44) for regulating the transfer of transport fluid to the dynamic filtration device (10). ).  (See Figure 4)  Preferably, the method for producing filtered silver nanowires having a high aspect ratio of the present invention further comprises: providing a liquid level detector (90) and a control circuit ( 95), wherein the liquid level detector 3037266 (90) and the control circuit (95) (preferably where the control circuit includes a programmable logic controller) are integrated with the dynamic filter device (10). ), the fluid moving device (80) (preferably a peristaltic pump or a system head pressure coupled with a fluid control valve (85)) and a liquid control valve (145) to maintain a stable liquid level (±) in the housing (20) such that the filtration interval (FG) remains filled by the mother liquor.  (See Figure 4)  Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the porous member (50) used in the dynamic filtration device (10) has a plurality of passages (55) extending therethrough from the first side (35) of the cavity (30) to the second side (45) of the cavity (30); wherein the passages (55) of this plurality of passages (55) are sufficiently large to allow the transfer of mother liquor and silver particles having a low aspect ratio and sufficiently small to block transfer of silver nanowires having a high aspect ratio.  More preferably, each passageway (55) in the plurality of passages (55) has a cross-sectional area, Xaire, perpendicular to the permeate flow through the thickness, T, of the porous member (0). ; wherein the cross-sectional area, Taire, is substantially constant over the thickness, T, of the porous element (S -. ).  Preferably, the porous member (50) has a pore size of 1 to 10 μm (more preferably 2 to 8 μm, more preferably 2 to 5 μm, most preferably 2.5 to 3.5 μm).  Preferably, the porous element is chosen from curved porous elements and flat porous elements.  More preferably, the porous element is a flat porous element.  Preferably, in the process for manufacturing silver nanowires having a high aspect ratio of the present invention, the porous element (50) used in the dynamic filtration device (10) is a porous membrane.  More preferably, the porous element (50) is a polycarbonate membrane made porous by track etch technology (PCTE).  (See Figures 1-3).  [C 7 -1] Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, shear stress is produced in the water present in the filtration range. , FG; wherein the shear stress induces sufficient movement in the water tangentially to the upper surface (52) of the porous member (50) to reduce or prevent clogging or fouling of the porous member.  Shear stress is produced by relative movement between the porous member (50) and the turbulence-inducing member (60) adjacent to the filtration gap, FG.  Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the porous element (50) is stationary relative to the cavity (30) and the element inducing turbulence (60) moves relative to the porous member (50).  Preferably, when the porous member (50) is a flat, stationary porous member, the turbulence inducing member (60) rotates in a plane near the upper surface (52) of the porous member (50).  More preferably, when the porous member (50) is a flat porous membrane, the turbulence inducing member (60) is a stirrer.  Preferably, the agitator is selected from the group consisting of a stirring bar, a stirring bar suspended and attached to (or in a piece with) a shaft, and an impeller mounted on a tree.  Preferably, the porous membrane is flat and has an upper surface (52) and a lower surface (54); wherein the upper surface (52) and the lower surface (54) are parallel; wherein the porous membrane has a thickness, measured from the upper surface (52) to the lower surface (54) along a line (A) perpendicular to the upper surface (52); and wherein the upper surface (52) faces the turbulence-inducing element (60).  Preferably, the turbulence-inducing member (60) provided with the flat porous membrane is a shaker with an impeller; wherein the impeller is rotated continuously in a plane disposed in the first side (35) of the cavity (30).  Preferably, the filtration interval is defined by the plane in which the pallet is continuously rotated and the upper surface (52) of the porous member (50) close to the pallet (more preferably, where the plane is parallel to the upper surface of the porous element).  (See Figures 1-3).  [0043] Preferably, in the process for making filtered silver nanowires having a high aspect ratio of the present invention, the turbulence-inducing element has a permeable surface.  More preferably, when the turbulence-inducing element has a permeable surface, the permeable surface is interposed between the first side of the cavity and the second side of the cavity and at least a certain fraction of the permeate removed from the dynamic filtration device passes through the permeable surface of the turbulence-inducing element from the first side of the cavity to the second side of the cavity.  Preferably, when the turbulence inducing member has a permeable surface, the permeable surface of the turbulence-inducing member faces the plurality of passages of the porous member.  Preferably, when the turbulence inducing member has a permeable surface, the permeable surface is curved and disposed about a central axis of rotation; where the turbulence inducing element rotates about the central axis.  More preferably, when the turbulence inducing member has a curved permeable surface disposed about a central axis of rotation; wherein the turbulence-inducing element rotates about the central axis; the porous member also has a curved surface disposed about a central axis of rotation; wherein the curved surface of the porous member has a plurality of passageways therethrough from the first side of the cavity to the second side of the cavity; wherein the porous member rotates about its central axis; wherein the curved permeable surface of the turbulence inducing member faces the curved surface of the porous member; wherein the space interposed between the curved permeable surface of the turbulence-inducing element and the curved surface of the porous element defines the filtration gap, FG.  Preferably, the central axis of rotation of the turbulence-inducing element and that of the porous element are parallel.  According to one variant, the turbulence-inducing element and the porous element rotate in the same direction.  According to another variant, the turbulence-inducing element and the porous element rotate in opposite directions.  [0044] Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, the filtration gap, FG, is disposed in the filter housing and is interposed between the first side (35) of the cavity (30) and the second side (45) of the cavity (30); where the filtration range, FG, is defined by two opposing surfaces; wherein at least one of the opposing surfaces is movable; and wherein the porous member (50) provides at least one of the opposing surfaces.  The filtration gap, FG, is typically formed between opposite, oppositely disposed surfaces which are separated from each other by a distance of from 1 to 25 mm (preferably from 1 to 20 mm). and more preferably from 1 to 15 mm, particularly preferably from 1 to 10 mm).  Preferably, the size of the filtration gap, FG, is substantially constant on the opposite surface formed by the porous member (50) (i.e., the largest dimension of the filtration gap, FGSL, and the smallest dimension of the filtration interval, F17. f. between the opposite surfaces 3037266 26 are linked in the following manner: 0.9 FGSL FGSs FGSL).  (See Figures 1 and 4).  [0045] Preferably, in the process for producing filtered silver nanowires having a high aspect ratio of the present invention, at least one of the porous element (50) and the turbulence-inducing element is moves relative to the other to produce a shear stress in water in a filtration gap, FG, between the opposed surfaces of the porous member (50) and the turbulence-inducing member (60).  More preferably, at least one of the porous element (50) and the turbulence-inducing element (60) moves continuously with respect to the other to produce shear stress in water in a filtration gap, FG, between the opposed surfaces of the porous element (50) and the turbulence-inducing element (r- ').  Preferably, the shear stress produced in the filtration gap, FG, induces sufficient movement in the water tangentially to the surface of the porous member that faces the first side (35) of the cavity (30). to reduce or prevent clogging or fouling of the porous element.  Preferably, the porous member (50) and the turbulence inducing member (60) move relative to each other at a relative velocity of 0.4 to 1.5 m / s (preferably still, from 0.6 to 1.3 m / s, particularly preferably from 0.9 to 1.1 m / s).  [46] Preferably, the shear stress produced in the water disposed in the filtration gap, FG, and the pressure drop across the porous member from the first side of the cavity to the second side of the cavity. the cavity are decoupled.  Particularly preferably, the shear stress produced in the water disposed in the filtration gap, FG, and the pressure drop across the porous member from the first side of the cavity to the second side of the chamber. cavity can be controlled independently.  Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the pressure source provides the primary driving force for permeate passage through the element. porous to the second side of the cavity.  Preferably, the pressure source is a gas pressure exerted on the first side of the cavity.  More preferably, the gas pressure exerted on the first side of the cavity is the pressure of an inert gas.  Particularly preferably, the gas pressure exerted on the first side of the cavity is a nitrogen pressure.  The gas pressure can be applied to the first side of the cavity as a gaseous free space above the liquid level in the cavity.  Alternatively, the first side of the cavity provided may further comprise a pocket; where the bag is pressurized with the gas.  Preferably, the pressure source induces a pressure drop across the porous element of 5 to 70 kPa (preferably 10 to 55 kPa, more preferably 15 to 40 kPa, most preferably 20 to 35 kPa).  [0048] Preferably, the method for producing high aspect ratio filtered silver nanowires of the present invention further comprises: periodically establishing an inverted flow through the porous member (50) from the second side (45) of the cavity (30) to the first side (35) of the cavity (30).  Those skilled in the art will be able to choose appropriate means for establishing the reverse current.  More preferably, the method for producing silver nanowires having a high aspect ratio of the present invention further comprises: periodically establishing an inverted stream through the porous member (50) since the second side (d-7) of the cavity (30) to the first side (35) of the cavity (30), where the reverse current is set for a period of 1 to 10 seconds (more preferably 2.5 at 7.5 seconds, particularly preferably from 3 to 5 seconds) every 10 to 60 seconds (more preferably every 15 to 40 seconds, particularly preferably every 20 to 30 seconds).  [0049] Preferably, the method for producing high aspect ratio filtered silver nanowires of the present invention further comprises: providing a conduit (120) for transferring permeate from the at least one outlet (47) from the second side (45) of the cavity (30) to a container (125) (preferably where there is an intermediate air layer (130) between the conduit (1. 7u) and the container (125).  More preferably, the method for manufacturing silver nanowires having a high aspect ratio of the present invention further comprises: providing a conduit (120) for transferring permeate from the at least one outlet (47); ) from the second side (45) of the cavity (30) to a container (125) (preferably where there is an intermediate air layer (130) between the conduit (120) and the container ( 125)); and periodically, reducing the momentary pressure of the first side (35) of the cavity (30) by releasing the pressure source (70) (for example by venting the first side of the cavity); wherein the conduit (120) contains a volume of permeate which is at a height which is higher than that of the liquid level (400) in the dynamic filtration device (10) (preferably, where the volume of permeate which is at a height which is higher than that of the liquid level (100) is at a higher height of 20 to 500 mm (more preferably 100 to 375 mm, particularly preferably 150 to 300 mm) such that, periodically, upon momentary pressure reduction of the first side (35) of the cavity (30) there is current reversal through the porous member (50) from the second side (45) from the cavity (30) to the first side (35) of the cavity).  Preferably, the periodic momentary pressure reduction is established for a period of 1 to 10 seconds (more preferably 2.5 to 7.5 seconds, particularly preferably 3 to 30 seconds). 10 to 60 seconds (more preferably every 15 to 40 seconds, particularly preferably every 20 to 30 seconds) of pressurization.  (See Figure 4)  [0050] Preferably, the method for producing filtered silver nanowires having a high aspect ratio of the present invention further comprises: providing a source of vibratory energy; and periodically applying vibratory energy from the vibratory energy source to the porous member.  [0051] Preferably, the method for producing filtered silver nanowires having a high aspect ratio of the present invention further comprises: providing a source of ultrasonic energy; and periodically applying ultrasonic energy from the ultrasonic energy source to the porous member.  [00: 2] Preferably, the method for making filtered silver nanowires having a high aspect ratio of the present invention further comprises: removing the silver solids from the permeate to provide a purified permeate; and recycling the purified permeate into the dynamic filtration device through the at least one inlet to the first side of the cavity (it may also be noted incidentally here that, of course, the raw feed, the transport fluid volume in cause, and the recycled permeate are not necessarily introduced into the dynamic filtration device by the same inlet in the first side of the cavity (they are however advantageously, very advantageously with the purified permeate in the transport fluid (see below). after)).  Preferably, the silver solids are removed from the permeate by any suitable method known to those skilled in the art to provide the purified permeate.  More preferably, the silver solids are removed by at least one method selected from filtration and centrifugation to provide the purified permeate.  Most preferably, the transport fluid comprises the purified permeate.  [0053] Preferably, the process for producing high aspect ratio filtered silver nanowires of the present invention provides a volumetric flow of permeate through the porous element of 20 to 1000 L / m2. hour (more preferably from 140 to 540 L / m2. hour ; Particularly preferably from 280 to 360 L / m2. hour).  Preferably, the initial water volume and additional water provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are each independently at least one water selected from deionized water and distilled water to limit the presence of accidental impurities.  More preferably, the initial water volume and additional water provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are both deionized and distilled.  Most preferably, the initial water volume and additional water provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are each ultrapure water which meets the requirements of the present invention. or exceeds the requirements for Type 1 water according to ASTM D1193-99e1 ("Standard Specification for Reagent Water").  [0055] Preferably, the initial reducing sugar and additional reducing sugar, if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are independently selected in the group consisting of at least one of the aldoses (e.g., glucose, glyceraldehyde, galactose, mannose); disaccharides with a free hemiacetal unit (eg, lactose and maltose); and sugars carrying a ketone (eg, fructose).  More preferably, the initial reducing sugar and the additional reducing sugar, if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are independently selected in the present invention. group 3037266 31 EN1655244 irregularity notification July 2016 No apparent changes consisting of at least one of an aldose, lactose, maltose and fructose.  More preferably, the initial reducing sugar and additional reducing sugar, if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are independently selected from the group consisting of at least one of glucose, glyceraldehyde, galactose, mannose, lactose, fructose and maltose.  Preferably, the initial reducing sugar and the additional reducing sugar, present, provided are the same.  Particularly preferably, the initial reducing sugar and the additional reducing sugar, if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention are each D -glucose.  [0056] Preferably, the initial polyvinylpyrrolidone (PVP) and the additional polyvinylpyrrolidone (PVP), if any, provided in the process for producing filtered silver nanowires having a high aspect ratio of the present invention. Each invention has a weight average molecular weight, Mw, of 20000 to 300000 u.  More preferably, the initial polyvinylpyrrolidone (PVP) and polyvinylpyrrolidone (PVP), if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention have each has a weight average molecular weight, Mw, of 30000 to 200000 u.  Particularly preferably, the initial polyvinylpyrrolidone (PVP) and polyvinylpyrrolidone (PVP), if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention. each have a weight average molecular weight, Mw, of 40000 to 60000 u.  Preferably, the initial copper (II) ion source and additional copper (II) ions, if any, provided in the process for making filtered silver nanowires having a ratio of High aspect of the present invention are independently selected from the group consisting of at least one of CuCl 2 and Cu (NO 3) 2.  More preferably, the initial copper (II) ion source and additional copper (II) ions, if any, provided in the process for making filtered silver nanowires having a high aspect ratio. of the present invention are independently selected from the group consisting of CuCl 2 and Cu (NO 3) 2.  Preferably, the source of copper (II) initial ions and the additional copper (II) ions present, provided, are the same.  Particularly preferably, the initial copper (II) ion source and additional copper (II) ions, if any, provided in the process for making filtered silver nanowires having an aspect ratio. of the present invention are each CuCl 2, where CuCl 2 is a copper (II) chloride dihydrate.  [_.  Preferably, the source of the initial halide ions and the additional halide ion source, if any, provided in the process for producing filtered silver nanowires having a high aspect ratio of the The present invention is independently selected from the group consisting of at least one of a chloride ion source, a fluoride ion source, a bromide ion source and an iodide ion source.  More preferably, the source of initial halide ions and the additional halide ion source, if any, provided in the process for producing high aspect ratio filtered silver nanowires of the present invention. are independently selected from the group consisting of at least one of a chloride ion source and a fluoride ion source.  More preferably, the source of the initial halide ions and the additional halide ion source, if any, provided in the process for making filtered silver nanowires having a high aspect ratio of the present invention. invention are each a source of chloride ions.  Preferably, the source of the initial halide ions and the additional source of halide ions present provided are the same.  Particularly preferably, the source of the initial halide ions and the additional halide ion source, if any, provided in the process for producing filtered silver nanowires having a high aspect ratio of the The present invention is each a source of chloride ions, wherein the source of chloride ions is an alkali metal chloride.  Preferably, the alkali metal chloride is selected from the group consisting of at least one of sodium chloride, potassium chloride and lithium chloride.  More preferably, the alkali metal chloride is selected from the group consisting of at least one of sodium chloride and potassium chloride.  Particularly preferably, the alkali metal chloride is sodium chloride.  Preferably, the initial silver ion source and the additional silver ion source, if any, provided in the process for producing filtered silver nanowires having a high aspect ratio of the present invention are each a silver complex.  More preferably, the initial silver ion source and the additional silver ion source, if any, provided in the process for producing filtered silver nanowires having a high aspect ratio of the present invention. Each invention is a silver complex, wherein the silver complex is selected from the group consisting of at least one of silver nitrate (AgNO3) and silver acetate (AgC2H302).  Particularly preferably, the initial silver ion source and the additional silver ion source, if any, provided in the process for producing filtered silver nanowires having a high aspect ratio of the The present invention is each silver nitrate (AgNO3).  Preferably, the initial silver ion source and the additional silver ion source, if any, provided in the process for making filtered silver nanowires having a high aspect ratio of the present invention. each has a silver concentration of from 0.005 to 1 times molar (M) (more preferably from 0.01 to 0.1 M, particularly preferably from 0.015 to 0.05 M).  [0060] Preferably, the initial water volume, the initial reducing sugar, the initial copper (II) ion source, the initial halide ion source and the pH adjusting agent, if there are, are added to the container in any order in an individual succession (i.e., one at a time), simultaneously (i.e., all at the same time), or semi-simultaneously (i.e. ie, some individually one at a time, some simultaneously simultaneously or in the form of sub-combinations).  More preferably, at least two of the initial water volume, the initial reducing sugar, the initial copper (II) ion source, the initial halide ion source and the pH adjusting agent are mixed together. to form a sub-combination prior to addition to the container.  [0061] Preferably, the initial volume of water is divided into multiple volumes (preferably at least two volumes of water, more preferably at least three volumes of water, particularly preferably at least five volumes). of water) which are then mixed with one or more of the initial reducing sugar, the initial copper (II) ion source, the initial halide ion source, the pH adjusting agent, There are some, the initial polyvinylpyrrolidone (PVP) supplied and the silver ion source supplied to form different sub-combinations which include water before addition to the container.  For example, the initial water volume is preferably divided into at least five volumes, where a first volume of water is combined with the initial reducing sugar to form a reducing sugar-containing sub-combination, where a second volume of water is added. The water is combined with the initial copper (II) ion source to form a sub-combination containing copper (II) ions, where a third volume of water is combined with the initial 3037266 halide ion source to form a sub-combination containing halide ions; wherein a fourth volume of water is combined with the supplied silver ion source to form a sub-combination containing silver ions (preferably, where the sub-combination containing silver ions is divided into a first part and a second one). part) ; and a fifth volume of water is combined with the initial polyvinylpyrrolidone (PVP) provided to form a polyvinylpyrrolidone (PVP) containing sub-combination (preferably, the polyvinylpyrrolidone-containing sub-combination (PVP) is divided into a first part and a second part).  These sub-combinations are then processed in a manner similar to the individual components in the previous discussion of the process for making filtered silver nanowires having a high aspect ratio of the present invention.  [2] The method for producing high aspect ratio filtered silver nanowires of the present invention preferably further comprises: providing a reducing agent; and adding the reducing agent to the creation mixture.  [C 1: 3] Preferably, the reducing agent provided in the process for producing high aspect ratio filtered silver nanowires of the present invention is selected from the group consisting of ascorbic acid, sodium borohydride (NaBH4), hydrazine, hydrazine salts, hydroquinone, C1-5 alkylaldehydes and benzaldehyde.  More preferably, the reducing agent provided in the process for producing high aspect ratio filtered silver nanowires of the present invention is selected from the group consisting of ascorbic acid, sodium borohydride (NaBH 4 ), hydrazine, hydrazine salts, hydroquinone, acetaldehyde, propionaldehyde and benzaldehyde.  Most preferably, the reducing agent provided in the process for producing high aspect ratio filtered silver nanowires of the present invention is selected from the group consisting of ascorbic acid and sodium borohydride. .  [0064] The method for producing filtered silver nanowires having a high aspect ratio of the present invention preferably further comprises: providing a pH adjusting agent; and adding the pH adjusting agent to the container.  The pH adjusting agent may be added to the container before the polyvinylpyrrolidone / mixed silver ion source is added to the container.  Preferably, when the pH adjusting agent is added to the combination prior to the addition of the polyvinylpyrrolidone / mixed silver ion source, the combination has a pH of 2.0 to 4.0 (preferably from 2.0 to 3.5, more preferably from 2.4 to 3.3, most preferably from 2.4 to 2.6) prior to addition of polyvinylpyrrolidone / mixed silver ion source to the container.  The pH adjusting agent can be added to the container simultaneously with the polyvinylpyrrolidone / mixed silver ion source.  Preferably, when the pH adjusting agent is added simultaneously with the polyvinylpyrrolidone / mixed silver ion source, the pH adjusting agent is added to the first part of the initial polyvinylpyrrolidone (PVP) before the mixing with the first portion of the silver ion source to form the polyvinylpyrrolidone / mixed silver ion source, wherein the first portion of the initial polyvinylpyrrolidone (PVP) has a pH of 2.0 to 4.0 (preferably, from 2.0 to 3.5, more preferably from 2.3 to 3.3, most preferably from 3.1 to 3.3).  Preferably, when the pH adjusting agent is added simultaneously with the polyvinylpyrrolidone / mixed silver ion source, the pH adjusting agent is also added to the second part of the initial polyvinylpyrrolidone (PVP), wherein the second portion of the initial polyvinylpyrrolidone (PVP) has a pH of 2.0 to 4.0 (preferably 2.0 to 3.5, more preferably 2.3 to 3.3; particularly preferably, from 3.1 to 3.3).  Preferably, the pH adjusting agent is added to the initial polyvinylpyrrolidone (PVP) supplied prior to division of the initial polyvinylpyrrolidone (PVP) provided in a first portion and a second portion, where the initial polyvinylpyrrolidone (PVP) provided at a pH of 2.0 to 4.0 (preferably 2.0 to 3.5, more preferably 2.3 to 3.3, most preferably 3.1 to 3 , 3).  [0065] Preferably, the pH adjusting agent provided in the process for producing filtered silver nanowires having a high aspect ratio of the present invention is an acid.  More preferably, the pH adjusting agent provided in the process for producing high aspect ratio filtered silver nanowires of the present invention is an acid, wherein the acid is selected from the group consisting of in at least one of the inorganic acids (eg, nitric acid, sulfuric acid, hydrochloric acid, fluorosulfuric acid, phosphoric acid, fluoroantimonic acid) and organic acids ( for example, methanesulfonic acid, ethanesulfonic acid, benzenesulfonic acid, acetic acid, fluoroacetic acid, chloroacetic acid, citric acid, gluconic acid, lactic acid).  Preferably, the pH adjusting agent provided in the process for making filtered silver nanowires having a high aspect ratio of the present invention has a pH value. <2.0. More preferably, the pH adjusting agent provided in the process for producing high aspect ratio filtered silver nanowires of the present invention includes nitric acid. Most preferably, the pH adjusting agent provided in the process for producing high aspect ratio filtered silver nanowires of the present invention is aqueous nitric acid. [0066] Preferably, the method for producing filtered silver nanowires having a high aspect ratio of the present invention further comprises: purging a gas space of the container in contact with the combination in the container to give a reduced oxygen gas concentration in the gas space of the container. Preferably, the step of purging the gas space of the container in contact with the combination in the container to give the reduced oxygen gas concentration in the container gas space includes: (i) isolation of the gas space of the container of a surrounding atmosphere outside the container; (ii) then pressurizing the vessel gas space with an inert gas (preferably, wherein the inert gas is selected from the group consisting of argon, helium, methane, and nitrogen (more preferably argon, helium and nitrogen, more preferably argon and nitrogen, particularly preferably nitrogen); and, (iii) thereafter purging the gas space of the vessel to provide the reduced oxygen gas concentration in the gas space of the vessel. Preferably, the gas space of the vessel is vented to a pressure in the vessel which is the atmospheric pressure of the surrounding atmosphere to give the reduced oxygen gas concentration in the gas space of the vessel. Preferably, the reduced oxygen gas concentration is 2000 ppm (more preferably 400 ppm, particularly preferably 20 ppm). More preferably, the step of purging the gas space of the container in contact with the combination in the container to give the reduced oxygen gas concentration in the gas space of the container, includes: (i) the isolating the gas space of the container from a surrounding atmosphere outside the container; (ii) then pressurizing the gas space 25 of the vessel with an inert gas (preferably, wherein the inert gas is selected from the group consisting of argon, helium, methane, and nitrogen (more preferably argon, helium and nitrogen, more preferably argon and nitrogen, particularly preferably nitrogen); and (iii) thereafter purging the gas space of the vessel to provide the reduced oxygen gas concentration in the gas space of the vessel 3037266 39 (preferably, where the gas space of the vessel is purged to at a pressure in the container which is> the atmospheric pressure of the surrounding atmosphere outside the container); and (iv) repeating steps (ii) and (iii) at least three times to give the reduced oxygen gas concentration in the container gas space (preferably, where the reduced oxygen gas concentration is .5 2000 ppm (more preferably 5,400 ppm, particularly preferably 5 ppm)). Preferably, the process for producing high aspect ratio filtered silver nanowires of the present invention further comprises: maintaining a reduced oxygen gas concentration in the container gas space during the period of time. addition of the polyvinylpyrrolidone / mixed silver ion source, during formation of the growth mixture, and during the holding period. [0067] Preferably, the method for producing filtered silver nanowires having a high aspect ratio of the present invention further comprises: bubbling into the initial silver ion source provided with an inert gas to extract by entraining the oxygen gas from the initial silver ion source and to give a low concentration of oxygen gas in a silver ion gas space in contact with the initial silver ion source. Preferably, the bubbling step in the initial silver ion source provided with an inert gas comprises (preferably consists of): bubbling into the initial silver ion source supplied with an inert gas (preferably wherein the inert gas is selected from the group consisting of argon, helium, methane, and nitrogen (more preferably argon, helium, and nitrogen, more preferably, argon and nitrogen, particularly preferably nitrogen) during a bubbling time of 5 minutes (more preferably from 5 minutes to 2 hours, particularly preferably from 5 minutes to 1.5 hours). ) prior to addition to the vessel for entrainment of oxygen gas from the supplied initial silver ion source and to give a low concentration of oxygen gas in the silver ion gas space. Preferably, the low oxygen gas concentration in the silver ion gas space is 10000 ppm (preferably 1000 ppm, more preferably 400 ppm, particularly preferably 20 ppm). Preferably, the method for producing filtered silver nanowires having a high aspect ratio of the present invention further comprises: maintaining the low oxygen gas concentration in the silver ion gas space up to the source of the initial silver ions supplied is added to the container. [0068] Preferably, the process for producing high aspect ratio filtered silver nanowires of the present invention further comprises: purging a polyvinylpyrrolidone (PVP) gas space in contact with the polyvinylpyrrolidone (PVP) provided to give a dilute oxygen gas concentration in the polyvinylpyrrolidone (PVP) gas space. Preferably, the step of purging the PVP gas space to provide the dilute oxygen gas concentration in the PVP gas space includes: (i) isolating the initial polyvinylpyrrolidone (PVP) provided; (ii) then pressurizing the PVP gas space with an inert gas (preferably, wherein the inert gas is selected from the group consisting of argon, helium, methane, and nitrogen (more preferably argon, helium and nitrogen, more preferably argon and nitrogen, particularly preferably nitrogen); and (iii) thereafter purging the PVP gas space to give the dilute oxygen gas concentration in the PVP gas space. Preferably, the PVP gas space is purged to a pressure that is> atmospheric pressure of the surrounding atmosphere to give the dilute oxygen gas concentration in the PVP gas space. More preferably, the step of purging the PVP gas space to provide the dilute oxygen gas concentration in the PVP gas space includes: (i) isolation of the initial polyvinylpyrrolidone (PVP) Provided; (ii) then pressurizing the PVP gas space with an inert gas (preferably, wherein the inert gas is selected from the group consisting of argon, helium, methane, and nitrogen (more preferably argon, helium and nitrogen, more preferably argon and nitrogen, particularly preferably nitrogen); (iii) then purging the PVP gas space to give the concentration of dilute oxygen gas in the PVP gas space (preferably, where the PVP gas space is purged to a pressure of inert gas which is> atmospheric pressure); and, (iv) repeating steps (ii) and (iii) at least three times to give the dilute oxygen gas concentration in the PVP gas space. Preferably, the dilute oxygen gas concentration in the PVP gas space is 10000 ppm (preferably 5000 ppm, more preferably 5.400 ppm, particularly preferably 20 ppm). Preferably, the process for producing high aspect ratio filtered silver nanowires of the present invention further comprises: maintaining the dilute oxygen gas concentration in the PVP gas space until the initial polyvinylpyrrolidone (PVP) supplied is added to the container. [C] Preferably, the process for producing high aspect ratio filtered silver nanowires of the present invention further comprises: venting a gas space from the container in contact with the combination into the container to give a reduced oxygen gas concentration in the container gas space; bubbling into the initial silver ion source provided with an inert gas to entrain the oxygen gas from the source of the initial silver ion supplied and to give a low concentration of oxygen gas in an ion gas space silver in contact with the original silver ion source provided; purging a polyvinylpyrrolidone (PVP) gas space in contact with the initial polyvinylpyrrolidone (PVP) provided to give a dilute oxygen gas concentration in the polyvinylpyrrolidone (PVP) gas space; maintaining the low oxygen gas concentration in the silver ion gas space and the dilute oxygen gas concentration in the polyvinylpyrrolidone (PVP) gas space; and maintaining the reduced oxygen gas concentration in the vessel gas space during the addition of the polyvinylpyrrolidone / mixed silver ion source, during formation of the growth mixture, and during the holding period. [C: 7 :)] Preferably, in the process for making filtered silver nanowires having a high aspect ratio of the present invention, the total glycol concentration in the container is <0.001% by weight at any time during the process. Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the initial polyvinylpyrrolidone (PVP) and the original silver ion source are added to weight ratio of polyvinylpyrrolidone (PVP) to silver ions of 4: 1 to 10: 1 (more preferably 5: 1 to 8: 1, particularly preferably 6: 1 to 7: 1). [0072] Preferably, in the process for producing high aspect ratio filtered silver nanowires of the present invention, the initial halide ion source and the initial copper (II) ion source are added. to the container in a ratio by weight of the halide ions to copper (II) ions of 1: 1 to 5: 1 (more preferably 2: 1 to 4: 1, particularly preferably 2.5: 1 to 3.5: 1). [0073] Preferably, the method for producing high aspect ratio filtered silver nanowires of the present invention provides a product where WA - - .rute <[- - Product. More preferably, the method for producing silver nanowires having a high aspect ratio of the present invention provides a product where S-drute <WFProduct 0.8. More preferably, the method of making silver nanowires having a high aspect ratio of the present invention provides a product where. WF - - .rute <WFProduct 0.85. Particularly preferably, the high aspect ratio silver nanowire manufacturing method of the present invention provides a product, where WF.rute <F. - -. - W -, product k 0.9. Some embodiments of the present invention will now be described in detail in the following examples. The water used in the following examples was obtained by means of a Barnstead NANOPure ThermoScientific purification system with a 0.2 μm pore size hollow fiber filter positioned downstream of the purification unit. some water. Example Si: halide ion sub-combination [0076] The halide ion sub-combination used herein in some examples was prepared by dissolving sodium chloride (0.2104 g available from Sigma Aldrich) in the following manner: water (900 mL). Example 52: Sub-combination of copper (II) ions The copper (II) ion sub-combination used here in some examples was prepared by dissolving copper (II) chloride dihydrate (0.6137). g; available from Sigma Aldrich) in water (900 mL). Example 53: reducing sugar / copper ions sub-combination (Mons halide [007] The reducing sugar / copper (II) ion / halide ion sub-combination used here in some examples was prepared: by adding 13.5 g of D-glucose to water (2159 mL) in a flask, then 21.3 mL of the halide ion sub-combination prepared according to Example Si was added to the flask, and 30.38266 added 21.3. mL of the copper (II) ion sub-combination prepared according to Example S2 to the flask Example S4: polyvinylpyrrolidone (PVP) sub-combination [L777.] The polyvinylpyrrolidone (PVP) sub-combination used here in some examples was prepared by addition of polyvinylpyrrolidone (52.2 g, weight average molecular weight of 50000 g / mol, Sokalan® K30 P available from BASF) to water (381 mL) in a flask and then rinse the transfer apparatus with water (203 mL) in the flask Example S5: arg ion sub-combination [00CC] The silver ion sub-combination used herein in some examples was prepared by the addition of AgNO3 (12.7 g; reactive grade 15 ACS, 99.0; available from Sigma Aldrich) to water (152 mL) in a flask. Example S6: Polyvinylpyrrolidone / mixed silver ion sub-combination [7.1] The polyvinylpyrrolidone / mixed silver ion sub-combination used here in some examples was prepared by combining the polyvinylpyrrolidone (PVP) sub-combination prepared according to the present invention. Example S4 with a silver ion sub-combination prepared according to Example S5 in a 1L conical bottom container and then successively by rinsing the flask containing the polyvinylpyrrolidone (PVP) sub-combination and the flask containing the sub-combination. combination of silver ions with water (102 mL) in the conical bottom container. The polyvinylpyrrolidone / mixed silver ion sub-combination contained in the conical bottom vessel was then gently bubbled continuously with nitrogen until it was transferred to the reactor.
[0004] Examples 1 and 2: Preparation of silver nanowires [0082] An 8 liter stainless steel pressure reactor equipped with a three blade propeller type stirrer, a temperature control unit with a External resistive heating mantle and an internal cooling tube to facilitate temperature control was used. A reducing sugar / copper (II) ion / halide ion sub-combination prepared according to Example S3 was added to the reactor. The transfer apparatus was then rinsed with water (152 mL) in the reactor. The reactor was then closed and the agitator was started at 200 rpm. The gas space in the reactor was then purged with> 620 x 103 Pa (90 psig) of nitrogen four times to a pressure> 414 x 103 Pa (60 psig) with holding under pressure for three minutes for each purge. The reactor was left with a nitrogen blanket at 111 x 103 Pa (16.1 psig) after the final purge. The set point for the temperature control unit was then set at 150 ° C. When the reactor contents reached a temperature of 150 ° C, 1 / 5th of a polyvinylpyrrolidone / mixed silver ion sub-combination prepared according to Example S6, after a pre-mixing time after its preparation, as noted in Table 1 was transferred to the reactor for a 1 minute charging time at a point below the surface of the combination in the reactor to form a creation mixture. Following a twenty-minute delay period, the remaining 4/5 of the polyvinylpyrrolidone / mixed silver ion sub-combination was transferred to the reactor for a feed time of 10 minutes at a point below the surface. of the creation mixture in the reactor to form a growth mixture. During the delay period, the set point for the temperature control device was lowered linearly from 150 ° C to 130 ° C, the lowering starting at 10 minutes in the delay period and ending with the period of delay. The growth mixture was then stirred for a hold time noted in Table 1 to form a raw feed. The raw feed was then cooled to room temperature. The agitator was stopped. The reactor was then vented to release any accumulated pressure in the vessel. The contents of the reactor were then transferred as raw feed into the dynamic filtration device. TABLE 1 Examples 3-4 [0083] In each of Examples 3-4, nitric acid was added to the combination in the reactor to adjust the pH of the combination to the pH noted in Table 2. Then, 1 Of a polyvinylpyrrolidone / mixed silver ion sub-combination prepared according to Example 56 as a result of a premixing time after its preparation, as noted in Table 2, was transferred to the reactor for a time charge 1 minute at a point below the surface of the combination in the reactor to form a creation mixture. Following a twenty-minute delay period, the remaining 4/5 of the polyvinylpyrrolidone / mixed silver ion sub-combination was then transferred to the reactor for a feed time of 10 minutes at a point below the surface. of the creation mixture to form a growth mixture. During the delay period, the set point for the temperature control device was lowered linearly by 10 minutes. Pre-mixing time holding time Example (min) (h) 1 <60 8 2 <60 18 3037266 47 150 ° C at the temperature noted in Table 2, the lowering starting at 10 minutes in the delay period and ending with the delay period. The growth mixture was then stirred for a hold time as noted in Table 2 to form a raw feed. The raw feed was then cooled to room temperature. The agitator was stopped. The reactor was then vented to release any accumulated pressure in the vessel.
[0005] TABLE 2 Pre-Mix Time Time Temp. EXAMPLE 5-8: Filtration [000] In Examples 5-8, raw feeds containing 15 percent of the feedings were prepared. silver solids including silver nanowires having a high aspect ratio and silver particles having a low aspect ratio prepared according to the synthesis examples as noted in Table 3 were filtered by means of a Advantec / MFS Model UHP 150 agitated cell filter case with a filtration area of 162 cm2 and 20 equipped with an impeller ("impeller") type cylindrical magnetic bar. The filter housing was placed on a Mettler model SB32001DR magnetic balance / stirring device. The porous medium used was a 3 μm filter membrane of hydrophilic polycarbonate made porous by track-etch technology (PCTE) supported in the bottom of the filter housing. Nitrogen pressure was used to create the motive force to produce a pressure drop across the porous medium. Nitrogen was introduced into the headspace of the filter housing. Head pressure was measured using a Cole-Parmer model 68075-16 pressure transducer. The nitrogen introduced into the filter housing was passed through a three-way ball valve mounted on the top of the filter housing. The three-way valve allowed for periodic interruption of the nitrogen stream and periodic release of pressure in the headspace of the filter housing to the atmosphere. This allowed for an inverted flow of gravity-induced filtrate material from the exhaust duct into the filter housing and up through the filter membrane. The three-way valve was controlled by means of a Camille process control computer in such a way that every 25 seconds the nitrogen supply to the filter housing was interrupted and the filter housing was turned off. atmosphere for 5 seconds before restoring the nitrogen supply. The raw feed identified in Table 3 for each of Examples 5-8 was poured into the filter housing. A carrier fluid having the composition noted in Table 3 for each of Examples 5-8 was then introduced into the filter housing by means of a Masterflex Model 77800-16 Easy-Load 3 Peristaltic Pump with a numerical control and a 16-gauge C-Flex pipe. The volume of transport fluid transferred to the filter housing was manually controlled to maintain a constant level in the filter housing throughout the filtration process. The filtrate leaving the bottom of the filter housing was made to mount into a flexible plastic tube of 4.1 mm internal diameter to reach the top of an open container at the top. The fluid column in the filtrate tube created the driving force for the discharge in the filter housing when the free space was periodically opened to the atmosphere with the three-way valve. Silver solids in the product filtrate were collected.
[0006] TABLE 3 Example Feeding Raw Transport Fluid 5 Aqueous solution product with 0.15% by weight of PVP Example 1 6 Aqueous solution product with 1.5% by weight of D-glucose Example 2 7 Purified Reaction Liquor Product Example 38 Product of aqueous solution with 140 mM PVP and 25 μM NaCl Example 4 Analysis of silver solids [0085] The silver solids from Examples 1-8 were were analyzed with a FEI Nova Nano SEM Field Emission Scanning Electron Microscope (SEM) using the FEL Automated Image Acquisition (AIA) program A drop of purified dispersion was It was taken from the UV / Vis cuvette and applied to an SEM sample holder covered with a silica wafer before being dried under vacuum. The backscattering electronic images were collected with a FEI Nova Nano SEM Field Emission Scanning Electron Microscope. FEI's Automated Image 15 Acquisition (AIA) acquisition program was used to move the deck, focus, and collect images. Eighteen images of each sample were acquired at a horizontal field width of 6 μm. Semi-automatic image analysis using the Image] software classified the objects as threads or particles based on an aspect ratio of 3. The 20 yarn widths were measured automatically as well as the total area of wires in the images. Particles were classified with respect to the individual size and the total area of particles in the images. The Image] software was also used to determine the diameter of the 3037266 silver nanowires in Table 4. It was observed that the average length of the silver nanowires exceeded 20 μm, based on the SEM images obtained for the diameter analysis. Image] was used to analyze the SEM images of the silver nanowires produced in each of Examples 1-8 to give a relative measure of the silver nanowires having an aspect ratio of> 3 in the samples. . The statistic used for this measurement is the fraction of nanowires, NWF, determined according to the following expression: NWF = NWAI TA; Where TA is the total surface area of the substrate which is occluded by a given deposited sample of silver solids; and NWA is the portion of the total occluded surface area attributable to silver nanowires having an aspect ratio> 3.
[0007] TABLE 4 Example Diameter of silver nanowires (nm) f Median Average Standard deviation 1 33.4 37.2 16.2 0.75 2 30.6 35.2 15.1 0.62 3 37.7 39, 9 12.1 0.82 4 35.0 39.9 17.0 0.71 5 32.5 36.0 20.4 0.87 6 29.3 32.7 15.0 0.81 7 33.4 35.0 10.7 0.94 8 36.2 36.3 7.1 0.95

权利要求:
Claims (10)
[0001]
REVENDICATIONS1. A process for producing filtered silver nanowires having a high aspect ratio, characterized by comprising: providing a container; the supply of an initial volume of water; the supply of an initial reducing sugar; providing an initial polyvinylpyrrolidone (PVP), wherein the initial polyvinylpyrrolidone (PVP) provided can be divided into a first portion of the initial polyvinylpyrrolidone (PVP) and a second portion of the initial polyvinylpyrrolidone (PVP); providing an initial copper (II) ion source; providing an initial halide ion source; providing an initial silver ion source, wherein the initial silver ion source provided can be divided into a first portion of the initial silver ion source and a second portion of the original silver ion source; adding the initial water volume, the initial reducing sugar, the initial copper (II) ion source and the initial halide ion source to the vessel to form a combination; heating the combination at a temperature between 110 and 160 ° C; mixing the first portion of the initial polyvinylpyrrolidone (PVP) with the first portion of the initial silver ion source to form a polyvinylpyrrolidone / mixed silver ion source; adding the polyvinylpyrrolidone / silver ion source mixed with the combination into the vessel to form a creation mixture; then, following a delay period, adding to the vessel the second portion of the initial polyvinylpyrrolidone (PVP) and the second portion of the original silver ion source to form a growth mixture; maintaining the growth mixture at a temperature between 110 and 160 ° C for a holding period of 2 to 30 hours to produce a raw feed (5) where the total glycol concentration in the container is <0.001% by weight; wherein the raw feed (5) produced comprises mother liquor and silver solids; where the mother liquor comprises the initial volume of water; and wherein the silver solids in the raw feed include silver nanowires having a high aspect ratio and silver particles having a low aspect ratio; providing a dynamic filtration device (10), wherein the dynamic filtration device (10) comprises: a housing (20), comprising: a cavity (30) having a first side (35) and a second side (45) ); wherein there is at least one inlet (32) in the first side (35) of the cavity (30), at least one product outlet (37) from the first side (35) of the cavity (30) and at least one a permeate outlet (47) from the second side (45) of the cavity (30); and a porous member (50) disposed in the cavity (30); a turbulence-inducing element (60) disposed in the cavity (30); and a pressure source (70); wherein the porous member (50) is interposed between the first side (35) of the cavity (30) and the second side (45) of the cavity (30); wherein the porous member (50) has a plurality of passages (55) therethrough from the first side (35) of the cavity (30) to the second side (45) of the cavity (30); wherein the passages (55) of this plurality of passages (55) are sufficiently large to allow transfer of mother liquor and silver particles having a low aspect ratio and sufficiently small to block the transfer of the silver nanowires 3037266 53 having a high aspect ratio; wherein the porous member (50) and the turbulence inducing member (60) cooperate to form a filtration gap (FG) and wherein at least one of the porous member (50) and the turbulence inducing member (60) is mobile; providing a transport fluid, wherein the transport fluid comprises an additional volume of water and an additional polyvinylpyrrolidone (PVP); transferring the raw feed (5) to the dynamic filtration device (10) through the at least one inlet (32) in the first side (35) of the cavity (30); transferring a volume (150) of the transport fluid to the dynamic filtration device (10) through the at least one inlet (32) in the first side (35) of the cavity (30); Where the filtration range (FG) is filled with water; wherein the porous member (50) and the turbulence inducing member (60) disposed in the cavity (30) are both in contact with water; pressurizing the first side (35) of the cavity (30) by means of the pressure source (70), which leads to a first-side pressure F5p in the first side (35) of the cavity ( 30) ; where the first side pressure, FSp, is higher than a second side pressure, 55p, in the second side (45) of the cavity (30), so that a pressure drop is created , PE, through the porous member (50) from the first side (35) of the cavity (30) to the second side (45) of the cavity (30); wherein the pressure source (70) provides a primary driving force for inducing a current from the first side (35) of the cavity (30) through the porous member (50) to the second side (45) of the cavity (30) producing a permeate; moving at least one of the porous member (50) and the turbulence inducing member (60) such that a shear stress is produced in the water within the range of filtration (FG) where the shear stress produced in water in the filtration gap (FG) acts to reduce fouling of the porous member (50); Removing the permeate from the at least one permeate outlet (47) from the second side (45) of the cavity (30), where the permeate comprises a second cut of the mother liquor and a second fraction of the silver solids ; where the second fraction of the silver solids is rich in silver particles having a low aspect ratio; and removing a product from the at least one product outlet (37) from the first side (35) of the cavity (30), wherein the product comprises a first cut of the mother liquor and a first fraction of the solids of the 'money; where the first fraction of the silver solids is depleted of silver particles having a low aspect ratio; and where the shear stress produced in water in the filtration gap (FG) and the pressure drop, PE, through the porous member (50) from the first side (35) of the cavity (30). ) to the second side (45) of the decoupled cavity (30).
[0002]
2. The process according to claim 1, characterized in that the transport fluid further comprises an additional halide ion source.
[0003]
3. Method according to claim 1 or 2, characterized in that the transport fluid further comprises an additional reducing sugar. 25
[0004]
4. Method according to any one of claims 1 to 3, characterized in that it further comprises: removal of silver solids from the permeate to provide a purified permeate; and recycling the purified permeate in the dynamic filtration device (10) through the at least one inlet (32) in the first side (35) of the cavity (30).
[0005]
5. Process according to claim 4, characterized in that the silver solids are removed from the permeate by centrifugation to provide the purified permeate.
[0006]
6. Method according to claim 4 or 5, characterized in that the transport fluid comprises the purified permeate,
[0007]
7. Process according to any one of claims 1 to 6, characterized in that the first part of the initial polyvinylpyrrolidone (PVP) represents 10 to 40% by weight of the polyvinylpyrrolidone (PVP) supplied; and the first portion of the initial silver ion source is 10 to 40% by weight of the silver ion source provided.
[0008]
8. A process according to any of claims 1 to 7, characterized in that it further comprises: providing a pH adjusting agent; adding the pH adjusting agent to the combination prior to adding the polyvinylpyrrolidone / mixed silver ion source; wherein the combination has a pH of 2.0 to 4.0 before the addition of the polyvinylpyrrolidone / silver ion source mixed with the container.
[0009]
9. Method according to any one of claims 1 to 8 characterized in that it further comprises: providing a reducing agent; adding the reducing agent to the creation mixture. 25
[0010]
The method according to any one of claims 1 to 9, characterized in that it further comprises: purging a gas space of the container in contact with the combination in the container to give a reduced oxygen gas concentration in the gas space of the container; Sparging in the initial silver ion source provided with an inert gas to drive the oxygen gas out of the supplied initial silver ion source and to give a low concentration of oxygen gas in a gas space of 30 ° C. silver ions in contact with the original silver ion source provided; purging a polyvinylpyrrolidone (PVP) gas space in contact with the initial polyvinylpyrrolidone (PVP) provided to give a dilute oxygen gas concentration in the polyvinylpyrrolidone (PVP) gas space; Maintaining the low oxygen gas concentration in the silver ion gas space and the dilute oxygen gas concentration in the polyvinylpyrrolidone (PVP) gas space; and maintaining the reduced oxygen gas concentration in the container gas space during the addition of the polyvinylpyrrolidone / mixed silver ion source, during formation of the growth mixture, and during the holding period.

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KR20160146544A|2016-12-21|

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引用文献:

---

公开号 | 申请日 | 公开日 | 申请人 | 专利标题

---

---

US5000848A|1987-01-28|1991-03-19|Membrex, Inc.|Rotary filtration device with hyperphilic membrane|

---

JPH02284609A|1989-04-27|1990-11-22|Toshiba Corp|Operation of ceramic filter|

---

US5143630A|1991-05-30|1992-09-01|Membrex, Inc.|Rotary disc filtration device|

---

US5254250A|1991-05-30|1993-10-19|Membrex, Inc.|Rotary filtration device and filter pack therefor|

---

FI106298B|1996-03-04|2001-01-15|Valmet Flootek Oy|Separation method and device|

---

EP0938365B1|1996-09-06|2006-11-29|Pall Corporation|Shear separation method and system|

---

US5993674A|1998-02-24|1999-11-30|Membrex, Inc.|Rotary disc filtration device with means to reduce axial forces|

---

US5944998A|1998-04-21|1999-08-31|Membrex, Inc.|Rotary filtration device with flow-through inner member|

---

EP1448725A4|2001-10-05|2008-07-23|Cabot Corp|Low viscosity precursor compositions and methods for the deposition of conductive electronic features|

---

JP2004042012A|2001-10-26|2004-02-12|Nec Corp|Separation apparatus, analysis system, separating method, and method of manufacturing the apparatus|

---

US7585349B2|2002-12-09|2009-09-08|The University Of Washington|Methods of nanostructure formation and shape selection|

---

WO2006076612A2|2005-01-14|2006-07-20|Cabot Corporation|A process for manufacturing application specific printable circuits and other custom electronic devices|

---

US7291292B2|2005-08-26|2007-11-06|E.I. Du Pont De Nemours And Company|Preparation of silver particles using thermomorphic polymers|

---

US7968008B2|2006-08-03|2011-06-28|Fry's Metals, Inc.|Particles and inks and films using them|

---

CN101269298B|2007-03-23|2011-06-01|中国科学院过程工程研究所|Membrane filtration method and device for polarization of concentration biomacromolecule with concentration|

---

US8018563B2|2007-04-20|2011-09-13|Cambrios Technologies Corporation|Composite transparent conductors and methods of forming the same|

---

US7922787B2|2008-02-02|2011-04-12|Seashell Technology, Llc|Methods for the production of silver nanowires|

---

JP5203769B2|2008-03-31|2013-06-05|富士フイルム株式会社|Silver nanowire and method for producing the same, aqueous dispersion and transparent conductor|

---

JP2009299162A|2008-06-16|2009-12-24|Fujifilm Corp|Silver nanowire, method for producing the same, water base dispersion product and transparent conductor|

---

BRPI0912901A2|2008-08-19|2015-10-06|Dow Global Technologies Llc|process for producing a graded catalyst composition, polymerization process, apparatus for producing a graded catalyst composition and method for determining the solids content in a paste|

---

JP5306760B2|2008-09-30|2013-10-02|富士フイルム株式会社|Transparent conductor, touch panel, and solar cell panel|

---

TWI372666B|2008-12-23|2012-09-21|Ind Tech Res Inst|Preparing composition of silver nanowire and method for forming silver nanowire|

---

US20100242679A1|2009-03-29|2010-09-30|Yi-Hsiuan Yu|Method for continuously fabricating silver nanowire|

---

JP5472299B2|2009-06-24|2014-04-16|コニカミノルタ株式会社|Transparent electrode, method for purifying conductive fiber used for transparent electrode, and organic electroluminescence device|

---

SG2014006001A|2009-08-24|2014-03-28|Cambrios Technologies Corp|Purification of metal nanostructures for improved haze in transparent conductors made from the same|

---

DE102010017706B4|2010-07-02|2012-05-24|Rent-A-Scientist Gmbh|Process for the preparation of silver nanowires|

---

CN101934378A|2010-09-10|2011-01-05|浙江大学|High-concentration fast preparation method for silver nanowires|

---

US9630250B2|2010-12-17|2017-04-25|Seiko Pmc Corporation|Process for producing silver nanowires and agent for controlling growth of silver nanowires|

---

CN102303124A|2011-08-24|2012-01-04|浙江科创新材料科技有限公司|Method for preparing length-diameter-ratio nano-silver wire by pH-value regulation solvothermal method|

---

JP2013073828A|2011-09-28|2013-04-22|Fujifilm Corp|Conductive composition, method for producing the same, conductive member, touch panel, and solar cell|

---

KR20130072956A|2011-12-22|2013-07-02|엘지이노텍 주식회사|Nanowire and method for manufacturing the same|

---

US9034075B2|2012-04-30|2015-05-19|Dow Global Technologies Llc|Methods of manufacturing high aspect ratio silver nanowires|

---

CN104583114B|2012-06-18|2017-04-05|苏州诺菲纳米科技有限公司|The agglomerated thing of the nanowire suspended liquid being stored in container is reduced|

---

WO2014013819A1|2012-07-19|2014-01-23|富士フイルム株式会社|Method for manufacturing fiber-containing dispersion liquid, electroconductive fiber-containing dispersion liquid, and method for manufacturing electroconductive layer|

---

WO2014138749A1|2013-03-08|2014-09-12|Innova Dynamics, Inc.|Production of nanostructures|

---

CN104511596B|2013-09-30|2017-01-18|中科院广州化学有限公司|Continuous preparation method and device for nano-silver wire|

---

CN103894624B|2014-04-03|2016-11-23|复旦大学|Screening technology is prepared in the filtration of a kind of nano-silver thread powder body|

---

US9897699B2|2014-07-09|2018-02-20|Massachusetts Institute Of Technology|Methods and apparatus for virtual sensor array|

---

DE102015013220A1|2014-10-28|2016-04-28|Dow Global Technologies Llc|Process for the preparation of silver nanowires|

---

DE102015013219A1|2014-10-28|2016-04-28|Dow Global Technologies Llc|Process for the preparation of silver nanowires|

---

DE102015013238A1|2014-10-28|2016-04-28|Dow Global Technologies Llc|Low oxygen concentration process for producing silver nanowires|

---

CN104607655B|2015-03-06|2016-08-24|苏州大学|A kind of preparation method of nano silver wire|

---

US10376898B2|2015-06-12|2019-08-13|Dow Global Technologies Llc|Method for manufacturing high aspect ratio silver nanowires|US9878306B2|2014-09-19|2018-01-30|Georgia Tech Research Corporation|Silver nanowires, methods of making silver nanowires, core-shell nanostructures, methods of making core-shell nanostructures, core-frame nanostructures, methods of making core-frame nanostructures|

---

US10376898B2|2015-06-12|2019-08-13|Dow Global Technologies Llc|Method for manufacturing high aspect ratio silver nanowires|

---

US20200030877A1|2017-03-14|2020-01-30|Dowa Electronics Materials Co., Ltd.|Method for producing silver nanowire dispersion liquid having good separability among wires|

---

WO2019121827A1|2017-12-19|2019-06-27|Rhodia Operations|Use of filtration media for purification of nanowires and process for the purification of nanowires|

---

CN111408176B|2020-03-06|2021-08-17|深圳第三代半导体研究院|Method and device for purifying multidimensional nano material|

法律状态:
2017-05-11| PLFP| Fee payment|Year of fee payment: 2 |

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2018-05-11| PLFP| Fee payment|Year of fee payment: 3 |

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2019-05-10| PLFP| Fee payment|Year of fee payment: 4 |

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2020-05-29| PLSC| Publication of the preliminary search report|Effective date: 20200529 |

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2021-03-12| ST| Notification of lapse|Effective date: 20210206 |

优先权:

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申请号 | 申请日 | 专利标题

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US201562174677P| true| 2015-06-12|2015-06-12|

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