• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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    • 专利摘要:
    The present disclosure describes an oxygen-generating composition comprising an oxygen source and a mixed metal oxide of the formula: (Li, Fe, Mg) O.
    公开号:FR3042485A1
    申请号:FR1660086
    申请日:2016-10-18
    公开日:2017-04-21
    发明作者:Christoph Kallfass；Artur Hejczyk；Ulla Simon
    申请人:Goodrich Lighting Systems GmbH；
    IPC主号:
    专利说明:

    Oxveene Generating Compositions Comprising (Li.Fe.Ma) O Technical Field
    The present invention relates to oxygen generating compositions and devices, i.e., chemical oxygen generators, as well as processes for their preparation.
    Historical
    Chemical oxygen generators are used for emergency systems, eg. in an aircraft, respirators for emergency services such as fire and rescue crews in mines, submarines, and other situations in which a compact emergency oxygen generator a long storage life is necessary. They release oxygen through a chemical reaction, usually oxygen sources are inorganic, especially alkali metals or alkaline earth metals, superoxides, chlorates or perchlorates.
    Chlorate candles, also known as oxygen candles, are examples of chemical oxygen generators that use chlorates or perchlorates as a source of oxygen. Chlorate candles can produce oxygen at a fixed rate of about 6.5 man-hours of oxygen per kilogram of the mixture and have a long shelf life.
    In addition to the oxygen-releasing compounds, additives having different properties are used in chemical oxygen generators, e.g. : fuels, catalysts, linkers and moderators. The fuels support the oxygen production reaction and are generally metal powders, e.g., iron, tin, manganese, cobalt, nickel, tungsten, titanium, magnesium, dusts powders. aluminum, niobium, zirconium and / or mixtures thereof.
    The transition metal oxides are generally used to catalyze the exothermic oxygen production reaction, particularly to reduce the temperature at which the reaction occurs and thereby reduce the heat released by the device in operation. A commonly used catalyst is cobalt oxide, because of its ability to reduce the temperature of the decomposition reaction, e.g. sodium chlorate from 290 to 400 ° C. Cobalt oxide is, however, toxic and expensive, and therefore it is necessary to use it in very small amounts. Although it is effective in very small amounts (e.g., 0.1% by weight), obtaining a uniform mixture at such low concentrations is difficult. Non-uniform mixing results in erratic performance, such as non-uniform oxygen production, which is clearly undesirable. Other catalysts commonly used are manganese oxides, although these can produce high concentrations of chlorine in the product oxygen. There is therefore a need to provide alternative catalysts for oxygen generation that overcome these problems.
    Chemical oxygen generators are necessary to produce a continuous oxygen flow that lasts over time. For this reason, moderators are also used, i.e., to avoid undesirable reaction products such as chlorine during the decomposition process and / or to provide sufficient and substantially uniform oxygen flow. Ba02 is generally used as a moderator, but it is toxic and waste disposal is expensive.
    Chemical oxygen generators, i.e., chemical oxygen generating devices, generally include molds, ie, containers or pellets that contain the chemicals; these molds, containers or pellets must obviously remain structurally stable before and during the use of the oxygen generator in order to avoid a failure during the initial firing process and to avoid the interruption of the flow of oxygen which could occur due to mechanical changes in the generator body induced by environmental effects or by the evolution of the reaction. Bonding agents are therefore used to stabilize the body of the chemical oxygen generator, e.g., the body of the chlorate candle, and to ensure that it does not present a hazard in use. Typical bonding agents are mica, glass powder, fiberglass, ceramic fiber, bentonite, kaolinite and mixtures thereof, although other inorganic bonding agents may also be suitable . These add an undesirable additional volume to the compositions used to produce oxygen.
    The decomposition of chlorates to release oxygen is exothermic, eg, sodium chlorate decomposes from 500 to 600 ° C. Due to the high temperatures involved, chemical oxygen generators require thermal insulation to protect the surrounding equipment. Such insulation adds further volume to the oxygen generator, which is clearly undesirable since it may be necessary to store them for extended periods of time, usually in locations (eg aircraft, -marines, fire trucks) in which space and capacity by weight are limited. There is therefore a need to reduce the size and / or the weight of the oxygen generators.
    The present inventors have discovered by chance that certain oxide compounds are multifunctional, acting as catalysts, linkers and fuels. These compounds therefore allow the production of lighter and more compact oxygen generators. In addition, since the compounds are nontoxic, the aforementioned problems with commonly used toxic catalysts can also be avoided.
    Thus, from this point of view, the present disclosure describes an oxygen generating composition comprising an oxygen source and a mixed metal oxide of the formula: (Li, Fe, Mg) O. Preferably, the mixed metal oxide is in the form of nanoparticles.
    The degree of crystallinity of the mixed metal oxides can be increased by heat treatment, eg by calcination. However, the best catalytic performance has been found for the oxides of the present disclosure which are non-crystalline, e.g., semi-crystalline or amorphous. The oxides of the present disclosure are therefore preferably non-calcined, i.e., they have not been thermally treated so that the degree of crystallinity is increased.
    Preferably, less than 90% (e.g.,% by weight), particularly less than 75%, especially less than 50%, especially preferably less than 25% or less than 10% of the mixed metal oxide material described herein. is in crystalline form. Especially preferably, the mixed metal oxide of formula: (Li, Fe, Mg) O is substantially semi-crystalline or substantially amorphous.
    The crystallinity is measured by X-ray diffraction (XRD) or by any other technique known in the art, such as differential scanning calorimetry. Crystallinity involves both a short-range and long-range order of atoms occurring periodically within the crystal lattice resulting in well-defined characteristic patterns on the X-ray powder diffractogram. Mixed metal oxides of formula: (Li, Fe, Mg) 0 which have not been subjected to a heat treatment demonstrate low degrees of crystallinity and may be called amorphous or semi-crystalline. Such materials only contain a short-range order of the atoms which results in non-defined X-ray powder diffractograms in which the larger reflexes found in the more crystalline forms are absent.
    Preferably, the mixed metal oxide, as described herein, is in the form of a powder. Preferably, the mixed metal oxide is in the form of nanoparticles, e.g., a nanoparticle powder.
    The formula "(Li, Fe, Mg) 0" is intended to describe a single chemical entity, rather than, for example, a mixture of lithium oxides, iron oxides and magnesium oxides. The compositions of the present disclosure therefore comprise a mixed metal of lithium iron magnesium oxide, rather than a mixture of these metal oxides. The oxides of the present disclosure can therefore be considered as Li-and Fe-doped MgO, ie, MgO in which certain magnesium cations are substituted with iron cations and lithium cations in the formula. crystal lattice. Although the oxide may be doped FeO, doping of MgO is, however, most preferred. In the oxides of the present disclosure, iron generally has an oxidation state of +2 and / or +3.
    The content of each element can be determined by standard techniques, e.g., atomic absorption spectroscopy or inductively coupled plasma atomic emission spectroscopy. Preferred examples of mixed metal oxide of the present disclosure are (Fe, Li, Mg) O, wherein the iron and lithium contents are independently from 0.01 to 30 atomic% (% .at), particularly from 0.05 to 20% .at. (e.g., 0.1 to 10 or 0.1 to 1 at%), especially preferably 0.1 to 0.5 at%, e.g., about 0.45 at%.
    An alternative notation would be (Fex, Liy Mgi.x.y) 0, wherein x and y are independently preferably 0.0002 to 0.6; especially 0.001 to 0.4, especially preferably 0.002 to 0.01, e.g., around 0.009. Especially preferably x = y, i.e. Li and Fe are substantially equimolar.
    Heat treatment below <1050 ° C does not alter the relative proportions of these metals.
    The inventors have developed a method for producing mixed metal oxides of the present disclosure in nanoparticulate form. The use of (or a method of using) such nanoparticles in the production of oxygen, eg as linkers, fuel and / or catalysts / moderators in the production of oxygen, is another new aspect of this disclosure. Thus, in a preferred aspect, the mixed metal oxides described herein are in the form of particles having a diameter (e.g., average particle diameter) less than or equal to 500 nm, preferably less than or equal to 300 nm, especially less than or equal to 200 nm. Smaller particles allow for better mixing in the oxygen generating compositions and, therefore, more uniform oxygen production.
    The mixed metal oxides of the present disclosure may be characterized using standard techniques, such as surface area analysis, absorption spectroscopy, inductively coupled plasma atomic emission spectroscopy, X-ray diffraction, electron paramagnetic resonance, nuclear magnetic resonance, scanning electron microscopy and / or transmission electron microscopy. The specific surface area of the materials of the mixed metal oxide of the present disclosure can be determined using standard techniques, eg, with a surface area analyzer with surface areas calculable by Brunauer's method, Emmett and Teller. Typical BET surface areas are in the range of 5 to 50 m 2 / g, e.g. 10 to 40 m 2 / g, especially 25 to 35 m 2 / g.
    The characterization of oxides by X-ray diffraction (XRD) is possible with the use of standard techniques, eg CuKal radiation, with a wavelength of 0.154 nm.
    EPR experiments can be performed in conventional continuous wave mode (CW) as well as in pulsation mode.
    In some aspects, the mixed metal oxide may comprise up to 70% by weight of the oxygen-generating composition, i.e., the composition may comprise from 0.1 to 70% by weight, preferably from 0.1 to 10% by weight, particularly preferably from 0.2 to 5% by weight, e.g. from 2 to 4% by weight, especially around 3% by weight of mixed metal oxide as described herein, wherein the amount of mixed metal oxide is expressed as a weight percent of the generating composition of oxygen as a whole (ie, taking into account the total weight of the oxygen source, the mixed metal oxide and any other component).
    The oxygen source may be any suitable compound for producing breathable oxygen. A metal (especially an alkali metal or an alkaline earth metal), halogenates (particularly chlorates, perchlorates or mixtures thereof), peroxides or superoxides are suitable, particularly those of lithium, sodium or potassium, eg, K02. Preferably, the oxygen source is, or comprises, one or more compounds selected from alkali metal chlorates, alkali metal perchlorates, alkaline earth metal chlorates, alkaline earth metal perchlorates, and mixtures thereof. of these, particularly preferably alkali metal chlorates and / or alkali metal perchlorates. Particularly preferred sources of oxygen are those comprising sodium or lithium, particularly sodium chlorate and lithium perchlorate, eg, the oxygen source is preferably sodium chlorate and / or lithium perchlorate.
    The oxygen generating composition of the disclosure generally comprises from 30 to 99.9% by weight of the oxygen source, preferably from 40 to 99% by weight, especially preferably from 70 to 99% by weight, e.g. at least 80% by weight or at least 95% by weight, especially 90 to 99.9% by weight, the amount of the oxygen source being expressed as a weight percent of the oxygen-generating composition in its full (ie, total weight of oxygen source, mixed metal oxide and any other component).
    A particularly preferred aspect of all the embodiments of this disclosure is that the produced oxygen is breathable, i.e., without further processing.
    As discussed in more detail in the Examples, it has been discovered by chance that the mixed metal oxides of the present disclosure are multifunctional, acting as a catalyst, a fuel, and a bonding agent. Thus, there is no need for additional combustion, bonding, catalyst or moderator components in the oxygen generating compositions of the present disclosure. This means that the compositions are simpler, their production is faster and less expensive than conventional oxygen generating compositions and they are more compact and lighter than those of the prior art (which require combustion components, liaison agent, catalyst and / or separate moderators). This gives lighter and more compact oxygen generators, eg, chlorate candles. Even more space and means savings are allowed by reducing the thermal insulation required for oxygen generators using the compositions of the present disclosure; less insulation is required due to the reduced temperature of the oxygen production reaction because of the catalytic properties of the mixed metal oxides disclosed herein. In addition, the mixed metal oxides of the present disclosure are non-toxic and allow for more uniform oxygen production because of the more efficient mixing that is possible due to their nanoparticulate nature.
    For example, as shown in Figure 2 and Example 2, uncalcined (Li, Fe, Mg) 0 reduces the decomposition temperature of sodium chloride to 340 to 400 ° C, i.e. -d., the decomposition process is completed at a lower temperature than with cobalt oxide as a catalyst. The mixed metal oxide of the present disclosure therefore performs better than cobalt oxide, which is generally considered to be the best catalyst for this reaction. In addition, the mixed metal oxide of the present disclosure also acts as a bonding agent and fuel, eliminating the need for other components to perform these functions, and is non-toxic.
    Because of the multifunctional nature of the oxides described herein, the oxygen generating compositions do not require the presence of separate fuels, catalysts, moderators or linkers. Preferably, therefore, the compositions described herein are composed of, or are essentially composed of (one or more, preferably one) oxygen source and (one or more, preferably one) of the metal oxide. mixed described here. However, even if the compositions of the present disclosure do not require the presence of other components, one or more additional components may be present. Thus, one aspect of the present disclosure relates to the compositions as described herein additionally comprising one or more additives, eg, fuels, catalysts, moderators and / or linkers.
    Thus, the compositions as described herein may also include one or more fuels. Metals or non-metals such as silicon, boron and / or carbon may be used. Preferably, the fuel is in powder form, particularly a metal powder, for example a powder of or comprising iron, tin, manganese, cobalt, nickel, tungsten, titanium, magnesium, aluminum, niobium, zirconium and / or mixtures thereof. The compositions may optionally comprise from 0 to 5 (e.g., 0.1 to 5) wt% of such fuel (expressed as percent by weight of the total weight of the additional fuels forming part of the composition in its composition. integrally), preferably 0 to 1 (e.g., 0.1 to 1) wt.%, particularly 0 to 0.5 (e.g., 0.1 to 0.5) wt.%.
    The compositions as described herein may also comprise one or more catalysts, eg, a transition metal oxide, preferably selected from manganese oxides (eg, MnO, Mn 2 O 3), iron oxides (eg, FeO and / or Fe203) cobalt oxide, copper oxide, nickel oxide and mixtures thereof. The compositions may optionally comprise from 0 to 5 (e.g., from 0.1 to 5) wt.% Of such catalyst (expressed as percent by weight of the total weight of the additional catalysts forming part of the composition. its entirety), preferably from 0 to 1 (e.g. from 0.1 to 1)% by weight, particularly from 0 to 0.5 (e.g., 0.1 to 0.5)% by weight .
    The compositions as described herein may also include one or more moderators, e.g., chlorine scavengers and / or reaction rate modifiers (e.g., inhibitors). These are preferably selected from oxides, peroxides and hydroxides of alkali or alkaline earth metals, preferably barium peroxide. These compounds are used to bind chlorine and carbon dioxide, which are sometimes produced in minute amounts, but which must not be present in respirable oxygen. They can also moderate oxygen production, ensuring a uniform supply. The compositions may optionally comprise from 0 to 5 (e.g. from 0.1 to 5) wt% of such moderators (expressed as percent by weight of the total weight of the additional moderators forming part of the composition in its entirety. ), preferably from 0 to 1 (eg from 0.1 to 1)% by weight, particularly from 0 to 0.5 (eg from 0.1 to 0.5)% by weight.
    The compositions as described herein may also comprise one or more binding agents, preferably selected from inorganic binding agents such as mica, glass powder, fiberglass, ceramic fiber, straw. iron, bentonite, kaolinite and mixtures thereof, although other inorganic binding agents may also be suitable.
    The oxygen generating compositions as described herein may be prepared by mixing the oxygen source with the mixed metal oxide (and any other components). The disclosure therefore also describes a method for preparing an oxygen generating composition as described herein, said method comprising mixing the oxygen source with a mixed metal oxide. Optionally, the oxygen source is mixed with, for example, from 1 to 5% by weight of water prior to mixing with the mixed metal oxide. In the case where the presence of any of the additional components mentioned herein is desirable in the composition, these will generally be mixed with the mixed metal oxide, preferably prior to mixing with the oxygen source. The components may be combined by any suitable method, eg by mixing. After mixing the components, the resulting oxygen generating composition can be dried and stored for later use, or placed in a mold to form part of an oxygen generator. The mixed metal oxide of the present disclosure may be prepared by any known route. Suitable routes for producing oxides of this type are described in Top. Catal. (2011) 54; 1266-1285. Ideally, the mixed metal oxide is prepared by co-precipitation, e.g., adding aqueous solutions of salts such as Mg (NO 3) 2.6H 2 O and Fe (NO 3) 3 .9H 2 O to a solution, preferably a ammonia solution (preferably at pH 11 or higher) to precipitate a semi-crystalline powder, which is then also mixed with LiOH.H 2 O. Other metal salts, eg, chlorides or phosphates can be used for the precipitation step, but nitrates are particularly preferred since they can be completely removed by heat treatment. In the same way, ammonia is the preferred medium of precipitation. If chlorides are used, the precipitates should be well washed to avoid the presence of chlorine.
    In order to produce nanoparticles, the product obtained can be deep-frozen with liquid N 2, followed by lyophilization, e.g., for more than 12 hours, especially more than 72 hours.
    The combination of precipitation, freezing and lyophilization produces homogeneous nanoparticles with high purity.
    The decomposition of the oxygen source of the compositions of the present disclosure results in the production of oxygen. Thus, from another aspect, the present disclosure discloses the use of a mixed metal oxide, as described herein, in a process for generating oxygen. The present disclosure also discloses the use of the mixed metal oxides, as herein described as multifunctional components, in oxygen generating compositions and oxygen generators, i.e .: single component with functions of catalyst, binding agent and fuel. Another aspect of the present disclosure relates to a method for generating oxygen, said method comprising decomposing an oxygen source as herein described in the presence of a mixed metal oxide, such as it is described here.
    The compositions of the present disclosure have utility in chemical oxygen generators, also referred to as "chemical oxygen generation devices", "chemical oxygen systems", "chemical oxygen generation systems", " oxygen generators ", etc.
    Thus, from another aspect, the present disclosure discloses a chemical oxygen generator comprising an oxygen generating composition as described herein. Preferably, said generator comprises a container for containing the oxygen-generating composition and a primer for initiating the decomposition of the oxygen-generating composition.
    The typical oxygen generators / chemical devices according to the present disclosure are fixed oxygen chemical generators and portable chemical oxygen generators. Especially preferably the chemical oxygen generator is, or includes, a chlorate candle.
    Stationary chemical oxygen generators are used in fixed systems, eg, those commonly used in aircraft carrying passengers. The system generally includes boxes, each containing an oxygen generator and one or more passenger masks. Generators are enabled when masks are presented. Thus, the present disclosure also discloses the use of compositions and generators as described herein in a fixed oxygen generating system, eg, an aircraft oxygen generating system. The present disclosure also discloses a method for producing oxygen, e.g., in an aircraft, comprising the use of the compositions and generators as described herein.
    An aircraft generally transports one or more oxygen generating systems selected from continuous flow systems, on-demand flow systems, diluent demand systems, and pressure demand systems. The generators and compositions of the present disclosure may be used in any such system. Thus, another aspect of the disclosure discloses an oxygen generating system, preferably an aircraft oxygen generating system, comprising a chemical oxygen generator or oxygen generating compositions as described herein.
    The present disclosure also discloses a kit for producing the oxygen generating composition as described herein or a kit for producing a chemical oxygen generator as described herein, said kit comprising an oxygen source as described herein and a mixed metal oxide as described herein.
    Chemical oxygen generating devices such as chlorate candles generally have a tapered cylindrical shape, with a recess at one end to contain an ignition pad. A typical candle configuration is shown in Figure 1 of SAE AIR1133. The ignition pad can be lit by lighting a primer. The heat coming from the ignition pad then ignites the reaction of the body of the candle and generates oxygen. The oxygen generating devices of the present disclosure therefore also preferably include an ignition pad and / or a primer. Suitable pellets and primers are known in the art.
    The oxygen generator, e.g., a candle, may comprise several layers of different compositions and thus different reaction rates. Multiple layers can be used to help meet oxygen generation requirements. Different applications have different requirements for oxygen generation. The shapes of the interface and the relative sizes and reactivities of the layers can be modified according to the requirements of the specific applications of the oxygen generating device.
    The oxygen generating devices of the present disclosure may therefore include compositions in addition to the oxygen generating composition as described herein. Furthermore, the devices could comprise a plurality of layers comprising the same composition or different compositions according to the present disclosure, eg layers comprising oxygen generating compositions as described herein which differ from each other according to one or more aspects such as: the identity / quantity of the oxygen source; the identity (eg, the specific proportion of metals in the oxide and / or the degree of crystallinity) / amount of mixed metal oxide present; and / or the quantity and / or identity of all possible components as described herein.
    The formation of the devices according to the present disclosure can be achieved by preparing the mixed metal oxide by any of the methods referred to herein and separately mixing the oxygen source with approximately 1 to 5 wt. water (water being used as a lubricant to facilitate the formation of generative nuclei or candles generating oxygen). The mixed metal oxide is then mixed with the moist oxygen source. The oxygen generating device, e.g., an oxygen generating candle, may be formed by compacting the wet mixture into a mold, which is then dried, eg at about 120 ° C, to remove the water that has been added during the mixing process.
    It will be understood that the disclosed uses and methods may take advantage of any of the products described above in connection with the compositions and products and vice versa.
    All references herein to the term "comprising" should be understood to encompass "including" and "containing" as well as "consisting of" and "consisting of essentially".
    Brief description of the illustrations
    One or more nonlimiting examples will now be described, with reference to the accompanying drawings, in which:
    Figure 1 illustrates a flowchart summarizing the process for preparing the mixed metal oxides of the present disclosure as further described in Example 1.
    Figure 2 illustrates the decomposition of sodium chlorate using (Li, Fe, Mg) O, non-calcined according to Example 2.
    Figure 3 illustrates the decomposition of lithium perchlorate using (Li, Fe, Mg) O, non-calcined according to Example 3.
    As shown in Figure 1, the mixed metal oxides according to the present disclosure can be formed by precipitation. An aqueous solution of Mg (NO 3) 2-6H 2 O is prepared by dissolving Mg (NO 3) 2-6H 2 O in distilled H 2 O. A solution of Fe (NO 3) 3-9H 2 O is prepared in the same way. The nitrate solutions are simultaneously added, dropwise, to a stirred ammonia solution while maintaining the pH value above 11. The gelatinous precipitates can be separated by centrifugation and rinsed with distilled H 2 O in a "cleaning" step. In order to incorporate the Li into the mixed metal oxide, the resulting precipitate is mixed with an aqueous solution of LiOH (LiOH xH 2 O) with appropriate Li concentrations (chosen to influence the amount of Li in the eventual oxide) in a tubular mixer and homogenized. In order to produce a nano-powder, the suspension can be frozen using liquid nitrogen. Then it can be lyophilized for at least 12 hours using a freeze-dryer. The combination of the aforementioned precipitation, freezing and lyophilization steps produces nanoparticles. Optionally, another grinding step can be used, even if the process allows the production of nanoparticles in the absence of grinding step.
    It will be understood that the foregoing description relates to a non-limiting example and that various changes and modifications may be made to the illustrated arrangement without departing from the scope of the disclosure, which is described in the appended claims.
    The disclosure will now be described in more detail with the following non-limiting Examples:
    Example 1
    Preparation of mixed metal oxides
    Aqueous solutions of Mg (NO 3) 2-6H 2 O are prepared by dissolving Mg (NO 3) 2 6H 2 O in distilled H 2 O. A solution of Fe (NO 3) 3-9H 2 O was prepared in the same way. The nitrate solutions were simultaneously added, dropwise, to a stirred ammonia solution while maintaining the pH value above 11. The gelatinous precipitates were rinsed with distilled H 2 O and mixed with an aqueous solution of LiOH (LiOH-1H2O) with appropriate concentrations of Li (selected to influence the amount of Li in the optional oxide) in a tubular mixer.
    Finally, the solution was frozen using liquid N 2. Then, it was lyophilized for at least 72 hours using a lyophilizer. Semi-crystalline powders of (Li, Fe, Mg) O were produced. Crystallinity "10%. The ratio of Li: Fe: Mg is determined by the preparation method.
    EXAMPLE 2 Decomposition of sodium chlorate using non-calcined (Li, Fe, Mg) 0 non-calcined (Li.Fe.MaK) 0 nano-sized and non-toxic (Li 0.5% .at, Fe 0.5 %, at) was prepared according to Example 1. It was combined with sodium chlorate (3% by weight of oxide with 97% by weight of sodium chlorate) by dry mixing (any method).
    The decomposition of sodium chlorate alone and in the presence of each of non-calcined, nano-sized, non-toxic (Li, Fe, Mg) 0 and cobalt oxide was monitored by comparing the reaction temperatures versus the The reaction heat developed in these reactions was determined by thermogravimetric differential scanning calorimetry (TG / DSC) measurements, recorded with a heating rate of 10 K / min in the reaction time, and the results are shown in FIG. temperature range of 20 ° C to 700 ° C. The weight of the sample (NaClO 3 + (Li, Fe, Mg) 0) was 40.0 mg.
    The decomposition process of pure sodium chlorate starts at 500 ° C and ends at 600 ° C (Figure 2, dashed line). The decomposition process of sodium chlorate in the presence of non-calcined, nano-sized, non-toxic (Li, Fe, Mg) 0 starts at 340 ° C and ends at 400 ° C (FIG 2, dashed line) . In comparison to what was considered one of the best catalysts, cobalt oxide (FIG.2 continuous line), the decomposition method using the oxide of disclosure is lowered, i.e. , ending at 400 ° C vs. 440 ° C. In addition, the mixed metal oxide of the present disclosure also acts as a bonding agent and a fuel, thus eliminating the need for other components to perform these functions, and it is non-toxic, and it is therefore preferable to cobalt oxide, which is commonly considered the best catalyst for this reaction.
    Example 3 Decomposition of Lithium Perchlorate Using Non-calcined (nonionic) Li-Fe calcined Li (Fe, Mg) 0 of nano-size and non-toxic (0.5% Li, 0.5% Fe) .at) was prepared according to Example 1. It was combined with lithium perchlorate (3% by weight of oxide with 97% by weight of sodium chlorate) by dry mixing (any method).
    The decomposition of lithium perchlorate alone and in the presence of each of non-calcined, non-toxic, nano-sized (Li, Fe, Mg) 0 and cobalt oxide was monitored by comparing the reaction temperatures versus the The reaction heat developed in these reactions was determined by thermogravimetric differential scanning calorimetry (TG / DSC) measurements, recorded with a heating rate of 10 K / min in the reaction time, and the results are shown in FIG. temperature range of 20 ° C to 700 ° C. The weight of the sample (LiClO 4 + (Li, Fe, Mg) O) was 40.0 mg.
    The decomposition method of pure lithium perchlorate starts at 480 ° C and ends at 510 ° C (FIG 3, dashed line). The process of decomposing lithium perchlorate in the presence of non-calcined, non-toxic, nano-sized (Li, Fe, Mg) 0 starts at 440 ° C and ends at 490 ° C (FIG 3, dashed line) . In comparison with what was considered one of the best catalysts, cobalt oxide (FIG.3 continuous line), the decomposition method using the oxide of disclosure is shifted to a slightly higher temperature, however, the mixed metal oxide of the present disclosure also acts as a bonding agent and a fuel, thus eliminating the need for other components to perform these functions, and it is non-toxic, and it is therefore preferable to cobalt oxide, which is commonly considered the best catalyst for this reaction.
    权利要求:
    Claims (15)
    [1" id="c-fr-0001]
    Claims:
    An oxygen generating composition comprising an oxygen source and a mixed metal oxide of the formula: (Li, Fe, Mg) 0.
    [2" id="c-fr-0002]
    A composition as claimed in claim 1, wherein less than 25% of the mixed metal oxide is in crystalline form.
    [3" id="c-fr-0003]
    A composition as claimed in claim 1 or claim 2, wherein less than 10% of the mixed metal oxide is in crystalline form.
    [4" id="c-fr-0004]
    A composition as claimed in any one of the preceding claims, wherein said mixed metal oxide comprises 0.1 to 1.0% Fe and 0.1 to 1.0% Li. .
    [5" id="c-fr-0005]
    A composition as claimed in any one of the preceding claims, wherein said mixed metal oxide is in the form of nanoparticles.
    [6" id="c-fr-0006]
    The composition as claimed in claim 5, wherein said nanoparticles have a diameter of less than or equal to 500 nm.
    [7" id="c-fr-0007]
    A composition as claimed in any one of the preceding claims, wherein said oxygen source is selected from alkali metal chlorates, alkali metal perchlorates, alkaline earth metal chlorates, metal perchlorates. alkaline earths and mixtures thereof.
    [8" id="c-fr-0008]
    A composition as claimed in any one of the preceding claims, wherein said oxygen source comprises sodium chlorate and / or lithium perchlorate.
    [9" id="c-fr-0009]
    A composition as claimed in any one of the preceding claims, wherein said composition is substantially composed of said oxygen source and said mixed metal oxide.
    [10" id="c-fr-0010]
    A composition as claimed in any one of the preceding claims, wherein 90 to 99.9% by weight of said composition is the source of oxygen.
    [11" id="c-fr-0011]
    A composition as claimed in any one of the preceding claims wherein 0.1 to 10% by weight of said composition is mixed metal oxide.
    [12" id="c-fr-0012]
    A process for generating oxygen, said process comprising decomposing an oxygen source as described in any one of claims 1 to 11 in the presence of a mixed metal oxide such as it is described in any one of claims 1 to 11.
    [13" id="c-fr-0013]
    A chemical oxygen generator comprising an oxygen generating composition as claimed in any one of claims 1 to 11.
    [14" id="c-fr-0014]
    A chemical oxygen generator as claimed in claim 13, wherein said generator comprises a container for containing the oxygen generating composition and a primer for initiating the decomposition of the oxygen generating composition.
    [15" id="c-fr-0015]
    15. The chemical oxygen generator as claimed in claim 13 or claim 14, wherein said chemical oxygen generator is a chemical oxygen candle.
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    同族专利:
    公开号 | 公开日
    FR3042485B1|2019-11-15|
    DE102015117831A1|2017-04-20|
    US10358348B2|2019-07-23|
    US20170107104A1|2017-04-20|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4086175A|1976-02-09|1978-04-25|Shell Oil Company|Activated bleaching process and compositions therefor|
    US4073741A|1976-03-05|1978-02-14|A-T-O Inc.|Cobalt oxide chlorate candle|
    US5049306A|1989-09-29|1991-09-17|Mine Safety Appliances Company|Oxygen generating candles|
    US5298187A|1992-03-13|1994-03-29|Puritan-Bennett Corporation|Non-toxic chemical oxygen generating compositions|
    US5279761A|1992-03-13|1994-01-18|Puritan-Bennett Corporation|Chemical oxygen generating compositions containing LI202|
    US5783105A|1995-11-09|1998-07-21|Nellcor Puritan Bennett|Oxygen generating compositions|
    US6007736A|1996-05-15|1999-12-28|Be Intellectual Property|Oxygen generating compositions catalyzed by copper and nickel oxides|
    US5882545A|1996-05-15|1999-03-16|Nellcor Puritan Bennett Incorporated|Oxygen generating compositions|
    RU2302993C2|2001-07-26|2007-07-20|Недерландсе Органисати Вор Тугепаст-Натюрветенсхаппелейк Ондерзук Тно|Chemical oxygen generator|
    WO2008094490A1|2007-01-26|2008-08-07|Avox Systems, Inc.|Oxygen generating composition|
    EP2490807A1|2009-10-23|2012-08-29|Massachusetts Institute Of Technology|Biotemplated inorganic materials|
    EP2851340B1|2013-09-23|2018-10-31|Goodrich Lighting Systems GmbH|Ortho-phosphate, ortho-vanadate or ortho-phosphate-vanadate components for use in solid chemical oxygen generators|
    DE102015117838A1|2015-10-20|2017-04-20|Goodrich Lighting Systems Gmbh|Oxygen generating compositions comprising thermally treated O|
    DE102015117835A1|2015-10-20|2017-04-20|Goodrich Lighting Systems Gmbh|Oxygen generating compositions comprising O|
    DE102015117839A1|2015-10-20|2017-04-20|Goodrich Lighting Systems Gmbh|Oxygen generating compositions comprising thermally treated O|DE102015117839A1|2015-10-20|2017-04-20|Goodrich Lighting Systems Gmbh|Oxygen generating compositions comprising thermally treatedO|
    DE102015117835A1|2015-10-20|2017-04-20|Goodrich Lighting Systems Gmbh|Oxygen generating compositions comprisingO|
    DE102015117838A1|2015-10-20|2017-04-20|Goodrich Lighting Systems Gmbh|Oxygen generating compositions comprising thermally treatedO|
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    优先权:
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    DE102015117831.1|2015-10-20|
    DE102015117831.1A|DE102015117831A1|2015-10-20|2015-10-20|Oxygen generating compositions comprisingO|
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