• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    A method and system for the extraction of isocyanuric acid is disclosed. According to the invention, the water containing the isocyanuric acid is passed through a bed with an adsorbent material, the bed is regenerated by the use of a liquid regeneration medium, the liquid regeneration medium containing the isocyanuric acid in solution, it is recovered by the addition of a complexing solid substance, the suspension obtained is passed through a filter medium and the isocyanuric acid and the regenerated extraction liquid medium is recovered. The system comprises an adsorption column, a reservoir of regenerating substance, a filter medium, a tank for dosing the regenerating substance, a compressor, a driving pump and a valve system for configuring the equipment according to the phase of the cycle in which have to operate. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2680486A1
    申请号:ES201730257
    申请日:2017-02-27
    公开日:2018-09-07
    发明作者:Carlos MACÍAS GÁLLEGO
    申请人:Diasa Ind S A；DIASA INDUSTRIAL SA；
    IPC主号:
    专利说明:

    DESCRIPTION

    PROCEDURE AND SYSTEM FOR THE EXTRACTION OF ISOCIANURIC ACID IN DISSOLUTION
     5
    Field of the Invention
    The present invention relates generally to the field of isocyanuric acid level control in swimming pool waters, and more particularly to a process and a system for the extraction of isocyanuric acid, keeping it within safe levels for the disinfectant action of chlorine. . 10
    Background of the invention
    The addition of chlorine in the form of trichloroisocyanuric acid is widespread in the world of swimming pools because it is the method that achieves a more effective chlorine action due to its slow and persistent release over time. However, the addition of chlorine in this form ends up causing the accumulation of isocyanuric acid in the water and from certain levels begins to inhibit the disinfectant action of chlorine by recombination.
    Currently, the method commonly used to control the concentration of isocyanuric acid in water is by replacing the corresponding volume of water with new water, which is a huge waste of this scarce resource.
    Some procedures for the removal of isocyanuric acid from water have been tested but none of them seems viable on an industrial scale per se.
    A method known in the prior art is the method according to patent application US2011259835, which is used to reduce the concentration of the isocyanuric acid level in the pool water to prevent chlorine blockage. The method comprises the steps of adding an effective amount of sodium hydroxide combined with an antimicrobial agent for the pool water and reacting the sodium hydroxide with the isocyanuric acid in it to reduce the concentration of isocyanuric acid. The antimicrobial agent reduces the amount of microorganisms that have accumulated in the pool water until the release of chlorine.
    From US5194162 a method is known to reduce the concentration of isocyanuric acid level in the pool water to prevent chlorine blockage. The method comprises the steps of adding an effective amount of sodium hydroxide to the pool water and reacting the sodium hydroxide with the isocyanuric acid 35 therein to reduce the isocyanuric concentration to a level between about 40 to 60 PPM.
    Another process known in the prior art is adsorption on activated carbon. Isocyanuric acid adsorbs well in this material when contaminated water is passed through a granular bed under the appropriate dynamic conditions; However, once the coal is saturated, its replacement is necessary, so unless an in situ regeneration method is available, the procedure is laborious and costly.
    Another known system of the prior art is the complexation of isocyanuric acid with melamine to form melamine isocyanurate which is in the form of
    microscopic crystals suspended in water. However, this system has several drawbacks: on the one hand, in the conditions of the pool water, the amount of melamine that reacts with cyanuric is low, so a high amount of melamine must be dosed to complex a significant amount of cyanuric, leading to problems of turbidity and toxicity in the pool since the combination of cyanuric and melamine is toxic. This mixture will remain in the pool constantly as the melamine is soluble in water at a rate of 3100 mg / L, which can also lead to water coloring problems. On the other hand, the crystals formed must be removed from the water, which is not feasible with the filter systems commonly used in swimming pools because they are excessively thin and deformable.
    Thus, there is still a need in the art for a procedure and a system that allows isocyanuric acid to be extracted from the water in an effective and viable way on an industrial scale, keeping it within safe levels for the disinfectant action of chlorine and also recovering it. for its subsequent use in the manufacture of other chemical components, such as for the manufacture of trichloroisocyanuric acid for the sterilization of swimming pools due to its high percentage of free chlorine. On the other hand, it would be desirable to have a procedure and system with a closed and ecological circuit.
    Summary of the invention 20
    To solve the problems of the prior art, in a first aspect the present invention discloses a process for the extraction of isocyanuric acid in solution comprising the following steps:
    (a) In a first step, this being the adsorption process, the water containing the isocyanuric acid is passed through a bed with an adsorbent material,
    (b) The water that passes through the bed is constantly returned to the source of origin so that the concentration of isocyanuric acid decreases over time,
    (c) Once the level of isocyanuric acid determined as a function of the needs has been reached, that is, at safe levels for the disinfectant action of the chlorine in the source of origin, the second step is taken, which is the regeneration of the bed by using a liquid regeneration medium, this being a polar solvent having an affinity for the isocyanuric acid greater than that of the adsorbent,
    (d) The liquid regeneration medium containing a concentration of isocyanuric acid in solution is collected and it is recovered in the third step of the process, by the addition of a solid complexing substance of the isocyanuric acid,
    (e) A crystal suspension is obtained, 40
    (f) The mixture obtained in step (e), in the third step, is passed through a filter medium of suitable mesh size for the retention of the solid mixture obtained,
    (g) The solid isocyanurate mixture, and the regenerated liquid extraction medium, is recovered.
    (h) The regenerated liquid extraction medium is returned to the system for
    next bed regeneration cycle.
    The combination of the steps and means used ensures a single procedure that eliminates the drawbacks of the prior art, while providing advantages for the user.
    The three steps of the procedure, that is, the adsorption, regeneration and filtration step are repeated cyclically, allowing the level of isocyanuric acid in pool water to be controlled. With the present invention, the excess of dissolved isocyanuric acid is extracted from the water and subsequently recovered in a solid mixture with other components. This mixture can in turn be used as a raw material for the manufacture of trichloroisocyanuric acid, thus recycling this compound instead of eliminating it from the environment with the pouring of water. It should be noted that there is no significant waste, no waste of water or other reagents used in the process, which is an important indicator when assessing the usefulness and application of the procedure.
    In summary, the process according to the present invention consists in passing the aqueous solution of the isocyanuric acid through an adsorbent bed, extracting the compound from the adsorbent bed by means of a liquid substance of greater affinity for the compound than the adsorbent and, finally, recovering the compound concentrated in the liquid substance by the addition of a solid powder substance that completely complexes the isocyanuric acid and is separated from the liquid substance by a suitable filtration system.
    According to another aspect, the present invention discloses a system for the extraction of isocyanuric acid in solution comprising:
    - a pump, which in the adsorption cycle, drives the water from the source of origin through means for regulating flow towards an adsorption column where isocyanuric acid is retained,
    - means for flow regulation that allow the return of isocyanuric acid free water to the source of origin,
    - a reservoir of liquid regeneration medium, connected to a dosing tank in which a complexing solid substance is added, optionally together with a filtration aid,
    - means for the regulation of flow that allow the passage of the liquid regeneration medium from the liquid regeneration tank to the dosing tank through other means for flow regulation,
    - a pump that drives the regeneration liquid from the reservoir of the regeneration liquid medium through means for the flow regulation to the dosing tank through other means for the flow regulation,
    - a solid mixture retention filter,
    - a metering pump, which in the regeneration cycle doses in line the suspension of the dosing tank to the retention filter, 40
    - means for the regulation of flow that allow the supply of the liquid medium from the dosing tank to the retention filter,
    - means for the regulation of flow which allow the regeneration liquid recovered from the retention filter to be supplied to the adsorption column in the opposite direction to the adsorption cycle, 45
    - means for flow regulation that return the regeneration liquid after passing through the adsorption column to the reservoir of regeneration liquid medium.
    The use of the system according to the present invention allows to reduce the level of isocyanuric acid in the source of origin and at the same time allows to obtain raw material for the manufacture of trichloroisocyanuric acid. The invention provides a closed circuit, thus, no waste of chemical means occurs. At the same time, the system is easy to implement and viable at the commercial level.
    Brief description of the figures
    The present invention will be better understood with reference to the following 10 figures illustrating a preferred embodiment of the invention, provided by way of example, and which should not be construed as limiting the invention in any way.
    Figure 1 is a view of the system according to the first preferred embodiment of the present invention. fifteen
    Figure 2 is a view of the system according to the second preferred embodiment of the present invention.
    Detailed description of the preferred embodiments
    A detailed description of the present invention is provided below. twenty
    The object of the present invention is a general procedure for the extraction and recovery of isocyanuric acid from an aqueous solution. This new procedure is mainly applicable to the control of the level of this compound in pool water, keeping it within safe levels for the disinfectant action of chlorine. 25
    The process for the extraction of isocyanuric acid in solution according to the present invention comprises the following steps:
    In step (a), this being the first step of the process called the adsorption process, the water containing the isocyanuric acid is passed through a bed with an adsorbent material. The adsorbent material used in this step is selected from the group of materials in the form of porous carbon having a high affinity for isocyanuric acid, preferably selected from the group comprising activated carbon, carbon airgel, carbon xerogel, carbon fibers activated, ordered mesoporous carbon (OMC) or graphene gels. In a preferred embodiment of the present invention, activated carbon is used. 35
    In step (b), the water that passes through the bed is constantly returned to the source of origin, this being usually a pool, so that the concentration of isocyanuric acid decreases over time.
    In step (c), once the level of isocyanuric acid determined has been reached, the appropriate levels being according to the current guidelines between 30 and 50 ppm, and not more than 100 ppm, the second main step of the procedure is that of regeneration. of the bed by the use of a liquid regeneration medium being this a polar solvent having an affinity for the isocyanuric acid greater than that of the adsorbent, so that the isocyanuric acid passes from the adsorbent to the liquid substance leaving the adsorbent clean for a next adsorption cycle Four. Five
    Preferably, the polar solvent used in the bed regeneration cycle is selected from the group comprising: HCl, NaOH, KOH or a polar hydrocarbon selected from the group comprising: acetone, diethylether, dimethyl formamide, dimethyl sulfoxide, methanol, ethanol and pyridine , or their mixtures. In a preferred embodiment of the present invention, methanol is used. 5
    In another preferred embodiment of the present invention, the polar hydrocarbon is mixed with water in a proportion of water between 50% (vol./vol.) And 10% (vol./vol.), Preferably in a proportion of 10 % (vol./vol.).
    In another preferred embodiment of the present invention, the polar hydrocarbon mixture with water has a pH between 4 and 10, and more preferably the pH is 10 8.
    The pH is regulated with the addition of NaOH or KOH. As examples, the final equilibrium concentrations for a 50% water / methanol mixture of 15 ml in contact with 1 g of carbon saturated with isocyanuric acid are 475, 485, 533, 470 and 490 mg / L for the pHs of 2.63, 4.25, 8, 10, 11.5 respectively. fifteen
    In step (d), the liquid regeneration medium that acquires a high concentration of isocyanuric acid in solution is collected and is recovered in the third step of the process, by the addition of an isocyanuric acid complexing substance. This substance in the liquid extraction medium reacts with the isocyanuric acid forming microscopic sized isocyanurate crystals.
    As a complexing substance, any molecule capable of forming multiple hydrogen bonds and with some symmetry can be used. Preferably, the isocyanuric acid complexing substance employed in step (d) is selected from the group comprising: melamine, amelide, ameline, bis-diaminotriazines, tris-diaminotriazines. In a preferred embodiment of the present invention, melamine is used.
    In step (e), a suspension of crystals is obtained, in a preferred embodiment, crystals of melamine isocyanurate are obtained, which, in an optional stage, is mixed with a filtration aid of similar particle size or somewhat higher of the crystals obtained.
    In a preferred embodiment, a mixture of the complexing solid substance and the filtration aid is added to the liquid regeneration medium containing a high concentration of isocyanuric acid in solution in the third step of the process to obtain a suspension of crystals. A mixture of approximately 50% can be used.
    Preferably, the filtration aid used in step (e) is selected from the group: natural diatomaceous earth, calcined or calcined to flow, perlite, cellulose or any of its mixtures.
    In step (f), the mixture obtained in step (e) is passed through a filter medium of mesh size suitable for retention of the solid mixture obtained.
    Preferably, the filter medium used has the permeability of the adjuvant between 0.04 Darcys and 10 Darcys, preferably 4 Darcys.
    In step (g), on the one hand, the solid mixture of isocyanurate and adjuvant is recovered if it is used, and on the other hand, the liquid extraction medium
    regenerate.
    In step (h), the regenerated liquid extraction medium is returned to the system for the next bed regeneration cycle.
    As a result of the process according to the present invention, the solid mixture can be used as raw material for the manufacture of trichloroisocyanuric acid and the regenerated liquid extraction medium can be used in a new extraction cycle.
    According to another aspect of the present invention, a system for practicing the procedure described above is disclosed. For this, the system for the extraction of isocyanuric acid in solution comprises:
    - a pump B01, which in the adsorption cycle, drives the water from the source of origin through means for the regulation of flow towards an adsorption column C01 where the isocyanuric acid is retained,
    - means for flow regulation that allow the return of isocyanuric acid free water to the source of origin, 15
    - a reservoir D01 of liquid regeneration medium, connected with a dosing reservoir D02 in which a complexing solid substance is added, and in an optional embodiment, together with a filtration aid. In this optional embodiment, an approximately 50% mixture can be used.
    - means for the flow regulation that allow the passage of the liquid regeneration medium 20 from the tank D01 to the dosing tank D02 through other means for the flow regulation,
    - a pump that drives the regeneration liquid from the tank D01 through means for flow regulation to the dose tank D02 through other means for flow regulation, 25
    - a solid mixture retention filter F01,
    - a dosing pump B02, which in the regeneration cycle, doses in line the suspension of the tank D02 towards the filter F01,
    - means for flow regulation that allow the supply of liquid medium from the dosing tank D02 to the filter F01, 30
    - means for the flow regulation that allow the regeneration liquid recovered from the filter F01 to be supplied to the adsorption column C01 in the opposite direction to the adsorption cycle,
    - means for flow regulation that return the regeneration liquid after passing through the adsorption column C01 to the tank D01. 35
    In this way, equipment specifically designed to maintain the level of isocyanuric acid in pool water is obtained within safe levels previously set. The equipment is designed to operate in automatic cycles requiring very little attention from the operator.
    The equipment consists of an adsorption column with a specific adsorbent, a reservoir of regenerating substance of the adsorbent, a filter for filtration of the regenerating substance, a tank with stirring containing a filtering substance to dose the regenerating substance, a compressor, a pump of impulsion and a system of valves to configure the equipment according to the phase of the cycle in which it has
    What to operate The equipment operates in three cycles: adsorption, regeneration and rinsing that will operate sequentially and in the same order.
    In Fig. 1 the system according to the first preferred embodiment of the present invention is shown.
    Specifically, the model comprises the parts enclosed in the box of Figure 1. According to the present invention, it is operated in three successive cycles: adsorption, regeneration and rinsing.
    The system for the extraction of isocyanuric acid in solution according to this preferred embodiment comprises:
    - a pump B01, which in the adsorption cycle, drives the water from the source source through a valve VA01 towards an adsorption column C01 where the isocyanuric acid is retained,
    - valves VA03, VA04 and VA12 to return isocyanuric acid free water to the source of origin,
    - a reservoir D01 of liquid regeneration medium, connected with a dosing reservoir D02 in which a complexing solid substance is added, preferably together with a filter aid,
    - a valve VA16 that allows the passage of the liquid regeneration medium from the tank D01 to the dosing tank D02 through valves VA08 and VA15, 20
    - a pump B01 that drives the regeneration liquid from the tank D01 through the valve VA16 to the dosing tank D02 through the valves VA08 and VA15,
    - a solid mixture retention filter F01,
    - a dosing pump B02, which in the regeneration cycle, doses the suspension of the tank D02 in line 25 towards the filter F01,
    - a VA09 valve that allows the supply of the liquid medium from the dosing tank D02 to the filter F01,
    - valves VA11, VA04 and VA03 for supplying the regeneration liquid recovered from the filter F01 to the adsorption column C01 in the opposite direction to the adsorption cycle 30,
    - valves VA13 and VA06 that return the regeneration liquid after passing through the adsorption column C01 to the tank D01.
    In the adsorption cycle a pump B01 drives the water from the source of origin, preferably this being a pool, through a valve VA01 towards an adsorption column C01 where the isocyanuric acid is retained by means of a specific adsorbent. Said valve may be piloted according to any of the modes known in the art such as, for example, hydraulically, pneumatically, electrically, electronically, but the use of other types of piloting is also contemplated, such as manually. Next, the water leaves column 40 C01 already free of isocyanuric acid and returns to the pool through valves VA03, VA04 and VA12. Only the mentioned valves remain open during this cycle. The water that returns to the pool without isocyanuric acid causes the concentration of this compound in the pool to decrease progressively.
    When the safety concentration set is reached, the equipment prepares to complete the adsorption cycle and move on to the next cycle.
    For this, the CM01 compressor that drives air through valves VA10 and VA02 is activated. The water evacuated from column C01 after the adsorption cycle, is returned to the pool through valves VA03, VA04 and VA12 and once empty, the CM01 compressor continues to blow for a while, which can be programmed in the equipment , to remove as much water as possible from column C01. During this part of the cycle the rest of the valves remain closed. After draining, water is passed through the C01 column to rinse the water through the valve VA07, this water being drained through the drain through the valve VA14 of the installation. The rinse time can be programmed in the control panel of the equipment.
    Once the rinsing of column C01 is finished, the regeneration cycle is started by activating the pump B01 that drives the regeneration liquid from the tank D01 through the valve VA16 to the dosing tank D02 through 15 valves VA08 and VA15.
    A solid powder substance, isocyanuric acid complexing, is added to the dosing tank D02, which is suspended with the aid of stirrer A01 in the regeneration liquid. At this time it is also possible to add the filter aid simultaneously to the dosing tank D02. Once the tank D02 is filled 20, the valve VA08 is closed and VA09 is opened, reaching the filter F01, and VA11, VA4, VA03 passing through the column C01 in the opposite direction to the adsorption cycle. The regeneration liquid extracts the isocyanuric acid from the adosrbente, leaves column C01 and passes through valves VA13 and VA06 returning to tank D01. Simultaneously to this process, the dosing pump 25 B02 injects the suspension of the tank D02 into the pipe section upstream of VA08, so that the regeneration liquid with dissolved isocyanuric acid is mixed with the complexing solid in suspension, both being retained in the filter F01. In this way, the regeneration liquid leaves the filter F01 clean and goes back through the column C01 to continue extracting isocyanuric acid from the adsorbent. 30 This process continues until no more isocyanuric acid is removed from the adsorbent of column C01, at which time the regeneration cycle ends and the rinse cycle begins to prepare column C01 for the adsorption cycle. At this time the column C01 is emptied by passing air from the CM01 compressor through the valves VA10 and VA02 by evacuating the regeneration liquid 35 from the column C01 after the regeneration cycle and returning it to the tank D01 through the valves VA03, VA05 and VA06. After evacuation, the CM1 compressor continues to run for a time that can be programmed in the equipment, to remove as much of the regeneration liquid as possible from column C01. During this part of the cycle the rest of the valves remain closed. After draining, the network water is passed through the column C01 to perform a rinse by passing the water through the valve VA07, this water being evacuated through the valve VA14 and through the installation drain. The rinsing time can be programmed in the control panel of the equipment, being recommended between 20 and 30 min. After the rinse of column C01, the equipment is ready to start a new adsorption cycle.
    The system also incorporates a VM01 sampling valve, for the control of isocyanuric acid at the exit of column C01. If its concentration reaches a predetermined value, for example, 15ppm, the change of the adsorbent bed must be carried out in a system maintenance work. fifty
    The system according to the second preferred embodiment of the present invention is shown in Fig. 2.
    Specifically, the model consists of the parts enclosed in the box of Figure 2. According to the present invention, it is operated in three successive cycles: adsorption, regeneration and rinsing, as in the first preferred embodiment of the present invention.
    The system for the extraction of isocyanuric acid in solution according to this preferred embodiment comprises:
    - a pump B01, which in the adsorption cycle, drives the water from the source of origin through a valve VA01 to a selector valve VS01 and towards a 10 adsorption column C01 where isocyanuric acid is retained,
    - valves VS01 and VA102 to return isocyanuric acid free water to the source of origin,
    - a reservoir D01 of liquid regeneration medium, connected with a dosing reservoir D02 in which a complexing solid substance is added, preferably together with a filter aid,
    - a valve VA104 that allows the passage of the liquid regeneration medium from the tank D01 to the dosing tank D02 through a valve VA105,
    - a pump B03 that drives the regeneration liquid from the tank D01 through the valve VA104 to the dosing tank D02 through 20 through the valve VA105,
    - a solid mixture retention filter F01,
    - a dosing pump B02, which in the regeneration cycle, drives the suspension of the tank D02 towards the filter F01,
    - a VA106 valve that allows the supply of liquid medium from the dosing tank D02 to the filter F01,
    - valves VA107, VA108 for supplying the regeneration liquid recovered from the filter F01 through the selector valve VS01 towards the adsorption column C01 in the opposite direction to the adsorption cycle,
    - VS01 and VA109 valves that return the regeneration liquid after its passage through the adsorption column C01 to the tank D01.
    In this variant of the equipment, column C01 can be operated by means of a five-way valve, this being the selector valve VS01 that simplifies the operation of the system, decreasing the number of valves used. The person skilled in the art will understand that it is also possible to use track valves with other types of configurations such as six-way, seven-way valves, etc.
    In the adsorption cycle, the pool water is driven by means of the pump B01 through the valve VA101 to the selector valve VS01 and passes through it to the adsorption column C01, where the isocyanuric acid is removed by medium of a specific adsorbent. The valve VA101 may be an actuated valve 40, but said valve may be piloted in any of the ways known in the art such as, for example, hydraulically, pneumatically, electrically, electronically. The use of other types of piloting is also contemplated, such as manually. Then the water leaves the column
    C01 already free of isocyanuric acid and returns to the pool through the valves VS01 and VA102. Only the mentioned valves remain open during this cycle. The water that returns to the pool without isocyanuric acid causes the concentration of this compound in the pool to decrease progressively. When the safety concentration set is reached, the equipment is prepared 5 to complete the adsorption cycle and move on to the next cycle. For this, the CM01 compressor that drives air through the VA108 valve is activated. The water evacuated from column C01 is returned to the pool through valves VS01 and VA102 and once empty, the CM01 compressor continues to blow for a while, which can be programmed in the equipment, to eliminate as much water as possible from column C01. 10 During this part of the cycle the remaining valves remain closed. After draining, water is passed through the C01 column to rinse the water through the VS01 VA103 valve, this water being evacuated through the drain of the installation. The rinse time can be programmed in the control panel of the equipment. Once the rinsing of column C01 is finished, the regeneration cycle is started by activating the pump B03 that drives the regeneration liquid from the tank D01 through the valve VA104 to the dose tank D02 through the valve VA105. A solid powder substance, isocyanuric acid complexing, is added to the dosing tank D02, which is suspended with the aid of stirrer A01 in the regeneration liquid. Once the tank D02 is filled, the valve VA105 is closed and VA106 is opened, reaching the filter F01, and VA107, VA108 passing through the selector valve VS01 to the column C01 in the opposite direction to the adsorption cycle. The regeneration liquid extracts the isocyanuric acid from the adsorbent, leaves the column C01 and passes through the valves VS01 and VA09 returning to the tank D01. Simultaneously to this process, the dosing pump 25 B02, injects the suspension of the tank D02 into the pipe section upstream of VA105, so that the regeneration liquid with dissolved isocyanuric acid is mixed with the complexing solid and the adjuvant in suspension. both retained in filter F01. In this way, the regeneration liquid leaves the filter F01 clean and goes back through the column C01 to continue extracting isocyanuric acid from the adsorbent. This process continues until no more isocyanuric acid is removed from the adsorbent of column C01, at which time the regeneration cycle ends and the rinse cycle begins to prepare column C01 for the adsorption cycle. At this time the column C01 is emptied by passing air from the CM1 compressor through the valves VA108 and VS01 35 by evacuating the regeneration liquid from the column C01 and returning it to the tank D01 through the valve VA109. After evacuation, the CM1 compressor continues to run for a time that can be programmed in the equipment, to remove as much of the regeneration liquid as possible from column C01. During this part of the cycle the rest of the valves remain closed. After draining, water from the network is passed through column C01 to rinse the water through the valve VA103, this water being evacuated through the drain of the installation. The rinsing time can be programmed in the control panel of the equipment, being recommended between 20 and 30 min. Once the rinse of column C01 is finished, the equipment is ready to start a new adsorption cycle. Four. Five
    In another variant of the equipment, manual valves can be used instead of operated. The person skilled in the art will understand that said valves can be piloted in any of the ways known in the art such as, for example, hydraulically, pneumatically, electrically, electronically.
    Example of embodiment of the invention 50
    In a first example, a 10 L solution of 35 mg / L acid was used
    isocyanuric by adding 625 mg of trichloroisocyanuric acid in 10 L of water. As an adsorbent an activated carbon treated with nitric acid was used to increase the affinity for isocyanuric acid. The amount of adsorbent used was 120 ml and was placed on a column 4.5 cm in diameter x 7 cm in height. The solution was passed through the column at a flow rate of 1.5 m / h 5, obtaining a concentration below the detection limit of the isocyanuric acid measuring equipment for the 10 L solution. This experiment was repeated several times to saturate the column and up to 95 L were passed before starting to detect isocyanuric acid at the exit of it. Water continued to pass until the output concentration matched that of the inlet, reaching 10 215 L in total. The column was then emptied and the regeneration was carried out by passing 600 ml methanol first through the bed of saturated carbon of isocyanuric acid and then and in the same process, by a ceramic filter dosing in line a 1: 1 mixture of melamine and diatom. The analysis of the isocyanuric acid content at the exit of the adsorption column gave a value above 15 the detection limit of the measuring equipment at the beginning of the regeneration process and the analysis at the exit of the filter gave a value below the limit detection. The process was maintained until the isocyanuric acid content at the exit of the adsorption column was below the detection limit of the measuring equipment, indicating the maximum extraction of the column. After the column regeneration process 20, the column was washed with running water to remove methanol residues and the adsorption process was restarted until saturation. 210 L of isocyanuric acid solution was passed until saturation of the column indicating a regeneration greater than 97%.
    In a preferred embodiment, in the system according to the present invention the adsorption column C01 contains an adsorbent material selected from the group of materials in the form of porous carbon, preferably the porous carbon is selected from the group comprising activated carbon, carbon airgel, Carbon xerogel, activated carbon fibers, ordered mesoporous carbon (OMC) or graphene gels.
    In another preferred embodiment, in the system according to the present invention the liquid regeneration medium is a polar solvent having an affinity for the isocyanuric acid greater than that of the adsorbent, preferably the polar solvent is selected from the group comprising: HCl, NaOH , KOH or a polar hydrocarbon selected from the group comprising: acetone, diethylether, dimethyl formamide, dimethyl sulfoxide, methanol, ethanol and pyridine, or mixtures thereof. 35
    In another preferred embodiment, in the system according to the present invention the solid complexing substance of the isocyanuric acid is selected from the group comprising: melamine, amelide, ameline, bis-diaminotriazines, tris-diaminotriazines.
    In another preferred embodiment, in the system according to the present invention the filtration aid is selected from the group: natural diatomaceous earth, calcined or flow calcined, perlite, cellulose or any of its mixtures
    In another preferred embodiment, in the system according to the present invention, the solid mixture retention filter F01 has the diatom permeability between 0.04 Darcys and 10 Darcys, preferably 4 Darcys.
    As defined above, the equipment developed according to the present invention consists of an adsorption column with a specific adsorbent, a reservoir of regenerating substance of the adsorbent, a filter for filtration of the regenerating substance, a tank with stirring containing a filter substance for dosing the regenerating substance, a compressor, a discharge pump and a
    valve system or other means for flow regulation to configure the equipment according to the phase of the cycle in which it has to operate. The person skilled in the art will understand that the means for flow regulation can be various valves or other equivalent means, which will be used according to the needs of each particular installation. Its function is to provide the connection between the elements of the present invention. They can be generally referred to as: means for regulating the flow of water between the source of origin and the adsorption column, means for regulating the flow between the reservoir of liquid regeneration medium and the dosing tank, means for the flow regulation between the dosing tank and the retention filter, means for regulating the regeneration liquid flow recovered 10 from the retention filter and the adsorption column, or means for the flow regulation that return the regeneration liquid after passing through the adsorption column to the liquid regeneration medium tank.
    Although the present invention has been described above with reference to specific embodiments thereof, the person skilled in the art may devise modifications and variations of said embodiment without thereby departing from the scope of the present invention.
    权利要求:
    Claims (34)
    [1]
    1. Procedure for the extraction of isocyanuric acid in solution, comprising the following steps:
    (a) Water containing isocyanuric acid is passed through a bed with an adsorbent material,
    (b) The water that passes through the bed is constantly returned to the source of origin,
    (c) Once the level of isocyanuric acid determined at the source of origin is reached, the bed is regenerated by using a liquid regeneration medium, this being a polar solvent having an affinity for the isocyanuric acid greater than that of the adsorbent,
    (d) The liquid regeneration medium containing a concentration of isocyanuric acid in solution is collected and it is recovered by the addition of an isocyanuric acid complexing substance,
    (e) A crystal suspension is obtained, which is mixed with a filter aid of particle size larger than the crystals obtained,
    (f) The mixture obtained in step (e) is passed through a filter medium of suitable mesh size for the retention of the solid mixture obtained,
    (g) The solid mixture of isocyanurate and adjuvant, and the regenerated liquid extraction medium, are recovered.
    (h) The regenerated liquid extraction medium is returned to the system for the next bed regeneration cycle.
    [2]
    2. Method according to claim 1, characterized in that the adsorbent material used in step (a) is selected from the group of materials in the form of porous carbon. 25
    [3]
    3. Method according to claim 2, characterized in that the porous carbon is selected from the group comprising activated carbon, carbon airgel, carbon xerogel, activated carbon fibers, ordered mesoporous carbon (OMC) or graphene gels.
    [4]
    4. Method according to claim 3, characterized in that activated carbon is used.
    [5]
    5. Method according to any of the preceding claims, characterized in that the polar solvent used in step (c) is selected from the group comprising: HCl, NaOH, KOH or a polar hydrocarbon selected from the group comprising: acetone, diethylether, dimethyl formamide, dimethyl sulfoxide, methanol, ethanol and pyridine, or mixtures thereof.
    [6]
    6. Process according to claim 5, characterized in that the polar solvent is methanol.
    [7]
    Method according to any one of claims 5 or 6, characterized in that the polar hydrocarbon is mixed with water in a proportion of water between 50% (vol./vol.) And 10% (vol./vol.) , preferably in a proportion of 10% (vol./vol.).
    [ 8]
     8. Method according to claim 7, characterized in that the
    mixture has a pH between 4 and 10, and preferably the pH is 8.
    [ 9]
     9. Method according to any of the preceding claims, characterized in that the isocyanuric acid complexing solid substance used in step (d) is selected from the group comprising: melamine, amelide, ameline, bis-diaminotriazines, tris-diaminotriazines. 5
    [10]
    10. Method according to claim 9, characterized in that melamine is used.
    [ 11]
     Method according to any of the preceding claims, characterized in that the crystal suspension of step (e) is mixed with a filter aid of particle size similar or larger than the crystals obtained.
    [12]
    12. Method according to claim 11, characterized in that the filtration aid used in step (e) is selected from the group: natural diatomaceous earth, calcined or calcined to flow, perlite, cellulose or any of its mixtures. fifteen
    [13]
    13. Method according to any of the preceding claims, characterized in that the filter medium of step (f) has the permeability of the adjuvant between 0.04 Darcys and 10 Darcys, preferably 4 Darcys.
    [14]
    14. System for the extraction of isocyanuric acid in solution comprising:
    - a pump B01, which in the adsorption cycle, drives the water from the source of origin through means for the regulation of flow and towards an adsorption column C01 where the isocyanuric acid is retained,
    - means for flow regulation that allow the return of isocyanuric acid free water to the source of origin, 25
    - a reservoir D01 of liquid regeneration medium, connected with a dosing tank D02 in which a complexing solid substance is added,
    - means for the flow regulation that allow the passage of the liquid regeneration medium from the tank D01 to the dosing tank D02 through other means for the flow regulation, 30
    - a pump that drives the regeneration liquid from the tank D01 through means for the flow regulation to the dose tank D02 through other means for the flow regulation,
    - a solid mixture retention filter F01,
    - a dosing pump B02, which in the regeneration cycle, doses the suspension of the tank D02 in line 35 towards the filter F01,
    - means for flow regulation that allow the supply of liquid medium from the dosing tank D02 to the filter F01,
    - means for the flow regulation that allow the regeneration liquid recovered from the filter F01 to be supplied to the adsorption column C01 in the opposite direction to the adsorption cycle,
    - means for flow regulation that return the regeneration liquid after passing through the adsorption column C01 to the tank D01.
    [15]
    15. System according to claim 14, characterized in that the complexing solid substance is added to the dosing tank D02, together with a filter aid.
    [ 16]
     16. System for the extraction of isocyanuric acid in solution according to claim 14, characterized in that it comprises:
    - a pump B01, which in the adsorption cycle, drives the water from the source of origin through a valve (actuated) VA01 towards an adsorption column C01 where the isocyanuric acid is retained,
    - valves VA03, VA04 and VA12 to return water free of isocyanuric acid to the source of origin, 10
    - a reservoir D01 of liquid regeneration medium, connected with a dosing tank D02 in which a complexing solid substance is added,
    - a valve VA16 that allows the passage of the liquid regeneration medium from the tank D01 to the dosing tank D02 through valves VA08 and VA15, 15
    - a pump B01 that drives the regeneration liquid from the tank D01 through the valve VA16 to the dosing tank D02 through the valves VA08 and VA15,
    - a solid mixture retention filter F01,
    - a dosing pump B02, which in the regeneration cycle, doses the suspension of the tank D02 to the filter F01 in 20 lines,
    - a VA09 valve that allows the supply of the liquid medium from the dosing tank D02 to the filter F01,
    - valves VA11, VA04 and VA03 to supply the regeneration liquid recovered from the filter F01 to the adsorption column C01 in the opposite direction to the 25 adsorption cycle,
    - valves VA13 and VA06 that return the regeneration liquid after passing through the adsorption column C01 to the tank D01.
    [17]
    17. System according to claim 16, characterized in that the complexing solid substance is added to the dosing tank D02, together with a filter aid 30.
    [18]
    18. System according to any of claims 16 or 17, characterized in that it comprises a CM01 compressor for propelling the air through the valves VA10 and VA02 and evacuating the water from the adsorption column C01 after the adsorption cycle, where the water evacuated, it returns to the source of origin through the 35 valves VA03, VA04 and VA12.
    [19]
    19. System according to any of claims 16 to 18, characterized in that it comprises a valve VA07 for rinsing the adsorption column C01 with water.
    [20]
    20. System according to any of claims 16 to 19, characterized in that it comprises an agitator A01 to facilitate suspension in the dosing tank D02.
    [21]
    21. System according to any of claims 16 to 20, characterized by
    that, the CM01 compressor drives the air through the VA10 and VA02 valves by evacuating the regeneration liquid from the adsorption column C01 after the regeneration cycle, where the regeneration liquid is returned to the tank D01 through the VA03 valves, VA05 and VA06.
    [22]
    22. System for the extraction of isocyanuric acid in solution according to claim 14, characterized in that it comprises:
    - a pump B01, which in the adsorption cycle, drives the water from the source of origin through a valve VA101 to the selector valve VS01 and towards an adsorption column C01 where the isocyanuric acid is retained,
    - valves VS01 and VA102 to return isocyanuric acid free water to the source of origin,
    - a reservoir D01 of liquid regeneration medium, connected with a dosing tank D02 in which a complexing solid substance is added,
    - a valve VA104 that allows the passage of the liquid regeneration medium from the tank D01 to the dosing tank D02 through a valve VA105, 15
    - a pump B03 that drives the regeneration liquid from the tank D01 through the valve VA104 to the dosing tank D02 through the valve VA105,
    - a solid mixture retention filter F01,
    - a dosing pump B02, which in the regeneration cycle, drives the tank suspension D02 towards the filter F01,
    - a VA106 valve that allows the supply of liquid medium from the dosing tank D02 to the filter F01,
    - valves VA107, VA108 for supplying the regeneration liquid recovered from the filter F01 through the connecting valve VS01 towards the adsorption column C01 in the opposite direction to the adsorption cycle,
    - VS01 and VA109 valves that return the regeneration liquid after passing through the adsorption column C01 to the tank D01.
    [23]
    23. System according to claim 22, characterized in that the complexing solid substance is added to the dosing tank D02, together with a filter aid 30.
    [24]
    24. System according to any of claims 22 to 23, characterized in that it comprises a CM01 compressor for propelling the air through the valve VA108 and evacuating the water from the adsorption column C01 after the adsorption cycle, where the evacuated water is returns to the source of origin through valves VS01 and 35 VA102.
    [25]
    25. System according to any of claims 22 to 24, characterized in that it comprises the VS01 valve and a VA103 valve for rinsing the adsorption column C01 with water.
    [26]
    26. System according to any of claims 22 to 25, characterized in that it comprises a stirrer A01 to facilitate suspension in the dosing tank D02.
    [27]
    27. System according to any of claims 22 to 26, characterized by
    that, the CM01 compressor drives the air through the VA108 and VS01 valves by evacuating the regeneration liquid from the adsorption column C01 after the regeneration cycle, where the regeneration liquid is returned to the tank D01 through a VA109 valve.
    [28]
    28. System according to any of claims 14-27, characterized in that the adsorption column C01 contains an adsorbent material selected from the group of materials in the form of porous carbon.
    [29]
    29. System according to claim 28, characterized in that the porous carbon is selected from the group comprising activated carbon, carbon airgel, carbon xerogel, activated carbon fibers, ordered mesoporous carbon (OMC) or graphene gels 10.
    [30]
    30. System according to any of claims 14-29, characterized in that the liquid regeneration medium is a polar solvent having an affinity for isocyanuric acid greater than that of the adsorbent.
    [31]
    31. System according to claim 30, characterized in that the polar solvent is selected from the group comprising: HCl, NaOH, KOH or a polar hydrocarbon selected from the group comprising: acetone, diethylether, dimethyl formamide, dimethyl sulfoxide, methanol, ethanol and pyridine, or mixtures thereof.
    [32]
    32. System according to any of claims 14-32, characterized in that the isocyanuric acid complexing solid substance is selected from the group comprising: melamine, amelide, ameline, bis-diaminotriazines, tris-diaminotriazines.
    [33]
    33. System according to any of claims 15, 17 and 23, characterized in that the filtration aid is selected from the group: natural diatomaceous earth, calcined or calcined to flow, perlite, cellulose or any of its mixtures
    [34]
    34. System according to any of claims 14-33, characterized in that the filter F01 of retention of the solid mixture has the permeability of the diatom between 0.04 Darcys and 10 Darcys, preferably 4 Darcys.
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    同族专利:
    公开号 | 公开日
    ES2680486B2|2019-05-06|
    CU20180021A7|2019-10-04|
    US20180244634A1|2018-08-30|
    IL257777D0|2018-04-30|
    ZA201801070B|2018-12-19|
    AU2018201053A1|2018-09-13|
    CO2018002058A1|2018-05-10|
    CN108502960A|2018-09-07|
    PE20181460A1|2018-09-13|
    EP3366650A1|2018-08-29|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    CN101565246A|2009-06-01|2009-10-28|南京大学|Method for removing cyanuric acid from swimming-pool water|
    CN102491565A|2011-12-28|2012-06-13|烟台大学|Method for recovering waste water from sodium dichloroisocyanurate production|
    US20130186837A1|2012-01-24|2013-07-25|Kik Custom Products Inc.|Method and Kit for Reducing Cyanuric Acid Levels in Pool Water|
    US20140076814A1|2012-09-19|2014-03-20|AquaNovus, LLC|Cyanuric acid removal|
    US5194162A|1991-07-05|1993-03-16|Hodak Frank J|Method for treating swimming pool water|
    ES2336185B1|2008-08-28|2011-01-21|Universidad De La Rioja|METHOD AND DEVICE FOR THE PARTIAL ELIMINATION OF ISOCIANURIC ACID IN POOL WATER.|
    US20110259835A1|2010-04-26|2011-10-27|David Hodak|Method for treating pool water containing high levels of isocyanuric acid and biological growth|
    CN102583628A|2012-02-28|2012-07-18|中南民族大学|Method for removing cyanuric acid in water by activated-carbon fibrofelt and for regenerating activated-carbon fibrofelt by electric desorption|
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    申请号 | 申请日 | 专利标题
    ES201730257A|ES2680486B2|2017-02-27|2017-02-27|PROCEDURE AND SYSTEM FOR THE EXTRACTION OF ISOCIANURIC ACID IN DISSOLUTION|ES201730257A| ES2680486B2|2017-02-27|2017-02-27|PROCEDURE AND SYSTEM FOR THE EXTRACTION OF ISOCIANURIC ACID IN DISSOLUTION|
    AU2018201053A| AU2018201053A1|2017-02-27|2018-02-13|Procedure and system for the extraction of isocyanuric acid in solution|
    ZA2018/01070A| ZA201801070B|2017-02-27|2018-02-16|Procedure and system for the extraction of isocyanuric acid in solution|
    EP18158364.2A| EP3366650A1|2017-02-27|2018-02-23|Procedure and system for the extraction of isocyanuric acid in solution|
    PE2018000303A| PE20181460A1|2017-02-27|2018-02-23|PROCEDURE AND SYSTEM FOR THE EXTRACTION OF ISOCYANURIC ACID IN SOLUTION|
    CONC2018/0002058A| CO2018002058A1|2017-02-27|2018-02-26|Procedure and system for the extraction of isocyanuric acid in solution|
    CU2018000021A| CU20180021A7|2017-02-27|2018-02-26|PROCEDURE AND SYSTEM FOR THE EXTRACTION OF ISOCYANURIC ACID IN SOLUTION|
    IL257777A| IL257777D0|2017-02-27|2018-02-27|Procedure and system for the extraction of isocyanuric acid in solution|
    CN201810161610.8A| CN108502960A|2017-02-27|2018-02-27|Method and system for extracting isocyanuric acid from solution|
    US15/905,943| US20180244634A1|2017-02-27|2018-02-27|Procedure and system for the extraction of isocyanuric acid in solution|
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