CN216273570U - Device for treating water-soluble organic phosphine in composite salt - Google Patents
Device for treating water-soluble organic phosphine in composite salt Download PDFInfo
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- CN216273570U CN216273570U CN202122577681.6U CN202122577681U CN216273570U CN 216273570 U CN216273570 U CN 216273570U CN 202122577681 U CN202122577681 U CN 202122577681U CN 216273570 U CN216273570 U CN 216273570U
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Abstract
The utility model discloses a device for treating water-soluble organic phosphine in composite salt. The device comprises a material tank, a filtering device, an adsorption tower, a steam generator, a reduced pressure distillation tank and a buffer tank. The material tank, the filtering device, the adsorption tower and the buffer tank are sequentially communicated, so that the sodium tetrachloroaluminate solution is continuously adsorbed and separated by the adsorption tower, organic phosphine impurities are selectively adsorbed in the adsorption tower, the content of organic phosphine in the treated sodium tetrachloroaluminate aqueous solution is less than 10ppm, and the loss of the sodium tetrachloroaluminate is less than 1%; form regeneration closed circuit through steam generator, adsorption tower and vacuum distillation jar through circulation pipeline, the steam that steam generator produced desorbs the organic phosphine impurity of adsorbing in the adsorption tower, and vacuum distillation jar evaporates water and returns recycle in the steam generator again, can realize separation purification continuous operation and energy consumption is little. The device has the characteristics of convenient operation, reliable operation and the like, and has low treatment cost and no secondary pollution.
Description
Technical Field
The utility model relates to the technical field of fine chemical equipment, in particular to a device for treating water-soluble organic phosphine in composite salt.
Background
In the process of producing methyldichlorophosphine by adopting a ternary complex method, sodium chloride is used for decomplexing the complex to obtain the methyldichlorophosphine and composite salt sodium tetrachloroaluminate, and because the sodium tetrachloroaluminate contains a small amount of organic phosphine impurities which are very easy to dissolve in water, the obtaining of high-purity sodium tetrachloroaluminate for subsequent deep processing has great difficulty.
MePCl4AlCl4+NaCl→MePCl2+NaAlCl4
Patent CN105217667A discloses a process for recycling sodium tetrachloroaluminate in glufosinate-ammonium production, and specifically discloses that the process of the recycling process is as follows: adding sodium tetrachloroaluminate into a mixed solvent of alcohol and ether, complexing with aluminum trichloride in the sodium tetrachloroaluminate by taking the ether as a complexing agent again to resolve sodium chloride and organic phosphine impurities, filtering out the sodium chloride, cooling filtrate to separate out the aluminum trichloride, further purifying the aluminum trichloride, then indiscriminately applying the aluminum trichloride to the synthesis of methyldichlorophosphine, reducing the complexing ability after the aluminum trichloride is applied for a plurality of times, and adding sodium hydroxide to prepare the polyaluminum chloride. The recycling process has the defects that aluminum trichloride is difficult to crystallize in mother liquor, precipitation is not thorough, crystal form is poor and better filtration cannot be achieved, meanwhile, a large amount of ether solvents are used in the process, peroxide generated in the recycling and applying process has great potential safety hazard in the specific industrial implementation process, aluminum trichloride with lowered complexing capacity is high in reprocessing cost and energy consumption, and organic phosphine impurities cannot be completely removed.
Patent CN109052444A discloses a method for preparing polyaluminium chloride by using by-products generated in the production of diethyl methylphosphite, and specifically discloses that the method comprises the following steps: dispersing the byproduct sodium tetrachloroaluminate in a solvent, then resolving, collecting filtrate, adding water into the filtrate, cooling to separate out aluminum chlorohydrate crystals, and then carrying out hydrolytic polymerization and curing on the aluminum chlorohydrate to obtain the polyaluminum chloride. The method uses a large amount of organic solvent, the organic solvent is easy to volatilize when the organic solvent is recycled, the method causes environmental pollution, the method is neither economical nor environment-friendly, and simultaneously, the method has the defects of long crystallization time of aluminum chlorohydrate after adding water into filtrate, incomplete precipitation, irregular crystallization, difficult precipitation, difficult filtration and the like, and organic phosphine impurities cannot be completely removed.
Patent CN111689508A discloses a method for treating tetrachloro sodium aluminate solid slag, and specifically discloses that the method comprises the following steps: mixing the tetrachloro sodium aluminate solid slag with water for dissociation, adding a separating agent to separate out aluminum chloride hexahydrate, or directly mixing the tetrachloro sodium aluminate solid slag with the separating agent for dissociation to separate out aluminum chloride hexahydrate, performing primary solid-liquid separation to obtain aluminum chloride hexahydrate solid and primary filtrate, and performing concentration crystallization and secondary solid-liquid separation on the primary filtrate to obtain sodium chloride solid and secondary filtrate. The treatment method is to realize the crystallization of the aluminum chloride hexahydrate in the concentrated hydrochloric acid by utilizing a classical aluminum chloride hexahydrate industrial production method, although a large amount of organic solvents are not needed, a large amount of hydrogen chloride gas or concentrated hydrochloric acid needs to be purchased, the cost of labor, energy consumption, equipment depreciation, rear-end environmental protection disposal and the like is considered, the treatment method cannot realize balance of income and expenditure and has limited economic value according to the price of the current aluminum chloride hexahydrate at a market terminal, and the phosphine-containing organic matters in the obtained aluminum chloride hexahydrate and sodium chloride are not completely removed, and the organic phosphine impurities are not enriched and further processed to become high-added-value products.
Patent CN111804704A discloses a method for treating tetrachloro sodium aluminate solid slag, and specifically discloses that the method comprises the following steps: mixing and dissociating the tetrachloro sodium aluminate solid slag with water, adding alkali for polymerization reaction, then carrying out concentration crystallization and solid-liquid separation to obtain sodium chloride solid and concentrated mother liquor, and then curing the obtained concentrated mother liquor to obtain a polymerized aluminum chloride liquid product. The treatment method is characterized in that relatively expensive sodium hydroxide is used for preparing polyaluminum chloride with low added value, an oxidant is added in the reaction process to oxidize an organic phosphorus compound into an inorganic phosphorus compound, sodium tetrachloroaluminate is dissolved in water to form strong acidity of the whole system, chloride ions in the strong acidity system are preferentially oxidized after the oxidant is added, extremely toxic chlorine gas can be generated, great potential safety hazard exists in large-scale application, and a large amount of oxidant is added for completely oxidizing organic phosphorus into inorganic phosphorus, so that the cost is high, and the method is not environment-friendly. In addition, the treatment method washes the obtained sodium chloride solid with water, so that a part of sodium chloride is left in mother liquor to form high-salt wastewater, incompletely oxidized organic phosphorus and inorganic phosphorus obtained by oxidation exist in the high-salt wastewater at the same time, thallus can be dead after entering a biochemical system, organic phosphorus wastewater can be generated without other treatment, and the wastewater cannot be directly discharged.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a device for treating water-soluble organic phosphine in a composite salt, aiming at the defects in the prior art.
In order to achieve the purpose, the utility model adopts the following technical scheme:
the utility model relates to a device for treating water-soluble organic phosphine in composite salt, which comprises a material tank, a filtering device, an adsorption tower, a steam generator, a reduced pressure distillation tank and a buffer tank, wherein the material tank is connected with the filtering device;
the material tank, the filtering device, the adsorption tower and the cache tank are sequentially communicated through a connecting pipeline along the liquid direction;
the steam generator, the adsorption tower and the reduced pressure distillation tank form a regeneration closed loop through a circulating pipeline;
and the connecting pipeline and the circulating pipeline are both provided with a chemical pump and a valve for opening or closing the chemical pump.
Further, a condenser is arranged on the regeneration closed loop, and the condenser is positioned between the adsorption tower and the reduced pressure distillation tank.
Furthermore, a heater is arranged on the connecting pipeline, the heater is located between the filtering device and the adsorption tower, the liquid inlet end of the heater is communicated with the filtering device, and the liquid outlet end of the heater is communicated with the adsorption tower.
Further, still be provided with the branch road on the connecting pipeline, the branch road be located the adsorption tower with between the buffer memory jar, the feed liquor end of branch road with the connecting pipeline communicates mutually, the play liquid end of branch road with the inlet of heater is linked together.
Furthermore, a packing chamber is arranged in the adsorption tower, and macroporous resin particles are paved in the packing chamber.
Further, the macroporous resin particles are macroporous resin of RDK02 type.
Furthermore, a sodium hydroxide feeding port is arranged at the top of the reduced pressure distillation tank.
Furthermore, a metering pump is further arranged on the connecting pipeline, the metering pump is located between the filtering device and the adsorption tower, the liquid inlet end of the metering pump is communicated with the filtering device, and the liquid outlet end of the metering pump is communicated with the adsorption tower.
Furthermore, the liquid outlet end of the metering pump is also connected with a speed regulating valve, and the liquid outlet end of the speed regulating valve is communicated with the adsorption tower.
Further, the material outlet of the reduced pressure distillation tank is connected with a hazardous waste tank.
The technical scheme provided by the utility model has the beneficial effects that:
(1) according to the utility model, the material tank, the filtering device, the adsorption tower and the buffer tank are sequentially communicated through the connecting pipeline, so that the sodium tetrachloroaluminate solution is continuously adsorbed and separated through the adsorption tower, organic phosphine impurities are selectively adsorbed in the adsorption tower, the content of organic phosphine in the treated sodium tetrachloroaluminate aqueous solution is less than 10ppm, and the loss of sodium tetrachloroaluminate is less than 1%;
(2) according to the utility model, a regeneration closed loop is formed by the steam generator, the adsorption tower and the reduced pressure distillation tank through the circulating pipeline, the steam generated by the steam generator desorbs the organic phosphine impurities adsorbed in the adsorption tower, and the water evaporated from the reduced pressure distillation tank returns to the steam generator again for recycling, so that the continuous operation of separation and purification can be realized, and the energy consumption is low;
(3) the device provided by the utility model has the characteristics of convenience in operation, reliability in operation and the like, can obviously reduce the content of organic phosphine impurities in sodium tetrachloroaluminate, can greatly reduce the treatment cost compared with the prior art, and has no secondary pollution.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for treating water-soluble organic phosphine in a composite salt according to the present invention.
1. A material tank; 2. a filtration device; 21. a metering pump; 22. a speed regulating valve; 3. an adsorption tower; 31. a packing chamber; 32. macroporous resin particles; 4. a steam generator; 5. a reduced pressure distillation tank; 51. a sodium hydroxide feeding port; 6. a buffer tank; 7. a condenser; 8. connecting a pipeline; 81. a branch circuit; 9. a regeneration closed loop; 91. a circulation line; 10. a heater; 11. and (5) hazardous waste tanks.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
As shown in fig. 1, the device for treating water-soluble organic phosphine in composite salt provided by the utility model comprises a material tank 1, a filtering device 2, an adsorption tower 3, a steam generator 4, a reduced pressure distillation tank 5 and a buffer tank 6, wherein the material tank 1, the filtering device 2, the adsorption tower 3 and the buffer tank 6 are sequentially communicated through a connecting pipeline 8 along the liquid direction; the steam generator 4, the adsorption tower 3 and the reduced pressure distillation tank 5 form a regeneration closed loop 9 through a circulating pipeline 91, and a chemical pump and a valve for opening or closing the chemical pump are arranged on the connecting pipeline 8 and the circulating pipeline 91. According to the utility model, the material tank 1, the filtering device 2, the adsorption tower 3 and the buffer tank 6 are sequentially communicated through the connecting pipeline, so that the sodium tetrachloroaluminate solution is continuously adsorbed and separated through the adsorption tower, organic phosphine impurities are selectively adsorbed in the adsorption tower, the content of organic phosphine in the treated sodium tetrachloroaluminate aqueous solution is less than 10ppm, the loss of sodium tetrachloroaluminate is less than 1%, and the sodium tetrachloroaluminate aqueous solution is stored in the buffer tank 6. Form regeneration closed circuit 9 through circulation pipeline 91 through steam generator 4, adsorption tower 3 and vacuum distillation jar 5, the steam that steam generator 4 produced desorbs the organic phosphine impurity of adsorption in the adsorption tower, and vacuum distillation jar 5 water of evaporating returns recycle back to steam generator again, can realize separation and purification continuous operation and energy consumption is little. The device provided by the utility model has the characteristics of convenience in operation, reliability in operation and the like, can obviously reduce the content of organic phosphine impurities in sodium tetrachloroaluminate, can greatly reduce the treatment cost compared with the prior art, and has no secondary pollution.
In order to more effectively separate out the organic phosphorus impurities, a condenser 7 can be arranged on the regeneration closed loop 9, the condenser 7 can be positioned between the adsorption tower 3 and the reduced pressure distillation tank 5, the steam generated by the steam generator 4 desorbs the organic phosphorus impurities adsorbed in the adsorption tower 3, the impurities are converted into gaseous state, the gaseous state is changed into liquid organic phosphorus impurities through the condensing pipe 7, and the liquid organic phosphorus impurities are converted into solid organic phosphorus impurities after the moisture is removed through the reduced pressure distillation tank 5.
In order to improve the adsorption efficiency of the adsorption tower, a heater 10 can be further arranged on the connecting pipeline 8, the heater 10 is positioned between the filtering device 2 and the adsorption tower 3, the liquid inlet end of the heater 10 is communicated with the filtering device 2, and the liquid outlet end of the heater 10 is communicated with the adsorption tower 3. The sodium tetrachloroaluminate solution is heated by the heater 10 and then enters the adsorption tower 3, the temperature can be controlled to be 5-45 ℃, and the adsorption quantity of the organic phosphorus impurities is effectively improved.
In order to improve the purity of the sodium tetrachloroaluminate, a branch 81 can be arranged on the connecting pipeline 8, the branch 81 is positioned between the adsorption tower 3 and the buffer tank 6, the liquid inlet end of the branch 81 is communicated with the connecting pipeline 8, and the liquid outlet end of the branch 81 is communicated with the heater 10. The sodium tetrachloroaluminate solution can continuously and circularly enter the adsorption tower 3 to adsorb organic phosphorus impurities, so that the purity of the sodium tetrachloroaluminate is effectively improved.
In order to improve the organic phosphorus adsorption efficiency, a packing chamber 31 may be provided inside the adsorption tower 3, and macroporous resin particles 32 may be laid in the packing chamber 31.
In order to improve the selectivity of the macroporous resin and ensure stable performance and reusability of the macroporous resin, the macroporous resin particles 32 can be RDK02 type macroporous resin.
In order to improve the separation efficiency of the organic phosphorus impurities, a sodium hydroxide feeding port 51 can be arranged at the top of the reduced pressure distillation tank 5, sodium hydroxide is added to maintain the pH value of desorption liquid flowing out of the condenser 7 at 10-12, organic phosphorus is prevented from being converted into a gaseous state when the desorption liquid is subjected to reduced pressure distillation, and solid organic phosphorus impurities are obtained by separation after moisture is removed.
In order to ensure that the device can continuously carry out adsorption separation work, a metering pump 21 can be arranged on the connecting pipeline 8, the metering pump 21 is positioned between the filtering device 2 and the adsorption tower 3, the liquid inlet end of the metering pump 21 is communicated with the filtering device 2, the liquid outlet end of the metering pump 21 is communicated with the adsorption tower 3,
in order to better control the flow rate of the sodium tetrachloroaluminate solution, the liquid outlet end of the metering pump 21 can be further connected with a speed regulating valve 22, the liquid outlet end of the speed regulating valve 22 is communicated with the adsorption tower 3, the flow rate of the sodium tetrachloroaluminate solution flowing into the adsorption tower 3 can be controlled through the regulating valve 22, and the adsorption and elution efficiency is further effectively improved.
In order to prevent environmental pollution, a material outlet of the reduced pressure distillation tank 5 can be connected with a dangerous waste tank 10, and organic phosphorus impurities enriched in the reduced pressure distillation tank 5 can be transferred into the dangerous waste tank 10 to be treated as dangerous waste to be sent to qualified units.
In order to better illustrate the working principle and the beneficial effects brought by the device for treating water-soluble organic phosphine in composite salt of the present invention, and facilitate the implementation of workers, the following description is made with reference to specific examples.
Example 1
Dissolving 100g of sodium tetrachloroaluminate containing organic phosphine impurities in 300g of water, stirring for 10 minutes to fully dissolve the sodium tetrachloroaluminate to obtain a sodium tetrachloroaluminate aqueous solution, and measuring the organic phosphine content of the sodium tetrachloroaluminate aqueous solution by using a total phosphorus measuring instrument to be 3500 ppm; filtering with filter 2 to remove solid impurities, continuously passing the sodium tetrachloroaluminate solution through adsorption tower 3, spreading RDK02 type macroporous resin particles in packing chamber 31 of adsorption tower 3, adsorbing and separating sodium tetrachloroaluminate solution with RDK02 type macroporous resin to adsorb organic phosphine impurities in macroporous resin, and allowing the flow rate of the sodium tetrachloroaluminate solution in macroporous resin column to be 3.0BV.h-1The adsorption process is carried out at 25 ℃ until the organic phosphine impurities in the effluent sodium tetrachloroaluminate aqueous solution reach 10 ppm; after adsorption saturation, continuously introducing water vapor into the macroporous resin column for desorption until no organic phosphine is detected in the collected desorption liquid through a condenser 7, wherein the collected desorption liquid is 3 BV; adding 3g of sodium hydroxide into the desorption solution obtained in the previous step, stirring, measuring the pH value to be 11, carrying out reduced pressure distillation on the desorption solution, keeping the internal temperature at 65 ℃ and the vacuum degree at-2.2 KPa, returning the distilled water to a steam generator again, and treating the organic phosphine impurities enriched after moisture removal as hazardous wastes to qualified units.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the utility model, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the utility model as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A device for treating water-soluble organic phosphine in composite salt is characterized in that: comprises a material tank (1), a filtering device (2), an adsorption tower (3), a steam generator (4), a reduced pressure distillation tank (5) and a buffer tank (6);
the material tank (1), the filtering device (2), the adsorption tower (3) and the buffer tank (6) are communicated in sequence along the liquid direction through a connecting pipeline (8);
the steam generator (4), the adsorption tower (3) and the reduced pressure distillation tank (5) form a regeneration closed loop (9) through a circulating pipeline (91);
and the connecting pipeline (8) and the circulating pipeline (91) are both provided with a chemical pump and a valve for opening or closing the chemical pump.
2. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 1, wherein: and a condenser (7) is arranged on the regeneration closed loop (9), and is positioned between the adsorption tower (3) and the reduced pressure distillation tank (5).
3. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 1, wherein: and a heater (10) is arranged on the connecting pipeline (8), and the heater (10) is positioned between the filtering device (2) and the adsorption tower (3).
4. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 3, wherein: still be provided with branch road (81) on connecting line (8), branch road (81) be located adsorption tower (3) with between buffer memory jar (6), the feed liquor end of branch road (81) with connecting line (8) are linked together, the play liquid end of branch road (81) with heater (10) are linked together.
5. The apparatus for treating water-soluble organophosphine in a complex salt according to any of claims 1 to 4, wherein: a packing chamber (31) is arranged in the adsorption tower (3), and macroporous resin particles (32) are paved in the packing chamber (31).
6. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 5, wherein: the macroporous resin particles (32) are of the type RDK 02.
7. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 1, wherein: and a sodium hydroxide feeding port (51) is also arranged at the top of the reduced pressure distillation tank (5).
8. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 1, wherein: still be provided with measuring pump (21) on connecting line (8), measuring pump (21) are located filter equipment (2) with between adsorption tower (3), the feed liquor end of measuring pump (21) with filter equipment (2) are linked together, the play liquid end of measuring pump (21) with adsorption tower (3) are linked together.
9. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 8, wherein: the liquid outlet end of the metering pump (21) is also connected with a speed regulating valve (22), and the liquid outlet end of the speed regulating valve (22) is communicated with the adsorption tower (3).
10. The apparatus for treating water-soluble organophosphine in a complex salt according to claim 1, wherein: and a material outlet of the reduced pressure distillation tank (5) is connected with a dangerous waste tank (11).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122577681.6U CN216273570U (en) | 2021-10-25 | 2021-10-25 | Device for treating water-soluble organic phosphine in composite salt |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122577681.6U CN216273570U (en) | 2021-10-25 | 2021-10-25 | Device for treating water-soluble organic phosphine in composite salt |
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| CN202122577681.6U Active CN216273570U (en) | 2021-10-25 | 2021-10-25 | Device for treating water-soluble organic phosphine in composite salt |
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