CN219682506U - Retrieve device of applying mechanically polyether polyol catalyst - Google Patents
Retrieve device of applying mechanically polyether polyol catalyst Download PDFInfo
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- CN219682506U CN219682506U CN202320663940.3U CN202320663940U CN219682506U CN 219682506 U CN219682506 U CN 219682506U CN 202320663940 U CN202320663940 U CN 202320663940U CN 219682506 U CN219682506 U CN 219682506U
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- reaction kettle
- polyether polyol
- pipeline
- filter
- recycling
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- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 52
- 229920000570 polyether Polymers 0.000 title claims abstract description 52
- 150000003077 polyols Chemical class 0.000 title claims abstract description 37
- 229920005862 polyol Polymers 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 100
- 238000010521 absorption reaction Methods 0.000 claims abstract description 25
- 239000004744 fabric Substances 0.000 claims abstract description 25
- 238000004064 recycling Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims description 22
- 238000011010 flushing procedure Methods 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 abstract description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000012065 filter cake Substances 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 4
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 abstract 2
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 22
- 239000007789 gas Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- PLLZRTNVEXYBNA-UHFFFAOYSA-L cadmium hydroxide Chemical compound [OH-].[OH-].[Cd+2] PLLZRTNVEXYBNA-UHFFFAOYSA-L 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000000391 magnesium silicate Substances 0.000 description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 description 2
- 235000019792 magnesium silicate Nutrition 0.000 description 2
- ZADYMNAVLSWLEQ-UHFFFAOYSA-N magnesium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[Mg+2].[Si+4] ZADYMNAVLSWLEQ-UHFFFAOYSA-N 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Polyethers (AREA)
Abstract
The utility model discloses a device for recycling polyether polyol catalyst, which comprises a pump, a valve, a cloth bag filter, a gas absorption tower, a plate filter, a knockout, a reaction kettle and a stirrer, wherein the catalyst is recycled and applied to filter residues obtained in the production process of polyether polyol, n-butanol is used for dissolving and separating residual polyether polyol in the filter cakes, then water is used for dissolving and separating potassium salt in the filter cakes, chlorate and cadmium ions are introduced to carry out filtration treatment through the two filters, impurity ions except the potassium ions are separated, new high-purity potassium hydroxide is generated for catalysis in the production process of polyether polyol, phosphoric acid capable of being used as a neutralizer is additionally generated, the recycling of materials is realized, the utilization rate and the productivity are improved, and the emission is reduced.
Description
Technical Field
The utility model belongs to the technical field of polyether polyol production, and particularly relates to a device for recycling a polyether polyol catalyst.
Technical Field
Polyether polyol is used as one of main raw materials of polyurethane, the demand of the polyether polyol in production and life is large, generally, the polyether polyol is a polymer formed by taking polyol or organic amine as an initiator and propylene oxide or propylene oxide and ethylene oxide, a certain amount of catalyst is required to be added for reaction catalysis in the process of production, the types of the catalyst are numerous, such as a strong base catalyst, an amine catalyst, a bimetallic catalyst and the like, but the catalyst has obvious advantages of low cost and easy obtainment by taking alkali as the catalyst, wherein potassium hydroxide is typically used widely in the process of producing polyether polyol as the strong base catalyst; before the finished polyether polyol is obtained, in the previous refining process, means of adding acid, adsorbent and filtering are adopted: firstly, neutralizing excessive potassium hydroxide serving as a catalyst, and secondly, removing viscosity impurities; during filtration, it is necessary to carry out a cyclic filtration to form a cake layer containing a large amount of polyether polyol, and the polyether content in the filter residue may be up to 30%, about 50% of potassium salt and 20% of magnesium silicate, depending on the viscosity of the polyether, because the usual neutralizing agent is phosphoric acid, and the potassium salt finally formed is monopotassium phosphate and other salt impurities represented by magnesium silicate. If the polyether filter residue is directly treated in the form of solid waste, the effects of low productivity and low economic benefit are caused, and the load of the phosphorus-rich solid waste on the environment is relatively large, so that the polyether filter residue needs to be further separated and recycled, each component in the polyether filter residue can be effectively separated, and the operation has huge economic benefit and environmental benefit.
In the prior art, the step is usually stopped to recycle polyether components in filter residues or further bring away monopotassium phosphate, but the separation is mainly performed, so that the environmental pressure is only reduced, the effective components cannot be recycled, the whole production system is wasted in resources, and the effective catalytic components cannot be returned to the production system, so that a continuous circulation production closed loop is formed.
For example, CN201320775560.5 describes a polyether residue treatment device, in which extraction of the polyether residue is achieved over a maximum area by means of an extraction recovery device using ethanol as solvent. No matter how the device for extraction has no mechanical disturbance, the filter cake layer is tightly accumulated and compacted, the polyether viscosity is high and other objective factors, so that the polyether is difficult to be fully dissolved in the recovery device, and the recovery efficiency of the polyether is affected.
For example, CN216092327U discloses a device for separating and recovering polyether polyol filter residues, which comprises an extraction kettle, a stirring device, a solvent recovery kettle, a solvent storage tank, a polyether polyol storage tank, an evaporator, a crystallizer, a phosphate storage bin, a filter and a polyether refiner storage bin; the phosphate in the filter residue and the polyether polyol are recovered by a series of devices, but this does not reuse these for the production of polyether polyols either, essentially without solving the above-mentioned problems.
Therefore, there is a need in the art to improve the above-mentioned technical problems, so that the materials recovered from the filter residues can be reused in the production system, the greatest environmental burden is imposed on the link, and the final purpose of the recycling operation is to produce continuous circulation and minimize material loss.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model provides a device for recycling polyether polyol catalyst.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
an apparatus for recovering polyether polyol catalyst comprising: the device comprises a first reaction kettle, a second reaction kettle, a third reaction kettle, a gas absorption tower, a cloth bag filter and a plate filter; the discharge port of the first reaction kettle is connected with a liquid separator through a pipeline, and a discharge pipe arranged at the bottom of the liquid separator is connected to the second reaction kettle; the upper end exhaust port of the second reaction kettle is connected to a gas absorption tower through an exhaust pipe, and the gas absorption tower is connected to the feed inlet of the second reaction kettle through a return pipe; the second reaction kettle is connected with the cloth bag type filter through a pipeline; the discharge port of the cloth bag type filter is connected with a third reaction kettle through a pipeline, and the bottom discharge port of the third reaction kettle is connected with a plate type filter through a pipeline.
Preferably, n-butanol is introduced into filter residues in the first reaction kettle, and then water is introduced; firstly introducing perchloric acid and then introducing concentrated hydrochloric acid into the second reaction kettle; cadmium hydroxide is firstly introduced into the third reaction kettle.
Further, the knockout is provided with a feed inlet of the second reaction kettle shared by a discharge pipe at the bottom of the knockout and a return pipe of the gas absorption tower; and a feed valve is arranged on a pipeline connected with the feed inlet of the liquid separator and the discharge outlet of the first reaction kettle.
By adopting the technical scheme, the sight glass is convenient for observing the liquid separation condition of the n-butanol phase and the water phase liquid level, reduces liquid impurities introduced into the second reaction kettle, the gas absorption tower absorbs overflowed gas chlorine in the second reaction kettle, balances the gas pressure in the second reaction kettle, and the chlorine absorbed in the gas absorption tower forms a recyclable hydrochloric acid solution for the reaction of the second reaction kettle to realize self circulation.
Preferably, a feeding port is arranged on the first reaction kettle, and the feeding port is connected with a circulating pump through a pipeline.
By adopting the technical scheme, the circulating pump enables the n-butanol in the first reaction kettle to be fully contacted with the filter residue, and simultaneously the heat of the filter residue is removed by applying the n-butanol, so that the subsequent damage to equipment is reduced, the ageing of the heat exchange device is omitted, and the cost is reduced.
Preferably, a return control valve is arranged on a pipeline connected with the discharge port of the liquid separator; and a check valve is arranged on a pipeline connected with the second reaction kettle at the discharge port of the liquid separator.
By adopting the technical scheme, the feed back control valve controls the discharge port in the liquid separator to be communicated with the circulating pump, so that the n-butanol solution containing polyether in the liquid separator is conveniently fed back to the first reaction kettle and oil phase separation is integrated; the check valve controls the pipeline of the water solution containing the monopotassium phosphate to be communicated with the circulating pump, and the water solution is directly sent into the second reaction kettle, so that the conveying function of the circulating pump is fully utilized.
Preferably, an anti-flushing device is arranged between the second reaction kettle and the gas absorption tower; a return valve is arranged on a return pipe between the gas absorption tower and a feed inlet of the second reaction kettle; the second reaction kettle is connected with a feed pump through a pipeline; further, the anti-flushing device is a metal plate with big meshes.
By adopting the technical scheme, the metal plate with large meshes is used as the anti-flushing device, so that the pressure holding and flushing caused by rapid separation when the second reaction kettle generates chlorine are simple and effective, and the recovery waste and the pollution of the gas absorption tower caused by flushing are avoided; the chlorine gas can not directly discharge polluted air, but is absorbed by water to be hydrochloric acid as the raw material of the second reaction kettle, so that the total use amount of the hydrochloric acid is reduced, and the method is economical and environment-friendly.
Preferably, the first reaction kettle and the third reaction kettle are respectively provided with a first stirrer and a second stirrer.
By adopting the technical scheme, solid materials with certain viscosity are not accumulated in the kettle body, so that the kettle is blocked, the full contact between the liquid reagent and the solid materials is further promoted, and the high-efficiency separation efficiency is maintained.
Preferably, a charging hopper is arranged at the top of the third reaction kettle and is used for charging cadmium hydroxide and precipitating chloride ions.
Preferably, a salt solution feed valve is arranged on a pipeline connected with the feed port of the third reaction kettle and the discharge port of the cloth bag filter; the discharge port of the cloth bag type filter is also connected with an in-line pipeline which is connected with a storage tank, and a discharge valve is arranged between the storage tank and the cloth bag type filter.
By adopting the technical scheme, the cloth bag type filter can directly throw the potassium perchlorate sediment in the second reactor into the second reactor again in a cloth bag replacement mode, so that potassium ions are effectively reserved, the equipment ageing is reduced, and the method is convenient and quick; the filtered mother liquor phosphoric acid is directly fed into a storage tank for collection.
The utility model has the beneficial effects that: 1) Polyether polyol in the filter cake can be efficiently separated and recovered from filter residues through n-butanol and water, and potassium salt is changed into strong alkali on the basis, so that the recovery and the application of the catalyst are realized; 2) Through the combination of the pump and the stirrer, the liquid phase and the solid phase are fully mixed, the effective components in the filter residues are dissolved to the greatest extent, and the recycling process is quickened; 3) The circulation and transportation functions of the electrode pump are matched with the valve and the pipeline, so that the ageing of the equipment is reduced, and the use cost is reduced; 4) The externally added hydrochloric acid is reasonably paved through equipment, so that self-circulation supply can be realized; 5) The potassium salt is converted into phosphate which flows down from the strong alkali overflow to be converted back into phosphoric acid, and the phosphate is reused as a neutralizer in the production link of polyether polyol, so that the continuous circulation and the small loss of materials and the small burden on the environment are achieved on the whole.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the device;
fig. 2 is an internal detail view of the device as a material flushing preventing device.
Reference numerals: 1. a first reaction kettle; 2. a second reaction kettle; 3. a third reaction kettle; 4. a knockout; 5. a cloth bag filter; 6. a panel filter; 7. a gas absorption tower; 8. a material flushing preventing device; 9. a charging hopper; 10. a viewing mirror; 11. a circulation pump; 12. a feed pump; 13. a first agitator; 14. a second stirrer; 15. a feed valve; 16. a feed back control valve; 17. a check valve; 18. a return valve; 19. a saline solution feed valve; 20. a discharge valve; 21. a storage tank.
The specific embodiment is as follows:
the utility model will be further described by means of specific examples, which do not limit the scope of the utility model.
An apparatus for recovering polyether polyol catalyst comprising: the device comprises a first reaction kettle 1, a second reaction kettle 2, a third reaction kettle 3, a liquid separator 4, a cloth bag type filter 5, a plate filter 6, a gas absorption tower 7, an anti-flushing device 8, a feeding hopper 9, a sight glass 10, a circulating pump 11, a feeding pump 12, a first stirrer 13, a second stirrer 14, a feeding valve 15, a feed back control valve 16, a check valve 17, a feed back valve 18, a saline solution feeding valve 19, a discharging valve 20 and a storage tank 21.
Referring to fig. 1, an apparatus for recovering polyether polyol catalyst comprising: the device comprises a first reaction kettle 1, a second reaction kettle 2, a third reaction kettle 3, a gas absorption tower 7, a cloth bag filter 5 and a plate filter 6; the discharge port of the first reaction kettle 1 is connected with a knockout 4 through a pipeline, and a discharge pipe arranged at the bottom of the knockout 4 is connected to a second reaction kettle 2; the upper end exhaust port of the second reaction kettle 2 is connected to a gas absorption tower 7 through an exhaust pipe, and the gas absorption tower 7 is connected to the feed inlet of the second reaction kettle 2 through a return pipe; the second reaction kettle 2 is connected with a cloth bag filter 5 through a pipeline; the discharge port of the cloth bag type filter 5 is connected with the third reaction kettle 3 through a pipeline, and the bottom discharge port of the third reaction kettle 3 is connected with the plate type filter 6 through a pipeline.
The knockout 4 is provided with a sight glass 10 which is used for separating the solution remained in the last butanol cycle from the aqueous phase potassium salt solution, and impurities are not introduced into the second reaction kettle 2; the discharge pipe at the bottom of the knockout 4 and the return pipe of the gas absorption tower 7 share the feed inlet of the second reaction kettle 2; a feed valve 15 is arranged on a pipeline of the feed inlet of the knockout 4 connected with the discharge outlet of the first reaction kettle 1.
The first reaction kettle 1 is provided with a feed port, and the feed port is connected with a circulating pump 11 through a pipeline and is used for circulating n-butanol in the kettle body to fully contact filter residues, taking away polyether polyol residues and reducing the polymerization of viscous polyether on the filter residues by utilizing impact force; meanwhile, the feed port can be used for feeding water to dissolve and separate the monopotassium phosphate in the filter residue.
A return control valve 16 is arranged on a pipeline connected with a discharge port of the liquid separator 4 by the circulating pump 11, and n-butanol phase separated from water phase enters the first reaction kettle 1 through the return control valve 16 and is pumped into the first reaction kettle 1 by the circulating pump 11; and a check valve 17 is arranged on a pipeline connected with the second reaction kettle 2 at the discharge port of the liquid separator 4 and is used for pumping the potassium salt solution into the second reaction kettle 2.
As shown in fig. 2, an anti-flushing device 8 is arranged between the second reaction kettle 2 and the gas absorption tower 7 to relieve bubbles and pressure surge caused by chlorine generation; a return valve 18 is arranged on a return pipe between the gas absorption tower 7 and the feed inlet of the second reaction kettle 2 and is used for returning hydrochloric acid with the concentration of 32% to the second reaction kettle 2 as a raw material; the second reaction kettle 2 is connected with a feed pump 12 through a pipeline; furthermore, the anti-flushing device 8 is a metal plate with large meshes, and the device is simple and high in efficiency.
The first reaction kettle 1 and the third reaction kettle 3 are respectively provided with a first stirrer 13 and a second stirrer 14. The top of the third reaction kettle 3 is provided with a feeding hopper 9 for throwing cadmium hydroxide into the third reaction kettle 3, and the stirrer is used for promoting material contact and accelerating reaction progress.
A salt solution feed valve 19 is arranged on a pipeline connected with the feed port of the third reaction kettle 3 and the discharge port of the cloth bag filter 5 and used for conveying potassium chloride solution into the third reaction kettle 3; the discharge hole of the cloth bag filter 5 is also connected with an in-line pipeline which is connected with a storage tank 21, so that phosphoric acid is conveniently and directly collected for recycling production; a drain valve 20 is arranged between the storage tank 21 and the bag filter 5.
The working process of the utility model comprises the following steps:
1) Feeding filter residues into a first reaction kettle 1, starting a circulating pump 11 to pump n-butanol into the first reaction kettle 1, dissolving polyether polyol remained in the filter residues, stopping feeding when the n-butanol reaches the volume of completely dissolving the polyether polyol, starting circulation to take away waste heat in the filter residues, starting a first stirrer 13 after the circulation is stopped, stirring for 60-100 min, starting a discharge hole of the first reaction kettle 1, and discharging the n-butanol solution containing polyether out of a kettle body;
2) After the water is input into the first reaction kettle 1 by opening the circulating pump 11 and the water amount is less than the water amount of n-butanol, starting the first stirrer 13 to stir, dissolving potassium dihydrogen phosphate in filter residues, standing for 20min, opening the feed valve 15 and the check valve 17 to communicate the feed back control valve 16, and sending the separated potassium salt solution into the second reaction kettle 2 by using the circulating pump 11; the potassium salt solution containing n-butanol with a certain volume remains in the knockout 4 for 10min, the situation of liquid separation is observed through the sight glass 10 to separate liquid, the check valve 17, the feed back control valve 16 and the circulating pump 11 are opened, and a small part of the potassium salt solution separated is pumped into the second reaction kettle 2; afterwards, pumping the n-butanol solution containing polyether back to the first reaction kettle 1, and entering the next separation cycle;
3) The potassium salt solution enters a second reaction kettle 2; introducing perchloric acid to form potassium ion sediment, introducing the reacted material into a cloth bag filter 5, separating potassium perchlorate sediment and phosphoric acid solution, opening a discharge valve 20, and collecting the phosphoric acid solution into a storage tank 21;
4) Replacing the cloth bag of the cloth bag filter 5, and putting the potassium perchlorate precipitate into the second reactor 2 again; the feeding pump 12 is started to input concentrated hydrochloric acid, generated chlorine enters the anti-flushing device 8 to be absorbed by the tail gas absorption tower 7, and after a certain amount of accumulated concentrated hydrochloric acid is changed into concentrated hydrochloric acid, the concentrated hydrochloric acid can enter the second reactor through the material returning valve 18, so that the use of the concentrated hydrochloric acid is reduced;
5) Opening a salt solution feeding valve 19 to introduce a potassium chloride solution into the third reaction kettle 3, adding cadmium hydroxide through a feeding hopper 9, and opening a second stirrer 14 to fully react to obtain chromium chloride precipitate and potassium hydroxide;
6) The product in the third reaction kettle 3 is filtered by a plate filter 6, potassium hydroxide is obtained by separation, and the potassium hydroxide can be sent into the production process of polyether polyol, so that catalyst circulation is realized.
Claims (8)
1. An apparatus for recovering polyether polyol catalyst, said apparatus comprising: the device comprises a first reaction kettle (1), a second reaction kettle (2), a third reaction kettle (3), a gas absorption tower (7), a cloth bag filter (5) and a plate filter (6); the discharge port of the first reaction kettle (1) is connected with a liquid separator (4) through a pipeline, and a discharge pipe arranged at the bottom of the liquid separator (4) is connected to the second reaction kettle (2); the exhaust port of the second reaction kettle (2) is connected to the gas absorption tower (7) through an exhaust pipe, and the gas absorption tower (7) is connected to the feed inlet of the second reaction kettle (2) through a return pipe; the second reaction kettle (2) is connected with the cloth bag type filter (5) through a pipeline; the discharge port of the cloth bag type filter (5) is connected with the third reaction kettle (3) through a pipeline, and the bottom discharge port of the third reaction kettle (3) is connected with the plate type filter (6) through a pipeline.
2. The device for recycling polyether polyol catalyst according to claim 1, wherein a sight glass (10) is arranged on the liquid separator (4), and a discharge pipe at the bottom of the liquid separator (4) and a return pipe of the gas absorption tower (7) share a feed inlet of the second reaction kettle (2); and a feeding valve (15) is arranged on a pipeline connecting the feeding port of the liquid separator (4) and the discharging port of the first reaction kettle (1).
3. The device for recycling polyether polyol catalyst according to claim 1, wherein a feed port is arranged on the first reaction kettle (1), and the feed port is connected with a circulating pump (11) through a pipeline.
4. A device for recycling polyether polyol catalyst according to claim 3, wherein a return control valve (16) is arranged on a pipeline connected with a discharge port of the knockout (4) of the circulating pump (11); and a check valve (17) is arranged on a pipeline connected with the second reaction kettle (2) at the discharge port of the liquid separator (4).
5. The device for recycling polyether polyol catalyst according to claim 4, wherein an anti-flushing device (8) is arranged between the second reaction kettle (2) and the gas absorption tower (7); a return valve (18) is arranged on a return pipe between the gas absorption tower (7) and the feed inlet of the second reaction kettle (2); the second reaction kettle (2) is connected with a feed pump (12) through a pipeline.
6. The device for recycling polyether polyol catalyst according to claim 1, wherein the first reactor (1) and the third reactor (3) are respectively provided with a first stirrer (13) and a second stirrer (14).
7. The device for recycling polyether polyol catalyst according to claim 6, wherein a feeding hopper (9) is arranged at the top of the third reaction kettle (3).
8. The device for recycling polyether polyol catalyst according to claim 7, wherein a salt solution feeding valve (19) is arranged on a pipeline connecting a feeding port of the third reaction kettle (3) and a discharging port of the cloth bag filter (5); the discharging hole of the cloth bag type filter (5) is further connected with a straight-line pipeline, the straight-line pipeline is connected with a storage tank (21), and a discharge valve (20) is arranged between the storage tank (21) and the cloth bag type filter (5).
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|---|---|---|---|
| CN202320663940.3U CN219682506U (en) | 2023-03-27 | 2023-03-27 | Retrieve device of applying mechanically polyether polyol catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202320663940.3U CN219682506U (en) | 2023-03-27 | 2023-03-27 | Retrieve device of applying mechanically polyether polyol catalyst |
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