CN109734912B - Polyphenylene sulfide separation and purification process - Google Patents
Polyphenylene sulfide separation and purification process Download PDFInfo
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- CN109734912B CN109734912B CN201811500818.4A CN201811500818A CN109734912B CN 109734912 B CN109734912 B CN 109734912B CN 201811500818 A CN201811500818 A CN 201811500818A CN 109734912 B CN109734912 B CN 109734912B
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 68
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 68
- 238000000926 separation method Methods 0.000 title claims abstract description 20
- 238000000746 purification Methods 0.000 title claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 45
- 238000002156 mixing Methods 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 230000001105 regulatory effect Effects 0.000 claims abstract description 16
- 241000953555 Theama Species 0.000 claims abstract description 15
- 239000011343 solid material Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims description 26
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000003912 environmental pollution Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 16
- 238000003756 stirring Methods 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- 230000000087 stabilizing effect Effects 0.000 description 6
- 238000009776 industrial production Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000009323 psychological health Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a polyphenylene sulfide separation and purification process, (1) a mixture containing polyphenylene sulfide is firstly separated into granular polyphenylene sulfide by a centrifuge, and the rest mixture is mixed with diatomite in a mixing kettle to prepare a mixture A; (2) an outlet of the mixing kettle is connected with a pump, an outlet of the pump is connected with an adjusting valve, the adjusting valve is connected with the Ama filter, the mixture A is conveyed to the Ama filter through the pump, and the mixture A is filtered to obtain a solid material and a filtrate B; (3) and (4) rectifying the filtrate B in a rectifying system. According to the invention, the self-operated regulating valve and the Ama filter are used together, and the diatomite is applied to the separation and purification process of the polyphenylene sulfide, so that the problems that the pump and the rectifying tower are blocked by materials, the tower equipment needs to be disassembled and cleaned or cleaned, the material leakage is caused can be effectively solved, the product loss can be reduced, the environmental pollution can be reduced, and the productivity can be improved.
Description
Technical Field
The invention belongs to the field of production processes of polyphenylene sulfide, and particularly relates to a separation and purification process of polyphenylene sulfide.
Background
After a mixture containing polyphenylene sulfide industrially produced in the prior art is cooled, filtered and washed, all mixed liquid is put into a horizontal spiral sedimentation separation centrifuge for solid-liquid separation, the polyphenylene sulfide belongs to particles, and part of the polyphenylene sulfide which does not grow into particles is polyphenylene sulfide oligomer powder (the polyphenylene sulfide oligomer powder has lower molecular weight and lower melting point than the granular polyphenylene sulfide), the polyphenylene sulfide oligomer powder is not easy to settle and floats in the liquid in the separation process, and after the polyphenylene sulfide oligomer powder enters a rectification system along with mother liquor, a reboiler of a rectification tower, internal parts of the tower (a filler and a redistributor) and an inlet pipeline of the centrifuge are easily blocked, so that the discharging and the separation can not be continuously carried out, and the normal production of the whole device is influenced.
In the prior art, a plate-and-frame filter press is mainly adopted for filtering and separating a mixture containing polyphenylene sulfide oligomer powder, and the problems of the prior art are as follows: the device is exposed in the air, and the odor of the solvent and the low polymer powder of the polyphenylene sulfide seriously pollute the environment and influence the physical and psychological health of operators; NMP (N-methyl pyrrolidone) solvent belongs to polar organic solvent, and filter cloth and a plate frame can be corroded or dissolved and deformed after long-term use, and often leak, so that oligomer enters a subsequent rectification system; the rubber ring inside the liquid discharge valve is also frequently damaged, so that the whole plate frame cannot stably bear pressure, the expected filtering effect cannot be achieved, and the production and maintenance cost is high. After the material containing polyphenylene sulfide oligomer powder which is not subjected to fine filtration enters a rectification system, a reboiler of a rectification tower, tower internals (a filler and a redistributor) and inlet pipelines of a centrifugal machine are often blocked, and the material is required to be disassembled during cleaning, so that material leakage in a material pipe can be caused in the cleaning and washing processes, and material loss and environmental pollution are caused.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a polyphenylene sulfide separation and purification process, and particularly relates to a gamma filter applied to the polyphenylene sulfide separation and purification process. The problem that the material blocks a pump and a rectifying tower, the cleaning or cleaning tower equipment needs to be disassembled and the material leakage is caused can be effectively solved, and the product loss and the environmental pollution can be reduced.
A separation and purification process of polyphenylene sulfide comprises the following specific steps:
(1) firstly, separating granular polyphenylene sulfide from a polyphenylene sulfide-containing mixture produced in industrial production through a centrifuge, and fully stirring and mixing the residual mixture and diatomite in a mixing kettle (model number BSJ, produced by Wunsinson pine mechanical Co., Ltd.) to prepare a mixture A;
(2) the outlet of the mixing kettle is connected with a pump, the outlet of the pump is connected with a self-operated regulating valve (provided by Beijing Navigation safety valve marketing Co., Ltd., model: ARC 200050X 50X 40PN1.0MPa), the self-operated regulating valve is connected with an Ama filter (produced by Senson pine machinery Co., Ltd., model: BSJ), the mixture A is conveyed to the Ama filter under the action of the pump, and the solid material and the filtrate B are obtained after filtration;
(3) and (4) rectifying the filtrate B in a rectifying system.
The rotating speed of the centrifuge in the step (1) is 1400-1500 rpm.
The remaining mixture in the step (1) contains, in terms of mass fraction, 5 to 12% (preferably 8%) of NaCl, 8 to 20% (preferably 15%) of NMP (N-methylpyrrolidone) as a solvent, 1 to 8% (preferably 3%) of an oligomer powder of polyphenylene sulfide, and the balance of water.
The mass ratio of the mixture containing polyphenylene sulfide to the diatomite in the step (1) is 100:0.5-2 (preferably 100: 1).
The mixing and stirring time in the step (1) is 15-30 minutes, and the stirring speed is 10-20 revolutions per minute (preferably 16.5 revolutions per minute).
Further, the stirring and mixing in the step (1) are carried out at 20 to 30 ℃.
Further, the working flow rate of the pump in the step (2) is 4-7m3H (preferably 6 m)3H) with a head of 45 to 55m (preferably 50 m).
Further, in the step (2), when the pressure of the Ama filter reaches 0.4-0.6MPa (preferably 0.5MPa), the filter cake becomes thicker and drier, so that the material entering the filter is gradually reduced, at the moment, the self-operated regulating valve is automatically opened, the mixture A is returned to the mixing kettle, the overpressure of equipment is avoided, the pump is not blocked when running at low flow, and the labor load of workers is greatly reduced.
Further, the temperature range of the mixture A filtered in the Ama filter in the step (2) is 20-30 ℃.
Further, the amador filter comprises a sealed mesh filter.
Further, the process that the mixture A enters the Ama filter in the step (2) comprises the following steps: mixture a entered a sealed mesh plate filter inside a ama filter.
Furthermore, the screen plate of the sealed screen plate filter is a fine stainless steel screen with 100 meshes and 150 meshes, and the polyphenylene sulfide oligomer powder can be filtered.
Further, when the pressure at the upper part of the sealed mesh plate filter is 0.4-0.6MPa (preferably 0.4-0.5MPa), indicating that a filter cake has been formed, after stabilizing the pressure for 15-45 minutes (preferably 30 minutes), the filter plate (filter cake on mesh plate, mesh plate mounted on filter plate) can be manually removed to obtain a solid material on the filter plate.
Further, the solid material includes an oligomer powder of polyphenylene sulfide. And if the centrifuge is abnormal, the solid material also comprises granular polyphenylene sulfide. The molecular weight of the granular polyphenylene sulfide is 4-6 ten thousand, the melting point is 285-300 ℃, and the melt index is 50-600; the molecular weight of the polyphenylene sulfide oligomer powder is less than 4 ten thousand, the melting point is less than 140 ℃ and 150 ℃, and the melt index is more than 600.
Further, the solvent NMP (N-methyl pyrrolidone) is obtained by rectification in the step (3), and the solvent NMP can be recycled.
Further, the rectified mixture is further concentrated by MVR (mechanical vapor recompression) to obtain industrial salt.
The diatomite in the mixture A cannot penetrate through the stainless steel wire mesh due to large volume, and finally a uniform diatomite filter layer is formed on the screen plate (the screen plate is arranged on the filter plate framework, and the diatomite filter layer is attached to the screen plate), the low polymer powder of the polyphenylene sulfide stays on the diatomite filter layer, the rest mixed liquor permeates through the stainless steel wire mesh and the diatomite filter layer, so that clear filtrate B is obtained, and the clear liquid smoothly enters a subsequent rectification system.
The invention has the following beneficial effects:
(1) the stainless steel wire mesh is used as the screen plate, so that filter cloth, filter paper and the like are not needed, the corrosivity of a solvent is not considered, and the filtering cost is greatly reduced.
(2) In the filtering process of production operation, the filtrate is not contacted with air, and the device belongs to a closed type, and has the advantages of very convenient operation, material leakage prevention, environmental pollution reduction, labor intensity reduction of workers and the like.
(3) The self-operated regulating valve is combined with the Ama filter for the first time, so that the overpressure of equipment is not avoided, and the condition that a pump is blocked when the pump runs at a low flow is also prevented.
(4) The filtrate entering the rectification system is clear and free of precipitation, prevents a reboiler of the rectification tower, internal parts (packing and redistributors) of the tower and inlet pipelines of a centrifugal machine from being blocked, reduces the product loss and the environmental pollution, reduces the labor intensity of operation, and improves the labor productivity and the device capacity.
(5) The diatomite has long continuous service time and can completely replace a plate and frame filter.
(6) The method can obtain granular polyphenylene sulfide and polyphenylene sulfide oligomer powder, can also obtain a pure solvent NMP through rectification, and further concentrate the rectified mixture through MVR (mechanical vapor recompression) to obtain the industrial salt.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, some examples are listed below.
Example 1
A separation and purification process of polyphenylene sulfide comprises the following specific steps:
(1) 1Kg of polyphenylene sulfide-containing mixture produced in industrial production is firstly separated into granular polyphenylene sulfide by a centrifuge, and the rest mixture and diatomite are fully stirred and mixed (the stirring time at 20-30 ℃ is 15 minutes, and the stirring speed is 16.5 revolutions per minute) in a mixing kettle (the mass ratio of the polyphenylene sulfide-containing mixture to the diatomite is 100:1) to prepare a mixture A;
(2) the outlet of the mixing kettle is connected with a pump, the outlet of the pump is connected with a self-operated regulating valve, the self-operated regulating valve is connected with a gamma filter, the mixture A is conveyed to the gamma filter under the action of the pump, and filtering is carried out to obtain polyphenylene sulfide oligomer powder and filtrate B;
(3) and (4) rectifying the filtrate B in a rectifying system.
The rotating speed of the centrifuge in the step (1) is 1400 revolutions per minute.
The working flow rate of the pump in the step (2) is 4m3H, the lift is 45 m.
And when the pressure of the upper part of the sealed screen plate filter is 0.4MPa, stabilizing the pressure for 15 minutes, taking out the filter plate, and recovering solid materials on the plate to obtain the polyphenylene sulfide oligomer powder.
Example 2
A separation and purification process of polyphenylene sulfide comprises the following specific steps:
(1) 1Kg of polyphenylene sulfide-containing mixture produced in industrial production is firstly separated into granular polyphenylene sulfide by a centrifuge, and the rest mixture and diatomite are fully stirred and mixed in a mixing kettle (the mass ratio of the polyphenylene sulfide-containing mixture to the diatomite is 100:0.5) in the mixing kettle (the stirring and mixing time is 30 minutes at 20-30 ℃, and the stirring speed is 10 r/min), so as to prepare a mixture A;
(2) the outlet of the mixing kettle is connected with a pump, the outlet of the pump is connected with a self-operated regulating valve, the self-operated regulating valve is connected with a gamma filter, the mixture A is conveyed to the gamma filter under the action of the pump, and filtering is carried out to obtain polyphenylene sulfide oligomer powder and filtrate B;
(3) and (4) rectifying the filtrate B in a rectifying system.
The rotating speed of the centrifuge in the step (1) is 1500 revolutions per minute.
The working flow rate of the pump in the step (2) is 7m3The head is 55 m.
And when the pressure of the upper part of the sealed screen plate filter is 0.6MPa, stabilizing the pressure for 45 minutes, taking out the filter plate, and recovering solid materials on the plate to obtain the polyphenylene sulfide oligomer powder.
Example 3
A separation and purification process of polyphenylene sulfide comprises the following specific steps:
(1) 1Kg of polyphenylene sulfide-containing mixture produced in industrial production is firstly separated into granular polyphenylene sulfide by a centrifuge, and the rest mixture and diatomite are fully stirred and mixed in a mixing kettle (the mass ratio of the polyphenylene sulfide-containing mixture to the diatomite is 100:2) in the mixing kettle (the stirring and mixing time at 25 ℃ is 20 minutes, and the stirring speed of the mixing kettle is 20 revolutions per minute) to prepare a mixture A;
(2) the outlet of the mixing kettle is connected with a pump, the outlet of the pump is connected with a self-operated regulating valve, the self-operated regulating valve is connected with a gamma filter, the mixture A is conveyed to the gamma filter under the action of the pump, and filtering is carried out to obtain polyphenylene sulfide oligomer powder and filtrate B;
(3) and (4) rectifying the filtrate B in a rectifying system.
The rotating speed of the centrifuge in the step (1) is 1450 revolutions per minute.
The working flow rate of the pump in the step (2) is 6m3The delivery lift is 50 m.
And when the pressure of the upper part of the sealed screen plate filter is 0.5MPa, stabilizing the pressure for 30 minutes, taking out the filter plate, and recovering solid materials on the plate to obtain the polyphenylene sulfide oligomer powder.
Comparative example 1
Compared with the example 3, the Ama filter is replaced by a plate frame filter in the comparative example 1, and the rest of the equipment and the operation process are the same.
Comparative example 2
Compared with example 3, the self-operated regulating valve is absent in comparative example 2, and the rest of the equipment is the same as the operation process.
Comparative example 3
In comparison with example 2, the working flow rate of the pump in comparative example 3 except for the step (2) was 8m3The delivery lift is 60 m. When the pressure of the upper part of the sealed screen plate filter is 0.5MPa, after stabilizing the pressure for 10 minutes, taking out the filter plate, and recovering the solid material on the plate to obtain the polyphenylene sulfide oligomer powder, wherein the rest parts are the same as those in the embodiment 2.
Comparative example 4
In comparison with example 3, the working flow rate of the pump in comparative example 3 except for the step (2) was 3m3The delivery lift is 40 m. When the pressure of the upper part of the sealed screen plate filter is 0.3MPa, after stabilizing the pressure for 60 minutes, taking out the filter plate, and recovering solid materials on the plate to obtain polyphenylene sulfide oligomer powder, wherein the rest parts are the same as those in the embodiment 3.
The oligomer powders of polyphenylene sulfide separated in examples 1 to 3 and comparative examples 1 to 4 are shown in Table 1.
Table 1:
as can be seen from the data in Table 1, the application of the Ama filter and the self-operated regulating valve to the separation and purification process of polyphenylene sulfide can obviously improve the separation amount of the low polymer powder of polyphenylene sulfide. From the experimental results of examples 2-3 and comparative examples 3-4, it can be seen that the working flow and the lift of the pump when the ama filter of the present invention is applied to the separation and purification process of polyphenylene sulfide, the upper pressure of the seal net plate filter and the pressure stabilization time have an important influence on the separation amount of the oligomer powder of polyphenylene sulfide. In addition, in comparative example 1, a reboiler, internal parts (a filler and a redistributor) of the rectifying tower and inlet pipelines of a centrifugal machine are easy to block, 10 tons of industrial production mixture containing polyphenylene sulfide is separated, in comparative example 1, the rectifying tower needs to be manually cleaned for 3-6 times, but in examples 1-3, the rectifying tower does not need to be manually cleaned.
In addition, it was also tested that example 3 and comparative example 1 were separated and purified for the same polyphenylene sulfide-containing mixture in a one-year period, and the annual yield of example 3 was 4 to 5 times that of comparative example 1.
The filtrate B filtered by the examples 1-3 enters a rectification system for rectification, the amount of the obtained solvent NMP is more than 140g, and the amount of the obtained solvent NMP in the comparative examples 1-4 is not more than 80 g.
The mixture after rectification in examples 1 to 3 was further concentrated by MVR (mechanical vapor recompression) to obtain a commercial salt in an amount exceeding 100g and comparative examples 1 to 4 to obtain a commercial salt in an amount not exceeding 60 g.
Claims (5)
1. A separation and purification process of polyphenylene sulfide is characterized by comprising the following steps:
(1) separating granular polyphenylene sulfide from the mixture containing polyphenylene sulfide by a centrifuge, and mixing the rest mixture and diatomite in a mixing kettle to prepare a mixture A;
(2) an outlet of the mixing kettle is connected with a pump, an outlet of the pump is connected with an adjusting valve, the adjusting valve is connected with the Ama filter, the mixture A is conveyed to the Ama filter through the pump, and the mixture A is filtered to obtain a solid material and a filtrate B;
the regulating valve is a self-operated regulating valve; when the pressure of the Ama filter is 0.4-0.6MPa, the self-operated regulating valve is automatically opened;
the working flow of the pump is 4-7m3H, the lift is 45-55 m;
the Ama filter comprises a sealed mesh plate filter, wherein the mesh plate of the sealed mesh plate filter is a stainless steel wire mesh which is 100-150 meshes; the pressure of the upper part of the sealed screen plate filter is 0.4-0.6MPa, and the solid material is obtained after the pressure is stabilized for 15-45 minutes;
(3) and (4) rectifying the filtrate B in a rectifying system.
2. The process for separating and purifying polyphenylene sulfide as claimed in claim 1, wherein the rotation speed of the centrifuge in step (1) is 1400-1500 rpm.
3. The process of claim 1, wherein the remaining mixture in step (1) comprises, in terms of mass fraction, 5-12% of NaCl, 8-20% of N-methylpyrrolidone as a solvent, 1-8% of polyphenylene sulfide oligomer powder, and the balance water.
4. The process for separating and purifying polyphenylene sulfide according to claim 1, wherein the remaining mixture in the step (1) is mixed with diatomaceous earth in a mass ratio of 100: 0.5-2.
5. The process of claim 1, wherein the solid material comprises an oligomer powder of polyphenylene sulfide.
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| CN201811500818.4A CN109734912B (en) | 2018-12-10 | 2018-12-10 | Polyphenylene sulfide separation and purification process |
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| CN112871124A (en) * | 2021-01-20 | 2021-06-01 | 珠海长先新材料科技股份有限公司 | Multifunctional comprehensive equipment for polyphenylene sulfide material production |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9409108B2 (en) * | 2012-04-06 | 2016-08-09 | Saint-Gobain Performance Pastics Corporation | Modular filter capsule apparatus |
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- 2018-12-10 CN CN201811500818.4A patent/CN109734912B/en active Active
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| CN101429288A (en) * | 2008-12-09 | 2009-05-13 | 江苏新中投资有限公司 | Method for treating process liquid generated in production process of polyphenylene sulfide |
| CN102863622A (en) * | 2012-09-25 | 2013-01-09 | 自贡鸿鹤化工股份有限公司 | Method for collecting polyphenylene sulfide resin from polyphenylene sulfide resin slurry |
| CN103333359A (en) * | 2013-07-04 | 2013-10-02 | 中国石油化工股份有限公司 | Method for solvent recovery in polyphenylene sulfide synthesis process |
| CN105214353A (en) * | 2015-11-06 | 2016-01-06 | 唐伟 | A kind of closed filter press carrying out plate compression for inflammable and explosive filtrate |
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| CN107141477A (en) * | 2017-06-14 | 2017-09-08 | 中国石油化工股份有限公司 | A kind of method of the high low molecule separation of polyphenylene sulfide |
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