CN103897188B - Polysulfones Macromolecular materials industry metaplasia production. art - Google Patents
Polysulfones Macromolecular materials industry metaplasia production. art Download PDFInfo
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- CN103897188B CN103897188B CN201410080113.7A CN201410080113A CN103897188B CN 103897188 B CN103897188 B CN 103897188B CN 201410080113 A CN201410080113 A CN 201410080113A CN 103897188 B CN103897188 B CN 103897188B
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- 229920002492 poly(sulfone) Polymers 0.000 title claims abstract description 82
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 206010054949 Metaplasia Diseases 0.000 title abstract description 5
- 230000015689 metaplastic ossification Effects 0.000 title abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 46
- 239000002904 solvent Substances 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 230000001376 precipitating effect Effects 0.000 claims abstract description 23
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 22
- 239000012530 fluid Substances 0.000 claims abstract description 14
- 239000006227 byproduct Substances 0.000 claims abstract description 4
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 238000012805 post-processing Methods 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 150000003457 sulfones Chemical class 0.000 claims description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 239000006166 lysate Substances 0.000 claims 1
- 231100000252 nontoxic Toxicity 0.000 claims 1
- 230000003000 nontoxic effect Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 12
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000000710 polymer precipitation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 10
- 238000009835 boiling Methods 0.000 description 9
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 7
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 229940106691 bisphenol a Drugs 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- GPAPPPVRLPGFEQ-UHFFFAOYSA-N 4,4'-dichlorodiphenyl sulfone Chemical compound C1=CC(Cl)=CC=C1S(=O)(=O)C1=CC=C(Cl)C=C1 GPAPPPVRLPGFEQ-UHFFFAOYSA-N 0.000 description 1
- 206010001606 Alcohol problem Diseases 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 208000028505 alcohol-related disease Diseases 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- FDPIMTJIUBPUKL-UHFFFAOYSA-N dimethylacetone Natural products CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000003359 percent control normalization Methods 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 150000003109 potassium Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- -1 salts potassium carbonate Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Polyethers (AREA)
Abstract
The invention discloses a kind of polysulfones Macromolecular materials industry metaplasia production. arts, include the following steps: that low moisture content solvent identical with polymerization solvent is added after the 1) macromolecular material polymerization reactions such as polysulfones, reduces reaction temperature, terminates the progress of polymerization reaction while reducing reaction fluid viscosity.2) reaction solution is filtered into unreacted catalyst, the by-product inorganic salts of reaction and mechanical admixture.3) filtered fluid is injected into the solvent different from reaction dissolvent as precipitating reagent, polysulfones is separated from filtered fluid in precipitating reagent.4) polysulfones separated washed once through precipitating reagent.5) polysulfones is dry, is granulated, packaging.Invention solves the problems, such as to wrap up inorganic salt particle in existing production technology polymer precipitation process, while solving the problems, such as that production technology solvent recovering rate is low, moisture is high.Using polysulfones high molecular material purity is high produced by the invention, performance is stable, solvent recovering rate is high, at low cost, pollution-free.
Description
Technical field
The present invention relates to the post-processing approach that Macromolecular materials industry metaplasia produces, and belong to technical field of polymer materials, especially
It is related to the post-processing approach and equipment of the high molecular materials industrialized production such as polysulfones, polyether sulfone.
Background technique
Polysulfones is high molecular polymer, is a kind of amorphous, thermoplastic resin.Its characteristic is: excellent in mechanical performance, rigidity
Greatly, wear-resisting, high-intensitive etc., due to its good characteristic, polysulfones has been widely used in medical instrument, space flight and aviation, electronics etc.
High-end field material.
The most advanced production technology of polysulfones high molecular material is one-step synthesis at present.One-step synthesis mainly divides polymerization workshop section
And treatment and finishing section.
Polymerization workshop section: primary raw material 4,4'- dichloro diphenyl sulfone, bisphenol-A, potassium carbonate or saleratus polymerize in a solvent,
Common solvent has dimethyl sulfoxide, n,N-Dimethylformamide, n,N-dimethylacetamide, N-Methyl pyrrolidone etc., optional
Toluene, dimethylbenzene etc. are selected as dehydrating agent.The treatment and finishing section of polymer is carried out after polymerization.
The treatment and finishing section of polymer: using viscous fluid injection and the different solvent of solvent of reaction addition after polymerization as
Precipitating reagent, domestic production factory often use water as precipitating reagent, and external polysulfones factory often uses ethyl alcohol or methanol as precipitating reagent, heavy
Polysulfones is separated from polymer solution in the agent of shallow lake.The polysulfones separated is purified, it is dry, be granulated and packaging.Wherein, gather
Sulfone separates from polymer solution and purifies particularly important, it influences the various performances of polysulfones.Polymer after polymerization
Contain unreacted inorganic salts potassium carbonate or saleratus, the side product chlorinated potassium of reaction, unreacted phenates, system in solution
With material bring colouring metal ions and other mechanical admixtures.They must be divided, and the polysulfones that could obtain high quality produces
Product.
The most commonly used is water-boiling methods for existing purification technique.Water-boiling method is the post-processing approach that domestic production producer generallys use,
This method: after polymerization reaction, the viscous fluid after polymerization is injected in water, while polysulfones is crushed with high speed disintegrator
At particle, the inorganic salt particle wrapped up in polymer is precipitated, removing inorganic salt particle need to high temperature, a large amount of water through 4 times or more
It washes, the pollution of environment caused by causing product purity not high and high energy consumption wastewater treatment etc..Polysulfone polymer after boiling is through dry
Dry, granulation, packaging.The solution of first time boiling is that the mixed liquor of water and solvent can be returned through vacuum distillation with recycling design, solvent
Yield is low, and the moisture content of recycling design is relatively high, generally requires second dehydration rear enclosure use.Drying equipment frequently with forced air drying,
Vacuum drying, vacuum spiral belt drying, drying process are to remove moisture to improve the purity of product, the drying time of water
It is long, increase production cost.
There is document report: after polymerization reaction, with chlorobenzene or dilution with toluene, being filtered to remove inorganic salts and other machinery is miscellaneous
Then matter is mixed with water, be settled out polysulfones.The polysulfones for being settled out polysulfones contains water and solvent, also needs to wash.Filtrate is through high-speed stirring
Standing is mixed, the separation of organic phase (chlorobenzene or toluene) and water phase (water and solvent) is carried out.Water phase recycling design, solvent recovering rate
Low, the moisture content of recycling design is relatively high, generally requires second dehydration rear enclosure use.Organic phase through being distilled to recover chlorobenzene or toluene,
The expense and equipment for increasing processing solvent, substantially increase production cost.
Summary of the invention
In order to solve existing technical problem: the inorganic salt particle wrapped up in polymer is precipitated, removing inorganic salt particle needs
Through high temperature, a large amount of washing, cause product purity not high and the pollution of the environment such as wastewater treatment, and solvent recovery energy after precipitating
The problems such as consumption is high, the rate of recovery is low.Using polysulfones high molecular material purity is high produced by the invention, performance stabilization, solvent recovering rate
It is high, at low cost, pollution-free, it can be applied to the high-end fields such as medical instrument, space flight and aviation, electronics.
A kind of post-processing approach that polysulfones Macromolecular materials industry metaplasia produces:
Solvent identical with polymerization liquid is added after the macromolecular material polymerization reactions such as polysulfones in polymeric kettle, it is molten
Agent moisture is 0.05 ~ 5%, is preferable over less than or equal to 0.5%.The progress that the addition of solvent reduces reaction temperature, terminates polymerization reaction
Reaction fluid viscosity is reduced simultaneously, and the additional amount of solvent is preceding 5% ~ 50% be added of polymerization, is preferable over 10% ~ 20% control temperature of charge
At 80 ~ 140 DEG C, it is preferable over 100 ~ 120 DEG C.Diluted reaction solution is entered by bottom pipeline in the enclosed filters of heat,
Filter unreacted catalyst, the by-product inorganic salts of reaction and mechanical admixture, the temperature of filter is maintained at 80 ~ 160 DEG C, excellent
It selects in 100 ~ 120 DEG C.Filters pressing, vacuum filter, centrifugal filtration can be selected in filter, is preferable over vacuum filter.Filtered fluid is injected
In precipitating reagent, polysulfones is precipitated out in precipitating reagent, while polysulfones is ground into particle with high speed disintegrator, centrifugation.After centrifugation
Polysulfones washed once through precipitating reagent, completely remove high boiling solvent.Solvent with the precipitating reagent boiling point temperature difference is larger can choose
Normal pressure, vacuum distillation.There is no moisture problems for solvent, the precipitating reagent isolated, and can directly apply.Polysulfones contains minimal amount of heavy
Shallow lake agent, through rapid draing.Polysulfones is granulated, packs.
It is difficult and existing that the present invention overcomes the problems, such as that the inorganic salt particle removal wrapped up in polymer is precipitated in existing production technology
There is the problem that production technology solvent recovering rate is low, moisture is high.Remove inorganic salt particle need to through 4 times or more high temperature, a large amount of washing,
The pollution of environment caused by causing product purity not high and high energy consumption wastewater treatment etc..Using polysulfones macromolecule produced by the invention
Material purity is high, performance is stable, solvent recovering rate is high, at low cost, pollution-free, can be applied to medical instrument, space flight and aviation, electronics
Etc. high-end zone material.
Specific embodiment
Embodiment 1
4,210 kilograms of 4- dichloro diphenyl sulfone, 160 kilograms of bisphenol-A, potassium carbonate 110 are added in 2000L polymerization reaction kettle
Kilogram, solvent dimethyl sulfoxide 1200L, 150 kilograms of toluene, be passed through nitrogen, heating starts to flow back in 110 DEG C, with dehydrating amount
Increase, remove in reacting temperature when temperature gradually rises to 155 DEG C and reach 160 DEG C for reaction system water base, and kept for 160 DEG C
The polysulfones solution of molecular weight is needed to acquisition.Dimethyl sulfoxide 150L is rapidly joined, polysulfones solution temperature is down to 130 DEG C.It opens
Polymerization kettle bottom valve, diluted reaction solution enter in vacuum filter, and the jacket temperature of filter at 130 DEG C, take out by the solution of filtering
Into solution kettle.
Filtered fluid is injected in acetone, polysulfones is precipitated out in acetone, while polysulfones is ground into high speed disintegrator
Particle, centrifugation.Polysulfones after centrifugation washed once through acetone reflux 30 minutes, and completely remove high boiling dimethyl sulfoxide.
Dimethyl sulfoxide and acetone select air-distillation.The problem of moisture content is not present in dimethyl sulfoxide, the acetone isolated, can be direct
It applies.Polysulfones is dried in vacuo 2 hours through 40 DEG C.Polysulfones is granulated, packs.It is 0.01% through detection polysulfones ash content, thermal deformation temperature
174 DEG C of degree.
Embodiment 2
4,210 kilograms of 4- dichloro diphenyl sulfone, 160 kilograms of bisphenol-A, saleratus are added in 2000L polymerization reaction kettle
220 kilograms, solvent n,N-Dimethylformamide 1200L are passed through nitrogen, and heating starts to flow back in 120 DEG C, with the increasing of dehydrating amount
Add, remove in reacting temperature when temperature gradually rises to 140 DEG C and reach 150 DEG C for reaction system water base, keep 150 DEG C to obtaining
Need the polysulfones solution of molecular weight.N,N-Dimethylformamide 120L is rapidly joined, polysulfones solution temperature is down to 120 DEG C.It opens
Polymerization kettle bottom valve, diluted reaction solution enter in centrifuge, and at 120 DEG C, the solution of centrifugation is extracted into molten the jacket temperature of centrifuge
In liquid kettle.
Filtered fluid is injected in ethyl alcohol, polysulfones is precipitated out in ethanol, while polysulfones is ground into high speed disintegrator
Particle, centrifugation.Polysulfones after centrifugation washed once through alcohol reflux 30 minutes, completely remove high boiling N, N- dimethyl methyl
Amide.N,N-dimethylformamide and ethyl alcohol select air-distillation.Isolate N,N-dimethylformamide, there is no moisture for ethyl alcohol
Problem can be applied directly.Polysulfones is dried in vacuo 2 hours through 40 DEG C.Polysulfones is granulated, packs.Being detected polysulfones ash content is
0.03%, 174 DEG C of heat distortion temperature.
Embodiment 3
4,210 kilograms of 4- dichloro diphenyl sulfone, 160 kilograms of bisphenol-A, potassium carbonate 110 are added in 2000L polymerization reaction kettle
Kilogram, solvent N-methyl pyrilidone 1200L, be passed through nitrogen, heating starts to flow back in 120 DEG C, with the increase of dehydrating amount, temperature
Remove in reacting temperature when degree gradually rises to 160 DEG C and reach 180 DEG C for reaction system water base, keep 180 DEG C to being needed
The polysulfones solution of molecular weight.N-Methyl pyrrolidone 240L is rapidly joined, polysulfones solution temperature is down to 150 DEG C.Open polymeric kettle
Bottom valve, diluted reaction solution enter in centrifuge, and at 150 DEG C, the solution of centrifugation is extracted into solution kettle the jacket temperature of centrifuge.
Filtered fluid is injected in methanol, polysulfones is precipitated out in methyl alcohol, while polysulfones is ground into high speed disintegrator
Particle, centrifugation.Polysulfones after centrifugation washed once through methanol eddy 30 minutes, completely remove high boiling N- crassitude
Ketone.N-Methyl pyrrolidone and methanol select air-distillation.N-Methyl pyrrolidone, methanol are isolated there is no moisture problem,
It can directly apply.Polysulfones is dried in vacuo 2 hours through 40 DEG C.Polysulfones is granulated, packs.It is 0.02% through detection polysulfones ash content, heat
174 DEG C of deformation temperature.
Claims (20)
1. polysulfones macromolecular material polymerization reaction post-processing approach, it is characterised in that through following steps:
1) it after polysulfones macromolecule material solution polymerization reaction, is added in polymeric kettle identical with polymerization solvent molten
Agent；
2) by diluted reaction solution by bottom pipeline enter closing, heat filter in, filter unreacted catalyst, anti-
The by-product inorganic salts and mechanical admixture answered；
3) filtered fluid is injected into the solvent different from reaction dissolvent as precipitating reagent, polysulfones is separated from filtered fluid in precipitating reagent
Out；
4) polysulfones separated washed once through precipitating reagent；
5) polysulfones is dry, is granulated, packaging.
2. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that be suitable for institute
There is the post-processing approach of macromolecule material solution polymerization reaction.
3. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that polymerization reaction
After identical with polymerization solvent solvent is added.
4. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 3, which is characterized in that polymerization reaction
After the moisture of solvent that is added be 0.05 ~ 5%.
5. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that polymerization reaction
After be added solvent amount be polymerize before additional amount 5% ~ 50%.
6. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that polymerization reaction
After be added solvent, control temperature of charge at 80 ~ 160 DEG C.
7. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 5, which is characterized in that solvent adds
Enter amount is preferably additional amount before polymerizeing 10% ~ 20%.
8. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 6, which is characterized in that control material
Preferably 100 ~ 140 DEG C of temperature.
9. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that will be diluted
Reaction solution by bottom pipeline enter closing, heat filter in, the temperature of filter is maintained at 80 ~ 160 DEG C.
10. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 9, which is characterized in that will dilute
Reaction solution by bottom pipeline enter closing, heat filter in, the temperature of filter is preferably at 100 ~ 140 DEG C.
11. the polysulfones macromolecular material polymerization reaction post-processing approach told according to claim 1, filter selects filters pressing, true
Sky filtering, centrifugal filtration.
12. the 1 polysulfones macromolecular material polymerization reaction post-processing approach told, filter preferably use vacuum according to claim 1
Filtering.
13. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that will be diluted
Reaction solution by bottom pipeline enter closing, heat filter in filter, filtered during nitrogen or argon gas are protected.
14. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, it is characterised in that infuse filtered fluid
Enter the solvent different from the solvent that reaction is added as precipitating reagent, polysulfones is separated from filtered fluid in precipitating reagent.
15. the 4 polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that precipitating reagent is
It dissolves each other with reaction dissolvent without the small organic molecule of lysate.
16. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 15, which is characterized in that precipitating reagent is excellent
It selects in nontoxic acetone, butanone, methanol or ethyl alcohol.
17. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, which is characterized in that separate
Polysulfones washed once through precipitating reagent.
18. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, it is characterised in that precipitating reagent washing
Polysulfones centrifugation afterwards, removes a large amount of precipitating reagents.
19. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, it is characterised in that poly- after centrifugation
Sulfone is dried in vacuo 2 ~ 6 hours, 40-100 DEG C of temperature.
20. polysulfones macromolecular material polymerization reaction post-processing approach according to claim 1, it is characterised in that recycling design,
Precipitating reagent selection normal pressure is recovered under reduced pressure.
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| CN104629055B (en) * | 2015-03-11 | 2017-03-08 | 威海帕斯砜新材料有限公司 | Industrialized production polysulfones macromolecular material method |
| CN106832286A (en) * | 2017-03-01 | 2017-06-13 | 山东浩然特塑股份有限公司 | A kind of sulfone birds of the same feather flock together compound industrialization blowing dispersing technology |
| CN107286345B (en) * | 2017-07-27 | 2023-08-18 | 上海帕斯砜材料科技有限公司 | Industrial production method of high-purity polysulfone, polyether sulfone and polyarylsulfone resin |
| CN108164746A (en) * | 2017-12-27 | 2018-06-15 | 赵洋 | The regeneration processing technology of waste and old polysulfones film product |
| CN108329472A (en) * | 2018-01-25 | 2018-07-27 | 威海帕斯砜新材料有限公司 | A kind of synthetic method of polysulfones series plastics |
| CN113416306B (en) * | 2020-08-14 | 2023-03-17 | 吉林大学 | Polyaryletherketone resin and preparation method thereof |
| CN116178719A (en) * | 2022-11-30 | 2023-05-30 | 山东海科创新研究院有限公司 | Polysulfone polymer purifying and molecular weight grading treatment process |
| CN115926167A (en) * | 2022-11-30 | 2023-04-07 | 山东海科创新研究院有限公司 | Purification method of polysulfone polymer |
| CN115850704A (en) * | 2022-11-30 | 2023-03-28 | 山东海科创新研究院有限公司 | Post-treatment method of polysulfone polymer |
| CN116178720A (en) * | 2022-11-30 | 2023-05-30 | 山东海科创新研究院有限公司 | Purification method of casting film grade polyethersulfone resin and obtained product |
| CN116478403B (en) * | 2023-04-07 | 2024-03-26 | 安徽卓润新材料科技有限公司 | Polysulfone resin preparation method and preparation device thereof |
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|---|---|---|---|---|
| EP0459620A2 (en) * | 1990-04-25 | 1991-12-04 | Kureha Kagaku Kogyo Kabushiki Kaisha | Production process of arylene thioether copolymer |
| CN101092479A (en) * | 2007-07-26 | 2007-12-26 | 四川大学 | Method for preparing polyphenylene oxide sulfide |
| CN101838390A (en) * | 2010-05-28 | 2010-09-22 | 电子科技大学 | Method for preparing poly(arylene ether nitrile) resin |
| CN102888003A (en) * | 2012-10-10 | 2013-01-23 | 四川飞亚新材料有限公司 | High polymer material precipitation method and industrial production method of polysulfone resin |
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