CN103788373B - The dewatering process of many water cures sodium in the synthesis of a kind of polyphenylene sulfide - Google Patents
The dewatering process of many water cures sodium in the synthesis of a kind of polyphenylene sulfide Download PDFInfo
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- CN103788373B CN103788373B CN201410060699.0A CN201410060699A CN103788373B CN 103788373 B CN103788373 B CN 103788373B CN 201410060699 A CN201410060699 A CN 201410060699A CN 103788373 B CN103788373 B CN 103788373B
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- polyphenylene sulfide
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 50
- 239000011734 sodium Substances 0.000 title claims abstract description 50
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 50
- 238000009156 water cure Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 24
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 24
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 31
- 230000018044 dehydration Effects 0.000 claims abstract description 19
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010792 warming Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000000391 smoking effect Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000012544 monitoring process Methods 0.000 claims description 14
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 abstract description 17
- 239000007789 gas Substances 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 19
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 7
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000006068 polycondensation reaction Methods 0.000 description 5
- 239000002341 toxic gas Substances 0.000 description 3
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 210000001061 forehead Anatomy 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002829 nitrogen Chemical class 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses the dewatering process of many water cures sodium in the synthesis of a kind of polyphenylene sulfide, in raw material many water cures sodium water smoking, many water cures sodium, catalyst, nmp solution are heated in a kettle. and stirs, continuous warming, temperature 150～200 DEG C, and it is passed through nitrogen.The dewatering process of the present invention can reduce the dewatering time of many water cures sodium in polyphenylene sulfide building-up process, improves dewatering efficiency and reduce energy consumption; and avoid N methyl pyrrolidone (NMP) and vulcanized sodium at high temperature, air easily decomposes, the problem of oxidation etc.; dehydration seldom produces NMP gas and other foreign gas; water vapour is taken out of by nitrogen, and technological process simplifies, is beneficial to industrialized production and environmental protection.
Description
Technical field
The present invention relates to polyphenylene sulfide synthesis technical field, be specifically related to the dehydration of many water cures sodium in the synthesis of a kind of polyphenylene sulfide
Technique.
Background technology
The at present synthesis of polyphenylene sulfide be mostly carry out being dehydrated with paracide and vulcanized sodium for raw material, the processing step such as polycondensation and
Prepare.Owing to the water imbibition of vulcanized sodium is strong, it is more difficult to preserve, and anhydrous sodium sulfide is expensive, and cost is the highest, therefore
The building-up process of polyphenylene sulfide generally uses the vulcanized sodium containing the crystallization water, that is to say many water cures sodium, therefore need in synthesis
Before polyphenylene sulfide, many water cures sodium is carried out processed.Conventional dewatering is to set up special dehydration facility to carry out
Dehydration, not only increases extra equipment investment cost, also greatly increases consumed energy.
The Chinese invention patent application of application number 201110199757.4 is introduced the many water cures sodium dehydration during polyphenylene sulfide produces
Technology, it will heat in reaction system of aqueous vulcanized sodium, 1-METHYLPYRROLIDONE and cosolvent sodium acetate, due to dehydration
Time length, dehydration temperaturre are high, and vulcanized sodium is exposed in air and can react the generation toxic gas such as sulfur dioxide, hydrogen sulfide, with
Time owing to heating-up temperature is higher than the boiling point of 1-METHYLPYRROLIDONE solution, therefore also have more 1-METHYLPYRROLIDONE quilt
Steaming, thus gas also needs to after discharging reactor separate through rectifying, there is dewatering time length, energy in whole technical process
Consume defect high, inefficient.The Chinese invention patent application of application number 201110229726.9 introduces a kind of polyphenylene sulfide
Many water cures sodium dewatering process process in synthesis technique, its complex process, operation easier are big, and equally exist because of N-first
Base pyrrolidones gas and the generation of hydrogen sulfide gas and need to separate through rectifying, need to increase extra equipment cost, de-
Water time length, energy consumption are high, efficiency is low.
In sum, the dewatering process of existing many water cures sodium is difficult to popularization and application in the industrial production, needs existing skill
Art improves, and works out a kind of dewatering process without increasing equipment cost, dewatering time is short, efficiency is high, energy consumption is low,
It is beneficial to industrialized production.
In order to overcome the technical problem of the above, the invention provides the dehydration of many water cures sodium in the synthesis of a kind of polyphenylene sulfide
Technique so that in polyphenylene sulfide synthesis, many water cures sodium dewatering time reduces, energy consumption reduces, efficiency is improved, and solves
Certainly 1-METHYLPYRROLIDONE (NMP) and vulcanized sodium at high temperature, the problem easily decomposing, aoxidize in air, technological process simplification,
It is beneficial to industrialized production and environmental protection.
Summary of the invention
In order to solve the problems referred to above, the present invention provides the dewatering process of many water cures sodium in the synthesis of a kind of polyphenylene sulfide,
In raw material many water cures sodium water smoking, many water cures sodium, catalyst, nmp solution are heated in a kettle. and stir,
Continuous warming, temperature 150～200 DEG C, and it is passed through nitrogen, described catalyst is selected from anhydrous Lithium chloride or lithium acetate.
The dehydrating process of the present invention, heats many water cures sodium and nmp solution in a kettle. and stirs, being omitted in
Increase dehydration facility outside reaction forehead to be dehydrated, save production cost and energy consumption.Catalyst is just added in the water smoking,
Then can be under catalyst action, vulcanized sodium and NMP combine and form complex compound, can improve the productivity of subsequent polymerisation reaction.
Being passed through nitrogen in dewatering process and can protect reaction, completely cut off air, therefore vulcanized sodium is at high temperature, also will not with in air
Oxygen reaction produces toxic gas sulfur dioxide, hydrogen sulfide etc. so that react safe and reliable；Nitrogen can also be under agitation
Take the moisture of many water cures sodium heating removing out of reactor, on-line monitoring moisture 0.9～1.0mol/molNa2S, make
The efficiency obtaining polycondensation reaction is improved.At 150～200 DEG C, steam is taken out of by nitrogen, without taking NMP out of
(boiling point 203 DEG C) and hydrogen sulfide, it is not necessary to increase atmospheric distillation tower and separate the steam produced in dehydration and NMP
And hydrogen sulfide gas, recycle.After dehydration, suitably it is cooled to 190 DEG C, raw material can be direct plungeed into two
Chlorobenzene starts polycondensation reaction, it is to avoid extra energy ezpenditure, and reaction efficiency is improved, and arriving of technological process is the simplest
Change.
Preferably, described nitrogen gas purity >=99.5%.Use highly purified nitrogen, reaction preferably can be protected,
So that the accessory substance of reaction reduces.
Preferably, nitrogen is passed through bottom reactor.Nitrogen is passed through from bottom, be possible not only to help stirring many water cures sodium,
Catalyst and the mixed solution of NMP, it is also possible to brought out by the water in solution, advantageously in the removing of many water cures sodium
Water.
Preferably, the flow of nitrogen is 5～50L/min.This nitrogen flow, in this scope, can fully take away steam,
Also will not waste the flow of nitrogen simultaneously, the most cost-effective, simultaneously effective to reaction.
Preferably, on-line monitoring system is near infrared moisture online monitoring system.On-line monitoring moisture, effectively controls
The effect of dehydration, thus judge to react the deadline so that the efficiency of polycondensation reaction is improved.
Preferably, the speed adding thermal agitation is 180～450rpm.Mixing speed in this scope, can be sufficiently mixed catalyst,
Vulcanized sodium and the mixed reaction solution of NMP, increase the contact area of reaction mixture and nitrogen simultaneously, be fully dehydrated.
Preferably, the time of raw material many water cures sodium dehydration is 40～60min.Dewatering time is in this scope, the effect of dehydration
Most preferably, saving energy consumption, dehydration is also the most effectively.
Preferably, the speed of continuous warming is 1～5 DEG C/min.Programming rate is in this scope, and reaction heats up uniformly, material
Being sufficiently mixed, dehydration reaches optimal effectiveness.
Compared with prior art, the invention has the beneficial effects as follows:
1, many water cures sodium, catalyst, nmp solution are heated to 150～200 DEG C by the present invention in a kettle., simultaneously
It is passed through nitrogen protection so that NMP and vulcanized sodium will not decompose, aoxidize, and only produces at a temperature of 150～200 DEG C
Having given birth to water vapour, and do not had other gas componant, such as NMP gas, hydrogen sulfide gas etc., water vapour is along with nitrogen stream
Going out in reactor, thus complete dehydration, whole process operation is simple, and spin cycle is short, and it is few, without increasing to consume energy
Add miscellaneous equipment, gas disadvantageous to environment or human body will not be produced.
2, the present invention just adds catalyst in many water cures sodium water smoking, then can be under catalyst action, vulcanized sodium
Combine with NMP and form complex compound, the productivity of subsequent polymerisation reaction can be improved.
3, being passed through nitrogen in dewatering process and can protect reaction, completely cut off air, therefore vulcanized sodium is at high temperature, also will not
Toxic gas sulfur dioxide, hydrogen sulfide etc. are produced so that react safe and reliable with oxygen reaction in air.
4, system does not also exist affect the material of polyphenylene sulfide polymerisation, after dehydration, be suitably cooled to 190 DEG C
, raw material paracide can be direct plungeed into and start polycondensation reaction, it is to avoid extra energy ezpenditure, reaction efficiency is improved,
Technological process is simplified greatly；And be dehydrated after vulcanized sodium will not oxidation stain, NMP also will not be decomposed, directly
Carry out polymerisation to reduce the generation of accessory substance, improve the condition of product, make product colour pure white, weight average molecular weight
Reach 50000, for fibre-grade product.
Detailed description of the invention
Below by embodiment, the present invention will be further described, and its purpose is only that and is best understood from present disclosure rather than limit
Protection scope of the present invention processed.
Specific embodiment 1
In the reactor of 10 liters, add Na2S·3H2O1,000g, catalyst 380g and NMP3,500g, pass to stream
Amount is about the nitrogen of 18L/min, in the case of low whipping speed is 250rpm, continuous warming, and programming rate is about 2 DEG C/min,
Between 163～198 DEG C, the moisture in vulcanized sodium is taken out of continuously by nitrogen, dewatering time 46min, and near infrared moisture is online
In monitoring still, moisture is 0.95mol/molNa2S, synthetic reaction gained polyphenylene sulfide is superior in quality, and condition is good, and color is pure white,
Weight average molecular weight reaches 50000, for fibre-grade product.
Specific embodiment 2
In the reactor of 10 liters, add Na2S·3H2O1,500g, catalyst 580g and NMP5,000g, pass to stream
Amount is about the nitrogen of 15L/min, and in the case of low whipping speed is 280rpm, continuous warming, programming rate is about 1.5 DEG C
/ min, between 150～200 DEG C, the moisture in vulcanized sodium is taken out of continuously by nitrogen, dewatering time 42min, near-infrared water
Dividing moisture in on-line monitoring still is 1mol/molNa2S, synthetic reaction gained polyphenylene sulfide is superior in quality, and condition is good, and color is pure
In vain, weight average molecular weight reaches 50000, for fibre-grade product.
Specific embodiment 3
In the reactor of 25 liters, add Na2S·3H2O3,200g, catalyst 1,200g and NMP11,000g are logical
Be about the nitrogen of 50L/min with flow, in the case of low whipping speed is 180rpm, continuous warming, programming rate is about 3 DEG C
/ min, between 160～196 DEG C, the moisture in vulcanized sodium is taken out of continuously by nitrogen, dewatering time 46min, near-infrared water
Dividing moisture in on-line monitoring still is 0.88mol/molNa2S, synthetic reaction gained polyphenylene sulfide is superior in quality, and condition is good, color
Pure white, weight average molecular weight reaches 50000, for fibre-grade product.
Specific embodiment 4
In the reactor of 25 liters, add Na2S·3H2O4,500g, catalyst 1,500g and NMP15,000g are logical
Be about the nitrogen of 50L/min with flow, in the case of low whipping speed is 360rpm, continuous warming, programming rate is about 3 DEG C
/ min, between 160～195 DEG C, the moisture in vulcanized sodium is taken out of continuously by nitrogen, dewatering time 52min, near-infrared water
Dividing moisture in on-line monitoring still is 0.92mol/molNa2S, synthetic reaction gained polyphenylene sulfide is superior in quality, and condition is good, color
Pure white, weight average molecular weight reaches 50000, for fibre-grade product.
Specific embodiment 5
In the reactor of 10 liters, add Na2S·3H2O800g, catalyst 290g and NMP2,500g, pass to flow
Being about the nitrogen of 5L/min, in the case of low whipping speed is 450rpm, continuous warming, programming rate is about 5 DEG C/min,
Between 150～196 DEG C, the moisture in vulcanized sodium is taken out of continuously by nitrogen, dewatering time 60min, and near infrared moisture is online
In monitoring still, moisture is 0.93mol/molNa2S, synthetic reaction gained polyphenylene sulfide is superior in quality, and condition is good, and color is pure white,
Weight average molecular weight reaches 50000, for fibre-grade product.
Specific embodiment 6
In the reactor of 10 liters, add Na2S·3H2O1,000g, catalyst 380g and NMP3,000g, pass to stream
Amount is about the nitrogen of 5L/min, in the case of low whipping speed is 400rpm, continuous warming, and programming rate is about 1 DEG C/min,
Between 150～199 DEG C, the moisture in vulcanized sodium is taken out of continuously by nitrogen, dewatering time 40min, and near infrared moisture is online
It is 0.96mol/molNa that moisture in still is surveyed in monitoring2S, synthetic reaction gained polyphenylene sulfide is superior in quality, and condition is good, and color is pure white,
Weight average molecular weight reaches 50000, for fibre-grade product.
The announcement of book and teaching according to the above description, above-mentioned embodiment can also be entered by those skilled in the art in the invention
Row change and amendment.Therefore, the invention is not limited in detailed description of the invention disclosed and described above, to the present invention
A little modifications and changes should also be as falling in the scope of the claims of the present invention.Although additionally, this specification employing
Some specific terms, but these terms are merely for convenience of description, and the present invention does not constitute any restriction.
Claims (3)
1. the dewatering process of many water cures sodium in a polyphenylene sulfide synthesis, it is characterised in that at raw material many water cures sodium
In the water smoking, many water cures sodium, catalyst, nmp solution are heated in a kettle. and stirs, continuous warming, rise continuously
The speed of temperature is 1～5 DEG C/min, temperature 150～200 DEG C, and is passed through nitrogen, and described nitrogen gas purity >=99.5%, nitrogen is from instead
Answering bottom portion to be passed through, described catalyst is selected from anhydrous Lithium chloride or lithium acetate, described in add the speed of thermal agitation be 180～450rpm,
The time of raw material many water cures sodium dehydration is 40～60min.
The dewatering process of many water cures sodium in a kind of polyphenylene sulfide the most according to claim 1 synthesis, its feature exists
Flow in nitrogen is 5～50L/min.
The dewatering process of many water cures sodium in a kind of polyphenylene sulfide the most according to claim 1 synthesis, its feature exists
Using on-line monitoring system monitoring moisture in described dewatering process, described on-line monitoring system is near infrared moisture on-line monitoring
System.
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| CN104262623B (en) * | 2014-08-28 | 2017-03-08 | 天津普莱化工技术有限公司 | Polyphenylene sulfide material crystal vulcanized sodium rectification under vacuum dehydrating process |
| CN108147372B (en) * | 2017-12-05 | 2020-01-17 | 宜宾天原集团股份有限公司 | Preparation method of sodium sulfide reaction precursor in polyphenylene sulfide production |
| CN110294844B (en) * | 2019-05-22 | 2022-03-18 | 四川中科兴业高新材料有限公司 | Method for synthesizing high molecular weight polyphenylene sulfide by controlling water content |
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|---|---|---|---|---|
| EP0353716A2 (en) * | 1988-08-05 | 1990-02-07 | Idemitsu Petrochemical Co. Ltd. | Process for preparing polyarylene sulfides |
| CN102432879A (en) * | 2011-08-11 | 2012-05-02 | 深圳市宝力特科技有限公司 | Dewatering process of polyhydrated sodium sulfide in synthetic process of polyphenylene sulfide resin |
| CN102888000A (en) * | 2011-07-18 | 2013-01-23 | 四川得阳特种新材料有限公司 | Dehydration technology of multi-water sodium sulfide in polyphenylene sulfide production |
-
2014
- 2014-02-21 CN CN201410060699.0A patent/CN103788373B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0353716A2 (en) * | 1988-08-05 | 1990-02-07 | Idemitsu Petrochemical Co. Ltd. | Process for preparing polyarylene sulfides |
| CN102888000A (en) * | 2011-07-18 | 2013-01-23 | 四川得阳特种新材料有限公司 | Dehydration technology of multi-water sodium sulfide in polyphenylene sulfide production |
| CN102432879A (en) * | 2011-08-11 | 2012-05-02 | 深圳市宝力特科技有限公司 | Dewatering process of polyhydrated sodium sulfide in synthetic process of polyphenylene sulfide resin |
Non-Patent Citations (1)
| Title |
|---|
| "聚苯硫醚的硫化钠法常压合成";冯辉霞等;《化工科技》;20071215;第15卷(第6期);第9-14页 * |
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Application publication date: 20140514 Assignee: Hengqin Financial Investment International Finance Leasing Co.,Ltd. Assignor: ZHUHAI CHANGXIAN NEW MATERIALS TECHNOLOGY Co.,Ltd. Contract record no.: X2023980044711 Denomination of invention: Dehydration process of polyhydrate sodium sulfide in the synthesis of polyphenylene sulfide Granted publication date: 20160824 License type: Exclusive License Record date: 20231026 |
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Denomination of invention: Dehydration process of polyhydrate sodium sulfide in the synthesis of polyphenylene sulfide Effective date of registration: 20231030 Granted publication date: 20160824 Pledgee: Hengqin Financial Investment International Finance Leasing Co.,Ltd. Pledgor: ZHUHAI CHANGXIAN NEW MATERIALS TECHNOLOGY Co.,Ltd. Registration number: Y2023980063341 |