CN103788373A - Dehydration process of multi-water sodium sulfide during polyphenyl thioether resin synthesis - Google Patents
Dehydration process of multi-water sodium sulfide during polyphenyl thioether resin synthesis Download PDFInfo
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- CN103788373A CN103788373A CN201410060699.0A CN201410060699A CN103788373A CN 103788373 A CN103788373 A CN 103788373A CN 201410060699 A CN201410060699 A CN 201410060699A CN 103788373 A CN103788373 A CN 103788373A
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- many water
- sodium
- polyphenylene sulfide
- water cure
- nitrogen
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 32
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 22
- 230000018044 dehydration Effects 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 title abstract description 4
- 238000003786 synthesis reaction Methods 0.000 title abstract description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 title abstract 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 title abstract 6
- 229920006389 polyphenyl polymer Polymers 0.000 title abstract 3
- 150000003568 thioethers Chemical class 0.000 title abstract 3
- 239000011347 resin Substances 0.000 title abstract 2
- 229920005989 resin Polymers 0.000 title abstract 2
- 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
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims description 36
- 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 claims description 30
- 229910052708 sodium Inorganic materials 0.000 claims description 30
- 238000009156 water cure Methods 0.000 claims description 30
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 26
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 26
- 238000012544 monitoring process Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 10
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- 230000000391 smoking effect Effects 0.000 claims description 4
- 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
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 abstract description 20
- 239000007789 gas Substances 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000009969 flowable effect Effects 0.000 abstract 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 38
- 235000010265 sodium sulphite Nutrition 0.000 description 19
- 239000000047 product Substances 0.000 description 16
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 7
- 238000006068 polycondensation reaction Methods 0.000 description 5
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000002341 toxic gas Substances 0.000 description 3
- 230000009471 action Effects 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
- 239000006227 byproduct Substances 0.000 description 2
- 150000001875 compounds Chemical class 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
- 230000001681 protective effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000001061 forehead Anatomy 0.000 description 1
- 238000009776 industrial production Methods 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
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229960004249 sodium acetate Drugs 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 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 a dehydration process of multi-water sodium sulfide during polyphenyl thioether resin synthesis. The dehydration process comprises the following steps of heating and stirring the multi-water sodium sulfide, a catalyst and an NMP (N-Methyl Pyrrolidone) solution in a reaction kettle in the dehydrating stage of the raw material multi-water sodium sulfide, continuously increasing temperature to 150-200 DEG C, and introducing nitrogen. The dehydration process disclosed by the invention can reduce the dewatering time of the multi-water sodium sulfide in the synthetic process of polyphenyl thioether, increase the dehydration efficiency, reduce the energy consumption, prevent the problems of easiness for decomposition and oxidation and the like of NMP (N-Methyl Pyrrolidone) and sodium sulfide at high temperature in air, generate extremely less NMP gas and other foreign gas in the dehydration process, can be used for carrying away the nitrogen through water vapors and is simplified in process flow and favorable to industrialized production and environmental protection.
Description
Technical field
The present invention relates to polyphenylene sulfide synthesis technical field, be specifically related to a kind of polyphenylene sulfide synthetic in the dewatering process of many water cure sodium.
Background technology
At present polyphenylene sulfide synthetic is mostly to make take santochlor and sodium sulphite as processing steps such as raw material dewaters, polycondensations.Because the water-absorbent of sodium sulphite is strong, be difficult to preserve, and Sodium sulphate anhydrous, 99min is expensive, cost is very high, therefore the general sodium sulphite that contains crystal water that uses in the building-up process of polyphenylene sulfide, that is to say many water cure sodium, therefore need to, before synthetic polyphenylene sulfide, carry out processed to many water cure sodium.Conventional dewatering is to set up special dehydration facility to dewater, and not only increases extra equipment investment cost, has also greatly increased consumed energy.
In the Chinese invention patent application of application number 201110199757.4, introduce the many water cure sodium dehydration technique in polyphenylene sulfide production, it is by moisture sodium sulphite, in the reaction system of N-Methyl pyrrolidone and solubility promoter sodium-acetate, heat, because dewatering time is long, dehydration temperaturre is high, sodium sulphite is exposed in air can reaction produce sulfurous gas, the toxic gases such as hydrogen sulfide, simultaneously because Heating temperature is higher than the boiling point of N-Methyl pyrrolidone solution, therefore also having more N-Methyl pyrrolidone is distilled out of, thereby also need through rectifying separation after gas discharge reactor, whole technological process exists dewatering time long, energy consumption is high, inefficient defect.The Chinese invention patent application of application number 201110229726.9 is introduced the many water cure sodium dewatering process process in a kind of polyphenylene sulfide synthesis technique, its complex process, operation easier are large, and same existence need to be passed through rectifying separation because of the generation of N-Methyl pyrrolidone gas and hydrogen sulfide, need to increase extra equipment cost, dewatering time is long, energy consumption is high, efficiency is low.
In sum, the dewatering process of existing many water cure sodium is difficult to apply in industrial production, need to improve prior art, work out a kind ofly without increasing equipment cost, dewatering time is short, efficiency is high, energy consumption is low dewatering process, be beneficial to suitability for industrialized production.
In order to overcome the technical problem of the above; the invention provides a kind of polyphenylene sulfide synthetic in the dewatering process of many water cure sodium; make polyphenylene sulfide synthetic in the minimizing of many water cure sodium dewatering time, Energy Intensity Reduction, efficiency be improved; and solve N-Methyl pyrrolidone (NMP) and sodium sulphite at high temperature, the problem easily decomposing, be oxidized in air, technical process simplification, be beneficial to suitability for industrialized production and environment protection.
Summary of the invention
In order to address the above problem, the invention provides a kind of polyphenylene sulfide synthetic in the dewatering process of many water cure sodium, in many water cure of raw material sodium water smoking, many water cure sodium, catalyzer, nmp solution are heated and stirred in reactor, continuous warming, 150～200 ℃ of temperature, and pass into nitrogen, described catalyzer is selected from Lithium chloride (anhydrous) or Lithium Acetate.
Dehydrating process of the present invention heats many water cure sodium and nmp solution and stirs in reactor, be omitted in reaction forehead increase outward dehydration facility dewater, save production cost and energy consumption.Just add catalyzer in the water smoking, can be under catalyst action, sodium sulphite and NMP, in conjunction with forming complex compound, can improve the productive rate of subsequent polymerisation reaction.In dewatering process, passing into nitrogen can protective reaction, isolated air, and therefore sodium sulphite at high temperature, also can not produce toxic gas sulfurous gas, hydrogen sulfide etc. with oxygen reaction in air, makes to react safe and reliable; Nitrogen also can heat by many water cure sodium the moisture removing and take reactor out of under stirring, and on-line monitoring moisture content 0.9～1.0mol/molNa2S, is improved the efficiency of polycondensation.At 150～200 ℃, nitrogen is taken water vapour out of, and can not take 203 ℃ of NMP(boiling points out of) and hydrogen sulfide, do not need to increase atmospheric distillation tower to separate the water vapour producing in dehydration and NMP and hydrogen sulfide, recycle.After dehydration, be suitably cooled to 190 ℃, can directly drop into raw material santochlor and start polycondensation, avoid extra energy expenditure, reaction efficiency is improved, and arriving greatly of technical process simplified.
Preferably, described nitrogen gas purity >=99.5%.Use highly purified nitrogen, reaction better can be protected, can make the by product of reaction reduce.
Preferably, nitrogen passes into from reactor bottom.Nitrogen passes into from bottom, not only can help to stir the mixing solutions of many water cure sodium, catalyzer and NMP, the water in solution can also be brought out, and is more conducive to the water that removes of many water cure sodium.
Preferably, the flow of nitrogen is 5～50L/min.This nitrogen flow, in this scope, can fully be taken away water vapour, also can not waste the flow of nitrogen simultaneously, saves cost, simultaneously to reacting effective.
Preferably, on-line monitoring system is near infrared moisture online monitoring system.On-line monitoring moisture content, effectively controls the effect of dehydration reaction, thereby judges the reaction deadline, and the efficiency of polycondensation is improved.
Preferably, the speed of heated and stirred is 180～450rpm.Stirring velocity is in this scope, and the fully mixed reaction solution of mixed catalyst, sodium sulphite and NMP increases the contact area of reaction mixture and nitrogen, fully dehydration simultaneously.
Preferably, the time of many water cure of raw material sodium dehydration is 40～60min.Dewatering time is in this scope, the best results of dehydration, and energy efficient, dehydration is also fully effectively.
Preferably, the speed of continuous warming is 1～5 ℃/min.Heat-up rate is in this scope, and reaction heats up evenly, and material fully mixes, and dehydration reaches optimal effectiveness.
Compared with prior art, the invention has the beneficial effects as follows:
1, many water cure sodium, catalyzer, nmp solution in reactor, are heated to 150～200 ℃ by the present invention; pass into nitrogen protection simultaneously; make NMP and sodium sulphite can not decompose, be oxidized; and at the temperature of 150～200 ℃, only produce water vapor; and there is no other gaseous constituent; as NMP gas, hydrogen sulfide etc.; water vapor is along with nitrogen flows out in reactor; thereby complete dehydration; whole process operation is simple, and spin cycle is short, and power consumption is few; also need not increase miscellaneous equipment, can not produce environment or the disadvantageous gas of human body.
2, the present invention just adds catalyzer in many water cure sodium water smoking, can be under catalyst action, and sodium sulphite and NMP, in conjunction with forming complex compound, can improve the productive rate of subsequent polymerisation reaction.
3, in dewatering process, passing into nitrogen can protective reaction, isolated air, and therefore sodium sulphite at high temperature, also can not produce toxic gas sulfurous gas, hydrogen sulfide etc. with oxygen reaction in air, makes to react safe and reliable.
4, in system, do not exist the material that affects polyphenylene sulfide polyreaction, after dehydration, be suitably cooled to 190 ℃, can directly drop into raw material santochlor and start polycondensation, avoid extra energy expenditure, reaction efficiency is improved, and technical process is simplified greatly; And sodium sulphite after dehydration can oxidation stain, NMP also can not be decomposed, and directly carries out the generation that polyreaction can reduce by product, the product phase that improves product, makes product colour pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
Embodiment
Below by embodiment, the present invention will be further described, and its object is only better to understand content of the present invention but not limits the scope of the invention.
Specific embodiment 1
In the reactor of 10 liters, add Na
2s3H
2o1,000g, catalyzer 380g and NMP3,500g, passes to the nitrogen that flow is about 18L/min, in the situation that low whipping speed is 250rpm, continuous warming, heat-up rate is about 2 ℃/min, and between 163～198 ℃, the moisture in sodium sulphite is taken out of continuously by nitrogen, dewatering time 46min, near infrared moisture on-line monitoring still, moisture is 0.95mol/molNa
2s, building-up reactions gained polyphenylene sulfide is superior in quality, product lover, color is pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
Specific embodiment 2
In the reactor of 10 liters, add Na
2s3H
2o1,500g, catalyzer 580g and NMP5,000g, passes to the nitrogen that flow is about 15L/min, in the situation that low whipping speed is 280rpm, continuous warming, heat-up rate is about 1.5 ℃/min, and between 150～200 ℃, the moisture in sodium sulphite is taken out of continuously by nitrogen, dewatering time 42min, near infrared moisture on-line monitoring still, moisture is 1mol/molNa
2s, building-up reactions gained polyphenylene sulfide is superior in quality, product lover, color is pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
Specific embodiment 3
In the reactor of 25 liters, add Na
2s3H
2o3,200g, catalyzer 1,200g and NMP11,000g, pass to the nitrogen that flow is about 50L/min, low whipping speed is in the situation of 180rpm, continuous warming, and heat-up rate is about 3 ℃/min, between 160～196 ℃, moisture in sodium sulphite is taken out of continuously by nitrogen, dewatering time 46min, and near infrared moisture on-line monitoring still, moisture is 0.88mol/molNa
2s, building-up reactions gained polyphenylene sulfide is superior in quality, product lover, color is pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
Specific embodiment 4
In the reactor of 25 liters, add Na
2s3H
2o4,500g, catalyzer 1,500g and NMP15,000g, pass to the nitrogen that flow is about 50L/min, low whipping speed is in the situation of 360rpm, continuous warming, and heat-up rate is about 3 ℃/min, between 160～195 ℃, moisture in sodium sulphite is taken out of continuously by nitrogen, dewatering time 52min, and near infrared moisture on-line monitoring still, moisture is 0.92mol/molNa
2s, building-up reactions gained polyphenylene sulfide is superior in quality, product lover, color is pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
Specific embodiment 5
In the reactor of 10 liters, add Na
2s3H
2o800g, catalyzer 290g and NMP2,500g, pass to the nitrogen that flow is about 5L/min, low whipping speed is in the situation of 450rpm, continuous warming, and heat-up rate is about 5 ℃/min, between 150～196 ℃, moisture in sodium sulphite is taken out of continuously by nitrogen, dewatering time 60min, and near infrared moisture on-line monitoring still, moisture is 0.93mol/molNa
2s, building-up reactions gained polyphenylene sulfide is superior in quality, product lover, color is pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
Specific embodiment 6
In the reactor of 10 liters, add Na
2s3H
2o1,000g, catalyzer 380g and NMP3,000g, passes to the nitrogen that flow is about 5L/min, in the situation that low whipping speed is 400rpm, continuous warming, heat-up rate is about 1 ℃/min, and between 150～199 ℃, the moisture in sodium sulphite is taken out of continuously by nitrogen, dewatering time 40min, it is 0.96mol/molNa that moisture in still is surveyed near infrared moisture on-line monitoring
2s, building-up reactions gained polyphenylene sulfide is superior in quality, product lover, color is pure white, and weight-average molecular weight reaches 50000, is fibre-grade product.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change and revise above-mentioned embodiment.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition,, although used some specific terms in this specification sheets, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (8)
- A polyphenylene sulfide synthetic in the dewatering process of many water cure sodium, it is characterized in that, in many water cure of raw material sodium water smoking, many water cure sodium, catalyzer, nmp solution are heated and stirred in reactor, continuous warming, 150～200 ℃ of temperature, and pass into nitrogen, described catalyzer is selected from Lithium chloride (anhydrous) or Lithium Acetate.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, it is characterized in that described nitrogen gas purity >=99.5%.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, it is characterized in that nitrogen passes into from reactor bottom.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, the flow that it is characterized in that nitrogen is 5～50L/min.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, it is characterized in that on-line monitoring system is near infrared moisture online monitoring system.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, the speed that it is characterized in that heated and stirred is 180～450rpm.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, it is characterized in that the time of many water cure of raw material sodium dehydration is 40～60min.
- A kind of polyphenylene sulfide according to claim 1 synthetic in the dewatering process of many water cure sodium, the speed that it is characterized in that continuous warming is 1～5 ℃/min.
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| CN201410060699.0A CN103788373B (en) | 2014-02-21 | 2014-02-21 | The dewatering process of many water cures sodium in the synthesis of a kind of polyphenylene sulfide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262623A (en) * | 2014-08-28 | 2015-01-07 | 天津普莱化工技术有限公司 | Reduced pressure rectification and dehydration technique of polyphenylene sulfide raw material (crystalline sodium sulfide) |
| CN108147372A (en) * | 2017-12-05 | 2018-06-12 | 宜宾天原集团股份有限公司 | The preparation method of vulcanized sodium reacting precursor in polyphenylene sulfide production |
| CN110294844A (en) * | 2019-05-22 | 2019-10-01 | 四川中科兴业高新材料有限公司 | A method of control water content synthesizes high molecular weight polyphenylene sulfide |
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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 |
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2014
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| 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262623A (en) * | 2014-08-28 | 2015-01-07 | 天津普莱化工技术有限公司 | Reduced pressure rectification and dehydration technique of polyphenylene sulfide raw material (crystalline sodium sulfide) |
| CN108147372A (en) * | 2017-12-05 | 2018-06-12 | 宜宾天原集团股份有限公司 | The preparation method of vulcanized sodium reacting precursor in polyphenylene sulfide production |
| CN110294844A (en) * | 2019-05-22 | 2019-10-01 | 四川中科兴业高新材料有限公司 | A method of control water content synthesizes high molecular weight polyphenylene sulfide |
| 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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| CN103788373B (en) | 2016-08-24 |
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