CN102731785B - Polyphenylene sulfide purifying method - Google Patents
Polyphenylene sulfide purifying method Download PDFInfo
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- CN102731785B CN102731785B CN201210189615.4A CN201210189615A CN102731785B CN 102731785 B CN102731785 B CN 102731785B CN 201210189615 A CN201210189615 A CN 201210189615A CN 102731785 B CN102731785 B CN 102731785B
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Abstract
The invention discloses a polyphenylene sulfide purifying method. The method comprises the steps that: (1) acid-base neutralization is carried out, wherein a polymerization reaction product polyphenylene sulfide is cooled, an acid is added to polyphenylene sulfide, the pH of the mixture is controlled at 3-4, and a reaction is carried out while stirring; (2) solid-liquid separation is carried out, wherein a reaction product obtained in the step (1) is cooled and is subjected to solid-liquid separation, such that polyphenylene sulfide solid is obtained; (3) solvent washing is carried out, wherein an organic solvent is added to the obtained polyphenylene sulfide solid, and washing is carried out while stirring; (4) steam distillation and washing are carried out, wherein the polyphenylene sulfide obtained by washing in the step (3) is subjected to steam distillation under a negative-pressure condition, the residual organic solvent in the polyphenylene sulfide solid particles is recovered during the steam distillation process, and the polyphenylene sulfide is washed by using steam condensation water with a temperature of 75-85 DEG C when the content of the organic solvent is lower than 1%; and (5) drying and packaging are carried out, wherein qualified polyphenylene sulfide obtained in the step (4) is separated, dried, and packaged. Polyphenylene sulfide obtained with the method is advantaged in high electrical insulating property and high mechanical strength.
Description
Technical field
The present invention relates to the production field of polyphenylene sulfide, refer more particularly to the purification process of polyphenylene sulfide.
Background technology
Polyphenylene sulfide (being called for short PPS) has good thermostability, good erosion resistance, hot and humid grade under environment, has good insulativity and dielectricity etc.Therefore polyphenylene sulfide is widely used in fiber and electronic devices and components.
It is raw material production that polyphenylene sulfide be take sodium sulphite and santochlor conventionally, completes polyreaction again through the dry polyphenylene sulfide finished product that obtains of purifying under high temperature (being generally 300 ℃ of left and right) high pressure.Because direct production polyphenylene sulfide out contains a large amount of mineral ion impurity, organic impurity and oligopolymer, can affect the use properties of follow-up polyphenylene sulfide, so must be through effective purifying.The purification process of polyphenylene sulfide generally adopts filtering separation and countercurrent washing at present.The shortcoming that above-mentioned purification process exists is: the polyphenylene sulfide after purifying still contains a large amount of mineral ion impurity, oligopolymer and organic impurity, has had a strong impact on electrical insulating property and the physical strength of polyphenylene sulfide.
Summary of the invention
The object of this invention is to provide a kind of purification process that can effectively reduce a kind of polyphenylene sulfide of mineral ion impurity, organic impurity and oligomer in polyphenylene sulfide.
For achieving the above object, the present invention has adopted following technical scheme.
A kind of purification process of polyphenylene sulfide, comprise the following steps: (1) acid-base neutralisation: the product polyphenylene sulfide generating after polyreaction is cooled to 100 ℃～120 ℃, add acid, control PH 3～4, low whipping speed is to react 25～35 minutes under the state of 20～30 revs/min of stirrings; (2) solid-liquid separation: the reaction product that (1) step is obtained is cooled to 75 ℃～85 ℃, by whizzer solid-liquid separation, obtains polyphenylene sulfide solid; (3) solvent wash: add organic solvent in the polyphenylene sulfide solid obtaining, temperature is controlled at 95 ℃～105 ℃, washs under whipped state, washs 10～20 minutes; (4) wet distillation and washing: the polyphenylene sulfide obtaining after (3) step is washed carries out wet distillation under the condition of negative pressure, and reclaim and residue in the organic solvent in polyphenylene sulfide solid particulate in still-process; After distillation for some time, sampling detects, when organic solvent content is less than 1%, with the vapour condensation water washing polyphenylene sulfide of 75 ℃～85 ℃; (5) dry packing: qualified polyphenylene sulfide that (4) step is obtained is separated, dry, packing.
Further, the purification process of aforesaid a kind of polyphenylene sulfide, wherein, described acid is hydrochloric acid, sulfuric acid or oxalic acid.
Further, the purification process of aforesaid a kind of polyphenylene sulfide, wherein, described organic solvent is hexamethylphosphorictriamide or N-Methyl pyrrolidone.
Further, the purification process of aforesaid a kind of polyphenylene sulfide, wherein, step is carried out wet distillation in (4) under the condition of negative pressure-80KPa～-60KPa, and distillation time is 40 minutes to 2 hours.
Beneficial effect of the present invention: in the polyphenylene sulfide after purifying, mineral ion impurity, oligopolymer and organic impurity content are low, electrical insulating property is strong and physical strength is high, is a kind of very excellent engineering plastics.And purifying process of the present invention can carry out under totally-enclosed condition of negative pressure, environmentally safe can be realized cleaner production.
Embodiment
Below in conjunction with preferred embodiment, the purification process of a kind of polyphenylene sulfide of the present invention is further described.
Embodiment mono-: a kind of purification process of polyphenylene sulfide, comprise the following steps: (1) acid-base neutralisation: the product polyphenylene sulfide generating after polyreaction is cooled to 100 ℃, add hydrochloric acid, controlling PH is 3, and low whipping speed is to react 25 minutes under the state of 20 revs/min of stirrings; (2) solid-liquid separation: the reaction product that (1) step is obtained is cooled to 75 ℃, by whizzer solid-liquid separation, obtains polyphenylene sulfide solid; (3) solvent wash: add organic solvent hexamethylphosphorictriamide in the polyphenylene sulfide solid obtaining, temperature is controlled at 95 ℃, washs under whipped state, washs 10 minutes; (4) wet distillation and washing: the polyphenylene sulfide obtaining after (3) step is washed carries out wet distillation under the condition of negative pressure-60KPa, and reclaim and residue in the organic solvent in polyphenylene sulfide solid particulate in still-process; Distillation for some time samples detection after being about 40 minutes, when organic solvent content is less than 1%, with the vapour condensation water washing polyphenylene sulfide of 75 ℃; (5) dry packing: qualified polyphenylene sulfide that (4) step is obtained is separated, dry, packing.
Embodiment bis-: a kind of purification process of polyphenylene sulfide, comprise the following steps: (1) acid-base neutralisation: the product polyphenylene sulfide generating after polyreaction is cooled to 110 ℃, add sulfuric acid, controlling PH is 3.5, and low whipping speed is to react 30 minutes under the state of 25 revs/min of stirrings; (2) solid-liquid separation: the reaction product that (1) step is obtained is cooled to 80 ℃, by whizzer solid-liquid separation, obtains polyphenylene sulfide solid; (3) solvent wash: add organic solvent N-Methyl pyrrolidone in the polyphenylene sulfide solid obtaining, temperature is controlled at 100 ℃, washs under whipped state, washs 15 minutes; (4) wet distillation and washing: the polyphenylene sulfide obtaining after (3) step is washed carries out wet distillation under the condition of negative pressure-70KPa, and reclaim and residue in the organic solvent in polyphenylene sulfide solid particulate in still-process; After approximately 1 hour for some time of distillation, sampling detects, when organic solvent content is less than 1%, with the vapour condensation water washing polyphenylene sulfide of 80 ℃; (5) dry packing: qualified polyphenylene sulfide that (4) step is obtained is separated, dry, packing.
Embodiment tri-: a kind of purification process of polyphenylene sulfide, comprise the following steps: (1) acid-base neutralisation: the product polyphenylene sulfide generating after polyreaction is cooled to 120 ℃, add oxalic acid, controlling PH is 4, and low whipping speed is to react 35 minutes under the state of 30 revs/min of stirrings; (2) solid-liquid separation: the reaction product that (1) step is obtained is cooled to 85 ℃, by whizzer solid-liquid separation, obtains polyphenylene sulfide solid; (3) solvent wash: add organic solvent hexamethylphosphorictriamide in the polyphenylene sulfide solid obtaining, temperature is controlled at 105 ℃, washs under whipped state, washs 20 minutes; (4) wet distillation and washing: the polyphenylene sulfide obtaining after (3) step is washed carries out wet distillation under the condition of negative pressure-80KPa, and reclaim and residue in the organic solvent in polyphenylene sulfide solid particulate in still-process; After approximately 2 hours for some time of distillation, sampling detects, when organic solvent content is less than 1%, with the vapour condensation water washing polyphenylene sulfide of 85 ℃; (5) dry packing: qualified polyphenylene sulfide that (4) step is obtained is separated, dry, packing.
Purification process of the present invention, in the polyphenylene sulfide after purifying, mineral ion impurity, oligopolymer and organic impurity content are low, and electrical insulating property is strong and physical strength is high, is a kind of very excellent engineering plastics.And purifying process of the present invention can carry out under totally-enclosed condition of negative pressure, environmentally safe can be realized cleaner production.
Claims (3)
1. the purification process of a polyphenylene sulfide; it is characterized in that: comprise the following steps: (1) acid-base neutralisation: the product polyphenylene sulfide generating after polyreaction is cooled to 100 ℃～120 ℃; add acid; control pH 3～4, low whipping speed is to react 25～35 minutes under the state of 20～30 revs/min of stirrings; (2) solid-liquid separation: the reaction product that step (1) is obtained is cooled to 75 ℃～85 ℃, by whizzer solid-liquid separation, obtains polyphenylene sulfide solid; (3) solvent wash: add organic solvent in the polyphenylene sulfide solid obtaining, temperature is controlled at 95 ℃～105 ℃ washs under whipped state, washs 10～20 minutes; (4) wet distillation and washing: the polyphenylene sulfide obtaining after step (3) washing is carried out to wet distillation under the condition of negative pressure, and reclaim and residue in the organic solvent in polyphenylene sulfide solid particulate in still-process; After distillation for some time, sampling detects, when organic solvent content is less than 1%, with the vapour condensation water washing polyphenylene sulfide of 75 ℃～85 ℃; (5) dry packing: the qualified polyphenylene sulfide separation that step (4) is obtained, dry, packing; Described organic solvent is hexamethylphosphorictriamide or N-Methyl pyrrolidone.
2. the purification process of a kind of polyphenylene sulfide according to claim 1, is characterized in that: described acid is hydrochloric acid, sulfuric acid or oxalic acid.
3. the purification process of a kind of polyphenylene sulfide according to claim 1 and 2, is characterized in that: in step (4), under the condition of negative pressure-80KPa～-60KPa, carry out wet distillation, distillation time is 40 minutes to 2 hours.
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| CN201210189615.4A CN102731785B (en) | 2012-06-11 | 2012-06-11 | Polyphenylene sulfide purifying method |
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| CN201210189615.4A CN102731785B (en) | 2012-06-11 | 2012-06-11 | Polyphenylene sulfide purifying method |
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| CN102731785A CN102731785A (en) | 2012-10-17 |
| CN102731785B true CN102731785B (en) | 2014-04-09 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103172863B (en) * | 2013-04-07 | 2015-02-25 | 百川化工(如皋)有限公司 | Method for improving washing and separating efficiency of polyphenylene sulfide particles |
| CN104072772A (en) * | 2014-07-11 | 2014-10-01 | 四川宝利丰科技有限公司 | Treatment method for polyphenylene sulfide resin slurry |
| CN104817696B (en) * | 2015-03-04 | 2018-10-19 | 常州大学 | Polymeric articles desalting purifying method in a kind of production of polyphenylene sulfide |
| CN105968356B (en) * | 2016-05-24 | 2018-02-09 | 四川大学 | A kind of environmental protection and economy type polyarylether and preparation method thereof |
| CN107151278A (en) * | 2017-04-26 | 2017-09-12 | 安徽华塑股份有限公司 | A kind of Corvic post-processing approach |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4424338A (en) * | 1982-09-10 | 1984-01-03 | Phillips Petroleum Company | Polymer treatment |
| EP0594192A1 (en) * | 1992-10-23 | 1994-04-27 | Phillips Petroleum Company | Production of poly(arylene sulfide)polymers containing reduced amounts of oligomers |
| CN1597736A (en) * | 2004-08-24 | 2005-03-23 | 四川大学 | Purification method of polyphenyl thioether |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000273175A (en) * | 1999-03-19 | 2000-10-03 | Idemitsu Petrochem Co Ltd | Purification of polyarylene sulfide resin |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4424338A (en) * | 1982-09-10 | 1984-01-03 | Phillips Petroleum Company | Polymer treatment |
| EP0594192A1 (en) * | 1992-10-23 | 1994-04-27 | Phillips Petroleum Company | Production of poly(arylene sulfide)polymers containing reduced amounts of oligomers |
| CN1597736A (en) * | 2004-08-24 | 2005-03-23 | 四川大学 | Purification method of polyphenyl thioether |
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Effective date of registration: 20200710 Address after: 215600 Donglai Jiangqiao, Yangshe Town, Zhangjiagang City, Jiangsu Province (in Zhangjiagang East China Marine Valve Manufacturing Co., Ltd.) Patentee after: Jiangsu Xinren Environmental Protection Technology Co.,Ltd. Address before: 215621, Zhangjiagang, Jiangsu, Suzhou Province Yu Yu Town Chemical Industry Park, Zhangjiagang Xin Sheng new materials Co., Ltd. Patentee before: ZHANGJIAGANG XINSHENG NEW MATERIAL Co.,Ltd. |
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