CN103242529A - Purifying refining method for high-molecular-weight polyphenylene sulfide - Google Patents
Purifying refining method for high-molecular-weight polyphenylene sulfide Download PDFInfo
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- CN103242529A CN103242529A CN2013102139508A CN201310213950A CN103242529A CN 103242529 A CN103242529 A CN 103242529A CN 2013102139508 A CN2013102139508 A CN 2013102139508A CN 201310213950 A CN201310213950 A CN 201310213950A CN 103242529 A CN103242529 A CN 103242529A
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Abstract
The invention relates to the production field of polyphenylene sulfide, in particular to a purifying refining method for high-molecular-weight polyphenylene sulfide. The method comprises the step of enabling oligomers and low-molecular-weight oligomers in the polyphenylene sulfide and small-molecular-weight polyphenylene sulfide to be gas through vaporizing or sublimating by high-temperature inert drying gas, wherein vaporized or sublimated gas is jacked out of the top of a device in a mode of being wrapped by the inert gas, enters the tube nest of a condenser and is subjected to fast cooling to become liquid or solid to be discharged out of the condenser. The method effectively eliminates the oligomers and low-molecular-weight oligomers in the polyphenylene sulfide and small-molecular-weight polyphenylene sulfide impurities by performing purifying and refining on the polyphenylene sulfide by the high-temperature inert drying gas, thus ensuring that high-quality polyphenylene sulfide fibers can be obtained in the subsequent spinning process of the polyphenylene sulfide purified by the method.
Description
Technical field
The present invention relates to the production field of polyphenylene sulfide, refer more particularly to a kind of process for purification refine of high molecular weight polyphenylene sulfide.
Background technology
Polyphenylene sulfide (being called for short PPS) has good thermostability, good anti-corrosion, has good insulativity and dielectricity etc. hot and humid the grade under the environment.The polyphenylene sulfide fibre of being made by polyphenylene sulfide is novel high added value speciality polymer material, have performances such as good thermotolerance, chemical resistance, flame retardant resistance, insulating property and dimensional stability, be widely used in fields such as environmental protection, electric power, machinery, space flight.
In the building-up process of polyphenylene sulfide, can derive the low molecule organic impuritys such as polyphenylene sulfide of oligopolymer and low-molecular-weight oligomer and small molecular weight, though through the process of washing, purifying, still have a spot of organic impurity to remain in the polyphenylene sulfide after polyphenylene sulfide is made.These impurity because distillation or vaporization will take place high temperature, cause cavity filament or column cap silk in the spinning process of polyphenylene sulfide, influence spinning properties and product quality, therefore must be further purified refining.
Therefore, in order to solve above technical problem, being necessary to have now design improves, designed a kind of process for purification refine of high molecular weight polyphenylene sulfide, present method is carried out purification refine by high temperature inert gas p-poly-phenyl thioether, effectively removed oligopolymer in the polyphenylene sulfide and the polyphenylene sulfide impurity of low-molecular-weight oligomer and small molecular weight, guaranteed in follow-up spinning process, to obtain high-quality polyphenylene sulfide fibre through the polyphenylene sulfide behind present method purifying.
Summary of the invention
In order to overcome the defective that exists in the background technology, the technical solution adopted for the present invention to solve the technical problems is: a kind of process for purification refine of high molecular weight polyphenylene sulfide the steps include:
(1) with in continuous adding one device of polyphenylene sulfide, make polyphenylene sulfide keep the kinestate of adding continuously, continuous output slowly mobile from top to bottom in device, the residence time of maintenance polyphenylene sulfide in installing is 18-50 hour;
(2) with speed be 2-10 cubic meter per minute, the temperature temperature is that 120-260 ℃ rare gas element is sent into from the bottom of this device, make rare gas element and polyphenylene sulfide form adverse current, and carry out thermal exchange, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight can be heated with polyphenylene sulfide, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight at high temperature can be vaporized or distil and is gas, gas after vaporization or the distillation can wrapped from the top of device by rare gas element and discharge, and enters in the tubulation of condenser;
(3) gas mixture that enters in the condenser tubulation is known from experience by fast cooling, the polyphenylene sulfide of oligopolymer wherein and low-molecular-weight oligomer and small molecular weight can become liquid or solid by gas, concentrate in the groove of condenser, automatically be disposed in the gathering barrel by magnetic valve again and focus on recycle again after the rare gas element in the mixed gas is recovered.
The process for purification refine of a kind of high molecular weight polyphenylene sulfide involved in the present invention, present method is carried out purification refine by high temperature inert gas p-poly-phenyl thioether, effectively removed oligopolymer in the polyphenylene sulfide and the polyphenylene sulfide impurity of low-molecular-weight oligomer and small molecular weight, guaranteed in follow-up spinning process, to obtain high-quality polyphenylene sulfide fibre through the polyphenylene sulfide behind present method purifying.
Embodiment
Be further described below in conjunction with the process for purification refine of preferred embodiment to a kind of high molecular weight polyphenylene sulfide of the present invention.
Embodiment one: a kind of process for purification refine of high molecular weight polyphenylene sulfide is characterized in that the steps include:
(1) with in continuous adding one device of polyphenylene sulfide, make polyphenylene sulfide keep the kinestate of adding continuously, continuous output slowly mobile from top to bottom in device, the residence time of maintenance polyphenylene sulfide in installing is 18 hours;
(2) with speed be 3 cubic metres of per minutes, the temperature temperature is that 120 ℃ rare gas element is sent into from the bottom of this device, make rare gas element and polyphenylene sulfide form adverse current, and carry out thermal exchange, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight can be heated with polyphenylene sulfide, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight at high temperature can be vaporized or distil and is gas, gas after vaporization or the distillation can wrapped from the top of device by rare gas element and discharge, and enters in the tubulation of condenser;
(3) gas mixture that enters in the condenser tubulation is known from experience by fast cooling, the polyphenylene sulfide of oligopolymer wherein and low-molecular-weight oligomer and small molecular weight can become liquid or solid by gas, concentrate in the groove of condenser, automatically be disposed in the gathering barrel by magnetic valve again and focus on recycle again after the rare gas element in the mixed gas is recovered.
Embodiment two: a kind of process for purification refine of high molecular weight polyphenylene sulfide is characterized in that the steps include:
(1) with in continuous adding one device of polyphenylene sulfide, make polyphenylene sulfide keep the kinestate of adding continuously, continuous output slowly mobile from top to bottom in device, the residence time of maintenance polyphenylene sulfide in installing is 35 hours;
(2) with speed be 7 cubic metres of per minutes, the temperature temperature is that 200 ℃ rare gas element is sent into from the bottom of this device, make rare gas element and polyphenylene sulfide form adverse current, and carry out thermal exchange, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight can be heated with polyphenylene sulfide, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight at high temperature can be vaporized or distil and is gas, gas after vaporization or the distillation can wrapped from the top of device by rare gas element and discharge, and enters in the tubulation of condenser;
(3) gas mixture that enters in the condenser tubulation is known from experience by fast cooling, the polyphenylene sulfide of oligopolymer wherein and low-molecular-weight oligomer and small molecular weight can become liquid or solid by gas, concentrate in the groove of condenser, automatically be disposed in the gathering barrel by magnetic valve again and focus on recycle again after the rare gas element in the mixed gas is recovered.
Embodiment three: a kind of process for purification refine of high molecular weight polyphenylene sulfide is characterized in that the steps include:
(1) with in continuous adding one device of polyphenylene sulfide, make polyphenylene sulfide keep the kinestate of adding continuously, continuous output slowly mobile from top to bottom in device, the residence time of maintenance polyphenylene sulfide in installing is 50 hours;
(2) with speed be 10 cubic metres of per minutes, the temperature temperature is that 260 ℃ rare gas element is sent into from the bottom of this device, make rare gas element and polyphenylene sulfide form adverse current, and carry out thermal exchange, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight can be heated with polyphenylene sulfide, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight at high temperature can be vaporized or distil and is gas, gas after vaporization or the distillation can wrapped from the top of device by rare gas element and discharge, and enters in the tubulation of condenser;
(3) gas mixture that enters in the condenser tubulation is known from experience by fast cooling, the polyphenylene sulfide of oligopolymer wherein and low-molecular-weight oligomer and small molecular weight can become liquid or solid by gas, concentrate in the groove of condenser, automatically be disposed in the gathering barrel by magnetic valve again and focus on recycle again after the rare gas element in the mixed gas is recovered.
The process for purification refine of a kind of high molecular weight polyphenylene sulfide involved in the present invention, present method is carried out purification refine by high temperature inert gas p-poly-phenyl thioether, effectively removed oligopolymer in the polyphenylene sulfide and the polyphenylene sulfide impurity of low-molecular-weight oligomer and small molecular weight, guaranteed in follow-up spinning process, to obtain high-quality polyphenylene sulfide fibre through the polyphenylene sulfide behind present method purifying.
Claims (1)
1. the process for purification refine of a high molecular weight polyphenylene sulfide is characterized in that the steps include:
(1) with in continuous adding one device of polyphenylene sulfide, make polyphenylene sulfide keep the kinestate of adding continuously, continuous output slowly mobile from top to bottom in device, the residence time of maintenance polyphenylene sulfide in installing is 18-50 hour;
(2) with speed be 2-10 cubic meter per minute, the temperature temperature is that 120-260 ℃ rare gas element is sent into from the bottom of this device, make rare gas element and polyphenylene sulfide form adverse current, and carry out thermal exchange, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight can be heated with polyphenylene sulfide, oligopolymer in the polyphenylene sulfide and low-molecular-weight oligomer, and the polyphenylene sulfide of small molecular weight at high temperature can be vaporized or distil and is gas, gas after vaporization or the distillation can wrapped from the top of device by rare gas element and discharge, and enters in the tubulation of condenser;
(3) gas mixture that enters in the condenser tubulation is known from experience by fast cooling, the polyphenylene sulfide of oligopolymer wherein and low-molecular-weight oligomer and small molecular weight can become liquid or solid by gas, concentrate in the groove of condenser, automatically be disposed in the gathering barrel by magnetic valve again and focus on recycle again after the rare gas element in the mixed gas is recovered.
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| CN2013102139508A CN103242529A (en) | 2013-05-31 | 2013-05-31 | Purifying refining method for high-molecular-weight polyphenylene sulfide |
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| CN2013102139508A CN103242529A (en) | 2013-05-31 | 2013-05-31 | Purifying refining method for high-molecular-weight polyphenylene sulfide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279692A (en) * | 2015-05-15 | 2017-01-04 | 江苏扬农化工集团有限公司 | A kind of method that polyphenylene sulfide oligomer recycles |
| CN107141477A (en) * | 2017-06-14 | 2017-09-08 | 中国石油化工股份有限公司 | A kind of method of the high low molecule separation of polyphenylene sulfide |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0025944A1 (en) * | 1979-09-21 | 1981-04-01 | RHEIN-CHEMIE RHEINAU GmbH | Process for preparing polysulfides |
| JPS62156134A (en) * | 1985-12-28 | 1987-07-11 | Idemitsu Petrochem Co Ltd | Purification of polyarylene sulfide resin |
| JPH01217095A (en) * | 1988-02-26 | 1989-08-30 | Seitetsu Kagaku Co Ltd | Reversible light shielding material |
| US5206439A (en) * | 1992-01-27 | 1993-04-27 | Phillips Petroleum Company | Preparation of high purity polysulfides |
| CN1624023A (en) * | 2004-11-02 | 2005-06-08 | 四川省纺织工业研究所 | Process for purification refine of macromolecular weight poly benzene thioether resin |
| CN101010360A (en) * | 2004-09-06 | 2007-08-01 | 株式会社吴羽 | Production method of polyarylene sulfide |
| CN102798278A (en) * | 2012-08-23 | 2012-11-28 | 江苏金达福高分子材料科技有限公司 | Continuous drying equipment and production method for polyphenylene sulfide slices |
| CN102863621A (en) * | 2012-09-25 | 2013-01-09 | 自贡鸿鹤化工股份有限公司 | Polyphenylene sulfide resin refining method |
-
2013
- 2013-05-31 CN CN2013102139508A patent/CN103242529A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0025944A1 (en) * | 1979-09-21 | 1981-04-01 | RHEIN-CHEMIE RHEINAU GmbH | Process for preparing polysulfides |
| JPS62156134A (en) * | 1985-12-28 | 1987-07-11 | Idemitsu Petrochem Co Ltd | Purification of polyarylene sulfide resin |
| JPH01217095A (en) * | 1988-02-26 | 1989-08-30 | Seitetsu Kagaku Co Ltd | Reversible light shielding material |
| US5206439A (en) * | 1992-01-27 | 1993-04-27 | Phillips Petroleum Company | Preparation of high purity polysulfides |
| CN101010360A (en) * | 2004-09-06 | 2007-08-01 | 株式会社吴羽 | Production method of polyarylene sulfide |
| CN1624023A (en) * | 2004-11-02 | 2005-06-08 | 四川省纺织工业研究所 | Process for purification refine of macromolecular weight poly benzene thioether resin |
| CN102798278A (en) * | 2012-08-23 | 2012-11-28 | 江苏金达福高分子材料科技有限公司 | Continuous drying equipment and production method for polyphenylene sulfide slices |
| CN102863621A (en) * | 2012-09-25 | 2013-01-09 | 自贡鸿鹤化工股份有限公司 | Polyphenylene sulfide resin refining method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279692A (en) * | 2015-05-15 | 2017-01-04 | 江苏扬农化工集团有限公司 | A kind of method that polyphenylene sulfide oligomer recycles |
| CN106279692B (en) * | 2015-05-15 | 2018-10-19 | 江苏扬农化工集团有限公司 | A kind of method that polyphenylene sulfide oligomer recycles |
| CN107141477A (en) * | 2017-06-14 | 2017-09-08 | 中国石油化工股份有限公司 | A kind of method of the high low molecule separation of polyphenylene sulfide |
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Address after: 215531 Jiangsu province Changshou City branch Tang Zhen He Su she Nan side of State Road 204 Applicant after: SUZHOU GOLD SPRING NEW MATERIAL CO., LTD. Address before: 215531 Jiangsu province Changshou City branch Tang Zhen He Su she Nan side of State Road 204 Applicant before: Changshu Gold Spring Chemical Fibers and Knittings Co., Ltd. |
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Application publication date: 20130814 |