CN106146826A - The purifying process of PEKK crude product - Google Patents
The purifying process of PEKK crude product Download PDFInfo
- Publication number
- CN106146826A CN106146826A CN201610505148.XA CN201610505148A CN106146826A CN 106146826 A CN106146826 A CN 106146826A CN 201610505148 A CN201610505148 A CN 201610505148A CN 106146826 A CN106146826 A CN 106146826A
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- CN
- China
- Prior art keywords
- crude product
- pekk
- purifying process
- product
- pekk crude
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/46—Post-polymerisation treatment, e.g. recovery, purification, drying
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing oxygen in addition to the ether group
- C08G2650/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing oxygen in addition to the ether group containing ketone groups, e.g. polyarylethylketones, PEEK or PEK
Abstract
The invention belongs to technical field of polymer materials, be specifically related to the purifying process of a kind of PEKK crude product.Described purifying process, comprises the following steps: joined by PEKK crude product in the adjacent phenylacetic acid aqueous solution of ethylenediamine two, backflow, and cooling is filtered, obtained Primary purification product;Joining in alkaline aqueous solution by Primary purification product, be passed through ozone backflow under ultraviolet light irradiates, cooling is filtered, and obtains secondary purification product;With the water secondary purification product of backflow washing, through filtering, being dried to obtain PEKK sterling.The present invention can be by the Al in PEKK crude product3+Content is down to below 50ppm, and the adjacent phenylacetic acid consumption of ethylenediamine two is few, low cost, and energy saving technology environmental protection is effectively increased product quality, reduces production cost.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to the purifying process of a kind of PEKK crude product.
Background technology
PEKK (PEKK) is the high-performance special engineering plastic of a kind of high temperature resistance, radiation hardness, acid and alkali-resistance, good flame resistance
Material, has important effect in fields such as Aero-Space, telecommunications, defence and military and civilian technology products.
PEKK is the product developed by DuPont, and its preparation method is divided into nucleophilic displacement of fluorine and electrophilic substitution
Two kinds.Electrophilic substitution reaction method typically uses the friedel-craft with aluminum trichloride (anhydrous) as catalyst to be synthesized, the polyether-ketone of synthesis
Having higher aluminium ion to remain in ketone crude product, make PEKK viscosity decline, molecular weight reduces, and product structure changes, and leads
When causing the polymer by following process, produce more side reaction.Therefore, it is possible to find the purification work of a kind of PEKK crude product
Skill, effectively removing the aluminium ion of residual in polymer is the key link of synthesized high-performance PEKK.
Summary of the invention
It is an object of the invention to provide the purifying process of a kind of PEKK crude product, effectively reduce gold in PEKK crude product
Belong to the content of ion.
The purifying process of PEKK crude product of the present invention, comprises the following steps:
(1) PEKK crude product is joined in the adjacent phenylacetic acid aqueous solution of ethylenediamine two, backflow, cooling, filter, obtain
Primary purification product;
(2) Primary purification product are joined in alkaline aqueous solution, under ultraviolet light irradiates, be passed through ozone backflow, cooling, mistake
Filter, obtains secondary purification product;
(3) with the water secondary purification product of backflow washing, through filtering, being dried to obtain PEKK sterling.
Wherein:
In step (1), PEKK crude product uses the electrophilic substitution reaction with aluminum trichloride (anhydrous) as catalyst to prepare, grain
Footpath is 0.1~2mm.
In step (1), the mass concentration of the adjacent phenylacetic acid aqueous solution of ethylenediamine two is 1~20%.
In step (1), the mass ratio of PEKK crude product phenylacetic acid aqueous solution adjacent with ethylenediamine two is 1:10~1:20.
In step (1), return time is 6~10 hours.
Step (2) neutral and alkali aqueous solution is with the aqueous solution that pH is 8~10 of ammonia regulation.
Step (2) neutral and alkali aqueous solution is 10:1~20:1 with the mass ratio of PEKK crude product in step (1).
Step (2) medium ultraviolet light wave a length of 280~320nm.
In step (2) under ultraviolet light irradiates, it is passed through ozone with the speed of 0.1~1L/h, refluxes 3~5 hours.
During in step (3), water consumption is step (1) 20~30 times of PEKK crude product quality.
Beneficial effects of the present invention is as follows:
The features such as the present invention has simple to operate, workable, low cost, and metal ion clearance is high, safety and environmental protection.
The adjacent phenylacetic acid chelating agen toxicity of ethylenediamine two is little, can form stable complex with the many kinds of metal ions such as ferrum, aluminum chelating, have
Effect removes the metal ion in PEKK.Ultraviolet light irradiates and weak basic condition, strengthens the oxidisability of ozone, utilizes ozone
Strong oxidizing property open the unstable impurity structure in reaction, eliminate the little molecule in product.The present invention can be by PEKK
Al in crude product3+Content is down to below 50ppm, and the adjacent phenylacetic acid consumption of ethylenediamine two is few, low cost, energy saving technology ring
Protect, be effectively increased product quality, reduce production cost.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Take Al3+The PEKK crude product 50g of content 4300ppm, the ethylenediamine two being added thereto to mass concentration 20% is adjacent
Phenylacetic acid aqueous solution 500g, 100 DEG C of return stirrings 6 hours, cooling, filter, obtain Primary purification product.
Primary purification product are joined in the 1000ml aqueous solution that pH is 8 with ammonia regulation, be the purple of 280nm at wavelength
Under outer light irradiates, it is passed through ozone with the speed of 1L/h and refluxes 3 hours, cooling, filter, obtain secondary purification product.
Secondary purification product join in 1000g water, backflow washing, through filtering, being dried, obtain white PEKK sterling.
Detect through ICP, its Al3+Content is 32ppm, meets PEKK applied at elevated temperature and processing request.
Embodiment 2
Take Al3+The PEKK crude product 50g of content 4300ppm, the ethylenediamine two being added thereto to mass concentration 10% is adjacent
Phenylacetic acid aqueous solution 750g, 100 DEG C of return stirrings 8 hours, cooling, filter, obtain Primary purification product.
Primary purification product are joined in the 750ml aqueous solution that pH is 9 with ammonia regulation, be the purple of 290nm at wavelength
Under outer light irradiates, it is passed through ozone with the speed of 0.5L/h and refluxes 4 hours, cooling, filter, obtain secondary purification product.
Secondary purification product join in 1250g water, backflow washing, through filtering, being dried, obtain white PEKK sterling.
Detect through ICP, its Al3+Content is 20ppm, meets PEKK applied at elevated temperature and processing request.
Embodiment 3
Take Al3+The PEKK crude product 50g of content 4300ppm, is added thereto to the adjacent benzene of ethylenediamine two of mass concentration 1%
Guanidine-acetic acid aqueous solution 1000g, 100 DEG C of return stirrings 10 hours, cooling, filter, obtain Primary purification product.
Primary purification product are joined in the 500ml aqueous solution that pH is 10 with ammonia regulation, be the purple of 320nm at wavelength
Under outer light irradiates, it is passed through ozone with the speed of 0.1L/h and refluxes 5 hours, cooling, filter, obtain secondary purification product.
Secondary purification product join in 1500g water, backflow washing, through filtering, being dried, obtain white PEKK sterling.
Detect through ICP, its Al3+Content is 45ppm, meets PEKK applied at elevated temperature and processing request.
Claims (10)
1. the purifying process of a PEKK crude product, it is characterised in that comprise the following steps:
(1) PEKK crude product is joined in the adjacent phenylacetic acid aqueous solution of ethylenediamine two, backflow, cooling, filter, obtain primary
Purification product;
(2) Primary purification product are joined in alkaline aqueous solution, under ultraviolet light irradiates, be passed through ozone backflow, cooling, filter,
To secondary purification product;
(3) with the water secondary purification product of backflow washing, through filtering, being dried to obtain PEKK sterling.
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: PEKK in step (1)
Crude product uses the electrophilic substitution reaction with aluminum trichloride (anhydrous) as catalyst to prepare, and particle diameter is 0.1~2mm.
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: ethylenediamine two in step (1)
The mass concentration of adjacent phenylacetic acid aqueous solution is 1~20%.
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: PEKK in step (1)
The mass ratio of crude product phenylacetic acid aqueous solution adjacent with ethylenediamine two is 1:10~1:20.
5. according to the purifying process of the arbitrary described PEKK crude product of Claims 1 to 4, it is characterised in that: step (1) is returned
The stream time is 6~10 hours.
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: step (2) neutral and alkali is water-soluble
Liquid is with the aqueous solution that pH is 8~10 of ammonia regulation.
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: step (2) neutral and alkali is water-soluble
Liquid is 10:1~20:1 with the mass ratio of PEKK crude product in step (1).
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: step (2) medium ultraviolet light wave
A length of 280~320nm.
9. according to the purifying process of the arbitrary described PEKK crude product of claim 6~8, it is characterised in that: in step (2)
Under ultraviolet light irradiates, it is passed through ozone with the speed of 0.1~1L/h, refluxes 3~5 hours.
The purifying process of PEKK crude product the most according to claim 1, it is characterised in that: in step (3), water consumption is
In step (1) 20~30 times of PEKK crude product quality.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1640911A (en) * | 2004-12-09 | 2005-07-20 | 四川大学 | Method for purifying poly ether-ether-ketone |
CN101486784A (en) * | 2009-02-19 | 2009-07-22 | 吉林金正高分子材料研发有限公司 | Method for effectively reducing metal content in polyetheretherketone |
CN101506268A (en) * | 2006-08-31 | 2009-08-12 | 旭硝子株式会社 | Method of purifying polyether compound |
CN102127219A (en) * | 2011-01-07 | 2011-07-20 | 金发科技股份有限公司 | Method for purifying polyether ketone/polyether sulfone polymers |
CN102766257A (en) * | 2012-05-02 | 2012-11-07 | 浙江鹏孚隆科技有限公司 | Method for reducing metal impurities in poly(aryl ether ketone) polymer |
CN104136490A (en) * | 2012-02-28 | 2014-11-05 | 沙伯基础创新塑料知识产权有限公司 | Poly (phenylene ether) process |
-
2016
- 2016-06-30 CN CN201610505148.XA patent/CN106146826A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1640911A (en) * | 2004-12-09 | 2005-07-20 | 四川大学 | Method for purifying poly ether-ether-ketone |
CN101506268A (en) * | 2006-08-31 | 2009-08-12 | 旭硝子株式会社 | Method of purifying polyether compound |
CN101486784A (en) * | 2009-02-19 | 2009-07-22 | 吉林金正高分子材料研发有限公司 | Method for effectively reducing metal content in polyetheretherketone |
CN102127219A (en) * | 2011-01-07 | 2011-07-20 | 金发科技股份有限公司 | Method for purifying polyether ketone/polyether sulfone polymers |
CN104136490A (en) * | 2012-02-28 | 2014-11-05 | 沙伯基础创新塑料知识产权有限公司 | Poly (phenylene ether) process |
CN102766257A (en) * | 2012-05-02 | 2012-11-07 | 浙江鹏孚隆科技有限公司 | Method for reducing metal impurities in poly(aryl ether ketone) polymer |
Non-Patent Citations (2)
Title |
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张思梅等: "《水处理工程技术》", 30 June 2015, 中国水利水电出版社 * |
杨全安等: "《油田实用清防蜡与清防垢技术》", 31 January 2014, 石油工业出版社 * |
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