CN106146826A - The purifying process of PEKK crude product - Google Patents

The purifying process of PEKK crude product Download PDF

Info

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
Authority
CN
China
Prior art keywords
crude product
pekk
purifying process
product
pekk crude
Prior art date
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.)
Pending
Application number
CN201610505148.XA
Other languages
Chinese (zh)
Inventor
薛居强
王军
孙庆民
王荣海
李光辉
张泰铭
黄桂青
李云龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Kaisheng New Materials Co Ltd
Original Assignee
Shandong Kaisheng New Materials Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shandong Kaisheng New Materials Co Ltd filed Critical Shandong Kaisheng New Materials Co Ltd
Priority to CN201610505148.XA priority Critical patent/CN106146826A/en
Publication of CN106146826A publication Critical patent/CN106146826A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/34Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
    • C08G65/46Post-polymerisation treatment, e.g. recovery, purification, drying
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/34Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
    • C08G65/38Macromolecular 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
    • C08G65/40Macromolecular 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
    • C08G65/4012Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2650/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G2650/28Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
    • C08G2650/38Macromolecular 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
    • C08G2650/40Macromolecular 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

The purifying process of PEKK crude product
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.
CN201610505148.XA 2016-06-30 2016-06-30 The purifying process of PEKK crude product Pending CN106146826A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610505148.XA CN106146826A (en) 2016-06-30 2016-06-30 The purifying process of PEKK crude product

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610505148.XA CN106146826A (en) 2016-06-30 2016-06-30 The purifying process of PEKK crude product

Publications (1)

Publication Number Publication Date
CN106146826A true CN106146826A (en) 2016-11-23

Family

ID=57350635

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610505148.XA Pending CN106146826A (en) 2016-06-30 2016-06-30 The purifying process of PEKK crude product

Country Status (1)

Country Link
CN (1) CN106146826A (en)

Citations (6)

* Cited by examiner, † Cited by third party
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
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 *

Similar Documents

Publication Publication Date Title
CN104192967B (en) A kind of Ti 3c 2the application of nanometer sheet high oxidative toxic metal ions in process water
CN106336055B (en) A kind of processing of acid-bearing wastewater utilizes technique
CN105152302B (en) A kind of processing method of phenyl amines organic wastewater
Wang et al. Comparison study on microwave irradiation-activated persulfate and hydrogen peroxide systems in the treatment of dinitrodiazophenol industrial wastewater
CN104607153A (en) Heavy metal ion adsorbent prepared from lotus leaves and preparation method thereof
CN104624163A (en) Heavy metal adsorbent prepared by cactus and preparation method for heavy metal adsorbent
Tomasi et al. Tannin-based coagulants: Current development and prospects on synthesis and uses
CN102153183A (en) Nano ferric oxide-cationic polyelectrolyte coupled multielement composite flocculant
CN105085332B (en) A kind of aromatic nitro compound method that selective reduction prepares arylamine when iron oxide/Fe (II) coexists
CN106311163A (en) Preparation method of chitosan/iron hydroxide composite adsorbent for adsorbing arsenic
Liu et al. High-efficient decomplexation of Cu-HA by discharge plasma: Process and mechanisms
CN104888693A (en) Heavy metal adsorbing granule containing ginkgo leaves and preparation method of heavy metal adsorbing granule
CN106146826A (en) The purifying process of PEKK crude product
CN105540982A (en) Resourceful treatment method for micromolecule amine salt-containing wastewater
CN105536728A (en) Grapevine adsorption granule for heavy metals and preparation method thereof
CN105457607A (en) Broad bean shell containing heavy metal adsorption granules and preparation method thereof
CN106008957A (en) Technology for purifying poly(ether-ketone-ketone) crude product by using amino tris(methylene phosphonic acid)
Mouton et al. A new water-soluble polycarbobetaine showing high selectivity toward copper
CN106008956B (en) The technique that polyether ketone ketone crude product is purified using chelating agent
CN106188526A (en) Use the technique that PEKK crude product is purified by polyamino many ethers tetramethylene phosphonic acid
CN106117546A (en) Use the technique that PEKK crude product is purified by diethylene triamine pentacetic acid (DTPA)
CN106046357A (en) Purification method of polyetherketone ketone crude product
CN105885032A (en) Technology for purifying poly(ether-ketone-ketone) crude product by adopting ethanediamine di-ortho-phenyl acetic acid
CN100567154C (en) A kind of synthetic method of sodium pentathiosulfate
CN107282023A (en) A kind of chemical waste fluid processing nano adsorber and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20161123

RJ01 Rejection of invention patent application after publication