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Preparation method of polyaryletherketone resin

A polyaryletherketone and resin technology is applied in the field of preparation of polyaryletherketone resin, which can solve the problems of difficult characterization of polymer molecular weight, difficult control of process conditions, fast reaction rate, etc., and achieves reduced characterization difficulty and strong controllability. , molecular weight easy effect

Inactive Publication Date: 2020-11-03
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing nucleophilic polycondensation process generally has the following defects: 1) In order to avoid polymer crystallization, the polymerization reaction is usually carried out in a high-boiling solvent at a relatively high temperature, and the energy consumption is high; 2) The reaction rate is fast at high temperature , It is difficult to control the process conditions, 3) Since polyaryletherketone is often crystalline and difficult to dissolve in conventional solvents, it is difficult to characterize the molecular weight of the polymer, and most of them use viscosity as the distinction between batches

Method used

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  • Preparation method of polyaryletherketone resin
  • Preparation method of polyaryletherketone resin
  • Preparation method of polyaryletherketone resin

Examples

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preparation example Construction

[0046] The invention provides a preparation method of polyaryletherketone resin, which comprises the following steps:

[0047] a) Under the action of an alkali catalyst, the dihalogen monomer of the structure represented by formula (i), the ketal diphenol monomer of the structure represented by formula (ii) and the copolymerized aromatic diphenol monomer of the structure represented by formula (iii) Carry out nucleophilic polycondensation in an organic solvent to obtain a ketal polymer of the structure represented by formula (I);

[0048] b) acidifying the ketal polymer in an acid solution to obtain a polyaryl ether ketone resin having a structure represented by formula (II);

[0049] X-Q-X formula (i); HO-R 3 -OH formula (iii);

[0050]

[0051] Wherein, Q is selected from one or more of the following substituents:

[0052]

[0053] X represents halogen, preferably -F or -Cl;

[0054] R 1 One or more of the following substituents:

[0055]

[0056] R 2 Selected from -CH 3 , -C 2 H 5 , ...

Embodiment 1

[0077] Choose The ketal bisphenol monomer (2,2-bis(4-hydroxyphenyl)-1,3-dioxolane) with m=1 and 4,4'-difluorobenzophenone were used for polycondensation to prepare polyarylene Ether ketone resin, the specific method is as follows:

[0078] Mix 25.83g (0.1mol) 2,2-bis(4-hydroxyphenyl)-1,3-dioxolane, 21.82g (0.1mol) 4,4'-difluorobenzophenone and 28.9g( 0.21mol) potassium carbonate was added to a three-necked flask with nitrogen protection, mechanical stirring, water separator and condenser, then added 100mL dimethyl sulfoxide and 50mL toluene, heated to 150℃, toluene refluxed with water for 6h, distilled After toluene was heated to 180°C for nucleophilic polycondensation, 300mL dimethyl sulfoxide was added to dilute after polycondensation for 2 hours, and the supernatant was settled into deionized water after centrifugation to obtain the crude ketal polymer. Such as Figure 1~2 Shown.

[0079] The crude ketal polymer prepared above was crushed and then acidified by boiling in 2mo...

Embodiment 2

[0084] With reference to the preparation method of Example 1, the difference is only that the polycondensation time is extended from "2h" to "4h" to prepare the polyaryletherketone resin.

[0085] GPC test was performed on the polyaryl ether ketone resin prepared in this example, and the result showed that the weight average molecular weight of the polymer was about 38000 (corresponding to n=96).

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Abstract

The invention belongs to the field of high polymer materials, and particularly relates to a preparation method of polyaryletherketone resin, which comprises the following steps: a) under the action ofan alkali catalyst, carrying out nucleophilic polycondensation on a dihalide monomer with a structure shown in a formula (i), a ketal diphenol monomer with a structure shown in a formula (ii) and a copolymerized aromatic diphenol monomer with a structure shown in a formula (iii) in an organic solvent to obtain a ketal polymer with the structure shown in the formula (I); and b) acidifying the ketal polymer in an acid solution to obtain the polyaryletherketone resin with the structure shown in the formula (II). The preparation method provided by the invention has the advantages of mild preparation conditions, low energy consumption, strong controllability and easy characterization of molecular weight. The formula (i) is X-Q-X; the formula (ii) is shown in the specification; the formula (iii) is HO-R3-OH; and the formula (I) and the formula (II) are shown in the specification.

Description

Technical field [0001] The invention belongs to the field of polymer materials, and particularly relates to a preparation method of polyaryletherketone resin. Background technique [0002] As a semi-crystalline polymer material, polyaryl ether ketone has the advantages of good strength, high modulus, high temperature steam resistance, solvent resistance, acid and alkali resistance, flame retardancy, etc. Therefore, as a special engineering plastic, polyaryl ether ketone has broad application prospects and extremely high commercial value in the fields of medical and health, electronic devices, aerospace, automobile manufacturing, petroleum industry, and nuclear energy. [0003] Polyaryl ether ketone polymers contain benzene ring, ether group and ketone group in the main chain of the molecule. According to the number and order of the ether group and ketone group in the repeating unit on the main chain of the molecule, it can be divided into polyether ketone (PEK) and polyether ketone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40C08G65/48
CPCC08G65/4012C08G65/405C08G65/48
Inventor 张所波孙宇轩
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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