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Preparation method of aromatic polyamic acid with characteristics of high relative molecular mass and narrow molecular weight distribution

A technology with narrow relative molecular weight and molecular weight distribution, which is applied in the field of polyamic acid preparation, can solve the problems that have not yet been published in literature or patent reports, and achieve the effects of preventing degradation, good performance and low investment cost

Active Publication Date: 2015-12-23
无锡高拓新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] A method for preparing aromatic polyamic acid with high relative molecular weight and narrow molecular weight distribution disclosed by the present invention has not been published in literature or patent reports

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At room temperature, put 40.00 kilograms (200 moles) of 4,4-diaminodiphenyl ether and 325.68 kilograms of dried N,N-dimethylacetamide into the reactor and stir, and add 41.42 kilograms ( 190 mol) of pyromellitic dianhydride was reacted in a temperature range of 40° C. for about 3 hours to obtain a polyamic acid oligomer solution containing 20% ​​by weight, and the bubbles in the solution were left to stand still.

[0030] Add 20.00 kg of dried N,N-dimethylacetamide and 22.61 kg of dimethyl sulfoxide into the dissolution kettle, add 2.18 kg (10 moles) of pyromellitic dianhydride under stirring at room temperature, and fully dissolve to obtain 4.87% by weight dianhydride solution.

[0031] Through the metering pump, the polyamic acid prepolymer is fed into the front inlet of the twin-screw mixing extruder at a flow rate of 454.5 grams per minute, and the dianhydride solution is simultaneously input at a flow rate of 50.0 grams per minute to achieve the flow rate of dianhy...

Embodiment 2

[0036] At room temperature, add 30.00 kg (150 moles) of 4,4'-diaminodiphenyl ether and 328.00 kg of dried N,N-dimethylacetamide into the reactor, stir, and add 31.72 kg ( 145.5 moles) of pyromellitic dianhydride was reacted in a temperature range of 30°C for 3 hours to obtain a polyamic acid prepolymer solution containing 15.84% by weight, which was allowed to stand still for defoaming.

[0037] Add 27.00 kg of dried dimethyl sulfoxide into the dissolution tank, add 0.98 kg (4.5 moles) of pyromellitic dianhydride with stirring at room temperature, and fully dissolve to obtain a dianhydride solution containing 3.5% by weight.

[0038] Through the metering pump, the polyamic acid prepolymer is fed into the front inlet of the twin-screw extruder at a flow rate of 417.8 grams per minute, and the dianhydride solution is fed into the front inlet of the twin-screw extruder at a flow rate of 30.0 grams per minute to achieve equimolar polymerization of dianhydride and diamine reaction ...

Embodiment 3

[0044] Add 240.00 kg (120 moles) of 4,4-diaminodiphenyl ether, 4.32 kg (40 moles) of 1,4-diaminobenzene and 232.00 kg of dried N,N-dimethylacetamide to the reaction kettle at room temperature Stir in medium, dissolve completely, continuously add 33.35 kilograms (153 moles) of pyromellitic dianhydride, react in 40 ℃ of temperature ranges for 3 hours, make the polyamic acid prepolymer solution containing 21% by weight, let it stand for defoaming .

[0045] At room temperature, add 20.80 kg of dried dimethyl sulfoxide into the dissolution tank, stir and add 1.53 kg (7 moles) of pyromellitic dianhydride, fully dissolve and prepare a 6.85% by weight dianhydride solution.

[0046] Through the metering pump, the polyamic acid prepolymer is fed into the twin-screw extruder at the flow rate of 526.0 grams per minute, and the dianhydride solution is simultaneously input into the twin-screw extruder at the flow rate of 40.0 grams per minute, and the diamine and the dianhydride are equimo...

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Abstract

The present invention discloses a preparation method of an aromatic polyamic acid with characteristics of high relative molecular mass and narrow molecular weight distribution. According to the preparation method, a low molecule prepolymer solution of an aromatic polyamic acid and an aromatic diacid anhydride solution are concurrently conveyed into a co-rotating twin-screw mixing extruder so as to be subjected to an equal equivalence synthesis reaction, wherein an aromatic dianhydride and an aromatic diamine react in a strongly-polar non-protonic organic solvent according to a molar ratio of 0.90-0.98:1 to prepare the low molecule prepolymer solution of the aromatic polyamic acid. With the method of the present invention, the polyamic acid resin with the characteristics of high relative molecular mass and narrow molecular weight distribution can be obtained so as to obtain the high-quality polyimide film.

Description

technical field [0001] The invention belongs to the field of polyamic acid synthesis, in particular to a method for preparing aromatic polyamic acid with high relative molecular weight and narrow molecular weight distribution. Background technique [0002] Polyamic acid is the precursor of polyimide. Taking advantage of the ease of processing of polyamic acid, it is the main method of producing polyimide film in China after it is salivated into a film and then heated and cyclized. The polyamic acid solution prepared by the polycondensation reaction of aromatic tetra-acid dianhydride and aromatic dibasic primary amine, because the unavoidable trace moisture in the reaction system will promote the hydrolysis of polyamic acid, so that its molecular weight will decrease and decrease with time. The extension of time increases, which in turn affects the performance of polyimide products. [0003] In industrial production, in order to obtain polyamic acid with high relative molecu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08
Inventor 沈国强
Owner 无锡高拓新材料股份有限公司
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