Preparation method of soluble polyimide resin

A soluble polyimide and polyimide technology, applied in the field of polyimide materials, can solve the problems of difficult drying and collection of flocculent resin, unfavorable industrial continuous production, incomplete cleaning, etc., and achieve good safety and industrial applicability, easy washing and drying, and less residue effect

Active Publication Date: 2015-06-17
长春聚明光电材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the above method for removing solvents and other substances is cumbersome, the cleaning is not thorough, and the irregular flocculent resin precipitated is not easy to dry and collect, and the resin yield is low, so it is not conducive to industrial continuous production

Method used

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  • Preparation method of soluble polyimide resin
  • Preparation method of soluble polyimide resin
  • Preparation method of soluble polyimide resin

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preparation example Construction

[0025] The embodiment of the present invention discloses a preparation method of a soluble polyimide resin, comprising the following steps:

[0026] (A) polyimide solution is subjected to vacuum defoaming treatment;

[0027] (B) continuously extruding the polyimide solution after the vacuum defoaming treatment in a polar solvent to obtain a tow-shaped resin with a diameter of 0.01 to 0.05 mm;

[0028] (C) washing the tow-shaped resin with water and drying to obtain a finished product of soluble polyimide resin.

[0029] In the present invention, it mainly relates to a method for obtaining a polyimide resin through processing a polyimide solution. According to the present invention, the source of the polyimide solution is not particularly limited, any polyimide solution that is obtained through polymerization well known to those skilled in the art and used to prepare soluble polyimide resins can be prepared by itself , You can also buy commercially available products.

[003...

Embodiment 1

[0039] A polyimide solution prepared by a high-temperature solution polymerization method is provided, and the polyimide solution is 3,3'-dimethyl-4,4'-diaminodiphenylmethane ( DMMDA) and 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA) are polymerized in phenol by heating at 180°C, and the apparent viscosity of the polyimide solution is 12000cp.

[0040] The polyimide solution was vacuum defoamed for 12 hours, the temperature of the solution was 25°C, and after filtration, it was poured into the resin former through a metering pump. The polyimide solution passes through the small holes and continuously separates out the tow-shaped resin in the precipitation tank. The precipitation tank is a mixed solvent of ethanol and DMAc, with a flow rate of 10m / min; the filamentous resin is washed at 80°C for 5 minutes at a speed of 2m / min, and washed with water at 25°C for 5min; the filamentous resin is washed at a speed of 2m / min After drying at 140° C. for 5 minutes and at 160° C. f...

Embodiment 2

[0056] Provides a polyimide solution prepared by chemical imidization, the polyimide solution is made of 1,4-bis(4-aminophenoxy)benzene (APB) in a molar ratio of 0.3:0.7:1 , 3,3'-diamino-4,4'-diaminodiphenylmethane (DMMDA) and 3,3',4,4'-diphenyl ether dianhydride (ODPA) in N,N-dimethylmethane Polymerization in amide (DMF) obtains, and the imide catalyst and the dehydrating agent adopted in the polymerization process are acetic anhydride and triethylamine respectively, and wherein the mol ratio of ODPA and acetic anhydride, triethylamine is 1:2:1; The described The apparent viscosity of the polyimide solution was 155000 cp.

[0057] The polyimide solution was vacuum defoamed for 12 hours, and the solution temperature was 25°C. After filtering, it was injected into the resin former through a metering pump. The polyimide solution passes through the small holes and continuously separates out the tow-shaped resin in the precipitation tank. The precipitation tank is a mixed solven...

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Abstract

The invention provides a preparation method of soluble polyimide resin. The preparation method comprises the following steps: performing vacuum defoamation treatment on a polyimide solution; continuously extruding the polyimide solution after the vacuum defoamation treatment in a polar solvent, so as to obtain tow-shaped resin with a diameter of 0.01-0.05 mm; washing the tow-shaped resin with water and drying, so as to obtain a finished product of the soluble polyimide resin. According to the preparation method disclosed by the invention, the polyimide solution is not required to be diluted but directly extruded and molded to form the tow-shaped resin, so that the usage of an organic solvent can be reduced, the follow-up water washing and drying can be convenient, and the residues of an organic reagent and an inorganic salt can be less; secondly, the preparation method can be used for implementing continuous production, and the resin is high in yield and good in safety and industrial application; furthermore, as for the soluble polyimide resin for preparing a colorless transparent polyimide material, the preparation method ensures that the resin is thoroughly cleaned and the solvent is removed cleanly, so that the thin film prepared by the resin is higher in light transmittance.

Description

technical field [0001] The invention relates to the field of polyimide materials, in particular to a preparation method of soluble polyimide resin. Background technique [0002] Soluble polyimide resin is a polymer obtained by changing the main chain of ordinary insoluble polyimide. Compared with ordinary polyimide, it not only has excellent chemical stability, thermal stability and mechanical performance, but also solubility. The discovery of soluble polyimide resin has expanded the application field of polyimide. In the field of optical communication, soluble polyimide resin can be used as optical waveguide material (waveguide), photoelectric packaging material, second-order nonlinear optical material (NLO), photorefractive material (photorefractive), photosensitive material (photosensitive) And photoelectric materials (electro-optic), etc. In these fields of application, polyimide resins are particularly required to have good solubility and excellent optical transparen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/00C08L79/08
Inventor 付饶刘洋许杨张海洋靳野郭百灵
Owner 长春聚明光电材料有限公司
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