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A kind of preparation method of highly cohesive phthalocyanine-containing polyimide resin

A phthalocyanine polyimide and high-adhesive technology, which is applied in the field of polyimide resin, can solve the problems of poor temperature resistance, poor solubility, and dispersibility of dyes, and overcome poor adhesion, Simple method, good adhesive effect

Active Publication Date: 2020-08-11
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of directly adding organic dyes has many disadvantages, such as poor temperature resistance and poor solubility of dyes; and adding inorganic pigments also has dispersibility problems

Method used

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  • A kind of preparation method of highly cohesive phthalocyanine-containing polyimide resin
  • A kind of preparation method of highly cohesive phthalocyanine-containing polyimide resin
  • A kind of preparation method of highly cohesive phthalocyanine-containing polyimide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) In a zero-degree ice-water bath, add 31.3g (50mmol) of trihydroxyphthalocyanine blue (M=Cu), 3.0616g (16mmol) of APDES and 6.25g (30mmol) of TEOS into 80mL of anhydrous THF, and mechanically stir. Slowly drop 14.5 g of deionized water, after the dropwise addition, react at zero temperature for 3 hours, then raise the temperature to 50°C for 8 hours. Distilled under reduced pressure at 55°C and 80mmHg to obtain blue powder, washed with ethanol several times to obtain aminosiloxane-modified phthalocyanine blue, the amino group content of the product was 0.5mmol / g as measured by elemental analysis.

[0036] (2) In 250mL of anhydrous NMP, sequentially add 12g of aminosiloxane-modified phthalocyanine blue in step (1), 12.4g of 1,4-di-(4-aminobenzoyloxy)benzene (ABHQ) , 17.8g of hexafluorodianhydride (6FDA), reacted at room temperature for 6h, then added 1.96g of maleic anhydride capping agent, continued to react for 5h at room temperature, added 25mL of acetic anhydride / ...

Embodiment 2

[0039] (1) In a zero-degree ice-water bath, add 25.7g (42mmol) aluminum dihydroxyphthalocyanine (M=Al), 2.87g (15mmol) APDES and 2.5g (12mmol) TEOS to 120mL anhydrous THF in turn, and stir mechanically. 10.2 g of deionized water was slowly added dropwise, and after the dropwise addition was completed, the reaction was carried out at zero temperature for 3 hours, and then the temperature was raised to 50° C. for 8 hours. Distilled under reduced pressure at 55°C and 80mmHg to obtain blue-green powder, washed with ethanol several times to obtain aminosiloxane-modified aluminum phthalocyanine, the amino group content of the product was 0.7mmol / g as measured by elemental analysis.

[0040] (2) In 250mL of anhydrous NMP, add 11.1g of aminosiloxane-modified aluminum phthalocyanine in step (1), 10.45g of bis(4-aminophenyl)-cyclohexane-1,4-bis Carboxylate (ES-C), 13.3g hexafluorodianhydride (6FDA), react at room temperature for 8h, then add 0.98g maleic anhydride capping agent, continu...

Embodiment 3

[0043] (1) In a zero-degree ice-water bath, add 22.58g (35mmol) of aluminum tetrahydroxyphthalocyanine (M=Al), 3.44g (18mmol) of APDES and 2.1g (10mmol) of TEOS into 120mL of anhydrous THF in sequence, and stir mechanically. 11.3 g of deionized water was slowly added dropwise, and after the dropwise addition was completed, the reaction was carried out at zero temperature for 3 hours, and then the temperature was raised to 50° C. for 8 hours. Distilled under reduced pressure at 55°C and 80mmHg to obtain blue-green powder, washed with ethanol several times to obtain aminosiloxane-modified aluminum phthalocyanine, the amino group content of the product was 0.9 mmol / g as measured by elemental analysis.

[0044] (2) In 250mL of anhydrous NMP, sequentially add 11.1g of aminosiloxane-modified aluminum phthalocyanine in step (2), 10.45g of bis(4-aminophenyl)-cyclohexane-1,4-di Carboxylate (ES-C), 13.3g hexafluorodianhydride (6FDA), react at room temperature for 8h, then add 0.98g maleic...

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Abstract

The invention relates to a preparation method for high-binding-property phthalocyanine-containing polyimide resin. The method comprises the following steps: synthesis of an amino siloxane-modified metal phthalocyanine, synthesis of a polyimide resin solution, and synthesis of the phthalocyanine-containing polyimide resin. The method provided by the invention is simple, and overcomes the disadvantages that the bonding property is not excellent, the chromatic light is single and the like in most conventional polyimide resin; and the prepared phthalocyanine-containing polyimide resin has good bonding property because of introduction of the siloxane and a phthalocyanine structure, and the phthalocyanine structure can change the resin spectral properties, so that the resin has richer chromaticlight selectivity, is directly used for preparation of colored polyimide films, tapes, adhesives, coatings and the like, and has bright application prospects.

Description

technical field [0001] The invention belongs to the field of polyimide resins, in particular to a preparation method of highly cohesive phthalocyanine-containing polyimide resins. Background technique [0002] Polyimide resin is a typical high-performance material, which has the characteristics of heat resistance, excellent mechanical properties, solvent resistance, radiation resistance, and good dielectric properties. It shows excellent comprehensive properties and can be used in composite materials, high temperature Filtration, military aerospace, fire protection and other technical fields. [0003] Among them, polyimide resin is widely used in the preparation of flexible copper clad laminates, and is used to prepare printed circuits and various electronic product devices. According to the preparation method and structural composition, copper clad laminates are divided into three-layer copper clad laminates and two-layer copper clad laminates. Generally speaking, three-la...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/12
CPCC08G73/125C08G73/126C08G73/128
Inventor 张清华李琇廷甘锋杨才冉董杰赵昕
Owner DONGHUA UNIV