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Method for preparing binder of polyimide of containing phenolic hydroxyl group

A technology of phenolic hydroxyl polyimide containing phenolic hydroxyl groups, which is applied in the field of chemical polymer adhesive preparation, which can solve the problems of decreased heat resistance of the adhesive system, restrictions on the use of printed circuit boards, and copper foil oxidation reactions. , to achieve the effect of improving the bonding strength, improving the oxidation resistance and reducing the curing temperature

Inactive Publication Date: 2007-07-25
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The disadvantage of this method is that due to the use of a large amount of aliphatic diamines, the heat resistance of the adhesive system is greatly reduced, and its glass transition temperature is between 150°C and 200°C, which limits the use of printed circuit boards in high temperature environments. use in
Its main disadvantage is that it needs long-term high-temperature curing at a high temperature of 350°C
This not only consumes energy, puts forward higher technical requirements for equipment, but also easily oxidizes copper foil

Method used

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  • Method for preparing binder of polyimide of containing phenolic hydroxyl group
  • Method for preparing binder of polyimide of containing phenolic hydroxyl group
  • Method for preparing binder of polyimide of containing phenolic hydroxyl group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 3.66 g (0.01 mol) of 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane (B3A4HPFP), 2.26 g (0.01 mol) of 3 , 3'-dimethyl 4,4'-diaminodiphenylmethane (DMMDA) and 5.85 grams (0.02 moles) of 1,3-bis(4-aminophenoxy)benzene (134BAPB) were added to the oil-water separation Then add 100 grams of N,N-dimethylacetamide (DMAc), stir at room temperature, make it dissolve completely, and cool in an ice-water bath To below 5°C, add 6.20 grams (0.02 moles) of 3,3',4,4'-tetracarboxylic diphenyl ether dianhydride (ODPA) and 6.44 grams (0.02 moles) of 3,3',4,4' -Tetraformic acid benzophenone dianhydride (BTDA), after stirring and reacting at 0° C. to 10° C. for 4 hours, a viscous polyhydroxyamic acid solution was obtained. Subsequently, nitrogen gas was introduced, 20 grams of toluene was added, and the temperature was raised to 120°C. After reflux and water separation for 2 hours, the heating system was turned off, stirred, and naturally cooled to room temperature to obtai...

Embodiment 2

[0034] 2.90 grams (0.01 moles) of 4,4'-diamino-4"-hydroxytriphenylmethane (DAHTM), 2.00 grams (0.01 moles) of 3,4'-diaminodiphenyl ether (34ODA), 5.18 grams (0.01 mol) 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane (4BAPOFP), 2.92 g (0.01 mol) 1,3-bis(4-aminophenoxy)benzene (134BAPB ) into the reaction flask with oil-water separator, reflux condenser, thermometer, nitrogen pipe and electric stirrer, then add 100 grams of N-methyl-2-pyrrolidone (NMP), stir at room temperature, make it completely After dissolving, cool in an ice-water bath to below 5°C, add 5.20 grams (0.01 moles) of bisphenol A diether dianhydride (BPADA), 6.44 grams (0.02 moles) of 3,3',4,4'-tetracarboxylic acid Benzophenone dianhydride (BTDA) and 2.49 grams (0.01 mole) biphenyl dianhydride (BPDA), after 8 hours of stirring reaction at 0 ℃~10 ℃, obtain the viscous polyhydroxyamic acid solution. Subsequently, Introduce nitrogen, add 60 grams of xylene, heat up to 140°C, reflux and separate water for 1 hour...

Embodiment 3

[0038] 3.66 grams (0.01 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane (B3A4HPFP), 4.10 grams (0.01 moles) of 2 , 2-bis[4-(4-aminophenoxy)phenyl]propane (BAPOPP), 2.00 g (0.01 mole) 3,4'-diaminodiphenyl ether (34ODA) and 2.00 g (0.01 mole) 4 , 4'-diaminodiphenyl ether (44ODA) was added to the reaction flask with oil-water separator, reflux condenser, thermometer, nitrogen pipe and electric stirrer, followed by adding 120 grams of N, N-dimethyl formaldehyde Amide (DMF), stirred at room temperature, after making it completely dissolved, cooled in an ice-water bath to below 5°C, and added 9.30 grams (0.03 moles) of 3,3',4,4'-tetracarboxylic diphenyl ether dianhydride ( ODPA) and 3.22 grams (0.01 mole) of 3,3',4,4'-tetracarboxylic acid benzophenone dianhydride (BTDA), after stirring and reacting at 0°C to 10°C for 6 hours, a viscous poly Hydroxyamic acid solution. Subsequently, nitrogen gas was introduced, 20 grams of toluene was added, the temperature ...

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Abstract

This invention discloses a method for preparing phenolic hydroxyl-containing polyimide adhesive. The method comprises: (1) reacting phenolic hydroxyl-containing aromatic diamine, or its mixture with other aromatic diamines, with aromatic dianhydride at a mol ratio of 1:1 in strongly polar non-proton organic solvent at 0-10 deg.C for 4-8 h to obtain uniform, transparent and viscose polyhydroxyamic acid solution; (2) adding azeotropic dehydrator in nitrogen atmosphere, heating, performing imidization reaction under refluxing and dehydration at 120-160 deg.C for 1-6 h, and cooling to room temperature to obtain phenolic hydroxyl-containing polyimide adhesive. The volume ratio of azeotropic dehydrator to strongly polar non-proton organic solvent is 1 :( 1-5). The method has such advantages as easy operation, no special requirement for equipment, and high product quality. The phenolic hydroxyl-containing polyimide adhesive has such advantages as short adhesion and curing time, low energy consumption, and high adhesiveness to copper foil and polyimide thin film, and can be used to produce bi-layer flexible printed circuit boards.

Description

technical field [0001] The invention belongs to the field of preparation methods of chemical polymer adhesives, in particular to a preparation method of polyimide adhesives containing phenolic hydroxyl groups. Background technique [0002] Polyimide is a class of polymers with excellent comprehensive properties. It has excellent heat resistance, low temperature resistance, solvent resistance, self-lubrication, radiation resistance and flame retardancy. At the same time, it also has very good mechanical and dielectric properties. Therefore, it is widely used in high-temperature and radiation-resistant materials such as spacecraft, satellites or space vehicles; advanced structural composite materials in aerospace, automotive, electromechanical, etc., C-level or 200-level electrical insulation materials, high-temperature resistant adhesives etc.; and FPC or PCB base materials in the field of electronic microelectronics, IC interlayer insulation materials, VLSI passivation coat...

Claims

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Application Information

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IPC IPC(8): C09J179/08
Inventor 虞鑫海徐永芬赵炯心
Owner DONGHUA UNIV
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