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Polyimide siloxane and carbon nanotube composite material and preparation method thereof

A technology of polyimide siloxane and nanocomposite materials, which is applied in the field of polyimide siloxane nanocomposites and its preparation, and can solve the problems of polyimide siloxane strength, stiffness, solvent resistance, size Poor stability and other issues, achieve performance improvement, improve dispersion uniformity, and simple process operation

Active Publication Date: 2013-01-16
丹阳新华美塑料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the presence of polysiloxane, the strength, stiffness, solvent resistance, and dimensional stability of polyimidesiloxane are relatively poor, so it needs to be further modified

Method used

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  • Polyimide siloxane and carbon nanotube composite material and preparation method thereof

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preparation example Construction

[0023] A preparation method of polyimide siloxane / carbon nanotube nanocomposite material, it comprises the following steps:

[0024] (1) Put the mixture of 1,3-bisaminopropyl-1,1,3,3-tetramethyldisiloxane and cyclosiloxane with a mass ratio of 1:3~15 into the reaction bottle , add 0.0001-0.1% of the total mass of the mixture of basic catalysts, inert gas protection, heat up to 80-180 ℃, react for 3-50 hours, stop the reaction, purify the sample, and obtain the terminal aminomethylphenylsiloxane alkanes prepolymers.

[0025] (2) In the reaction flask, control the ratio of total amine group and dianhydride to 1:1 to 1.3, and the ratio of amino-terminated polysiloxane prepolymer to aromatic diamine monomer is 1: 0.1~5, dissolve the amino-terminated dimethyldiphenylsiloxane prepolymer, aromatic dianhydride and aromatic diamine in o-dichlorobenzene 5 times its mass, and then and slowly adding the surface-modified carbon nanotubes to control the weight content of the carbon nanotu...

Embodiment 1

[0029] 1) Put 183g of 1,3-bisaminopropyl-1,1,3,3-tetramethyldisiloxane and hexamethylcyclotrisiloxane in a mass ratio of 1:3 into a reaction flask , add 0.032g of potassium hydroxide as a catalyst, under inert gas protection, heat up to 80°C, react for 20 hours, cool to room temperature, stop the reaction, wash with water, separate, and remove unreacted substances and small ring-shaped molecules under reduced pressure to obtain terminal The number average molecular weight of the aminomethylphenylsiloxane prepolymer measured by the end group analysis method is 850.

[0030] (2) In the reaction flask, control the ratio of total amine groups and dianhydride to 1:1, mix 708g of amino-terminated dimethyldiphenylsiloxane prepolymer, 520g of bisphenol A dianhydride and 18 g of p-phenylenediamine was dissolved in 6.23 Kg of o-dichlorobenzene, and then 1.2 g of nylon 6 graft-modified carbon nanotubes were gradually added and dispersed and mixed uniformly.

[0031] (3) The above mixtur...

Embodiment 2

[0033]1) Put 358.5g of 1,3-bisaminopropyl-1,1,3,3-tetramethyldisiloxane and hexamethylcyclotrisiloxane with a mass ratio of 1:15 into the reaction bottle , add 0.184g of potassium hydroxide as a catalyst, under inert gas protection, heat up to 150°C, react for 20 hours, cool to room temperature, stop the reaction, wash with water, separate, and remove unreacted substances and small ring-shaped molecules under reduced pressure to obtain The amino-terminated methylphenylsiloxane prepolymer has a number average molecular weight of 3500 as tested by the terminal group analysis method.

[0034] (2) In the reaction flask, control the ratio of total amine groups and dianhydride to 1:1.3, mix 105g of amino-terminated dimethyldiphenylsiloxane prepolymer, 405g of bisphenol A dianhydride and 32.4 g of p-phenylenediamine was dissolved in 1.63 Kg of o-dichlorobenzene, and then 57 g of nylon 6 graft-modified carbon nanotubes were gradually added and dispersed and mixed uniformly.

[0035] ...

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Abstract

The invention relates to a polyimide siloxane and carbon nanotube composite material and a preparation method thereof. The composite material is prepared through an in-situ blending method by using polyimide siloxane as matrixes and surface-modified carbon nanotubes as nano fillers, wherein the surface-modified carbon nanotubes are carbon nanotubes which are grafted with nylon 6 molecular chains through a surface chemical method, and the weight of the surface-modified carbon nanotubes is 0.1-20 percent of the weight of the polyimide siloxane and carbon nanotube composite material. In the composite material, the surface-modified carbon nanotubes are evenly distributed, the strength of the composite material is high, the toughness is good, and the flame retardation, the processing performance and the size stability are excellent. By adopting the in-situ blending method, since the preparation of the polyimide siloxane and the preparation of the nano composite material are completed in one step, the preparation technology of the composite material is greatly simplified and the preparation cost of the composite material is decreased.

Description

technical field [0001] The invention relates to a polyimide siloxane nanocomposite material and its preparation, in particular to a polyimide siloxane / carbon nanotube nanocomposite material and an in-situ blending preparation method thereof. Background technique [0002] Polyimide siloxane uses silicon-containing dianhydride or silicon-containing diamine as a monomer, and introduces flexible, asymmetric and side group polysiloxane chain links into the polyimide skeleton structure. The resulting polymer is a high-performance thermoplastic resin that can maintain strength without damage for a long time at high temperatures, has long-term heat resistance, has excellent processing performance and electrical properties, and has both flame retardancy and combustion properties. Less smoke and high radiation resistance. However, due to the presence of polysiloxane, the strength, stiffness, solvent resistance, and dimensional stability of polyimidesiloxane are relatively poor, so it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K9/04C08K7/00C08K3/04C08G73/10
Inventor 闫东广黄明越李世云解庆福
Owner 丹阳新华美塑料有限公司