Method for preparing flame-retardant thermoplastic polyimide resin

A polyimide and polyesterimide technology, applied in the field of preparation of high-performance flame-retardant thermoplastic polyimide resin, can solve the problems of poor compatibility, deteriorated mechanical properties and electrical properties of materials, etc. The effect of good capacitance, high industrial application value and good compatibility

Active Publication Date: 2014-02-05
宏威高新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the addition of these metal compounds can improve the flame retardancy, their compatibility with TPI is poor, which will deteriorate the mechanical and electrical properties of the material to a certain extent.

Method used

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  • Method for preparing flame-retardant thermoplastic polyimide resin
  • Method for preparing flame-retardant thermoplastic polyimide resin
  • Method for preparing flame-retardant thermoplastic polyimide resin

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preparation example Construction

[0042] A preparation method of flame-retardant thermoplastic polyimide resin, comprising the following steps:

[0043] A. Preparation of Phosphorus-Silicon Synergistic Flame Retardant Thermotropic Liquid Crystalline Polyesterimide

[0044](1) With p-hydroxymethylbenzoic acid as mesogen, PEtI-TLCP is formed by copolymerization of dichlorobisphthalimide, hydroxy acid, phosphorus-containing and silicon-containing monomers; its basic segment structure is as follows :

[0045]

[0046] where R is C 1 -C 3 chain alkyl, R 1 are the same or different methyl, ethyl, and phenyl groups, x is 8-12, y is 5-10, and z is 1-3. T selected from:

[0047]

[0048] (2) The molar percentage of hydroxy acid in the present invention is 30-40%, the molar percentage of said hydroxy acid is 30-35%, the molar percentage of dichlorobisphthalimide is 35-40%, and the phosphorus-containing mono The molar ratio of bulk DOPO and its derivatives to dihydroxysiloxane is 1:3-3:1. Add the above-menti...

Embodiment 1

[0067] (1) Preparation of phosphorus-silicon synergistic flame-retardant thermotropic liquid crystal polyesterimide

[0068] Stirring at a speed of 60-120 rpm, mix 3000mol p-hydroxybenzoic acid (p-HBA), 3500mol dichlorobisphthalimide, 1000mol DOPO, chlorosiloxane containing 2500mol hydroxyl equivalent, 0.4 Add kg esterification catalyst antimony acetate and 0.5 kg polycondensation catalyst antimony trioxide to the reactor with fractionation condenser strong stirrer nitrogen conduit at one time, stir and mix for 10-20 minutes, heat to 180°C for reaction, under nitrogen protection, The by-products formed are carried out with nitrogen. As the viscosity of the reaction system gradually increased, a "rod climbing" phenomenon (indicating the formation of a liquid crystal phase) appeared. The reaction temperature was gradually increased to 290°C, the vacuum was pumped to above 100Pa, and the reaction was carried out for 30 minutes. A light brown solid product was obtained through tr...

Embodiment 2

[0076] The processing parameter of embodiment 2 is exactly the same as embodiment 1, and difference is that the phosphorus silicon flame-retardant type polyester imide liquid crystal (PEtI-TLCP-I) addition amount prepared by embodiment 1 is 40% (by mass percentage) ) mixed with thermoplastic polyimide 60%, the performance test results of the prepared materials are listed in Table 1.

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Abstract

The invention discloses a flame-retardant thermoplastic polyimide resin. The method comprises the following steps: (1) introducing a monomer which has a flame-retardant effect and contains a DOPO and siloxane structure and synthesizing thermotropic liquid crystal polyester-imide PEtI-TLCP which has flame retardant property and liquid crystal characteristics and has a chemical structure similar to thermoplastic polyimide; and (2) performing in-situ synthesis on the prepared PEtI-TLCP and the thermoplastic polyimide (TPI), thus obtaining the flame-retardant thermoplastic polyimide resin. The method can be suitable for a process for producing a high-performance flame-retardant thermoplastic polyimide resin in a severe environment. The prepared flame-retardant thermoplastic polyimide resin has excellent mechanical property, thermal performance, processability, flame-retardant property and resistance to heat and humidity, can be used for preparing high-temperature protective textiles and special electrical insulation films and has extremely high commercial value.

Description

technical field [0001] The invention belongs to the flame-retardant field of polymer materials, and in particular relates to a preparation method of a high-performance flame-retardant thermoplastic polyimide resin suitable for harsh environments. The high-performance polyimide resin prepared by the invention can be used to spin high-temperature-resistant non-combustible fibers required for high-temperature protective products or to prepare special high-temperature-resistant non-combustible electrical insulating films through biaxial stretching. Background technique [0002] Polyimide refers to a class of aromatic heterocyclic polymers containing imide rings in the main chain. It is widely used for its excellent mechanical, dielectric, radiation resistance, and corrosion resistance at high temperatures. In addition, it is a self-extinguishing material, which can meet the flame retardant requirements of most fields. However, the application in special fields such as high-temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/16C08L79/08
Inventor 阳龑李晓敏黄渝鸿袁彬彬黄小诚李旺曹君李涛杨帆陈凤韩青霞
Owner 宏威高新材料有限公司
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