Preparation method of polyamide-imide copolymer

A technology of polyamide-imide copolymer and trimellitic anhydride acid chloride, which is applied in the field of preparation of polyamide-imide, can solve the problems of product performance damage, plasticizer migration, etc., achieve short reaction time, high temperature retention rate, and easy Processing effect

Active Publication Date: 2013-04-03
SHANGHAI PLASTICS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Speaking of its shortcomings, I am worried that a small amount of plasticizer rem

Method used

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  • Preparation method of polyamide-imide copolymer
  • Preparation method of polyamide-imide copolymer
  • Preparation method of polyamide-imide copolymer

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0028] Example 1

[0029] Add 660g of N-methylpyrrolidone to a 3-liter reactor equipped with a stirrer, temperature regulator, dropping funnel and cooler, followed by 100g (0.5mol) 4,4'-diaminodiphenyl ether, 100g (0.5 mol) 3,4'-diaminodiphenyl ether and 10.8g m-phenylenediamine were stirred and dissolved at 10°C, followed by adding 211g (1.1mol) trimellitic anhydride acid chloride (TMAc), where TMAc was divided into 10 batches, each time Add 21.1g at an interval of 10 minutes, and react for 3 hours after the addition of the materials. Then add 2.3g of hydroxyphthalic anhydride, stir for 1.5 hours, the reaction is over, add 1600ml of deionized water, stir to precipitate the polymer, filter, Wash with water, filter, dry and imidize at 250°C for 2 hours, in N-methylpyrrolidone at 30°C, with a concentration of 0.5g / dl, and determine the intrinsic viscosity to be 0.65dl / g, Tg: 275°C.

[0030] According to injection molding conditions, dry at 150°C for 5 hours with a moisture content o...

Example Embodiment

[0035] Example 2

[0036] In addition to adding 120g (0.6mol) 4,4'-diaminodiphenyl ether, 80g (0.4mol) 3,4'-diaminodiphenyl ether, the polymerization temperature is 5℃, and the blocking agent hexahydrophthalic anhydride 0.9g is added, The end-capping reaction was performed for 1 hour, and the dry imidization was carried out at 230° C. for 2 hours, and the other formulations and operation steps were the same as in Example 1. Results: The intrinsic viscosity was 1.0 dl / g, the Tg was 285°C, and the performance indicators of the injection sample were the same as in Example 1.

Example Embodiment

[0037] Example 3

[0038] Except that the polymerization temperature is 25°C, 1 g of 1-methylhexahydrophthalic anhydride is added, the end-capping reaction is 2 hours, and the imidization reaction is 2 hours at 220°C, the other formulations and operation steps are the same as in Example 1. Results: The intrinsic viscosity was 0.72dl / g, Tg: 260°C. The performance indicators of the injection sample were the same as in Example 1.

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Abstract

The invention relates to a preparation method of a polyamide-imide copolymer, reacting trimellitic anhydride acyl chloride, 4,4'-diaminodiphenyl ether, 3,4'-diaminodiphenyl ether and m-phenylenediamine according to equal anhydride/amine mol ratio at 5-25 DEG C for 3 hours to prepare polyamide imide acid; and adding 0.5-3 wt% of blocking agent to react for 1-2 hours, precipitating in water, filtering, and drying at 220-250 DEG C for imidization for 3 hours to prepare the polyamide-imide copolymer. The polyamide-imide copolymer has the characteristics of high temperature resistance, low disproportionation degree, favorable flowability in machining, favorable alkali resistance and the like; the inherent viscosity is 0.5-1.0dl/g, and the Tg is 265-285 DEG C; and the properties of the injected sample piece are as follows: the tensile strength is 152 MPa, the bending strength is 241 MPa, the notched Izod impact strength is 140 J/m, the surface resistivity is 5.0*10<18> Omega, the volume resistivity is 2.0*10<17> Omega.cm, the dielectric constant (60Hz) is 4.20, the dielectric loss tangent (60Hz) is 0.026, and the heat-deformation temperature (1.8 MPa) is 278 DEG C.

Description

1. Technical field [0001] The present invention relates to a kind of preparation method of polyamide-imide, relate to a kind of preparation method of polyamide-imide copolymer more precisely. 2. Background technology [0002] Polyamide-imide (PAI) is the first industrialized injection-moldable polyimide plastic. Its thermal deformation temperature is as high as 275-280°C. It has excellent physical and mechanical properties retention under high temperature conditions; it is a candidate material to replace metals. Molded parts are widely used in the automotive, aerospace and electronics industries. [0003] Due to the high viscosity of polyamideimide at high temperature and its reactivity at high temperature, it is necessary to prevent processing by increasing the temperature and reducing the viscosity. Requires heavy-duty, high-speed injection molding machine processing, and hydraulic accumulators must be used to ensure high-speed injection. However, it is shear sensitive,...

Claims

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Application Information

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IPC IPC(8): C08G73/14
Inventor 黄慧琳胡志强
Owner SHANGHAI PLASTICS RES INST CO LTD
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