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A kind of high molecular weight high temperature resistant polyamide resin and its preparation method

A polyamide resin, high molecular weight technology, applied in the field of polyamide resin, can solve the problems of high price, high cost of PA46, inability to produce, etc., and achieves the effects of good crystallinity, simple preparation process and excellent heat resistance.

Active Publication Date: 2017-09-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the production of butyldiamine is monopolized by a small number of multinational companies, there is no domestic manufacturer, resulting in the domestic market with almost no supply of butyldiamine and production cannot be produced; the price of butyldiamine is high, resulting in high cost of PA46. greatly limit its wide application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 800ml and 116.2g of hexamethylenediamine to a 2L four-neck round bottom flask equipped with a mechanical stirrer and a condenser tube, and replace nitrogen 3 times. After heating to 60°C, 146 g of dimethyl succinate was added dropwise through a constant pressure funnel under stirring and nitrogen flow; thereafter, the temperature was raised to reflux of toluene and refluxed for 4 hours; subsequently, 59 mg of CuI was added and toluene was distilled out, and the pressure was gradually reduced After reaching 500-100Pa, it was gradually heated to 315°C and polymerized in a molten state for 2 hours, and cooled to obtain 197g of light yellow PA64 product.

[0035] Its relative viscosity was determined to be 2.1, and its melting point was 289°C. The product was dissolved in deuterated sulfuric acid at room temperature, 1 H-NMR confirmed the presence of methyl ester end groups (its CH 3 The peak area of ​​the CH in the succinic acid unit is about 2 CH 2 0.4% of peak ar...

Embodiment 2

[0037] Add 800ml and 116.2g of hexamethylenediamine to a 2L four-neck round bottom flask equipped with a mechanical stirrer and a condenser tube, and replace nitrogen 3 times. After heating to 80°C, 146 g of dimethyl succinate was added dropwise through a constant pressure funnel under stirring and nitrogen flow; then, the temperature was raised to reflux of toluene and refluxed for 4 hours; subsequently, 594 mg of CuI was added and toluene was distilled off to obtain a prepolymer 196g; put the prepolymer into the solid phase polymerization tube, gradually reduce the pressure to 200-100Pa, then heat from room temperature to 170, 200, 230, 260°C and polymerize at each temperature for 30 minutes, and finally raise the temperature to 280°C and Solid state polymerization was carried out at 280° C. for 4 hours, and 186 g was obtained by cooling.

[0038] Its relative viscosity was determined to be 2.7, and its melting point was 302°C. The product was dissolved in deuterated sulfur...

Embodiment 3

[0040] After adding 116.2 g of hexamethylenediamine to a 1L four-neck round-bottom flask equipped with a mechanical stirrer and a condenser tube, nitrogen was replaced three times. After heating to 70°C, under stirring and nitrogen flow, 174g of diethyl succinate was dropped through a constant pressure funnel; then, 1200mg of CuI was added, gradually heated to 315°C and polymerized in a molten state for 4 hours, and cooled to obtain 192g of yellow PA64 product.

[0041] Its relative viscosity was determined to be 3.1, and its melting point was 301°C.

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Abstract

The invention discloses a high molecular weight high temperature resistant polyamide resin and a preparation method thereof. The main chain of the polyamide resin contains succinic acid units; the concentration of the polyamide resin prepared with 96wt% sulfuric acid as a solvent is 1.0g / dl, and the relative viscosity at 25°C is 1.5-6.0; The melting point of the polyamide resin is above 280°C. The preparation method is as follows: polyamide resin is prepared by solution polymerization at 20-200°C in a monomer system containing succinate, or at 100-350°C by melt polymerization. The invention has the characteristics of good crystallization performance, excellent heat resistance, etc., has a simple preparation process, and can be widely used in various fields of automobiles and electronic appliances.

Description

technical field [0001] The invention relates to a polyamide resin, in particular to a high molecular weight polyamide resin containing succinic acid units and a preparation method thereof. Background technique [0002] Since DuPont developed polyamide (commonly known as nylon, hereinafter referred to as PA) in 1939, it has a history of more than 70 years. During this period, nylon developed from the initial fiber to other fields. Especially in the second half of the last century, nylon was widely used to replace metal due to its high strength, good toughness, and wear resistance, and was processed into wear-resistant and high-strength parts, such as turbines, gears, bearings, etc. With the great increase in its demand, PA6, PA66, PA11, PA12, PA610, PA612, MXD6 and other nylons have come out one after another, thus making nylon materials occupy an important position in engineering plastics. [0003] In the past 30 years, due to the miniaturization and high-performance requi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/26C08G69/28
Inventor 赵国欣何勇郑楚昱钱瑞伟沈愉峰朱波
Owner DONGHUA UNIV