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Bio-based semi-aromatic polyamide and its synthesis method

A semi-aromatic and synthetic method technology, applied in the field of materials, can solve the problems of restricting the large-scale promotion of solid-phase polymerization, accelerating the discharge of small molecules of by-products, and many solid-phase polymerization production processes, so as to achieve excellent processing performance, increase productivity, The effect of reducing the process

Active Publication Date: 2017-10-10
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since solid-phase polymerization is generally carried out at 15-30°C below the melting point of the prepolymer, the reaction rate is slow and the reaction time is long, and the production process of solid-phase polymerization is complicated and the process is complicated. The requirements for equipment parameters are high, and the reaction is slow. It is necessary to ensure that the ratio of functional groups is close to 1:1, and the viscosity-increasing stage requires vacuum or air flow to accelerate the discharge of small molecules of by-products, thereby increasing the molecular weight of polycondensation products. Therefore, the above conditions limit the large-scale promotion of solid-phase polymerization

Method used

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  • Bio-based semi-aromatic polyamide and its synthesis method
  • Bio-based semi-aromatic polyamide and its synthesis method
  • Bio-based semi-aromatic polyamide and its synthesis method

Examples

Experimental program
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Effect test

Embodiment 1

[0076] The raw material composition and synthetic steps of the polyester amide used in the present embodiment are as follows:

[0077] (1) Vacuum-dried monomer 2: 1006.6g (5mol) 11-aminoundecanoic acid, 456.6g (4mol) 6-caprolactone, 270.3g (1.25mol) 2,2'-(1,3 -Phenylene)-bisoxazoline was added to the stirred polymerization reactor, and tetrabutyl titanate (17.3 g) of 1% of the total weight of monomer 2 was added as a catalyst, and 500 mL of water was added as a mass transfer and heat transfer Then vacuumize for 5 minutes, pass nitrogen for 5 minutes, and circulate like this for 6 times, so that the reactant exists in the environment under nitrogen protection, and the system pressure in the stirred polymerization reactor is controlled to be 0.2MPa;

[0078] (2) within 2.5 hours, heat the stirred polymerization reactor to 250°C at a uniform speed, and adjust the stirring speed of the stirred polymerization reactor to 40r / min, wherein, when the temperature of the stirred polymeri...

Embodiment 2

[0083] The raw material composition and synthesis steps of the polyester amide used in this example are the same as those in Example 1.

[0084] A synthetic method of a bio-based semi-aromatic polyamide in this embodiment comprises the following steps:

[0085] (1) Vacuum-dried monomer 1: 172.3g (1mol) decanediamine, 116.3g (0.7mol) terephthalic acid, 60.7g (0.3mol) sebacic acid were added to the stirred polymerization reactor, 8% (27.9g) of polyesteramide, 8% (27.9g) of organic montmorillonite, 3% (10.5g) of benzoic acid, 0.3% (1.0g) of N,N `-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phthalamide, add 100mL water as the medium for mass transfer and heat transfer; then vacuumize for 5min, and nitrogen for 5min , so circulated 6 times, so that the reactant exists in the environment under the protection of nitrogen, and the system pressure in the control stirred polymerization reactor is 0.2MPa;

[0086] (2) within 2 hours, heat the stirred polymerization reactor to 270°C at a...

Embodiment 3

[0088] The raw material composition and synthesis steps of the polyester amide used in this example are the same as those in Example 1.

[0089] A synthetic method of a bio-based semi-aromatic polyamide in this embodiment comprises the following steps:

[0090] (1) Vacuum-dried monomer 1: 172.3g (1mol) decanediamine, 149.5g (0.9mol) terephthalic acid, 20.2g (0.1mol) sebacic acid were added to the stirred polymerization reactor, 2% (6.8g) of polyesteramide, 0.5% (1.7g) of organic montmorillonite, 0.5% (1.7g) of benzoic acid, 0.2% (0.7g) of N,N `-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phthalamide, add 100mL water as the medium for mass transfer and heat transfer; then vacuumize for 5min, and nitrogen for 5min , so circulated 6 times, so that the reactant exists in the environment under the protection of nitrogen, and the system pressure in the control stirred polymerization reactor is 0.3MPa;

[0091] (2) within 3.5 hours, heat the stirred polymerization reactor to 280°C a...

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Abstract

The invention relates to a bio-based semi-aromatic polyamide and a synthesis method thereof. The bio-based semi-aromatic polyamide has the following structure of formula I: in formula I, a=10-100, b=10-200, c=10-100, d=10-100, and R is polyester amide. The bio-based semi-aromatic polyamide of the present invention has high mechanical properties and heat resistance, low water absorption, excellent processing performance and the characteristics of biological origin, and can be applied to the fields of electronic appliances, LED, automobile, aerospace and other fields. military field, etc.

Description

technical field [0001] The invention relates to the field of materials, in particular to a bio-based semi-aromatic polyamide and a synthesis method thereof. Background technique [0002] In recent years, in order to meet the higher performance requirements in the fields of electronics, electrical appliances, automobiles, etc., especially with the development of Surface Mount Technology (SMT), the common high-temperature-resistant engineering plastic polyphenylene sulfide (PPS ) and liquid crystal polymer (LCP) can no longer fully meet their requirements, so it is necessary to develop engineering plastics with higher heat resistance. [0003] Semi-aromatic polyamides are usually prepared by polycondensation of aliphatic diamines or diacids and diacids or diamines with aromatic rings. Due to the introduction of aromatic rings into the main chain of the polyamide molecule, its heat resistance And the mechanical properties have been improved, and the water absorption rate has b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/28C08G69/44C08G69/48C08K3/34C08K5/3435
Inventor 胡国胜王忠强张静婷石哲平师文博方春晖刘冰肖许和伟
Owner ZHONGBEI UNIV
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