Semi-aromatic polyamide and synthesis method thereof

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 by-product small molecules, 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: 2016-02-24
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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  • Semi-aromatic polyamide and synthesis method thereof
  • Semi-aromatic polyamide and synthesis method thereof
  • Semi-aromatic polyamide and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0073] The raw material composition and synthesis steps of the polyester amide used in this embodiment are as follows:

[0074] (1) The monomer after vacuum drying 2: 1006.6g (5mol) 11-aminoundecanoic acid, 456.6g (4mol) 6-caprolactone, 270.3g (1.25mol) 2,2'-(1,3 -Phenylene)-Dioxazoline was added to the stirred polymerization reactor, while adding 1% of the total weight of monomer 2 to tetrabutyl titanate (17.3g) as a catalyst, and 500mL of water as mass transfer and heat transfer The medium; then vacuum for 5min, nitrogen gas for 5min, so cycle 6 times, so that the reactants exist in the environment under the protection of nitrogen, control the system pressure in the stirred polymerization reactor to 0.2MPa;

[0075] (2) In 2.5 hours, heat the agitated polymerization reactor to 250℃ in an airtight manner and adjust the stirring speed of the agitated polymerization reactor to 40r / min. When the temperature of the agitated polymerization reactor reaches 210℃, vent gas To 1.6MPa, and...

Embodiment 2

[0080] The raw material composition and synthesis steps of the polyester amide used in this example are the same as those in Example 1.

[0081] The method for synthesizing semi-aromatic polyamide in this embodiment includes the following steps:

[0082] (1) Add the vacuum-dried monomer 1:172.3g (1mol) decane diamine, 166.1g (1mol) terephthalic acid, 40.3g (0.2mol) 11-aminoundecanoic acid into the stirred polymerization reactor Add 8% (30.3g) of polyester amide, 8% (30.3g) of organic montmorillonite, 3% (11.4g) of benzoic acid, and 0.3% (1.1g) of N ,N`-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phthalamide, add 100mL water as the mass and heat transfer medium; then vacuum for 5min, pass Nitrogen for 5 minutes, circulate 6 times in this way so that the stirred polymerization reactor exists in an environment protected by nitrogen, and the system pressure in the stirred polymerization reactor is controlled to 0.2 MPa;

[0083] (2) Within 2 hours, heat the stirred polymerization reacto...

Embodiment 3

[0085] The raw material composition and synthesis steps of the polyester amide used in this example are the same as those in Example 1.

[0086] The method for synthesizing semi-aromatic polyamide in this embodiment includes the following steps:

[0087] (1) Add the vacuum-dried monomer 1:172.3g (1mol) decanediamine, 166.1g (1mol) terephthalic acid, 20.1g (0.1mol) 11-aminoundecanoic acid into the stirred polymerization reactor Add 2% (7.2g) of polyester amide, 0.5% (1.8g) of organic montmorillonite, 0.5% (1.8g) of benzoic acid, and 0.2% (0.7g) of N ,N`-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phthalamide, add 100mL water as the mass and heat transfer medium; then vacuum for 5min, pass Nitrogen is applied for 5 minutes and circulates 6 times in this way, so that the reactants exist in the environment under the protection of nitrogen, and the system pressure in the stirred polymerization reactor is controlled to 0.3MPa;

[0088] (2) In 3.5 hours, heat the stirred polymerization rea...

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Abstract

The invention relates to semi-aromatic polyamide and a synthesis method thereof. The semi-aromatic polyamide has the structure shown in the formula I (shown in the description); in the formula I, a is equal to 10-200, b is equal to 10-200, c is equal to 10-100 and R is polyesteramide. The semi-aromatic polyamide has a relatively high mechanical property, relatively high heat resistance, low water absorption, excellent processability and biologically-derived characteristics, and can be applied to the fields of electronics and electrical appliances, LEDs, automobiles, aerospace, military and the like.

Description

Technical field [0001] The invention relates to the field of materials, in particular to semi-aromatic polyamides and their synthesis methods. Background technique [0002] In recent years, in order to meet higher performance requirements in the fields of electronics, electrical appliances, automobiles, etc., especially with the development of Surface Mount Technology (SMT), ordinary high-temperature resistant engineering plastics polyphenylene sulfide (PPS) and The heat resistance of liquid crystal polymer (LCP) can no longer fully meet its requirements, so it is inevitable 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 in the main chain of the polyamide molecule, its heat resistance And the mechanical properties have been improved, and the water absorption rate has been red...

Claims

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Application Information

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IPC IPC(8): C08G69/36C08G69/44C08G69/48C08K5/3435
CPCC08G69/36C08G69/44C08G69/48C08K5/3435
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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