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High-temperature-resistant long-carbon-chain polyamide and synthesis method thereof

A synthesis method and high-temperature-resistant 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 having many solid-phase polymerization production processes, so as to facilitate management and control, improve productivity, and reduce processes. Effect

Active Publication Date: 2016-02-03
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • High-temperature-resistant long-carbon-chain polyamide and synthesis method thereof
  • High-temperature-resistant long-carbon-chain polyamide and synthesis method thereof
  • High-temperature-resistant long-carbon-chain polyamide and synthesis method thereof

Examples

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Effect test

Embodiment 1

[0075] The raw material composition and synthetic steps of the polyester amide used in the present embodiment are as follows:

[0076] (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;

[0077] (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

[0082] The raw material composition and synthesis steps of the polyester amide used in this example are the same as those in Example 1.

[0083] The synthetic method of a kind of long carbon chain high temperature resistant polyamide of this embodiment comprises the following steps:

[0084] (1) Add monomer 1 after vacuum drying: 116.2g (1mol) hexamethylenediamine, 91.4g (0.55mol) terephthalic acid, 103.6g (0.45mol) dodecanedioic acid to the stirred polymerization reactor 8% (24.9g) of polyester amide, 8% (24.9g) of organic montmorillonite, 3% (9.3g) of benzoic acid, 0.3% (0.9g) of the total weight of monomer 1 were added simultaneously. 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, Pass nitrogen for 5 minutes, and circulate like this 6 times, so that the reactant exists in the environment under the protection of nitrogen, and the system pressure in the stirred polymeriz...

Embodiment 3

[0087] The raw material composition and synthesis steps of the polyester amide used in this example are the same as those in Example 1.

[0088] The synthetic method of a kind of long carbon chain high temperature resistant polyamide of this embodiment comprises the following steps:

[0089] (1) Add monomer 1 after vacuum drying: 116.2g (1mol) hexamethylenediamine, 116.3g (0.7mol) terephthalic acid, 69.1g (0.3mol) dodecanedioic acid to the stirred polymerization reactor 2% (6.0g) of polyesteramide, 0.5% (1.5g) of organic montmorillonite, 0.5% (1.5g) of benzoic acid, 0.2% (0.6g) 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, Nitrogen was passed for 5 minutes, and this cycle was repeated 6 times, so that the reactants were present in the environment under the protection of nitrogen, and the system pressure in the stirred polymerization reactor was controlled to be 0.3MPa...

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Abstract

The invention discloses a high-temperature-resistant long-carbon-chain polyamide and a synthesis method thereof. The structure of the high-temperature-resistant long-carbon-chain polyamide is as shown in the following formula (I) which is as shown in the specification, wherein a is 10-100, b is 10-200, c is 10-100, d is 10-100, and R refers to polyesteramide. The high-temperature-resistant long-carbon-chain polyamide disclosed by the invention has high mechanical properties and heat resistance, low water absorption and excellent processability, and can be applied to the fields such as electrical and electronic fields, LED field, automotive filed, aerospace and military fields, and the like.

Description

technical field [0001] The invention relates to the field of materials, in particular to a long carbon chain high temperature resistant 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), 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 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 impro...

Claims

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Application Information

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IPC IPC(8): C08G69/26C08G69/28C08G69/44C08K3/34C08K5/09C08K5/3435
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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