Preparation method of semi-aromatic polyamide

A semi-aromatic and polyamide technology, applied in the field of semi-aromatic polyamide preparation, can solve the problems of side reactions, inability to ensure the molar ratio balance of monomeric dicarboxylic acid and diamine, increase the reaction pressure, etc., and achieve The effect of high crystallinity, good processing stability and low active end group content

Inactive Publication Date: 2010-06-30
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Increasing the pre-polymerization temperature will lead to the occurrence of side reactions, and will also increase the reaction pressure, and the requirements for equipment will also increase accordingly
Draining the water in the reaction will volatilize the unreacted diamine, resulting in a large difference between the monomer unit ratio of the prepolymer and the initial monomer ratio added to the reactor, and it cannot guarantee that the monomer dicarboxylic acid and Molar ratio balance of diamines

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 3323g (20mol) terephthalic acid, 17230g (20mol) decanediamine concentrated solution (concentration 20wt%), 73.27 g (0.6mol) benzoic acid, 6.77g (0.1wt% based on the total weight of the raw material) sodium hypophosphite, and start to heat up after nitrogen purging. The temperature was raised to 220°C with stirring over 2 hours, the reaction mixture was stirred at 220°C for 1 hour, then the temperature of the reactants was raised to 230°C with stirring. The reaction was continued for 2 hours at a constant temperature of 230°C and a constant pressure of 2.5 MPa, and the pressure was kept constant by removing the formed water. After the reaction was completed, the material was discharged, thereby obtaining a pre-prepared material with an intrinsic viscosity [η] of 0.150dl / g. Polymer. The prepolymer was vacuum-dried at 80°C for 24 hours, and then solid-phase tackified at 260°C for 10 hours under a nitrogen atmosphere to obtain a PA10T resin with a melting point of 321°...

Embodiment 2

[0045] Repeat Example 1, the difference is that the concentration of decanediamine concentrated solution is changed to 50wt%, and the weight is changed to 6892g. The results are shown in Table 1.

Embodiment 3

[0047] Repeat Example 1, the difference is that the concentration of decanediamine concentrated solution is changed to 80wt%, and the weight is changed to 4307.5g. The results are shown in Table 1.

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Abstract

The invention discloses a preparation method of semi-aromatic polyamide. In the method, aromatic dicarboxylic acid and a recovery aliphatic diamine concentrated solution containing 4-14 carbon atoms are used for preparing the semi-aromatic polyamide, thereby reducing the waste of raw material diamine in production, reducing the production cost and simultaneously lightening the influence of environmental pollution. The semi-aromatic polyamide has higher crystallinity, inherent viscosity and heat-resistance temperature, good hue, low active terminal group content, good processing stability and no corrosion to moulds. Through a prepolymerization reaction, a prepolymer with the inherent viscosity [eta] within the range of 0.06-0.3dl/g measured in 96 percent sulfuric acid at 25 DEG C can be obtained. After a tackification reaction, the inherent viscosity [eta] of the semi-aromatic polyamide is 0.8-2.5dl/g, the melting point of the semi-aromatic polyamide is 270-330 DEG C, the content of terminal carboxyl groups is 15-80mol/t, and the content of terminal amino groups is 15-80mol/t.

Description

technical field [0001] The present invention relates to the preparation technology of semi-aromatic polyamide. Background technique [0002] Aliphatic polyamides, such as PA6 and PA66, have excellent mechanical strength, heat resistance, chemical resistance, wear resistance and self-lubricating properties, and low coefficient of friction. Their applications include electronic appliances, automotive parts, furniture , building materials and fibers, has become one of the most important engineering plastics. [0003] Semi-aromatic polyamide is a polyamide resin prepared by polycondensation of diamines or dicarboxylic acids with aromatic rings and aliphatic dicarboxylic acids or diamines, and is one of the aromatic polyamides. Due to the introduction of aromatic rings into the main chain of polyamide molecules, the heat resistance and mechanical properties are improved, the water absorption rate is reduced, and it has a more suitable performance / price ratio. It is between gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28
Inventor 罗湘安夏世勇蔡彤旻曾祥斌曹民
Owner KINGFA SCI & TECH CO LTD
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