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Environmental-protection bio-based semi-aromatic PA10T/11 copolymerization material and preparation method thereof

A semi-aromatic, bio-based technology, applied in the field of environmentally friendly bio-based semi-aromatic PA10T/11 copolymer materials and its preparation, can solve the problems of low water absorption, narrow processing window, poor toughness, etc., and achieve low water absorption, polymerization The effect of short cycle time and high production efficiency

Inactive Publication Date: 2017-07-04
SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects of narrow processing window and poor toughness in the post-processing of PA10T, provide an environmentally friendly bio-based semi-aromatic PA10T / 11 copolymer material and its synthesis method, so that the processing temperature of PA10T is reduced to a certain extent, thereby Improve the processing stability of the material, and improve its toughness to a large extent. In addition, the synthetic material has relatively low water absorption, so the dimensional stability is good

Method used

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  • Environmental-protection bio-based semi-aromatic PA10T/11 copolymerization material and preparation method thereof
  • Environmental-protection bio-based semi-aromatic PA10T/11 copolymerization material and preparation method thereof
  • Environmental-protection bio-based semi-aromatic PA10T/11 copolymerization material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 20 mol of terephthalic acid, 20 mol of decanediamine, 0.05 mol of barium sulfate as a nucleating agent, and 0.002 mol of catalyst sodium hypophosphite and mix them evenly, then add them into a high-pressure polymerization reactor equipped with a high-efficiency stirring device, and weigh Take 250 mol of solvent deionized water in the reaction kettle, seal the high-pressure polymerization reaction kettle, start stirring and raise the temperature to 90°C, and then stir at this temperature for 2 hours to make the two fully salt.

[0038] Open the reactor again, add 1mol of 11-aminoundecanoic acid into it, seal the high-pressure polymerization reactor, use high-purity inert gas to replace the air in the reactor for 3 times, and finally reserve 0.05MPa inert gas as a protective gas .

[0039] Turn on the stirring, control the heating rate, and raise the temperature to 290°C at a constant speed in 2 hours, and when the pressure in the kettle is 3.5MPa, the reaction kettl...

Embodiment 2

[0042] Take 20mol of terephthalic acid, 19.2mol of decanediamine, 0.075mol of titanium dioxide as a nucleating agent, and 0.003mol of calcium hypophosphite as a catalyst and mix evenly, then add it to a high-pressure polymerization reactor equipped with a high-efficiency stirring device, and weigh Take 300 mol of solvent deionized water in the reaction kettle, seal the high-pressure polymerization reaction kettle, start stirring and raise the temperature to 105°C, and then stir at this temperature for 1.5h to make the two fully salt-formed.

[0043] Open the reactor again, add 3mol of 11-aminoundecanoic acid into it, seal the high-pressure polymerization reactor, use high-purity inert gas to replace the air in the reactor for 4 times, and finally reserve 0.15MPa inert gas as a protective gas .

[0044]Start stirring, control the heating rate, and use 1.75h to raise the temperature to 280°C at a constant speed, and when the pressure in the kettle is 3.0MPa, the reaction kettle ...

Embodiment 3

[0047] Take 20 mol of terephthalic acid, 18.5 mol of decane diamine, 0.1 mol of nucleating agent silicon dioxide, and 0.005 mol of catalyst potassium hypophosphite, mix them evenly, and then add them into a high-pressure polymerization reactor equipped with a high-efficiency stirring device , Weigh 300 mol of solvent deionized water in the reaction kettle, seal the high-pressure polymerization reaction kettle, start stirring and raise the temperature to 120°C, and then stir at this temperature for 1 hour to make the two fully salt.

[0048] Open the reactor again, add 4.5mol of 11-aminoundecanoic acid into it, seal the high-pressure polymerization reactor, use high-purity inert gas to replace the air in the reactor for 5 times, and finally reserve 0.25MPa inert gas as a protection gas.

[0049] Start stirring, control the heating rate, and use 1.5 hours to raise the temperature to 270°C at a constant speed, and when the pressure in the kettle is 2.5MPa, the reaction kettle is ...

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Abstract

The present invention relates to an environmental-protection bio-based semi-aromatic PA10T / 11 copolymerization material and a preparation method thereof, wherein the environmental-protection bio-based semi-aromatic PA10T / 11 copolymerization material is prepared from the following components by mole: 20 parts of terephthalic acid, 18.5-20 parts of diaminodecane, 1-4.5 parts of 11-aminoundecanoic acid, 0.05-0.1 part of a nucleating agent, 0.002-0.005 part of a catalyst, and 250-300 parts of a solvent. Compared to the material in the prior art, the material of the present invention has the following characteristics that the monomer 11-aminoundecanoic acid in the PA10T / 11 provides the flexible chain segment to the main chain molecule, such that the flexibility of the main chain molecule is increased, the toughness is improved, the obtained product has the wide processing window, and the molding processing difficulty is lower than the molding processing difficulty of PA10T; and the synthesis material has characteristics of low water absorption and good material stability. According to the present invention, the PA10T / 11 is prepared by using the one-step melt condensation polymerization method so as to continuously perform the whole polymerization process, wherein the one-step melt condensation polymerization method has advantages of less process step, short polymerization period, high production efficiency, low production cost and the like, and creates the conditions for the future continuous industrial production.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and relates to an environment-friendly bio-based semi-aromatic PA10T / 11 copolymer material and a preparation method thereof. Background technique [0002] With the continuous development of industrial technology, more and more attention has been paid to semi-aromatic polyamides, and there are more and more types of products. Among them, PA4T of DSM Engineering Plastics, PA6T / 66 of Mitsui Chemicals and PA9T of Kuraray are representative. Among the semi-aromatic polyamides that have been industrially produced, PA9T has the best comprehensive performance in all aspects. However, the monomer nonanediamine of PA9T is obtained through petroleum refining. Petroleum is a non-renewable resource, and the production process of nonanediamine is complicated, the equipment requirements are high, and the synthesis technology is monopolized by Japan Kuraray Company, resulting in high cost and price of PA9T. No ...

Claims

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Application Information

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IPC IPC(8): C08G69/36
CPCC08G69/36
Inventor 杨桂生柯昌月
Owner SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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