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Long-carbon-chain semi-aromatic nylon PA14T and preparation method thereof

A semi-aromatic, long carbon chain technology, applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of long synthesis route and continuous production difficulties, and achieve high molecular weight, low price and raw material source. rich effects

Active Publication Date: 2015-02-04
HENAN JUNHENG IND GRP BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such a synthetic route is relatively long and it is difficult to carry out continuous production.

Method used

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  • Long-carbon-chain semi-aromatic nylon PA14T and preparation method thereof
  • Long-carbon-chain semi-aromatic nylon PA14T and preparation method thereof
  • Long-carbon-chain semi-aromatic nylon PA14T and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of long carbon chain semi-aromatic nylon PA14T, its preparation method is:

[0029] (1) Add 1,14-tetradecanediamine into water and heat to 85°C. After the tetradecanediamine is completely dissolved, add 1,4-terephthalic acid to react under stirring. The reaction time After 2 hours, the pH value of the solution was stable at 7.1, and then cooled to room temperature, suction filtered and dried to obtain the PA14T salt in the form of white powder. Wherein, the mass ratio of 1,14-tetradecanediamine to water is 1:10, and the molar ratio of 1,14-tetradecanediamine to 1,4-terephthalic acid is 1:1.05.

[0030] (2) Add the prepared PA14T salt and absolute ethanol into a stainless steel polymerization kettle at a solid-to-liquid ratio of 1:1 by mass. After replacing the air in the kettle with carbon dioxide for 3 times, the system pressure is 0.3MPa. Stir for 2 hours Gradually heat up to 200°C, control the pressure in the kettle to 1.5 MPa, keep the pressure for 2 hours, ...

Embodiment 2

[0037] Embodiment 2 comparative test

[0038] A kind of long carbon chain semi-aromatic nylon PA14T, its preparation method is:

[0039] (1) The preparation method is the same as step (1) in Example 1;

[0040] (2) Add the prepared PA14T salt and absolute ethanol into a stainless steel polymerization kettle at a solid-to-liquid ratio of 1:1 by mass, replace the air in the kettle with carbon dioxide for 3 times, and gradually heat up to 200 °C within 2 hours under stirring. ℃, control the pressure in the kettle to 1.5 MPa, keep the pressure for 2 hours, then slowly release the gas to make the pressure in the kettle drop to normal pressure within 2 hours, then raise the temperature to 230℃, continue the reaction for 3 hours, and obtain a light yellow powder The semi-aromatic nylon PA14T has a melting point of 297°C. The intrinsic viscosity is 1.63 dL / g, and its physical and mechanical properties are tested, and the results are listed in Table 2.

[0041] Table 2 The physica...

Embodiment 3

[0045] A kind of long carbon chain semi-aromatic nylon PA14T, its preparation method is:

[0046] (1) Add 1,14-tetradecanediamine into water and heat to 90°C. After the tetradecanediamine is completely dissolved, add 1,4-terephthalic acid to react under stirring. The reaction time After 2 hours, the pH value of the solution was stable at 7.2, then cooled to room temperature, suction filtered and dried to obtain white powder PA14T salt. Wherein, the mass ratio of 1,14-tetradecanediamine to water is 1:8, and the molar ratio of 1,14-tetradecanediamine to 1,4-terephthalic acid is 1:1.02.

[0047] (2) Add the prepared PA14T salt and absolute ethanol into the stainless steel polymerization kettle according to the mass ratio of 1:1.5, replace the air in the kettle with carbon dioxide for 3 times, the system pressure is 0.3MPa, and gradually heat up within 2 hours under stirring To 215°C, control the pressure inside the kettle to 1.5 MPa, keep the pressure for 3 hours, then slowly re...

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Abstract

The invention relates to a long-carbon-chain semi-aromatic nylon PA14T and a preparation method thereof, belonging to the field of high polymer material synthetic technologies. The repeat unit is shown in the specification, and the degree of polymerization of the long-carbon-chain semi-aromatic nylon PA14T is n which is equal to 2 to 200. The preparation method comprises the following steps: (1) preparing nylon PA14T salt: adding 1,4-terephthalic acid and 1,14-tetradecanedioic diamine into water to perform salt forming reaction; (2) preparing semi-aromatic nylon PA14T: adding the nylon PA14T salt obtained in step (1) and a solvent into a polymerizer, heating up a reaction still to be at 200-240 DEG C under a condition of shielding gas, reacting for 1-4 hours under the pressure of 1.2 to 3 MPa, deflating until normal pressure is achieved and vacuumizing, and then carrying out polymerization reaction to obtain the semi-aromatic nylon PA14T. The PA14T is excellent in performance and is easy to process and form, and has the good market prospect, especially in electronic and electrical, automotive industries and the like; and besides, the long-carbon-chain semi-aromatic nylon PA14T is simple in technology, moderate in reaction condition, short in reaction time and low in energy consumption.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and relates to a semi-aromatic nylon and a preparation method thereof, in particular to a long carbon chain semi-aromatic nylon PA14T and a preparation method thereof. Background technique [0002] Semi-aromatic nylon is made by polycondensation of aliphatic diamine or diacid and diacid or diamine with aromatic ring. It is a kind of aromatic nylon. Due to the introduction of the aromatic ring structure into the main chain of the nylon molecule, the heat resistance and mechanical properties of the nylon product have been improved, and the water absorption rate has also been reduced to varying degrees, and it has a better cost performance. It is mainly used in the automotive and electrical and electronic industries. According to product performance requirements, various manufacturers have developed various brands of semi-aromatic nylon products. With the rapid development of high-tech an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28C07C211/09C07C209/48
Inventor 张振国张振辉杨韶辉高元英吴自胜
Owner HENAN JUNHENG IND GRP BIOTECH CO LTD
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