Novel phosphorus and nitrogen containing flame-retardant thermotropic liquid crystal copolyester with low melting point and synthesis method thereof

A technology of thermotropic liquid crystal and low melting point, which is applied in the field of chemical synthesis, can solve problems such as the complex structure and reduction of the flexible unit imide diacid that are not conducive to the melting point of TLCP, and achieve high yield, good reproducibility, and synthetic The effect of simple method

Inactive Publication Date: 2011-08-03
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the structure of the flexible unit imide diacid (IA6) in this TLCP is relatively complex, and there are other ring structures besi

Method used

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  • Novel phosphorus and nitrogen containing flame-retardant thermotropic liquid crystal copolyester with low melting point and synthesis method thereof
  • Novel phosphorus and nitrogen containing flame-retardant thermotropic liquid crystal copolyester with low melting point and synthesis method thereof
  • Novel phosphorus and nitrogen containing flame-retardant thermotropic liquid crystal copolyester with low melting point and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0032] Example 1,

[0033] Weigh 0.013mol p-acetoxybenzoic acid (p-AHB) and 0.004mol 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa10-phosphaphenanthrene-10-oxide respectively Diacetate (ODOPB), 0.003mol terephthalic acid (TPA) and the condensation product of 0.002mol terephthalic acid and 1,6-hexanediamine. The reaction raw materials were put into a three-necked flask, and a nitrogen flow device was installed. Repeatedly pass nitrogen and vacuum to exhaust the oxygen in the three-neck bottle. The oil bath was heated to 170°C, the reaction was carried out under strong stirring and nitrogen protection, and the temperature was raised at a heating rate of 1°C / 2min. When the temperature rises to 250°C, the reaction system has obvious stirring opalescence, the viscosity is high, and the small molecule by-product acetic acid is not easy to escape. At this time, the nitrogen flow is stopped and the oil pump is used to vacuum. Continue to heat up to 270°C, and the pressure in the reaction fl...

Example Embodiment

[0034] Example 2,

[0035] Weigh p-AHB 0.015mol, ODOPB 0.005mol, TPA 0.002mol and the condensation product of terephthalic acid and 1,6-hexanediamine 0.002mol. The reaction raw materials were put into a three-necked flask, and a nitrogen flow device was installed. Repeatedly pass nitrogen and vacuum to exhaust the oxygen in the three-neck bottle. The oil bath was heated to 165°C, the reaction was carried out under strong stirring and nitrogen protection, and the temperature was raised at a heating rate of 1°C / 2min. When the temperature rises to 243°C, the reaction system has obvious stirring opalescence, the viscosity is high, and the small molecule by-product acetic acid is not easy to escape. At this time, the nitrogen flow is stopped and the oil pump is used to vacuum. Continue to heat up to 268°C, and the pressure in the reaction flask remains basically unchanged, indicating that small acetic acid molecules are no longer generated. When the reaction is over, the heating is...

Example Embodiment

[0036] Example 3.

[0037] Weigh p-AHB 0.013mol, ODOPB 0.004mol, TPA 0.003mol, and the condensation product of terephthalic acid and 1,7-heptanediamine 0.002mol. The reaction raw materials were put into a three-necked flask, and a nitrogen flow device was installed. Repeatedly pass nitrogen and vacuum to exhaust the oxygen in the three-neck bottle. The oil bath was heated to 172°C, the reaction was carried out under strong stirring and nitrogen protection, and the temperature was raised at a heating rate of 1°C / 2min. When the temperature rises to 248°C, the reaction system appears obvious agitated opalescence, the viscosity is high, and the small molecule by-product acetic acid is not easy to escape. At this time, the nitrogen flow is stopped and the oil pump is used to vacuum. Continue to heat up to 275°C, and the pressure in the reaction flask remains basically unchanged, indicating that small acetic acid molecules are no longer generated. When the reaction is over, the heat...

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Abstract

The invention discloses a phosphorus and nitrogen containing flame-retardant thermotropic liquid crystal copolyester with low melting point and a synthesis method thereof; the phosphorus and nitrogen containing flame-retardant thermotropic liquid crystal copolyester with low melting point is synthesized by taking diacetic ester of 10-(2, 5-dyhydroxy phenyl group)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide, p-acetoxy-benzoic acid, terephthalic acid and a condensation product of terephthalic acid and aliphatic series diamine with methylene flexible chain as reactive monomers which undergo melt phase polycondensation. The main chain of the molecules of the hermotropic liquid crystal copolyester contains methylene flexible chains; therefore, compared with the common liquid crystal copolyester, the transition temperature of the liquid crystal is greatly reduced and can be matched with the processing temperature of most general-purpose plastics. As the thermotropic liquid crystal copolyester contains halogen free and flame-retardant elements such as phosphorous and nitrogen, the thermotropic liquid crystal copolyester achieves the purpose of high efficiency flame retardant while reinforcing general-purpose plastics. The synthesis method for thermotropic liquid crystal copolyester is simple, is easy to operate, has high reaction speed and high yield, avoids the using of large quantity of solvents and is in line with the requirements of sustainable development.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a phosphorus-nitrogen-containing thermotropic liquid crystal copolyester with low melting point and high-efficiency flame-retardant performance and a synthesis method thereof. Background technique [0002] Thermotropic liquid crystal polymers (TLCPs) have unique anisotropy. It has high strength, high modulus, self-reinforcing properties, outstanding heat resistance and excellent corrosion resistance. When blended with thermoplastic resins, TLCP will undergo in-situ fiber formation and thus play a reinforcing role. [0003] But a fly in the ointment, the rigidity of TLCP molecular chain is bigger, causes its melting point (T m ) is high, which brings difficulties to melt processing. In order to obtain TLCP with a low melting point, researchers continue to improve production technology, try new monomers, and develop new varieties of TLCP, so that they can exhibit a s...

Claims

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Application Information

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IPC IPC(8): C08G63/692C08G63/78
Inventor 夏英葛雪明侯传金王晨马文文张丹
Owner DALIAN POLYTECHNIC UNIVERSITY
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