Liquid crystal epoxy resin with branched chain, its preparing method, composition and use

A composition and compound technology, applied in liquid crystal materials, chemical instruments and methods, other chemical processes, etc., can solve the problems of insufficient adjustment of molecular chains, difficult to control curing reaction, high melting point, high shape memory recovery temperature, avoidance of High temperature curing defects, low deformation effect

Inactive Publication Date: 2005-06-29
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are rigid mesogens in the molecular structure of liquid crystal epoxy monomers, and the molecules are symmetrical, so most of the liquid crystal epoxy monomers have high melting points. Even if they are cured at the low temperature end of the liquid crystal phase temperature, due to the high reaction temperature, the curing reaction It is very fast, and the molecular chain is too late to be fully adjusted, which is not conducive to the formation of highly ordered liquid crystal epoxy cured products, but also makes the curing reaction difficult to control, resulting in defects such as pores in the liquid crystal epoxy cured products
This is also the main reason why there are few reports on the macroscopic mechanical properties (such as strength, modulus, etc.) of liquid crystal epoxy resin materials in the current literature.

Method used

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  • Liquid crystal epoxy resin with branched chain, its preparing method, composition and use
  • Liquid crystal epoxy resin with branched chain, its preparing method, composition and use
  • Liquid crystal epoxy resin with branched chain, its preparing method, composition and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]Add 0.01mol allyl chloride, 0.01mol methyl p-hydroxybenzoate, 1g 18-crown-6-ether and 10g potassium carbonate to 100mL acetone, and react at 50°C for 20 hours to obtain p-benzoic acid allyl ether. 0.01mol of 2,5-dihydroxybenzoic acid and 0.01mol of n-octanol were reacted at 80°C for 7 hours under the action of 6mL of concentrated sulfuric acid, extracted with 1000mL of solvent, the volume ratio of ethanol and water in the solvent was 3:1, In 2,5-dihydroxybenzoic acid n-octyl. 0.01mol p-benzoic acid allyl ether was acylated with 20mL thionyl chloride at 90°C, and the obtained acylated product was mixed with 0.01mol n-octyl 2,5-dihydroxybenzoate in 0.4g N,N-dimethyl Under the action of aminopyridine, react at 0°C to get m=1, R=C 8 h 17 The compound of formula (4). 0.01mol of this compound was reacted with 0.03mol of o-chloroperoxybenzoic acid at 45°C for 120 hours with 100mL of dichloromethane as a solvent, and the obtained product was confirmed to be R=C by nuclear mag...

Embodiment 2

[0037] Add 0.01mol 4-chloro-1-butene, 0.01mol methyl p-hydroxybenzoate, 1.5g dibenzo-18-crown-6-ether, 10g potassium carbonate to 150mL acetone and react at 65°C for 20 hours to obtain Butyl p-benzoate. 0.01mol of 2,5-dihydroxybenzoic acid and 0.01mol of n-tetradecyl alcohol were reacted at 120°C for 6 hours under the action of p-toluenesulfonic acid, extracted with 1000mL solvent, and the volume ratio of ethanol and water in the solvent was 5: 1. Obtain n-tetradecyl 2,5-dihydroxybenzoate. 0.01mol of butyl p-benzoate was acylated in thionyl chloride at 90°C, and the obtained acylated product was mixed with 0.01mol of n-tetradecyl 2,5-dihydroxybenzoate in 1g of N,N-di Under the action of methylaminopyridine, react at -5°C for 16 hours to obtain m=2, R=C 14 h 29 The compound of formula (4). 0.01mol of this compound was reacted with 0.03mol of o-chloroperoxybenzoic acid at 40°C for 150 hours with 100ml of dichloromethane as a solvent, and the obtained product was confirmed to...

Embodiment 3

[0040] Add 0.01mol allyl chloride, 0.01mol methyl p-hydroxybenzoate, 0.7g 15-crown-5-ether, 6g sodium hydroxide to 100mL deionized water, and react at 50°C for 20 hours to obtain allyl p-benzoate base ether. 0.01mol of 2,5-dihydroxybenzoic acid and 0.01mol of 1-bromo-n-butane were reacted in 100mL of triethylamine at 30°C for 6 hours, rinsed with 1000mL of solvent, the solvent was 5% aqueous sodium bicarbonate, and then vacuum-dried , to obtain n-butyl 2,5-dihydroxybenzoate. 0.01mol p-benzoic acid allyl ether and 20ml thionyl chloride were acylated at 85°C, and the obtained acylated product was mixed with 0.01mol 2,5-dihydroxybenzoic acid n-butyl ester in 1g catalyst N,N-dimethyl Under the action of aminopyridine, react at -5°C for 20 hours to obtain m=1, R=C 4 h 9 The compound of formula (4). 0.01mol of this compound was reacted with 0.03mol of o-chloroperoxybenzoic acid at 50°C for 36 hours with 100mL of dichloromethane as a solvent, and the obtained product was confirme...

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Abstract

The invention relates to liquid crystal epoxide resin wit branch chain, its (1) is shown at the right: R is alkyl containing 1-16 carbon atom, m=1-10, also it relates to the method to prepare the compound, the combination and its application. The invention has the characteristic that the product etherealized and then esterified of methyl p-hydroxybenzoate and alkenyl alkyl halide has reaction with the product of 2,5-dihydroxy-benzoic acid and alkyl alcohol or alkyl halide, the compound generated then reacts with peroxiding agent, making the liquid crystal epoxide resin with branch chain, and the productivity is as high as 70-85%, much higher than the conventional dirct esterification method. The invention has the performance of liquid crystal, and lower melt point than that without branch chain, can be solified by many curing agent in lower temperature for producing electronic enclosing material and shape-mambering material with outstanding performance.

Description

technical field [0001] The present invention relates to a novel liquid crystal epoxy resin and its preparation method, as well as the epoxy resin composition and its use, especially to a branched liquid crystal epoxy resin and its preparation method, composition and use . Background technique [0002] Liquid crystal polymer is a polymer that exists in a liquid crystal state under specific conditions. Compared with general polymers, it has the molecular orientation and position orientation unique to liquid crystal phases. Compared with small molecule liquid crystal compounds, it has polymers Quality and properties of polymeric compounds. Because of its excellent mechanical properties or incomparable physical properties of other materials, liquid crystal polymers have received common attention and attention from academia and industry. [0003] According to the formation conditions of liquid crystals, liquid crystal polymers are classified into thermotropic and lyotropic type...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B29C61/06C08G59/12C09K3/10C09K19/38
Inventor 郑一泉吕满庚
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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