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Preparation method of aryl-containing boron thermoplastic phenolic resin

A phenolic resin and thermoplastic technology, which is applied in the field of preparation of aryl boron-containing thermoplastic phenolic resin, can solve the problems of high curing temperature, poor processing technology and mechanical properties, and unstable product quality of boric acid-modified thermoplastic phenolic resin. Superior manufacturability, both manufacturability and low free phenol content

Active Publication Date: 2014-02-05
XI AN JIAOTONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to provide a kind of preparation method of aryl boron-containing thermoplastic phenolic resin, while this method solves the problems such as high free phenol content, low molecular weight, poor thermal performance and unstable product quality of traditional thermoplastic phenolic resin, it can also Preparation of high ortho aryl boron-containing thermoplastic phenolic resins to solve the problems of high curing temperature, poor processing technology and mechanical properties of boric acid modified thermoplastic phenolic resins

Method used

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  • Preparation method of aryl-containing boron thermoplastic phenolic resin
  • Preparation method of aryl-containing boron thermoplastic phenolic resin
  • Preparation method of aryl-containing boron thermoplastic phenolic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) According to the number of parts by mass, weigh 18.82 parts of phenol, 0.05 parts of zinc acetate, 0.23 parts of oxalic acid and 1.88 parts of phenylboronic acid respectively; % formalin solution;

[0040] 2) Add phenol and zinc acetate into a four-neck flask equipped with a condenser, a stirring paddle, a thermometer and a thermocouple, raise the reaction temperature to 50°C and stir to heat and melt the phenol to obtain a mixture; divide the formalin solution into two After adding 75% of the total mass of the formalin solution for the first time, stir to make it fully mixed with the material in the flask, raise the reaction temperature to 70°C, react at 70°C for 1.5h, and then Add 25% of the total mass of formalin solution and oxalic acid at a time, increase the reaction temperature to reflux state, reflux reaction for 2 hours, and finally reduce the reaction temperature to 60°C and then distill under reduced pressure (pressure 30-100mmHg) to remove the reaction ge...

Embodiment 2

[0050] 1) By mass parts, weigh 45.6 parts of bisphenol A, 0.26 parts of sodium acetate, 0.77 parts of phosphoric acid with a mass concentration of 85%, and 6.84 parts of hydroxymethylphenylboronic acid; meanwhile, according to the ratio of 1:1.2 Phenol A and formaldehyde molar ratio take by weighing the formalin solution that mass concentration is 37%;

[0051]2) Add bisphenol A and sodium acetate into a four-necked flask equipped with a condenser, a stirring paddle, a thermometer and a thermocouple, raise the reaction temperature to 50°C and stir to heat and melt bisphenol A to obtain a mixture; The formalin solution was added to the mixture twice. After adding 80% of the total mass of the formalin solution for the first time, stir to make it fully mixed with the material in the flask, raise the reaction temperature to 65°C, and react at 65°C for 1h. Then add 20% of the total mass of formalin solution and phosphoric acid for the second time, raise the reaction temperature to ...

Embodiment 3

[0054] 1) In parts by mass, weigh 22.02 parts of catechol, 0.13 parts of manganese acetate, 0.27 parts of citric acid, and 2.64 parts of carboxyphenylboronic acid; Take by weighing the formalin solution that mass concentration is 37%;

[0055] 2) Add catechol and manganese acetate into a four-necked flask equipped with a condenser, a stirring paddle, a thermometer and a thermocouple, raise the reaction temperature to 40° C. and stir to heat and melt the catechol to obtain a mixture; The formalin solution was added to the mixture twice, the first time adding 85% of the total mass of the formalin solution, stirring to make it fully mixed with the material in the flask, raising the reaction temperature to 65°C, and reacting at 65°C for 1.5 h, then add 15% of the total mass of formalin solution and citric acid for the second time, raise the reaction temperature to reflux state, reflux reaction for 2h, finally reduce the reaction temperature to 65°C and then distill under reduced p...

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Abstract

A preparation method of an aryl-containing boron thermoplastic phenolic resin. The method is as below: adding a phenolic compound and a divalent metal salt catalyst into a reaction kettle, adding an aldehyde compound by two times, wherein after the first addition, reacting at 50-70 DEG C for 0.5-2 h, and after the second addition, adding an acidic catalyst, heating to a reflux reaction state for reaction, then removing generated water and unreacted phenolic compounds to obtain the thermoplastic phenolic resin; and adding a boronic acid-containing compound into the thermoplastic phenolic resin, then heating to 100-120 DEG C, removing generated water to obtain the aryl-containing boron thermoplastic phenolic resin; or directly mixing the thermoplastic phenolic resin with the boric acid-containing compound in a solvent evenly and drying to obtain the aryl-containing boron thermoplastic phenolic resin. As the added boronic acid-containing compound contains aryl boric acid, the prepared aryl-containing boron thermoplastic phenolic resin has low water absorption rate and low curing temperature, not only has excellent thermal properties but also shows superior processing and mechanical properties.

Description

technical field [0001] The invention belongs to the field of new materials, and in particular relates to a preparation method of aryl boron-containing thermoplastic phenolic resin. Background technique [0002] Due to the easy availability of raw materials, low cost, and good mechanical properties, heat resistance, and electrical properties, thermoplastic phenolic resins are widely used as matrix resins for resin-based composite materials and carbon / carbon composite materials. Material. In recent years, the rapid development of aerospace and related technical fields has placed higher requirements on the performance of ablation-resistant materials. However, the existing thermoplastic phenolic resins still have deficiencies such as high free phenol content, low carbon residue rate, low softening point and unstable product quality, which lead to high porosity of composite materials, low product quality reliability, interlayer shear and so on. However, problems such as low she...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
Inventor 井新利王淑娟辜朝辉王勇司晶晶李瑜
Owner XI AN JIAOTONG UNIV
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