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Aryl boron-containing phenolic resin and preparation method thereof

A technology of phenolic resin and aryl boron, which is applied in the field of aryl boron-containing phenolic resin and its preparation, can solve the problems of low char formation rate, unstable product quality, poor processability and mechanical properties, etc. Insufficient char formation rate and thermal decomposition temperature, superior processability

Active Publication Date: 2013-09-11
浙江世涛鼎革新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to solve the problems of low char formation rate, poor manufacturability and mechanical properties, and unstable product quality of traditional boron phenolic resins, and provides a kind of aryl-containing boron phenolic resin and its preparation method, according to the preparation method of the present invention The obtained aryl boron-containing phenolic resin can balance heat resistance, processability and mechanical properties

Method used

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  • Aryl boron-containing phenolic resin and preparation method thereof
  • Aryl boron-containing phenolic resin and preparation method thereof
  • Aryl boron-containing phenolic resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] According to the molar ratio of phenol / aldehyde=1:1.25. First, add 18.82g (0.2mol) of phenol and 2.96g of barium hydroxide into a four-necked flask equipped with a stirring paddle, a thermometer, a thermocouple and a condenser tube, raise the temperature to 40°C and stir to heat and melt the phenol. Then, dropwise add 20.29g37% formalin solution (0.25mol formaldehyde) in the flask, stir to make it fully mix with the material in the flask, heat up to 85°C, keep the heat for about 2.5h, and distill under reduced pressure under vacuum ( Pressure 30 ~ 100mmHg) to remove the water generated by the reaction, and the water content is less than 4%. Finally, slowly add 4.5g of phenylboronic acid into the flask, increase the reaction temperature to 115°C, and conduct the second vacuum distillation (pressure 30-100mmHg) dehydration after the heat preservation reaction for about 2 hours, and unreacted phenol with low water content The content of free phenol is less than 0.1%, and ...

Embodiment 2

[0038] According to the molar ratio of phenol / aldehyde=1:0.85. First, add 19.48g (0.46mol) of 1,4-benzenediol and 3.25g of acid catalyst (a mixture of oxalic acid and hydrochloric acid) into a four-necked flask equipped with a stirring paddle, a thermometer, a thermocouple and a condenser, and raise the temperature to 50 Stir at ℃ to heat and melt 1,4-benzenediol. Then, slowly add 8.71g of aryl boron compound (2,4,6-triphenylboroxine) into the flask, stir to make it fully mixed with the contents of the flask, raise the reaction temperature to 160°C, and keep the heat for about After 2.5 hours, after the reaction temperature drops to 55°C, vacuum distillation (pressure 30-100mmHg) removes the water generated by the reaction, and the water content is less than 4%. Finally, when the reaction temperature rose to 100°C, 20.29g of 37% formalin solution (0.25mol formaldehyde) was added dropwise to the flask, the temperature was raised to 90°C, and the second vacuum distillation (pre...

Embodiment 3

[0040] According to the molar ratio of phenol / aldehyde=1:1.25. First, add 20.02g (0.2mol) of catechol and 4.25g of sodium hydroxide into a four-neck flask equipped with a stirring paddle, thermometer, thermocouple and condenser, raise the temperature to 45°C and stir to heat and melt the catechol . Then, slowly add 3g of aryl boron compound (4-hydroxymethylphenylboronic acid) into the flask, stir to make it fully mixed with the contents of the flask, raise the reaction temperature to 180°C, and keep the reaction for about 3.5h. Add 3g of 10% concentrated sulfuric acid to the two-layer mixture to reduce the pH value of the reaction product to 6-7. After the reaction temperature drops to 45°C, distill under reduced pressure (pressure 30-100mmHg) to remove the water generated by the reaction. The water content is lower than 4%. Finally, when the reaction temperature rose to 100°C, 20.29g of 37% formalin solution (0.25mol formaldehyde) was added dropwise to the flask, the temper...

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Abstract

The invention discloses a phenolic resin containing aryl boron and a preparation method thereof, especially to an aryl boron-containing phenolic resin with good thermal stability and high char yield and a preparation method thereof. Directed at the disadvantages that a common phenolic resin has poor thermal behaviors (e.g., low char yield) and a boric acid modified phenolic resin has poor manufacturability and mechanical properties, the invention brings forward the method which introduces borophenylic acid and a derivative thereof in synthesis of the aryl boron-containing phenolic resin. The obtained aryl boron-containing phenolic resin not only has excellent thermal behaviors such as high thermal decomposition temperature and high char yield but also has superior manufacturability and good mechanical properties. Since the aryl boron-containing phenolic resin has high char yield and superior inoxidizability and manufacturability, the aryl boron-containing phenolic resin is especially applicable to ablation-resistant resin matrix composites, carbon / carbon composites, high temperature braking materials, friction materials, heat-insulating materials, adhesives, coatings, flame-retardant materials, etc.

Description

technical field [0001] The invention belongs to the field of new materials, and in particular relates to an aryl boron-containing phenolic resin and a preparation method thereof. Background technique [0002] Resins with high heat resistance and high char formation rate are widely used in the fields of ablation-resistant composite materials, carbon / carbon composite materials, high-temperature brake materials, friction materials, heat insulation materials, adhesives and coatings. As one of the three synthetic thermosetting resins, phenolic resin is widely used in aviation due to its easy availability of raw materials, low cost, simple production process, low investment in manufacturing and processing equipment, and good heat resistance, flame retardancy, electrical insulation and chemical resistance. Aerospace, military equipment, electronics, transportation, and manufacturing have an irreplaceable position. They are still used as matrix resins for composite materials, and th...

Claims

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Application Information

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IPC IPC(8): C08G8/28
Inventor 井新利王淑娟司晶晶王勇
Owner 浙江世涛鼎革新材料有限责任公司
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