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Preparation method of organic-inorganic hybrid biomass phenolic resin ablation-resistant material

A technology of phenolic resin and biomass, which is applied in the field of preparation of modified biomass phenolic hybrid materials, which can solve the problems of poor high temperature resistance and heat resistance to oxygen degradation, decreased overall performance of resin crosslinking density, and poor manufacturability, etc. , to achieve good heat resistance and thermal oxygen aging performance

Pending Publication Date: 2021-11-09
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, more widely natural phenols and aldehydes, especially biomass phenolic resins headed by aromatic aldehydes or fused-ring natural phenols, have poor reactivity due to large steric hindrance and require higher The temperature and longer reaction time make the reaction complete, otherwise the resin crosslinking density will decrease and the overall performance will decrease; however, the increase of the reaction temperature and the extension of the reaction time also bring about the increase of viscosity and the deterioration of manufacturability These factors lead to these aromatic aldehydes or natural phenols having higher carbon content, but the prepared biomass phenolic resin has poor high temperature resistance and thermal oxygen degradation ability, and it is difficult to use it as a raw material for the synthesis of phenolic resin

Method used

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  • Preparation method of organic-inorganic hybrid biomass phenolic resin ablation-resistant material
  • Preparation method of organic-inorganic hybrid biomass phenolic resin ablation-resistant material
  • Preparation method of organic-inorganic hybrid biomass phenolic resin ablation-resistant material

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Step 1, preparation of organosilicon-modified urethane-based biomass phenolic resin

[0042] Add 10-25 parts by weight of phenol, 1-4 parts by weight of paraformaldehyde, 2-5 parts by weight of ethanol, 5-8 parts by weight of furfural, and 0.1-2 parts by weight of ammonia water in the reactor, and react at 60-75 °C for 0.5- After 1.5 hours, remove small molecules by distillation under reduced pressure, add 5-15 parts by weight of acetone, 1-5 parts by weight of isocyanatotrimethoxysilane, and 0.1-1 parts by weight of dibutyltin dilaurate, react at 40°C for 6 hours, and the reaction ends After vacuum distillation, a light yellow organosilicon-modified urethane-based biomass phenolic resin was obtained.

[0043] Step 2, preparation of borosilicate resin oligomer

[0044] 1 to 6 parts by weight of hydroxyphenylboronic acid, 5 to 15 parts by weight of methyltrimethoxysilane, 1 to 3 parts by weight of methyldimethoxysilane, 2 to 6 parts by weight of phenyltrimethoxysilane, ...

Embodiment 2

[0048] Step 1, preparation of organosilicon-modified urethane-based biomass phenolic resin

[0049] Add 10 parts by weight of phenol, 2 parts by weight of paraformaldehyde, 3 parts by weight of ethanol, 6 parts by weight of vanillin, and 0.5 parts by weight of ammonia water into the reactor, react at 70°C for 1h, add 3 parts by weight of resorcinol and continue at 70°C After reacting for 30 minutes and removing small molecules by distillation under reduced pressure, add 10 parts by weight of acetone, 3 parts by weight of isocyanatotrimethoxysilane, and 0.5 parts by weight of dibutyltin dilaurate, and react at 40°C for 6 hours. After the reaction is completed, distill under reduced pressure to obtain Silicone-modified urethane-based biomass phenolic resin.

[0050] Step 2, preparation of borosilicate resin oligomer

[0051] With 3 parts by weight of chlorophenylboronic acid, 10 parts by weight of methyltrimethoxysilane, 2 parts by weight of methyldimethoxysilane, 4 parts by we...

Embodiment 3

[0055] Step 1, preparation of organosilicon-modified biomass phenolic resin

[0056] Add 10-25 parts by weight of phenol, 1-4 parts by weight of paraformaldehyde, 2-6 parts by weight of ethanol, 5-8 parts by weight of benzaldehyde, and 0.1-2 parts by weight of ammonia water into the reactor, and react at 60-75°C 0.5-1.5h, remove small molecules by distillation under reduced pressure, add 1-5 parts by weight of aminopropylmethyldiethoxysilane and 1 wt% organometallic catalyst of phenolic resin quality, and react at 50-80°C for 0.5-1h to obtain Silicone grafted biomass phenolic resin.

[0057] Step 2, preparation of borosilicate resin oligomer

[0058] Add 1 to 8 parts by weight of chlorophenylboronic acid, 1 to 20 parts by weight of methyltrichlorosilane, and 0.5 to 3 parts by weight of dimethyldichlorosilane in the reactor, gradually add 3 to 8 parts by weight of water, and stir for 1 After ~5h, let stand to separate and take the organic phase, wash it several times with wat...

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Abstract

The invention discloses a preparation method of an organic-inorganic hybrid biomass phenolic resin ablation-resistant material. The method comprises the following steps of: 1, preparing low-viscosity resol through addition and condensation reaction of phenols and aldehydes under alkali catalysis, adding a catalyst for phenolic grafting and an organosilicon compound, and carrying out copolymerization to obtain an organic silicon modified biomass phenolic resin; 2, preparing a borosilicate resin oligomer through co-hydrolytic condensation or non-hydrolytic copolymerization of trifunctional silane, bifunctional silane and an organic boron compound under acid catalysis; and 3, dissolving the organic silicon modified biomass phenolic resin and the borosilicate resin oligomer in a cosolvent, adding silazane or a nitrogen-containing compound, and stirring to obtain the organic-inorganic hybrid biomass phenolic resin. The organic-inorganic hybrid biomass phenolic resin prepared by the method has excellent high temperature resistance, and has high carbon yield at high temperature.

Description

technical field [0001] The invention relates to a preparation method of an organic-inorganic hybrid resin ablation-resistant material, in particular to a preparation method of a modified biomass phenolic hybrid material with a high carbon residue rate. Background technique [0002] The most commonly used raw materials used in phenolic resins are phenol and formaldehyde, among which the raw materials such as benzene and propylene used in the preparation of phenol are important products of petrochemical industry, and the CO and H used in the preparation of formaldehyde 2 And other raw materials also need to consume huge industrial production capacity. Petroleum, as a non-renewable resource, is one of the most important sources of raw materials in the chemical industry at present. Seeking new, cheap, green and natural phenolic resin raw materials that can replace or partially replace phenol and formaldehyde has great impact on energy conservation, emission reduction and It is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/14C08L83/14C08L83/16
CPCC08L61/14C08L83/14C08L2201/08C08L83/16
Inventor 姜波刘涛李楠杨剑曹庆元朱小飞姜文红黄玉东
Owner HARBIN INST OF TECH