Silicon-boron-modified thermosetting phenolic resin hollow microsphere, and preparation method and application thereof

A phenolic resin and thermosetting technology, which is applied in the field of thermosetting phenolic resin hollow microspheres and its preparation, can solve the problems of mechanical property damage, decreased thermal insulation performance, and phenolic resin hollow microspheres cannot meet the ablation resistance and other problems, and achieves mechanical properties. The effect of excellent, excellent ablation resistance

Inactive Publication Date: 2019-10-22
RES & DEV INST OF NORTHWESTERN POLYTECHNICAL UNIV IN SHENZHEN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Phenolic resin hollow microspheres have good ablation resistance and heat insulation properties, but the phenolic resin hollow microspheres are cracked during the ablation process to form carbon spheres with a large amount of amorphous carbon layer, which is easy to be absorbed by the air flow Mechanical peeling occurs under the action of mechanical shear, so that the spherical structure is destroyed, the mechanical properties are destroyed, and the thermal insulation performance is greatly reduced
Therefore, with the development of high-tech fields such as aerospace, phenolic resin hollow microspheres can no longer meet the needs of higher ablation resistance.

Method used

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  • Silicon-boron-modified thermosetting phenolic resin hollow microsphere, and preparation method and application thereof
  • Silicon-boron-modified thermosetting phenolic resin hollow microsphere, and preparation method and application thereof
  • Silicon-boron-modified thermosetting phenolic resin hollow microsphere, and preparation method and application thereof

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preparation example Construction

[0044] The present invention also provides a method for preparing silicon-boron modified thermosetting phenolic resin hollow microspheres described in the above technical solution, comprising the following steps:

[0045] After mixing water, core material and surfactant, adding silicon boron-modified thermosetting phenolic resin for preforming to obtain a preforming mixture;

[0046] After mixing the preformed mixed solution with an accelerator, precure to obtain precured microspheres;

[0047] The pre-cured microspheres are subjected to deep curing molding to obtain silicon-boron-modified thermosetting phenolic resin hollow microspheres.

[0048]In the invention, after mixing water, core material and surface active agent, silicon boron modified thermosetting phenolic resin is added for preforming to obtain a preforming mixed liquid. In the present invention, the water, core material and surfactant are mixed to form an "oil-in-water" emulsified dispersion system, wherein the ...

Embodiment 1

[0063] (1) Preparation of silicon boron modified thermosetting phenolic resin:

[0064] According to the ratio of phenol:boric acid molar ratio of 5:1, add it into a three-necked flask equipped with a thermometer, condensing device, and stirring device, control the temperature at 90°C, react for 6h, then cool down to 70°C, and add at 70°C with a mass concentration of 20% sodium hydroxide aqueous solution and paraformaldehyde, wherein the mass of sodium hydroxide aqueous solution accounts for 4% of phenol, and the molar ratio of paraformaldehyde and phenol is 1.3:1. After continuing to react for 6 hours, press phenyltriethoxysilane : Add phenylethoxysilane with a phenol molar ratio of 1:7, continue the reaction for 1 hour, and vacuum dehydrate to obtain SiBPR-1;

[0065] (2) Preparation of thermosetting phenolic resin hollow microspheres modified by silicon boron

[0066] 1) Add 40g of deionized water, 10g of tetraethyl orthosilicate and 22g of polyacrylic acid into a three-ne...

Embodiment 2

[0077] (1) Preparation of silicon boron modified thermosetting phenolic resin:

[0078]According to the ratio of phenol:boric acid molar ratio of 3:1, add it into a three-necked flask equipped with a thermometer, a condensing device, and a stirring device, control the temperature at 90°C, react for 6h, then cool down to 70°C, and add a concentration of 20 at 70°C % sodium hydroxide aqueous solution and paraformaldehyde, wherein the quality of sodium hydroxide aqueous solution is 4% of phenol, the molar ratio of paraformaldehyde and phenol is 1.3:1, after continuing to react for 6h, press phenyltriethoxysilane : Add phenyltriethoxysilane at a phenol molar ratio of 1:9, react for 1 hour, and vacuum dehydrate to obtain SiBPR-2.

[0079] (2) Preparation of thermosetting phenolic resin hollow microspheres modified by silicon boron

[0080] 1) Add 40g of deionized water, 12g of methyl silicone oil and 25g of polyvinyl alcohol into a three-necked flask, control the stirring speed at...

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Abstract

The invention provides a silicon-boron-modified thermosetting phenolic resin hollow microsphere, and a preparation method and an application thereof, and belongs to the technical field of aerospace materials. rovided by the invention still maintain a spherical shape by calcination, and have excellent mechanical properties, indicating that they have excellent ablation resistance. The silicon-boron-modified thermosetting phenolic resin hollow microsphere is prepared from a silicon-boron-modified thermosetting phenolic resin, and the silicon-boron-modified thermosetting phenolic resin is preparedby a bulk polymerization technology. The silicon-boron-modified thermosetting phenolic resin hollow microsphere has excellent ablation resistance, and undergoes ceramic transformation in the ablationprocess to form a silicon-boron oxycarbide ceramic structure, and the ceramic structure has a pinning effect when dispersed in a resin matrix as second phase particles to effectively fix carbon formed after resin cracking. Experimental results show that the silicon-boron-modified thermosetting phenolic resin hollow microsphere still keeps spherical and has excellent mechanical performances afterbeing calcined, so the hollow microsphere has excellent ablation resistance.

Description

technical field [0001] The invention relates to the technical field of aerospace materials, in particular to a silicon-boron modified thermosetting phenolic resin hollow microsphere and a preparation method and application thereof. Background technique [0002] Due to its unique hollow structure, phenolic resin hollow microspheres have become the focus of development in the field of materials at home and abroad. It has the characteristics of low density, low thermal conductivity, excellent thermal stability, etc., and has excellent electrical insulation, mechanical properties, flame retardancy and ablation resistance of phenolic resin. Therefore, it is often dispersed in the resin matrix and used as the ablation layer on the surface of aerospace equipment to isolate the huge heat generated by the intense friction between the spacecraft and the atmosphere, and to protect the normal operation of the internal components of the spacecraft. [0003] Phenolic resin hollow microsp...

Claims

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Application Information

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IPC IPC(8): B01J13/14C08G8/28
CPCB01J13/025B01J13/14C08G8/28
Inventor 陈立新叶文龙赵嘉
Owner RES & DEV INST OF NORTHWESTERN POLYTECHNICAL UNIV IN SHENZHEN
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