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Cage-shaped oligomerization silsesquioxane hybridized phenolic resin with eight phenolic hydroxyl groups and preparation method thereof

The technology of polysilsesquioxane and octaphenol hydroxyl cage is applied in the field of octaphenol hydroxyl cage oligomeric silsesquioxane hybrid phenolic resin and its preparation, and can solve the problem of increasing the thermal and mechanical properties of resin, POSS Agglomeration, affecting performance and other problems, to achieve the effect of increasing thermal properties and tensile properties, improving oxidation resistance, and improving inherent properties

Active Publication Date: 2016-01-20
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The oxidation resistance and mechanical modulus of the phenolic resin physically doped with POSS are increased, especially the increase of its modulus is the most significant, and the tensile properties of the material are basically unchanged, because POSS has a similar polymer chain segment The nanometer size, so it can control the chain segment movement of the polymer, maintain its mechanical properties, and greatly increase the thermal and mechanical properties of the resin. However, the phenolic resin physically doped by POSS is prone to agglomeration, which affects its performance.
Based on the above objectives, the development of a new type of POSS hybrid phenolic resin grafted with phenolic hydroxyl groups to solve the problem that physical doping will cause POSS to a large extent to be agglomerated has become an urgent problem to be solved.

Method used

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  • Cage-shaped oligomerization silsesquioxane hybridized phenolic resin with eight phenolic hydroxyl groups and preparation method thereof
  • Cage-shaped oligomerization silsesquioxane hybridized phenolic resin with eight phenolic hydroxyl groups and preparation method thereof
  • Cage-shaped oligomerization silsesquioxane hybridized phenolic resin with eight phenolic hydroxyl groups and preparation method thereof

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preparation example Construction

[0043] The preparation method of octaphenol hydroxyl cage oligomeric silsesquioxane hybridized thermosetting phenolic resin of the present invention comprises the following steps:

[0044] (1), dissolve 100~200 parts of phenols in 85~175 parts of formaldehyde solution by mass ratio, add 1~50 parts of octaphenol hydroxyl cage oligomeric silsesquioxane as reactants, 40~50 ℃ Stir in a water bath for 10 to 30 minutes, then add 0.2 to 3 parts of barium hydroxide octahydrate to adjust the pH of the solution to 8 to 9, slowly heat up to 60 to 70°C, and carry out a constant temperature reaction for 1 to 3 hours; the heating rate is 0.16 to 0.33°C / min;

[0045] (2), slowly warming up the solution obtained in step (1) from 60~70 ℃ to 85~98 ℃, carry out constant temperature reaction 1~3h, and heating rate is 0.16~0.33 ℃ / min;

[0046] (3), add 0.3~3.5 parts of phosphoric acid solution, adjust the pH value of the solution obtained in step (2) to be 5~6, after stirring for 10~20min, under...

Embodiment 1

[0068] According to mass parts, 130 parts of phenol were dissolved in 140 parts of formaldehyde solution, and 20 parts of octaphenol hydroxyl clathrate oligomeric silsesquioxane were added, stirred in a water bath at 40°C for 30 minutes, and then 1.4 parts of barium hydroxide octahydrate was added to adjust the solution The pH value of the solution is 8 to 9, and the temperature is slowly raised to 60 °C, and the constant temperature reaction is carried out for 3h; the heating rate is 0.25 °C / min; the mass concentration of the formaldehyde solution is 37%.

[0069] The above solution was slowly heated from 60°C to 95°C, and a constant temperature reaction was carried out for 1 h, and the heating rate was 0.25°C / min;

[0070] Add 1.6 parts of phosphoric acid solution, adjust the pH value of the above solution to 5-6, stir for 15 minutes, stir and dehydrate in a water bath at 95°C for 1 hour under vacuum conditions, stand, precipitate, filter, cool to room temperature, and take o...

Embodiment 2

[0080] According to parts by mass, dissolve 100 parts of phenol in 85 parts of formaldehyde solution, add 1 part of octaphenolic hydroxyl clathrate oligomeric silsesquioxane, stir in a water bath at 40°C for 30 minutes, and then add 0.2 parts of barium hydroxide octahydrate to adjust the solution The pH value of the mixture is 8-9, and the temperature is slowly raised to 60° C., and the constant temperature reaction is carried out for 1-3 hours; the heating rate is 0.16° C. / min; the mass concentration of the formaldehyde solution is 35%.

[0081] Slowly raise the temperature of the above solution from 60°C to 95°C, carry out constant temperature reaction for 1 hour, and the heating rate is 0.16°C / min;

[0082] Add 0.3 parts of phosphoric acid solution, adjust the pH value of the above solution to 5-6, stir for 15 minutes, and dehydrate in a water bath at 95°C under vacuum for 3 hours, let stand, precipitate, filter, cool to room temperature, and take out the upper layer of pure...

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Abstract

The invention relates to cage-shaped oligomerization silsesquioxane hybridized phenolic resin with eight phenolic hydroxyl groups and a preparation method thereof. The phenolic resin is prepared by taking, by mass, 100-200 parts of phenol, 85-175 parts of formaldehyde solutions and 1-50 parts of cage-shaped oligomerization silsesquioxane as the reactants and taking, by mass, 0.2-3 parts of barium hydroxide octahydrate and 0.3-3.5 parts of phosphoric acid solutions as conditioning agents to adjust the PH value of the reactants. By means of the cage-shaped oligomerization silsesquioxane hybridized phenolic resin with the eight phenolic hydroxyl groups and the preparation method thereof, the dispersity problem of physical doped POSS in the phenolic resin is solved, the phenolic resin material which is better in dispersity and evener is obtained, and the oxidation resistance, the thermal property and the mechanical property are improved.

Description

technical field [0001] The invention relates to an octaphenol hydroxyl polyhedron cage silsesquioxane (OP-POSS) hybridized phenol-formaldehyde phenolic resin and a preparation method thereof, which are used for ablation of a heat-resistant resin-based composite material. Background technique [0002] Faced with the increasingly demanding requirements for ablative and heat-resistant composite materials in the aerospace and military industries, higher requirements have been placed on the oxidation resistance, ablation resistance and mechanical properties of the phenolic resin matrix. In recent years, the structural modification of phenolic resins become a research hotspot in this field. Since the U.S. Air Force Laboratory used polyhedral oligomeric silsesquioxane (POSS) to prepare high-temperature aerospace materials in the 1990s, the related research on POSS and its graft-modified polymer-doped phenolic resin has been widely studied. s concern. [0003] It can be considered...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08G8/10
Inventor 胡宏林冯志海余瑞莲师建军王伟
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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