High silica fiber reinforced reactive silsesquioxane modified hybrid phenolic aldehyde composite material and preparation method thereof

A technology of silsesquioxane and high silica fiber, which is applied in the field of hybrid phenolic composite materials and preparation, can solve the problems of high price, monopoly of synthesis methods, cumbersome purchasing routes, etc., and achieves low chemical toxicity and improved heat resistance. , the effect of suitable for large-scale production

Active Publication Date: 2020-12-29
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the vast majority of literature, POSS is provided by Hybird Plastics of the United States, and the price is high, and the purchase method is cumbersome, and the related synthesis method is monopolized by Hybird Plastics

Method used

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  • High silica fiber reinforced reactive silsesquioxane modified hybrid phenolic aldehyde composite material and preparation method thereof
  • High silica fiber reinforced reactive silsesquioxane modified hybrid phenolic aldehyde composite material and preparation method thereof
  • High silica fiber reinforced reactive silsesquioxane modified hybrid phenolic aldehyde composite material and preparation method thereof

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preparation example Construction

[0038] The present invention provides a method for synthesizing silsesquioxane described in the above technical scheme, comprising the following preferred steps:

[0039]In a nitrogen-protected three-necked flask equipped with a magnet and a condenser, first add isopropanol (120-150mL), then phenyltrimethoxysilane (24.0g, 121mmol), deionized water (2.5g, 139mmol ) and NaOH (3.2 g, 80 mmol) were added successively, and the mixture was reacted under reflux for 4 hours, then cooled to room temperature and reacted for 15-18 hours. After the reaction, remove most of the isopropanol with a rotary evaporator, filter to obtain a white solid, and vacuum-dry at 60° C. for 12 to 24 hours to obtain octaphenylcyclotetrasiloxane sodium tetrasilicate (DDONa) with a yield of 90 ~98%. Dissolve the above DDONa (11.6g, 10mmol) in a one-necked flask equipped with tetrahydrofuran and a magnet, add a certain amount of glacial acetic acid (3.0mL, 53mmol) and stir for 15-30 minutes, then add a certa...

Embodiment 1

[0056] In a nitrogen-protected three-necked flask equipped with a magnet and a condenser, first add isopropanol (120mL), then phenyltrimethoxysilane (24.0g, 121mmol), deionized water (2.5g, 139mmol) and NaOH (3.2 g, 80 mmol) was added successively, and the mixture was reacted under reflux for 4 hours, then cooled to room temperature and reacted for 15 hours. After the reaction was completed, most of the isopropanol was removed by a rotary evaporator, and a white solid was obtained by filtration, and vacuum-dried at 60° C. for 12 hours to obtain sodium octaphenylcyclotetrasiloxane tetrasilicate (DDONa), with a yield of 98%. Dissolve the above DDONa (11.6g, 10mmol) in a single-necked flask equipped with tetrahydrofuran and a magnet, add a certain amount of glacial acetic acid (3.0mL, 53mmol) and stir for 30 minutes, then add a certain amount of saturated sodium bicarbonate solution (10mL) to neutralize the unreacted acid, add (20mL) n-hexane to the flask, stop stirring, let stan...

Embodiment 2

[0058] (1) Weigh 0.954g of tetrasilanol octaphenylsilsesquioxane, dissolve it in 3.816g of acetone, stir and oscillate until completely dissolved, and obtain a silsesquioxane solution with a mass fraction of 20%;

[0059] (2) Weigh 52.5g of phenolic resin solution with a solid content of 59.4%, add the above-mentioned tetrasilanol octaphenylsilsesquioxane solution into the phenolic resin solution, stir with a homogeneous stirrer for 30 minutes until uniformly mixed, Obtain a modified phenolic resin solution (silsesquioxane accounts for 3% of the total mass except the solvent);

[0060] (3) Put the modified phenolic resin into a 75°C vacuum oven to remove the solvent for 4 hours. During the solvent removal process, the vacuum should be released at any time to remove the extracted solvent;

[0061] (4) The above-mentioned modified resin after removing the solvent is directly cured in stages: 100° C. / 3 hours; 130° C. / 2 hours; 150° C. / 2 hours; 170° C. / 2 hours; natural cooling. Th...

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Abstract

The invention relates to a high silica fiber reinforced reactive silsesquioxane modified hybrid phenolic composite material and a preparation method thereof. Hybrid phenolic resin is prepared from POSS modified phenolic resin with a silicon hydroxyl structure, high silica fiber is impregnated with the hybrid phenolic resin to prepare a prepreg, and the fiber reinforced composite material is prepared through hot press molding. POSS and phenolic resin are subjected to a cross-linking reaction, and introduction of POSS hybrid molecules plays a role in nanoparticle reinforcement. The mass loss ofthe hybrid resin is 5%, the temperature is increased to 385.5 DEG C from 306.6 DEG C, and the heat resistance of the material is improved. The linear ablation rate of the fiber reinforced composite material is reduced from 0.191 mm/s to 0.163 mm/s, the mass ablation rate is reduced from 0.0703 g/s to 0.0643 g/s, and the ablation resistance of the material is remarkably improved. The high silica fiber reinforced POSS modified phenolic resin-based composite material provided by the invention has a wide application prospect in the fields of aerospace craft resin-based advanced thermal protectionmaterials and engine exhaust nozzle thermal insulation materials.

Description

technical field [0001] The invention belongs to the technical field of ablation-resistant composite materials, and relates to a high-silica fiber-reinforced reactive silsesquioxane (POSS) modified hybrid phenolic composite material and a preparation method. Background technique [0002] As a synthetic resin, phenolic resin has been widely used as an ablation-resistant matrix resin material for aerospace shell heat due to its simple synthesis, convenient use, excellent instantaneous temperature resistance and high thermal residual rate. Protective layer and engine exhaust nozzle, etc. With the development of aerospace science and technology, higher requirements are put forward for the heat resistance and ablation resistance of phenolic resins, which has become a hot spot in the research on the modification of phenolic resins in recent years. Because phenolic resin has a high carbon residue rate, it is difficult to further improve its heat resistance and ablation performance....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/14C08K7/10C08G8/28C08G77/04C08G77/06
CPCC08K7/10C08G8/28C08G77/045C08G77/06C08L2201/10C08L61/14
Inventor 马晓燕牛肇淇申帅李璐阳
Owner NORTHWESTERN POLYTECHNICAL UNIV
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