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A kind of method of sol-gel method modified benzoxazine resin/epoxy resin copolymer

A technology of sol-gel method and epoxy resin, which is applied in the field of preparation of organic polymer compounds, can solve the problems of low thermal stability of the blend system, toughness is not as good as that of pure epoxy resin, and does not maximize its advantages, and achieves thermal stability. Excellent stability, reduced thermal stability, and improved toughness

Active Publication Date: 2019-04-09
江苏君澄空间科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the traditional benzoxazine resin / epoxy resin co-curing system improves the toughness of the benzoxazine resin to a certain extent, and the thermal stability of the mixture is higher than that of the corresponding epoxy resin cured product, however, simple co-curing Mixed curing is only a compromise between the advantages of the two resins. The thermal stability of the blended system is lower than that of pure benzoxazine resin, and its toughness is not as good as that of pure epoxy resin. It does not maximize the advantages of the two resins.

Method used

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  • A kind of method of sol-gel method modified benzoxazine resin/epoxy resin copolymer

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Experimental program
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Effect test

Embodiment 1

[0039] Step 1. with bisphenol F epoxy resin (epoxy value 0.51), 3-isocyanopropyltriethoxysilane is mixed with molar ratio 15: 1, and adding quality is 0.2% of the above-mentioned reactant quality sum Dibutyltin laurate (catalyst) was reacted at 50° C. for more than 5 hours to obtain a siloxane-modified glycidyl ether epoxy resin (a).

[0040] Step 2. Silicone-modified glycidyl ether epoxy resin (a), bisphenol A benzoxazine resin (b), and tetraethyl orthosilicate (c) are mixed according to the molar ratio of 1.5:0.8:0.2 , dissolved in acetone, heated to 50°C, the amount of the acetone added is twice the sum of the mass of the siloxane-modified glycidyl ether epoxy resin, the benzoxazine resin and the silica precursor.

[0041] Step 3. adding an aqueous acetic acid solution with a pH of 3-4 to the solution obtained in step 2, the amount of the aqueous acetic acid solution being 5% of the total mass of the reactants in step 2.

[0042] Step 4. After reacting for 3 hours, remove ...

Embodiment 2

[0046] Step 1. with bisphenol F epoxy resin (epoxy value 0.51), 3-isocyanopropyltriethoxysilane is mixed with molar ratio 10:1, and adding quality is 0.2% of the above-mentioned reactant quality sum Dibutyltin laurate was reacted at 50° C. for more than 5 hours to obtain a siloxane-modified glycidyl ether epoxy resin (a).

[0047] Step 2. Silicone-modified glycidyl ether epoxy resin (a), bisphenol A benzoxazine resin (b), and tetraethyl orthosilicate (c) are mixed according to the molar ratio of 2:1:0.3 , dissolved in acetone, the solution is heated to 50 ° C, the addition of the acetone is siloxane-modified glycidyl ether epoxy resin, benzoxazine resin and silica precursor mass sum of 4 times.

[0048] Step 3. adding an aqueous acetic acid solution with a pH of 3-4 to the solution obtained in step 2, the amount of the aqueous acetic acid solution being 4% of the total mass of the reactants in step 2.

[0049] Step 4. After reacting for 3 hours, water and acetone were remove...

Embodiment 3

[0052] Step 1. with bisphenol F epoxy resin (epoxy value 0.51), 3-isocyanopropyltriethoxysilane is mixed with molar ratio 10:1, and adding quality is 0.2% of the above-mentioned reactant quality sum Dibutyltin laurate was reacted at 50° C. for more than 5 hours to obtain a siloxane-modified glycidyl ether epoxy resin (a).

[0053] Step 2. Silicone-modified glycidyl ether epoxy resin (a), bisphenol A benzoxazine resin (b), and tetraethyl orthosilicate (c) are mixed according to the molar ratio of 1:1:0.1 , dissolved in acetone, and the solution was heated to 50°C. The amount of acetone added is twice the sum of the mass of the siloxane-modified glycidyl ether epoxy resin, the benzoxazine resin and the silica precursor.

[0054] Step 3. adding an aqueous acetic acid solution with a pH of 3-4 to the solution obtained in step 2, the amount of the aqueous acetic acid solution being 4% of the total mass of the reactants in step 2.

[0055] Step 4. After reacting for 3 hours, water...

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Abstract

The invention provides a method used for modifying a benzoxazine resin / epoxy resin copolymer via sol-gel method. The method comprises following steps: 1, siloxane-modified glycidyl ether epoxy resin, benzoxazine resin, and silicon dioxide precursor are mixed, and are dissolved in acetone, and an obtained mixture is heated to 50 DEG C; 2, an acetic acid aqueous with a pH value ranging from 3 to 4 is added, wherein the adding amount of the acetic acid aqueous accounts for 4 to 6% of the total mass amount of the reagents in step 1; and 3, after 3h of reaction, water and acetone are removed via pressure reduction so as to obtain the modified benzoxazine resin / epoxy resin copolymer. According to the method, chemical method is adopted, so that flexible silicon oxygen bonds are introduced into the benzoxazine resin / epoxy resin copolymer network successfully, toughness and thermal stability are both increased obviously because of introduction of silicon oxygen bonds, and performance advantages of the two resins in the matrix are achieved as far as possible.

Description

technical field [0001] The invention belongs to the field of preparation of organic polymer compounds, and in particular relates to a method for modifying a benzoxazine resin / epoxy resin copolymer by a sol-gel method. Background technique [0002] In recent years, the demand for composite materials in the aerospace field has been increasing, and due to the special conditions of use, more stringent requirements have been put forward for their performance. Compared with ordinary composite materials, composite materials based on aerospace applications must not only meet the basic mechanical performance requirements, but also have good high temperature resistance. The heat resistance of composite materials largely depends on the structure of the matrix resin and the formulation of the curing system. [0003] As a new type of thermosetting resin, benzoxazine resin has attracted more and more attention because of its excellent performance and flexibility in molecular design. Ben...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G59/14
CPCC08G59/1405C08G59/1438C08G81/00
Inventor 武湛君彭聪刘新孙涛
Owner 江苏君澄空间科技有限公司
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