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Preparation method for composite resin system copolymerized by silicon dioxide and epoxy resin and compatible with liquid oxygen

A technology of epoxy resin and silicon dioxide, which is applied in the field of preparation of organic polymer compounds, can solve problems such as unusable resin materials, and achieve the effects of improved toughness, high efficiency and mild reaction conditions

Active Publication Date: 2017-04-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Because resin materials and liquid oxygen have far more serious compatibility problems than metal materials, it has been generally believed that resin materials cannot be used as liquid oxygen structural materials for a long time.

Method used

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  • Preparation method for composite resin system copolymerized by silicon dioxide and epoxy resin and compatible with liquid oxygen
  • Preparation method for composite resin system copolymerized by silicon dioxide and epoxy resin and compatible with liquid oxygen
  • Preparation method for composite resin system copolymerized by silicon dioxide and epoxy resin and compatible with liquid oxygen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1. Mix bisphenol F epoxy resin (epoxy value 0.51mol / 100g), 3-chloropropyltriethoxysilane in a molar ratio of 15:1, add 0.2% dibutyltin dilaurate of total mass (catalyst), and reacted at 50° C. for 2 hours to obtain a siloxane-modified glycidyl ether epoxy resin (a).

[0030] Step 2. Mix 21.6g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 21g of allyltriethoxysilane, add 30ml of toluene solvent, heat up to 80°C, and Under the reflux condensing device, stir with a magnetic stirrer for 10 minutes to completely dissolve 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and add 0.2 g of azobisisobutyronitrile as a catalyst. Reaction 2h. Distill under reduced pressure to remove the solvent to obtain a light yellow viscous modified phosphorus-containing antioxidant (b).

[0031] Step 3. Mix 46g of silane-modified epoxy resin (a), 4g of silane-modified antioxidant (b), and 2.1g of tetraethyl orthosilicate into 100ml of solvent acetone, and stir well to make th...

Embodiment 2

[0036] Step 1. Mix bisphenol F epoxy resin (epoxy value 0.51mol / 100g) and dichlorodimethylsilane at a molar ratio of 10:1, and react at 30°C for 2 hours to obtain siloxane-modified glycidol Ether epoxy resin (a).

[0037] Step 2. Mix 20g of diphenylphosphine and 21g of allyltriethoxysilane, add 30ml of toluene solvent, heat up to 80°C, and stir for 10min with a magnetic stirrer under the reflux condensing device to make diphenylphosphine Oxygen was completely dissolved, and 0.2 g of azobisisobutyronitrile was added as a catalyst for 2 hours of reaction. Distill under reduced pressure to remove the solvent to obtain a light yellow viscous modified phosphorus-containing antioxidant (b).

[0038] Step 3. Mix 40g of silane-modified epoxy resin (a), 4g of silane-modified antioxidant (b), and 2.4g of trimethoxysilane into 100ml of solvent acetone, and stir well to make the components evenly mixed.

[0039] Step 4. Add 1.5g deionized water and 0.1g acetic acid, react at 30°C for 3h...

Embodiment 3

[0043] Step 1. Mix bisphenol A epoxy resin (epoxy value 0.51mol / 100g), 3-chloropropyltriethoxysilane in a molar ratio of 15:1, add 0.2% dibutyltin dilaurate of total mass (catalyst), and reacted at 50° C. for 2 hours to obtain a siloxane-modified glycidyl ether epoxy resin (a).

[0044] Step 2. Mix 20g of diphenylphosphine and 21g of allyltriethoxysilane, add 30ml of toluene solvent, heat up to 80°C, and stir for 10min with a magnetic stirrer under the reflux condensing device to make diphenylphosphine Oxygen was completely dissolved, and 0.2 g of azobisisobutyronitrile was added as a catalyst for 2 hours of reaction. Distill under reduced pressure to remove the solvent to obtain a light yellow viscous modified phosphorus-containing antioxidant (b).

[0045] Step 3. Mix 46g of silane-modified epoxy resin (a), 4g of silane-modified antioxidant (b), and 2.1g of tetraethyl orthosilicate into 100ml of solvent acetone, and stir well to make the components evenly mixed.

[0046] S...

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Abstract

The invention discloses a preparation method for a composite resin system copolymerized by silicon dioxide and epoxy resin and compatible with liquid oxygen. The preparation method comprises the following steps: 1, subjecting glycidyl ether epoxy resin and silane to a reaction so as to prepare silane modified epoxy resin; 2, subjecting a phosphorus-containing antioxidant substance and silane to a reaction so as to prepare a silane modified antioxidant; 3, mixing the silane modified epoxy resin, the silane modified antioxidant and a silicon dioxide precursor, dissolving the mixture into a solvent, and carrying out heating to 40 to 60 DEG C; and 4, adding deionized water and a catalyst, carrying out a reaction for 1 to 5 hours, and carrying out decompressing so as to remove product water and the solvent. According to the invention, a nanometer silicon dioxide unit and antioxidant molecules are covalently introduced into the epoxy resin system, and well-known mechanical strength may not be decreased after introduction, so the antioxidant may not be precipitated and leaked out of a resin substrate; and through the introduction of the silicon dioxide unit, the toughness of the cured resin is significantly improved, and the use safety of the epoxy resin used as a substrate material of a liquid oxygen storage tank is greatly improved.

Description

technical field [0001] The invention belongs to the field of preparation of organic macromolecular compounds, and in particular relates to a synthesis method of a composite resin system in which silicon dioxide and epoxy resin are copolymerized and are compatible with liquid oxygen. Background technique [0002] As a power source for spacecraft flight, liquid oxygen is indispensable in the field of aerospace. Traditional liquid oxygen storage tanks are made of metal materials. With the intensification of international competition in the space field, reducing the launch cost of space vehicles and improving the carrying capacity have become the goals pursued by every space power. The new generation of reusable spacecraft and low-cost spacecraft put forward higher requirements for light weight and low cost of materials, and the main structural components of the aircraft have to rely on various composite materials with excellent light weight and high performance. If resin-base...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/14
CPCC08G59/1433C08G59/1438C08G59/1488C08G59/1494
Inventor 武湛君彭聪孙涛王智刘新
Owner DALIAN UNIV OF TECH
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