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In-situ ceramizable anti-oxidation resin, resin matrix, ceramic material and resin preparation method

A technology of anti-oxidation and ceramicization, applied in the field of composite materials, to achieve the effects of cost reduction, convenient operation and good compatibility

Active Publication Date: 2020-02-14
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, this method and the currently existing methods for preparing SiBCN resins generally require the use of solvents, and both utilize polycondensation reactions to polymerize. In the process of preparing polymers, volatile small molecule by-products will be produced. Therefore, the solvent and by-products Product removal is an unavoidable problem for this type of method

Method used

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  • In-situ ceramizable anti-oxidation resin, resin matrix, ceramic material and resin preparation method
  • In-situ ceramizable anti-oxidation resin, resin matrix, ceramic material and resin preparation method
  • In-situ ceramizable anti-oxidation resin, resin matrix, ceramic material and resin preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Example 1. Preparation of PBSCN-1-1 resin

[0085] Take 85g of silazane resin 1 (structure shown in formula V) and put it into a 250ml three-necked flask, install magnet and thermometer. Use oil field heating, while stirring, increase the temperature until the temperature of the system reaches 80°C. Weigh 15 g of carborane monomer (structure shown in IV), quickly add it to the flask, increase stirring, and keep heating. After the resin system becomes homogeneous, keep it warm and stir for 60 minutes to obtain PBSCN-1-1 resin. Infrared spectra such as figure 1 Shown.

[0086] Prepare the resin matrix (resin cured product) according to the curing system of (140℃, 3h) + (180℃, 3h) + (240℃, 2h). Use N 2 TGA under air atmosphere characterizes its heat resistance, the heating rate is 10℃ / min, and the temperature range is 25-900℃. The test result is like image 3 As shown, image 3 The PBSCN-1-1 resin prepared in Example 1 of the present invention is in N 2 TG / DTG curve under ai...

Embodiment 2

[0088] Example 2: Preparation of PBSCN-1-2 resin

[0089] Take 71 g of silazane resin 1 (structure as V) into a 250ml three-necked flask, install magnet and thermometer. Use oil field heating, while stirring, raise the temperature until the system heats up to 80°C. Weigh 29 g of carborane monomer (structure as shown in IV), quickly add it to the flask, increase stirring, and keep heating. After the resin system is in a homogeneous phase, keep it warm and stir for 60 minutes to obtain PBSCN-1-2 resin.

[0090] Prepare the resin matrix (resin cured product) according to the curing system of (140℃, 3h) + (180℃, 3h) + (240℃, 2h). Use N 2 TGA under air atmosphere characterizes its heat resistance, the heating rate is 10℃ / min, and the temperature range is 25-900℃. The cured product is in N 2 T in the atmosphere d5 (The thermal decomposition temperature at 5% weight loss of the resin) is 391°C; the carbon residue rate at 900°C is 65.8%.

[0091] TGA under air atmosphere is used to charac...

Embodiment 3

[0092] Example 3. Preparation of PBSCN-2-1 resin

[0093] Take 85g of silazane resin 2 (structure as VI) and put it into a 250ml three-necked flask, and install a magnet and a thermometer. Use oil field heating, while stirring, increase the temperature until the temperature of the system reaches 80°C. Weigh 15 g of carborane monomer (structure shown in IV), quickly add it to the flask, increase stirring, and keep heating. After the resin system becomes homogeneous, keep it warm and stir for 30 minutes, and finally get PBSCN-2-1 resin. Infrared spectra such as figure 2 Shown.

[0094] Prepare resin cured product according to the curing system of (140℃, 3h) + (180℃, 3h) + (240℃, 2h). Use N 2 TGA under air atmosphere characterizes its heat resistance, the heating rate is 10°C / min, and the temperature range is 25-900°C. The cured product is in N 2 T in the atmosphere d5 (The thermal decomposition temperature at 5% weight loss of the resin) is 464°C; the carbon residue rate at 900°C...

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Abstract

The invention relates to in-situ ceramization type anti-oxidant resin, resin matrix and ceramic material, as well as a preparation method of the resin. Carborane and silazane serve as raw materials, a solvent is not used in the preparation process, Diels-Alder addition reaction and cross-linking solidification are conducted through vinyl under the action of an initiator, the raw materials and the vinyl perform hydrosilylation reaction when the raw materials contain a Si-H group, and the two kinds of reaction form a compact three-dimensional space network structure, so that the resin has excellent heat resistance; micromolecular byproducts in the condensation polymerization process are avoided by utilizing vinyl addition and hydrosilylation reaction; in addition, the resin system has high oxidation resistance, can be subjected to in-situ ceramization under the action of high temperature, is high in ceramic yield, and can serve as a resin matrix or a ceramic precursor of a heat-resistant composite material to be applied to the fields of national defense, aviation, spaceflight and the like.

Description

Technical field [0001] The invention relates to an in-situ ceramicization type antioxidant resin, a resin matrix, a ceramic material and a resin preparation method, and belongs to the technical field of composite materials. Background technique [0002] With the continuous deepening of human exploration, the demand for high-temperature materials has become more and more demanding. Existing phenolic and other resin-based thermal insulation composite matrixes are difficult to further meet the future needs of aviation and aerospace due to their relatively high density, high thermal conductivity and insufficient carbon residue rate. Therefore, a new type of High temperature resistant resins are urgent. In recent years, the organic-inorganic hybrid resin of the Si-CN system has become the focus of attention in the research field of high temperature resins due to its excellent thermal stability, such as high temperature resistance and oxidation resistance, and mechanical properties su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/398C04B35/589
CPCC04B35/589C04B2235/3821C08G77/398
Inventor 冯志海姚祺左小彪颜雪王筠孔磊
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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