In-situ ceramization type anti-oxidant resin, resin matrix and ceramic material, as well as preparation method of resin

A technology of anti-oxidation and ceramicization, applied in the field of composite materials, to achieve the effect of convenient operation, good compatibility and simple curing method

Active Publication Date: 2017-06-27
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 ceramization type anti-oxidant resin, resin matrix and ceramic material, as well as preparation method of resin
  • In-situ ceramization type anti-oxidant resin, resin matrix and ceramic material, as well as preparation method of resin
  • In-situ ceramization type anti-oxidant resin, resin matrix and ceramic material, as well as preparation method of resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Embodiment 1, preparation PBSCN-1-1 resin

[0085] Take 85 g of silazane resin 1 (structure shown in formula V) and put it into a 250 ml three-necked flask, and install a magnet and a thermometer. Heating in an oil field, heating up while stirring, until the temperature of the system reaches 80°C. Take by weighing 15g of carborane monomer (structure as shown in IV), quickly add to the flask, increase the stirring force, keep heating, wait for the resin system to be homogeneous and then insulate and stir for 60min, finally obtain PBSCN-1-1 resin, its Infrared spectrum such as figure 1 shown.

[0086] Prepare the resin matrix (resin cured product) according to the curing system of (140°C, 3h)+(180°C, 3h)+(240°C, 2h). Use N 2 TGA under air atmosphere characterizes its heat resistance performance, the heating rate is 10°C / min, and the temperature range is 25-900°C. Test results such as image 3 as shown, image 3 The PBSCN-1-1 resin prepared for the embodiment of the...

Embodiment 2

[0088] Embodiment 2, preparation PBSCN-1-2 resin

[0089] Take 71 g of silazane resin 1 (structure shown in V) and put it into a 250 ml three-necked flask, and install a magnet and a thermometer. Heating in an oil field, heating up while stirring, until the temperature of the system reaches 80°C. Weigh 29g of carborane monomer (structure as shown in IV), quickly add to the flask, increase the stirring force, keep heating, and keep stirring for 60min after the resin system is homogeneous, finally get PBSCN-1-2 resin.

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

[009...

Embodiment 3

[0092] Embodiment 3, preparation PBSCN-2-1 resin

[0093] Take 85 g of silazane resin 2 (structure as shown in VI) and put it into a 250 ml three-necked flask, and install a magnet and a thermometer. Heating in an oil field, heating up while stirring, until the temperature of the system reaches 80°C. Take by weighing 15g of the carborane monomer (structure shown in IV), add it into the flask quickly, increase the stirring force, keep heating, and wait for the resin system to be homogeneous and then insulate and stir for 30min to finally obtain the PBSCN-2-1 resin. Infrared spectrum such as figure 2 shown.

[0094] According to the curing system of (140°C, 3h)+(180°C, 3h)+(240°C, 2h), the cured resin was prepared. Use N 2 TGA under air atmosphere characterizes its heat resistance performance, the heating rate is 10°C / min, and the temperature range is 25-900°C. The cured product in N 2 T in air atmosphere d5 (The thermal decomposition temperature when the weight loss of ...

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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 ceramizable anti-oxidation resin, a resin matrix, a ceramic material and a resin preparation method, belonging to the technical field of composite materials. Background technique [0002] With the deepening of human exploration, the demand for high temperature resistant materials is becoming more and more stringent. Due to the relatively high density, high thermal conductivity and insufficient carbon residue rate of the existing resin-based heat-resistant composite material matrix such as phenolic formaldehyde, it is difficult to further meet the future use requirements in the aviation and aerospace fields. Therefore, a new type of heat-resistant composite material is developed High temperature resistant resins are urgently needed. In recent years, organic-inorganic hybrid resins of the Si-C-N system have become the focus of attention in the field of high-temperature resistant resins because of their excellent therm...

Claims

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Application Information

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Patent Type & Authority Applications(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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