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Novel method for environmentally and efficiently preparing polycarbosilane

A polycarbosilane and polysilane technology, which is applied in the field of preparation of organosilicon polymer precursors, can solve the problems of long PDMS production cycle and environmental pollution, and achieve the effects of shortening post-processing time, improving recycling rate, and being easy to clean.

Active Publication Date: 2014-02-05
宿迁澳鑫斯新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of long production cycle and environmental pollution in the existing industrial production of PDMS, the present invention provides an environmentally friendly and efficient PDMS synthesis method, which can greatly shorten the post-processing time of PDMS, improve the recycling rate of solvents, and avoid the production of The washed product of pollutants has the advantages of high production efficiency, energy saving and environmental protection

Method used

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  • Novel method for environmentally and efficiently preparing polycarbosilane
  • Novel method for environmentally and efficiently preparing polycarbosilane
  • Novel method for environmentally and efficiently preparing polycarbosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Under the protection of high-purity nitrogen, add refined and purified anhydrous xylene and metal sodium into a three-necked flask, heat until the metal sodium melts, start stirring, and then add dichlorodimethylsilane dropwise after the sodium is dispersed. The crude product of polydimethylsilane was obtained; after cooling to room temperature, the solvent xylene was removed by suction filtration, and the excess sodium was washed with ethanol;

[0027] Add the crude PDMS product into a three-necked flask, pump it with high-purity nitrogen after vacuuming, start stirring and heating, and raise the temperature to different temperature ranges to collect ethanol and xylene respectively. When the temperature of the system rose to 320°C, PDMS began to break and crack, and white vapor appeared in the flask. The vapor was cooled by the condenser tube and collected in the receiving bottle. After the system temperature reaches 420°C, the white vapor decreases, and the N 2 The f...

Embodiment 2

[0030] Under the protection of high-purity argon, add refined and purified anhydrous toluene and metal sodium into the three-necked flask, heat until the metal sodium melts, start stirring, and then add dichlorodimethylsilane dropwise after the sodium is dispersed. The crude product of polydimethylsilane was obtained; after cooling to room temperature, the solvent toluene was removed by suction filtration, and excess sodium was washed with methanol;

[0031] Put the crude PDMS product into a three-necked flask, vacuumize and pass high-purity argon, start stirring and heating, and raise the temperature to different temperature ranges to collect methanol and toluene respectively. When the temperature of the system rose to 320°C, PDMS began to break and crack, and white vapor appeared in the flask. The vapor was cooled by the condenser tube and collected in the receiving bottle. After the system temperature reaches 420°C, the white vapor decreases, and the flow rate of argon gas ...

Embodiment 3

[0034] Under the protection of high-purity nitrogen, add refined and purified anhydrous xylene and metal sodium into a three-necked flask, heat until the metal sodium melts, start stirring, and then add dichlorodimethylsilane dropwise after the sodium is dispersed. The crude product of polydimethylsilane was obtained; after cooling to room temperature, the solvent xylene was removed by suction filtration, and the excess sodium was washed with ethanol;

[0035]Add the crude PDMS product into a three-necked flask, pump it with high-purity nitrogen after vacuuming, start stirring and heating, and raise the temperature to different temperature ranges to collect ethanol and xylene respectively. When the temperature of the system rose to 320°C, PDMS began to break and crack, and white vapor appeared in the flask. The vapor was cooled by the condenser tube and collected in the receiving bottle. After the system temperature reaches 420°C, the white vapor decreases, and the N 2 The fl...

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Abstract

The invention relates to a method for environmentally and efficiently preparing polycarbosilane, comprises the following steps: enabling a reactant dimethyl dichlorosilane to react with metallic sodium in an organic solvent to prepare polysilane, removing the solvent, reacting with residual metallic sodium by using alcohol, directly feeding into a cracking kettle to prepare low-molecular weight liquid state cyclic polysilane, and finally preparing polycarbosilane from the liquid state cyclic polysilane. The method has the advantages that the processes of washing and drying the polysilane for a plurality of times, which are long in time-consuming and capable of producing industrial wastewater, are avoided in an existing process route of producing the polycarbosilane; meanwhile, the solvent and the alcohol adsorbed in the polysilane can be subjected to secondary recycling in the process of preparing the liquid state polysilane. The pilot scale test data shows that compared with the prior art, the method has the advantages that the production period is saved by 30-50%, the solvent recycling rate is increased by 10-20%, the industrial wastewater containing a benzene organic solvent cannot be produced, the working environment is purified, and the reaction residue is fluffy solid residue, and can be easily cleaned from a reaction still.

Description

technical field [0001] The invention belongs to the preparation technology of precursors required in the production of ceramic materials, and in particular relates to the preparation technology of organosilicon polymer precursors. Background technique [0002] The preparation of ceramic materials by the precursor conversion method is an important change in the field of material manufacturing. This method uses organometallic polymers as precursors. After molding using its soluble or fusible properties, it is transformed from organic matter into inorganic ceramic materials through high-temperature cracking. , the production of this method has low requirements on the reaction device, low investment cost, high production efficiency, and is suitable for large-scale production; and the produced fiber diameter is fine, the weaving performance is good, and it is easy to form complex components. In addition, this method can change the composition, structure, and crystal state of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/565
Inventor 杜亮董小虎冯春祥田秀梅
Owner 宿迁澳鑫斯新材料有限公司
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