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Method for polymethylsilane scale production

A technology of polymethylsilane and toluene, applied in the field of polysilane preparation, can solve the problems of inability to expand production, low safety factor, low output, etc., and achieve the effects of reducing risk, increasing output, and increasing surface area

Active Publication Date: 2016-01-06
湖南前驱新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of low output, inability to expand production, and low safety factor in the existing PMS preparation process, the present invention proposes a new process with low cost, high safety and large-scale production

Method used

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  • Method for polymethylsilane scale production
  • Method for polymethylsilane scale production
  • Method for polymethylsilane scale production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] step one:

[0044] Production of sodium sand: Submerge about 20kg of sodium block in a 100L glass kettle filled with 50L of toluene, install a condensing device and a stirring device, and start heating. pass a certain N 2 Flow rate, start heating, heat for about ten minutes to observe whether the sodium block is dissolved, if it has been dissolved, start to slowly turn on the stirring device, gradually increase the stirring, turn off the heating after stirring for about three minutes, when stirring to powder fine sand , turn off the stirring, and cool down to room temperature.

[0045] Step two:

[0046] Sodium sand pretreatment: Add about 1.5Kg of aluminum powder with a particle size of 50 μm to the glass kettle of sodium sand, and the whole reaction kettle is still under N 2 In the atmosphere, turn on the stirring and make it stir at room temperature for about 48h until the sodium sand turns into a fine powder.

[0047] Step three:

[0048] Feed: Vacuumize the 30...

Embodiment 2

[0062] step one:

[0063] Production of sodium sand: Submerge about 22kg of sodium block in a 100L glass kettle filled with 50L of toluene, install a condensing device and a stirring device, and start heating. pass a certain N 2 Flow rate, start heating, heat for about ten minutes to observe whether the sodium block is dissolved, if it has been dissolved, start to slowly turn on the stirring device, gradually increase the stirring, turn off the heating after stirring for about three minutes, when stirring to powder fine sand , turn off the stirring, and cool down to room temperature.

[0064] Step two:

[0065] Sodium sand pretreatment: Add about 1.8Kg of aluminum powder with a particle size of 40 μm to the glass kettle of sodium sand, and the whole reaction kettle is still under N 2 In the atmosphere, turn on the stirring and make it stir at room temperature for about 48h until the sodium sand turns into a fine powder.

[0066] Step three:

[0067] Feed: Vacuumize the 30...

Embodiment 3

[0081] step one:

[0082] Production of sodium sand: Submerge about 23kg of sodium block in a 100L glass kettle filled with 50L of toluene, install a condensing device and a stirring device, and start heating. pass a certain N 2 Flow rate, start heating, heat for about ten minutes to observe whether the sodium block is dissolved, if it has been dissolved, start to slowly turn on the stirring device, gradually increase the stirring, turn off the heating after stirring for about three minutes, when stirring to powder fine sand , turn off the stirring, and cool down to room temperature.

[0083] Step two:

[0084] Add about 2.0Kg of aluminum powder with a particle size of 30 μm to the glass kettle made of sodium sand, and the whole reaction kettle is still under N 2 In the atmosphere, turn on the stirring and make it stir at room temperature for about 48h until the sodium sand turns into a fine powder.

[0085] Step three:

[0086] Feed: Vacuumize the 300L reactor, and then ...

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Abstract

The invention relates to a method for polymethylsilane (PMS) scale production, and belongs to the technical field of polysilane preparation. The method comprises the steps that sodium sand added with aluminum powder serves as standby sodium sand; after the standby sodium sand and monomers are prepared according to the Na-Si mole ratio of 2.5:1-2:1, under a protection atmosphere, the sodium sand is firstly contained in a reaction kettle, and then organic solvent is added into the reaction kettle; stirring is performed, the temperature is increased to 70 DEG C-85 DEG C, then the mixed monomers are dropwise added into the reaction kettle at least for two times, stirring is performed, and a reflux reaction is performed; an after-reaction solution is obtained, and PMS is obtained after reaction and separation are performed. The method is simple in technology, low in cost, high in safety coefficient and capable of being directly applied to scale production and application.

Description

technical field [0001] The invention relates to a method for large-scale production of polymethylsilane (PMS), belonging to the technical field of polysilane preparation. Background technique [0002] Polysilane is a kind of polymer whose main chain is completely composed of silicon atoms. The 3d empty orbitals of silicon atoms cause σ electrons to be widely delocalized along the Si-Si main chain, thus endowing polysilane with many excellent photoelectric properties, making it as It has broad application prospects in functional materials such as semiconductors, photoconductors and nonlinear optical materials. At the same time, polysilane can also be converted into SiC ceramics after high temperature conversion, and ceramic materials also have great commercial value. [0003] Polymethylsilane (polymethylsilane, PMS) is the simplest composition polysilane, and its basic structural unit is -SiCH 3 H-, C / Si=1 in the molecule, viscous liquid state at room temperature, soluble a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
Inventor 张西岩刘沙金辉亚赵倩倩
Owner 湖南前驱新材料有限公司
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