New process for industrialized production of ultralow-oxygen narrow-MWD (Molecular Weight Distribution) polydimethylsilane

A technology of polydimethylsilane and narrow molecular weight distribution, which is applied in the field of new industrial production process of polydimethylsilane with narrow molecular weight distribution in ultra-low oxygen, and can solve the problems of unsuitable industrial production, difficult control, and small synthesis scale.

Inactive Publication Date: 2013-02-06
江西星火狮达科技有限公司
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Problems solved by technology

Among them, the synthesis of polysilane by Wurtz coupling method is the earliest and most commonly used method for synthesizing polysilane. The polysilane synthesized has stable performance. At the same time, the Wurtz method has the advantages of simple method and strong operability; but due to the violent reaction of this method , releases a lot of heat and is difficult to control, so the synthesis scale is very small, generally the output of each synthesis is only 10 g~15 g, and the yield is only about 50%, which is not suitable for industrial production

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  • New process for industrialized production of ultralow-oxygen narrow-MWD (Molecular Weight Distribution) polydimethylsilane
  • New process for industrialized production of ultralow-oxygen narrow-MWD (Molecular Weight Distribution) polydimethylsilane

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Embodiment Construction

[0013] The technical content of the present invention will be further described in conjunction with the accompanying drawings.

[0014] Such as figure 1 As shown, the new industrial production process of polydimethylsilane with ultra-low oxygen and narrow molecular weight distribution is synthesized by Wurtz method: 1. First, the used solvent xylene is dehydrated with anhydrous calcium chloride to reduce the water content to below 5ppm; 2. Add 1,000 kg of dewatered xylene into the frequency conversion rake reactor, then add 300 kg of metallic sodium, heat to 110°C, and start the high-speed stirring paddle to beat it into "sodium sand" after the sodium is melted, and reflux 24 hours to fully dry the solvent and remove harmful impurities; 3. Under the protection of inert gas, add pre-refined dimethyl dichlorosilane to the frequency conversion rake reactor for reaction, and open the external multi-stage cooling circulation system, The reactant turns from gray to purple. After re...

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Abstract

The invention provides a new process for industrialized production of ultralow-oxygen narrow-MWD (Molecular Weight Distribution) polydimethylsilane. The ultralow-oxygen narrow-MWD polydimethylsilane is synthesized by adopting a Wurtz method. The new process comprises the following processing steps of: firstly drying a solvent required for reaction, carrying out secondary rectification for dimethyl dichlorosilane in advance to improve the purity of dimethyl dichlorosilane, installing a temperature and humidity controller in a factory to ensure that the environmental humidity is below 40%, and the like, so that the oxygen content in produced polydimethylsilane is minimized (only 0.1%), the polydimethylsilane can reach the product performance of developed countries, and more qualified silicon carbide ceramic fiber can be prepared; an external multi-stage cooling circulatory system is adopted to timely discharge heat released in the Wurtz synthesis method so as to guarantee safe and smooth industrial production; a reactor has the dual advantages of the stability of glass and metal strength, thus being excellent corrosion-resistant equipment, fully meeting the requirements of the Wurtz method, and realizing the industrialized application of the Wurtz coupling method to synthesizing polydimethylsilane.

Description

technical field [0001] The invention relates to an industrialized production process of polymer materials, in particular to a new industrialized production process of polydimethylsilane with ultra-low oxygen and narrow molecular weight distribution. Background technique [0002] Polydimethylsilane is a polymer material whose main chain is composed of silicon atoms. Due to Si's low electronegativity and 3d empty orbitals, electrons can be widely delocalized along the Si-Si main chain, and it also contains abundant Si-H bonds, so that polydimethylsilane can be used in photoconductive, Light-emitting diodes, nonlinear optical materials, and SiC ceramic preparation and functional materials all have very good application prospects. As a new type of functional polymer material, polydimethylsilane is of great significance both in theory and in practice. Polydimethylsilane chemistry has become a hot spot in the field of organosilicon. Research is very active. With the deepening o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
Inventor 游孟松
Owner 江西星火狮达科技有限公司
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