氯硅烷中甲基二氯硅烷的转化反应工艺 急
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TQ127.2

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国家自然科学基金项目(面上项目,重点项目,重大项目)


Conversion reaction process of methyldichlorosilane in chlorosilane
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The National Natural Science Foundation of China (General Program, Key Program, Major Research Plan)

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    摘要:

    为了除去多晶硅原料中主要含碳杂质甲基二氯硅烷,通过催化反应将其转化为高沸点物质甲基三氯硅烷。采用浸渍法制备了Pd/Al2O3催化剂,采用X射线荧光光谱(XRF)、X射线粉末衍射(XRD)、N2吸附脱附(BET)、光电子能谱仪(XPS)、H2-脉冲化学吸附等分析手段对催化剂物化性质进行表征。在氯源物质为四氯化碳条件下,利用固定床反应器,对比了制备的Pd/Al2O3催化剂与树脂A催化剂和AlCl3/ Al2O3催化剂的催化效果,考察了Pd/Al2O3催化条件下,反应温度、反应物配比、反应空速及催化剂稳定性对甲基二氯硅烷转化率的影响,得到了最佳工艺条件。Pd/Al2O3催化剂相比于树脂A催化剂和AlCl3/ Al2O3催化剂,Pd/Al2O3催化剂具有更好的催化效果;在反应温度为140℃、n(甲基二氯硅烷):n(四氯化碳)=3:1、反应液时空速为5.0h-1时,甲基二氯硅烷转化率最高可以达到69.76%。

    Abstract:

    In order to remove the main carbon impurity methyldichlorosilane in the polysilicon raw material, it is converted into a high boiling point substance methyltrichlorosilane by a catalytic reaction. Pd/Al2O3 catalyst was prepared by impregnation method, and its physicochemical properties were characterized by X-ray fluorescence (XRF), X-ray powder diffraction (XRD), N2 adsorption desorption (BET), photoelectron spectroscopy (XPS) and H2 pulse chemisorption. Using a fixed-bed reactor under conditions where the chlorine source material is carbon tetrachloride, the catalytic effect of Pd/Al2O3 catalyst, The resin A catalyst and AlCl3/Al2O3 catalyst were compared. The effects of reaction temperature, reactant ratio, reaction space velocity and catalyst stability on the conversion of methyldichlorosilane were studied. The best process conditions were obtained. Pd/Al2O3 catalyst has better catalytic effect than The resin A catalyst and AlCl3/Al2O3 catalyst. When the chlorine source material is carbon tetrachloride, the reaction temperature is about 140 ℃、n(CH3Cl2SiH):n(CCl4)=3:1 and the space-time velocity of reaction solution is 5.0h-1, the maximum conversion rate of methyldichlorosilane can reach 69.76%.

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张明鑫,黄国强.氯硅烷中甲基二氯硅烷的转化反应工艺 急[J].精细化工,2020,37(4):

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  • 收稿日期:2019-11-26
  • 最后修改日期:2020-01-10
  • 录用日期:2020-01-14
  • 在线发布日期: 2020-03-23
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