引用本文: | 李季,张磊,杨春晖.直接法制备三甲氧基硅烷的正交实验研究[J].材料科学与工艺,2011,19(5):6-11.DOI:10.11951/j.issn.1005-0299.20110502. |
| LI Ji,ZHANG Lei,YANG Chun-hui.Direct synthesis of trimethoxysilane in orthogonal experiment[J].Materials Science and Technology,2011,19(5):6-11.DOI:10.11951/j.issn.1005-0299.20110502. |
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摘要: |
为提高产率、降低成本,采用反歧化法制备了催化剂氯化亚铜,研究了硅粉和氯化亚铜经过微波预处理直接法合成三甲氧基硅烷,利用XRD、XRF、SEM对催化剂进行了表征.用正交实验方法探索了不同工艺条件对硅粉转化率、产物选择性和产物收率的影响.正交实验表明,各因素对产物收率影响的由大至小顺序为:硅粉占溶剂质量比例、反应温度、甲醇加入速度、催化剂占硅粉质量比例、微波预处理时间、搅拌速度.在优化后的工艺条件下,三甲氧基硅烷的产物收率最高达到84.94%. |
关键词: 三甲氧基硅烷 氯化亚铜 微波 正交实验 |
DOI:10.11951/j.issn.1005-0299.20110502 |
分类号:TQ264.1 |
基金项目:国家科技支撑计划资助项目(2006BAE01B09) |
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Direct synthesis of trimethoxysilane in orthogonal experiment |
LI Ji, ZHANG Lei, YANG Chun-hui
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School of Chemical Engineering & Technology,Harbin Institute of Technology,Harbin 150001,China
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Abstract: |
To improve the product yield and reduce industrial cost,the reaction of silicon with methanol using copper(I) chloride prepared by inverse disproportionation as a catalyst has been investigated.The Si-CuCl mixture is pretreated by microwave prior to feeding methanol.The catalyst is characterized by X-Ray Diffractomer(XRD),X-Ray Fluorescence Spectrometer(XRF),Scanning Electron Microscopy(SEM).Orthogonal experiment is used to explore the influences of some factors on the silicon conversion and trimethoxysilane selectivity and yield.Orthogonal experimental results show that effect order of factors on the triethoxysilane yield is as follows: mass ratio of silicon in solvent,reaction temperature,dropping rate of methanol,mass ratio of catalysts in silicon,time of microwave pretreating and stirring rate.Under the optimized conditions,the trimethoxysilane yield efficiency can be as high as 84.94%. |
Key words: trimethoxysilane copper(I) chloride microwave orthogonal experiment |