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作 者:王文金 姚中鹏 辛梓杰 匡建国 WANG Wenjin;YAO Zhongpeng;XIN Zijie;KUANG Jianguo(Hubei Xingrui Silicon Material Co.,Ltd.,Yichang 443007,Hubei)
机构地区:[1]湖北兴瑞硅材料有限公司,湖北宜昌443007
出 处:《有机硅材料》2022年第5期62-66,共5页Silicone Material
摘 要:以一甲基三氯硅烷(一甲)和甲醇为原料,采用塔式反应器连续合成甲基三甲氧基硅烷(MTMS),探讨了原料配比、下塔温度、上塔温度、反应塔压力、粗品回流比和甲醇含水量对MTMS收率及酸值的影响。结果表明:随着一甲与甲醇质量比的增大,MTMS收率先升后降,酸值先降后升;随着下塔温度的升高,MTMS收率升高并趋于稳定,酸值降低并趋于稳定;随着上塔温度的升高,MTMS收率先升后降,酸值降低;随着反应塔压力的升高,MTMS收率先升后降,酸值升高;随着粗品回流比的增大,MTMS收率和酸值均先升后降;随着甲醇含水量的升高,MTMS收率降低,酸值变化不明显;MTMS的较佳合成条件为:一甲与甲醇质量比1.5∶1,下塔温度85~90℃,上塔温度60~64℃,反应塔压力10~20 kPa,粗品回流比0.5~1,甲醇含水量≤500×10^(-6)。Using monomethyltrichlorosilane(monomethyl)and methanol as raw materials,a tower reactor was used to synthesize methyltrimethoxysilane(MTMS)continuously.The effects of raw material ratios,temperature of lower tower and upper tower,tower pressure,reflux ratio and water content of methanol on the yield and acid value of MTMS were discussed.The results show that with the increase of the mass ratio of monomethyl and methanol,the MTMS yield increases first and then decreases,and the acid value first decreases and then increases.With the increase of lower tower temperature,the yield of MTMS increases and tends to be stable,and the acid value decreases and tends to be stable.As the temperature in the upper tower elevates,the MTMS yield first increases and then decreases,and the acid value decreases.As the pressure in reaction tower rise,the MTMS yield first increases and then decreases,and the acid value increases.As the reflux ratio of the crude goes up,the MTMS yield and the acid value both increases first and then decreases.As the water content in methanol increase,the yield of MTMS decreases,and the acid value keep unchanged.The optimal synthesis conditions of MTMS are as follows:the mass ratio of monomethyl to methanol is 1.5:1,the temperature of the lower tower is 85-90℃,the temperature of the upper tower is 60-64℃,the pressure of the reaction tower is 10-20 kPa,the reflux ratio of the crude product is 0.5-1,the moisture content of methanol is≤500×10^(-6).
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