摘要
该文对格氏试剂合成四丁基锡的工艺进行了研究，提出了混合溶剂一步法合成工艺。采用正交实验及单因素法研究了合成过程中反应时间、反应温度、反应物用量等因素对四丁基锡收率的影响，获得了控制反应过程的最佳参数，并用气相色谱法对产物的成分进行了定量分析。研究结果表明，采用混合溶剂一步法合成工艺，当四氯化锡加入量达到理论量的90％时，产物中四丁基锡的质量分数大于97％，收率大于97％；用该工艺在500t／a规模的工业装置上生产时，产品四丁锡质量分数为87．2％～96．2％，收率为85．8％～94．3％。
A new one-step synthesis process of tetrabutyhin through Grignards reagent was put forward. Factors influencing the reaction such as reaction time, reaction temperature and amounts of the reactants were investigated. Gas chromatography was used to determine quantitatively the constituents of the product. The results show that, adopting the one-step process and using mixed solvent, amount of stannic chloride added can reach 90% as much as the theoretical amount, content of tetrabutyltin in the final product is higher than 97%, and the yield of tetrabutyltin is over 97%. This new process was applied in industrial production of 500 t/a, the content of tetrabutyhin in the product was 87.2% - 96. 2% ,and the yield was 85.8% -94. 3%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2006年第7期698-701,共4页
Fine Chemicals
关键词
格氏反应
四丁基锡
一步法工艺
Grignard reaction
tetrabuytyltin
one-step process
