有机硅材料
有機硅材料
유궤규재료
SILICONE MATERIAL
2014年
5期
358-361,362
,共5页
吴艳金%王三跃%欧阳建松%贺志江
吳豔金%王三躍%歐暘建鬆%賀誌江
오염금%왕삼약%구양건송%하지강
固体超强酸%二氧化锆%硫酸%七甲基三硅氧烷%含氢硅油%六甲基二硅氧烷
固體超彊痠%二氧化鋯%硫痠%七甲基三硅氧烷%含氫硅油%六甲基二硅氧烷
고체초강산%이양화고%류산%칠갑기삼규양완%함경규유%륙갑기이규양완
solid super acid%zirconium dioxide%sulfuric acid%1,1,1,3,5,5,5-heptamethyltrisiloxane%hydrogen silicone fluid%hexamethyldisiloxane
以含氢硅油和六甲基二硅氧烷(MM)为原料,在SO42-/ZrO2固体超强酸催化下进行调聚反应,制得1,1,1,3,5,5,5-七甲基三硅氧烷(MDH M)。考察了原料配比、反应温度、反应时间及催化剂用量对MDH M收率的影响,并用红外光谱及气相色谱-质谱联用分析对产物进行了表征。结果表明,MDH M的最佳合成工艺为:反应温度70℃,反应时间7 h,MM与含氢硅油的质量比4∶1,SO42-/ZrO2固体超强酸用量为投料总质量的4%;在此条件下,MDH M的收率为31%~34%,固体超强酸的使用次数达到16次,产品质量较高。
以含氫硅油和六甲基二硅氧烷(MM)為原料,在SO42-/ZrO2固體超彊痠催化下進行調聚反應,製得1,1,1,3,5,5,5-七甲基三硅氧烷(MDH M)。攷察瞭原料配比、反應溫度、反應時間及催化劑用量對MDH M收率的影響,併用紅外光譜及氣相色譜-質譜聯用分析對產物進行瞭錶徵。結果錶明,MDH M的最佳閤成工藝為:反應溫度70℃,反應時間7 h,MM與含氫硅油的質量比4∶1,SO42-/ZrO2固體超彊痠用量為投料總質量的4%;在此條件下,MDH M的收率為31%~34%,固體超彊痠的使用次數達到16次,產品質量較高。
이함경규유화륙갑기이규양완(MM)위원료,재SO42-/ZrO2고체초강산최화하진행조취반응,제득1,1,1,3,5,5,5-칠갑기삼규양완(MDH M)。고찰료원료배비、반응온도、반응시간급최화제용량대MDH M수솔적영향,병용홍외광보급기상색보-질보련용분석대산물진행료표정。결과표명,MDH M적최가합성공예위:반응온도70℃,반응시간7 h,MM여함경규유적질량비4∶1,SO42-/ZrO2고체초강산용량위투료총질량적4%;재차조건하,MDH M적수솔위31%~34%,고체초강산적사용차수체도16차,산품질량교고。
1 ,1 ,1 ,3 ,5 ,5 ,5-heptamethyltrisiloxane was prepared with hexamethydisiloxane and methyl-hydrogen silicone fluid as the starting materials and SO2-4 /ZrO2 solid super acid as the catalyst. The influences of reactant mass ratio,reaction temperature,reaction time and catalyst dosage on the yield of 1,1,1,3,5,5,5-heptamethyltrisiloxane were investigated,the optimal conditions for synthesis were as follows:the reaction tem-perature was 70℃,the mass ratio of MM and methyl-hydrogen silicone fluid was 4∶1 ,the reaction time was 7 hours,and the mass fraction of SO2-4 /ZrO2 solid super acid was 4%. Under the optimal conditions,the yield of 1,1,1,3,5,5,5-heptamethyltrisiloxane was 31% ~34%,and solid super acid can be used for 16 times, with good quality.