陕西科技大学学报(自然科学版)
陝西科技大學學報(自然科學版)
협서과기대학학보(자연과학판)
JOURNAL OF SHAANXI UNIVERSITY OF SCIENCE & TECHNOLOGY
2015年
4期
65-69
,共5页
长链烷基聚醚共改性硅油%含氢硅油%硅氢化加成%表征
長鏈烷基聚醚共改性硅油%含氫硅油%硅氫化加成%錶徵
장련완기취미공개성규유%함경규유%규경화가성%표정
long chain epoxy-modified silicone oil%hydrogen silicone%hydrosilylation%char-acterization
将含氢硅油(PHMS)、烯丙基环氧聚醚(AEH)和1‐十六碳烯(C16)等,在Pt催化下经硅氢加成反应制得长链烷基环氧基聚醚改性硅油(PC A ),再将其与聚醚胺进行开环反应,合成了一种新型长链烷基聚醚改性硅油(PCAD ).采用红外光谱( FT‐IR )和核磁共振氢谱(1 HNMR)等对产物结构进行了表征.通过正交试验对合成中间体PCA的反应条件进行了探讨.当n(Si-H )∶ n(C=C)=1∶1.1、反应时间为2 h、催化剂用量为反应物质量的0.004%、溶剂异丙醇用量为反应物质量的30%时,为合成中间体PC A的最佳反应条件;还通过单因素实验确定了氨解反应的最佳条件,即 n(环氧基)∶ n(聚醚胺)=1∶1.08、反应温度为80℃、反应时间为5h.
將含氫硅油(PHMS)、烯丙基環氧聚醚(AEH)和1‐十六碳烯(C16)等,在Pt催化下經硅氫加成反應製得長鏈烷基環氧基聚醚改性硅油(PC A ),再將其與聚醚胺進行開環反應,閤成瞭一種新型長鏈烷基聚醚改性硅油(PCAD ).採用紅外光譜( FT‐IR )和覈磁共振氫譜(1 HNMR)等對產物結構進行瞭錶徵.通過正交試驗對閤成中間體PCA的反應條件進行瞭探討.噹n(Si-H )∶ n(C=C)=1∶1.1、反應時間為2 h、催化劑用量為反應物質量的0.004%、溶劑異丙醇用量為反應物質量的30%時,為閤成中間體PC A的最佳反應條件;還通過單因素實驗確定瞭氨解反應的最佳條件,即 n(環氧基)∶ n(聚醚胺)=1∶1.08、反應溫度為80℃、反應時間為5h.
장함경규유(PHMS)、희병기배양취미(AEH)화1‐십륙탄희(C16)등,재Pt최화하경규경가성반응제득장련완기배양기취미개성규유(PC A ),재장기여취미알진행개배반응,합성료일충신형장련완기취미개성규유(PCAD ).채용홍외광보( FT‐IR )화핵자공진경보(1 HNMR)등대산물결구진행료표정.통과정교시험대합성중간체PCA적반응조건진행료탐토.당n(Si-H )∶ n(C=C)=1∶1.1、반응시간위2 h、최화제용량위반응물질량적0.004%、용제이병순용량위반응물질량적30%시,위합성중간체PC A적최가반응조건;환통과단인소실험학정료안해반응적최가조건,즉 n(배양기)∶ n(취미알)=1∶1.08、반응온도위80℃、반응시간위5h.
In the presence of Pt catalyst ,a kind of long‐chain alkyl polyether modified epoxy silicone oil (PCA) was synthesized from hydrogen silicone oil(PHMS) ,allyl epoxy polyether (AEH) and 1‐hexadecene (C16 ) by hydrosilylation reaction ,and then reacted with a polyether amine to prepare a long‐chain alkyl polyether/amino silicon (PCAD) .The chemical structure of PCAD was characterized by means of nfrared spectroscopy (FT‐IR) and nuclear magnetic resonance spectroscopy (1 HNM R) .By orthogonal experiments to explore the conditions of synthesis intermediates ,the results showed that the optimum conditions for the preparation of intermediates of PCA∶ n(Si-H)∶ n(C=C)=1∶1 .1 ,reaction time is 2 h ,the amount of catalyst is 0 .004% ,the amount of solvent is 30% .The optimum conditions for ammonolysis reaction have been determined by single factor experiment as follow s :the molar ratio of ep‐oxy to polyether amines is 1∶1 .08 ,the reaction temperature is 80 ℃ ,the reaction time is 5 h.