Please wait a minute...
浙江大学学报（理学版）
浙江大学学报（理学版）  2016, Vol. 43 Issue (4): 416-419    DOI: 10.3785/j.issn.1008-9497.2016.04.007
化学     
1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷的制备
黄允河1, 何冰晓1, 陈关喜1,2, 吴清洲1,2, 冯建跃1,2
1. 浙江大学 化学系, 浙江 杭州 310027;
2. 浙江大学 分析测试中心, 浙江 杭州 310027
Preparation of 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane
HUANG Yunhe1, HE Bingxiao1, CHEN Guanxi1,2, WU Qingzhou1,2, FENG Jianyue1,2
1. Department of Chemistry, Zhejiang University, Hangzhou 310027, China;
2. Center of Analysis and Measurement, Zhejiang University, Hangzhou 310027, China
 全文: PDF(735 KB)  
摘要： 以二甲基氯硅烷和γ-氯丙烯为原料，经硅氢加成、水解缩合两步反应得到双官能团有机硅烷单体1，3-双（γ-氯丙基）-1，1，3，3-四甲基二硅氧烷，总产率为81.0%.对第1步硅氢加成反应进行了条件优化，确定最佳条件为：反应时间5 h，催化剂用量2×10-5 g·mL-1，反应物配比1∶1，此时产率可达83.8%；第2步水解缩合反应产率为96.7%.采用红外光谱、核磁共振、气相色谱-质谱联用等检测方法对产物进行了结构鉴定.
关键词： 二甲基氯硅烷;  γ-氯丙烯;  1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷;  硅氢加成;  水解缩合    
Abstract: 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane is a reactive functional group terminated siloxane, which is synthesized using dimethylchlorosilane and allyl chloride as starting materials. Through hydrosilylation and hydrolytic condensation, 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane was prepared in a total yield of 81%. The optimal conditions of hydrosilylation were studied. The yield of hydrosilylation was 83.8% when the reaction time was 5 h, the amount of platinum catalyst was 2×10-5 g·mL-1 and the ratio of reactants was 1∶1. The yield of hydrolytic condensation was 96.7%. Additionally, IR, 1H NMR and gas chromatography-mass spectrometer were used to characterize the structure of target product.
Key words: dimethylchlorosilane    allyl chloride    1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane    hydrosilylation    hydrolytic condensation
收稿日期: 2015-10-10 出版日期: 2016-04-28
CLC:  O621.3  
基金资助: 浙江省重大科技专项重点工业项目（2013C01087）.
通讯作者: 冯建跃,ORCID:http://orcid.org/0000-0002-1484-5392,E-mail:jyfeng@zju.edu.cn.     E-mail: jyfeng@zju.edu.cn
作者简介: 黄允河(1990-),http://orcid.org/0000-0002-6225-7368,女,硕士生,主要从事功能有机硅化合物的合成与分析研究.
服务　　
把本文推荐给朋友
加入引用管理器
E-mail Alert
RSS
作者相关文章　　
黄允河
何冰晓
陈关喜
吴清洲
冯建跃

引用本文:

黄允河, 何冰晓, 陈关喜, 吴清洲, 冯建跃. 1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷的制备[J]. 浙江大学学报（理学版）, 2016, 43(4): 416-419.

HUANG Yunhe, HE Bingxiao, CHEN Guanxi, WU Qingzhou, FENG Jianyue. Preparation of 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane. Journal of ZheJIang University(Science Edition), 2016, 43(4): 416-419.

链接本文:

https://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2016.04.007    或    https://www.zjujournals.com/sci/CN/Y2016/V43/I4/416

[1] 来国桥,幸松民.有机硅合成工艺及产品应用[M].第2版.北京:化学工业出版社,2010. LAI Guoqiao, XING Songmin. Organic Silicon Synthesis Technology and Product Application[M]. 2nd ed. Beijing: Chemical Industry Press,2000.
[2] 胡江华,甘书官,甘俊,等.一种正丁基氨丙基三烷氧基硅烷的合成方法:CN 103333200A[P].2013-07-22. HU Jianghua, GAN Shuguan, GAN Jun, et al. A Synthesis Method of n-butylaminopropyltrialkoxysilane: CN 103333200A[P].2013-07-22.
[3] 周振宇,王政,顾晓丹,等.几种含α-官能团的二硅氧烷的合成与表征[J].有机硅材料,2009,23(5):288-292. ZHOU Zhenyu, WANG Zheng, GU Xiaodan, et al. Preparation and characterization of several bis(α-functional group) contained disiloxanes[J]. Silicone Material,2009,23(5):288-292.
[4] 姜红芹,张墩明,蔡锡群,等.1,3-双(3-羟丙基)-1,1,3,3-四甲基二硅氧烷的制备[J].精细化工,2004,21(3):232-240. JIANG Hongqin, ZHANG Dunming, CAI Xiqun, et al. Preparation of 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetrameth-yldisiloxane[J]. Fine Chemicals,2004,21(3):232-240.
[5] JANKOWIAK M, MACIEJEWSKI H, GULINSKI J. Catalytic reactions of hydrosiloxanes with allylchloride[J]. Journal of Organometallic Chemistry,2005,690(20):4478-4487.
[6] 曾小剑,王传虎,葛金龙.γ-氯丙基二甲基氯硅烷的催化合成[J].有机硅材料,2009,23(2):95-97. ZENG Xiaojian, WANG Chuanhu, GE Jinlong. Study on catalytic synthesis of γ-chloropropyldimethylchlorosilane [J]. Silicone Material,2009,23(2):95-97.
[7] CHALK A J, HARROD J F. Homogeneous catalysis. II. The mechanism of the hydrosilation of olefins catalyzed by group VⅢ metal complexes[J]. Journal of the American Chemical Society,1965,87(1):16-21.
No related articles found!