优质失水山梨醇倍半油酸酯的合成
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摘要
从理论上分析了失水山梨醇倍半油酸酯的合成,并通过变量法试验对影响反应的温度、时间、催化剂用量等条件进行考察。用得到的失水山梨醇倍半油酸酯制备乳胶基质,测试乳胶基质的储存稳定性,以此得到优良的失水山梨醇倍半油酸酯合成条件。结果表明:采用醚化温度155℃、醚化时间90 min、醚化催化剂磷酸(质量分数0.5%)、酯化温度205℃、酯化时间4 h、酯化催化剂Na OH(质量分数0.3%)为合成条件时,能够得到优良的失水山梨醇倍半油酸酯。用其制备的乳胶基质在高低温循环测试中,循环次数可达20次。
Synthesis of sorbitan sesquioleate was theoretically analyzed,and the effect of temperature,time,catalyst amount and other reaction conditions were investigated by variable method. The stability of emulsion matrix prepared by sorbitan sesquioleate was tested. Better conditions to synthesize sorbitan sesquioleate were obtained. Optimal reaction conditions are that: the etherification temperature is 155 ℃,the etherification time is 90 min,the etherification catalyst is phosphorous acid,and the mass ratio of catalyst is 0. 5%; the esterification temperature is 205 ℃,the esterification time is4 h,the esterification catalyst is Na OH,and the mass ratio of catalyst is 0. 3%. The emulsion matrix prepared by sorbitan sesquioleate with optimal reaction conditions was tested by high and low temperature cycling,and the number of cycles will be up to 20.
Synthesis of sorbitan sesquioleate was theoretically analyzed,and the effect of temperature,time,catalyst amount and other reaction conditions were investigated by variable method. The stability of emulsion matrix prepared by sorbitan sesquioleate was tested. Better conditions to synthesize sorbitan sesquioleate were obtained. Optimal reaction conditions are that: the etherification temperature is 155 ℃,the etherification time is 90 min,the etherification catalyst is phosphorous acid,and the mass ratio of catalyst is 0. 5%; the esterification temperature is 205 ℃,the esterification time is4 h,the esterification catalyst is Na OH,and the mass ratio of catalyst is 0. 3%. The emulsion matrix prepared by sorbitan sesquioleate with optimal reaction conditions was tested by high and low temperature cycling,and the number of cycles will be up to 20.
引文
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[2]Stockburger G J,George J.Porcess for preparing sorbitan esters:US,4297290[P].1981-10-27.
[3]朱建民,王春艳,王风杰.山梨醇失水反应及Span-80合成的研究[J].精细化工,1992,9(5-6):43-47.Zhu Jianmin,Wang Chunyan,Wang Fengjie.Studies on the dehydration reaction of sorbitol and the synthesis of Span-80[J].Fine Chemicals,1992,9(5-6):43-47.
[4]谢银宝,徐新生,杨锦宗,等.失水山梨醇油酸酯合成反应动力学研究[J].日用化学工业,1995(6):1-7.
[5]吕春绪,刘祖亮,倪欧琪.工业炸药[M].北京:兵器工业出版社,1994.
[6]王荟慧.可聚合性Span80的合成研究[D].南京:南京理工大学,2008.Wang Huihui.Study on preparation of Span80 which has polymerizable reactivity[D].Nanjing:Nanjing Universty of Science and Technology,2008.
[7]毛连山,王加国,向昭旺,等.优质失水山梨醇单硬脂酸酯的合成[J].化学工业与工程技术,2005,26(1):19-22.Mao Lianshan,Wang Jiaguo,Xiang Zhaowang,et al.Synthesis of high quality of sorbitan monostearate[J].Journal of Chemical Industry&Engineering,2005,26(1):19-22.
[8]高昌文,殷雅婷.Span-80的合成工艺研究[J].煤矿爆破,2013(3):28-31,34.Gao Changwen,Yin Yating.Research on the synthesis technology of Span-80[J].Coal Mine Blasting,2013(3):28-31,34.
[9]董宇清.山梨醇酐单油酸酯的合成及其乳化炸药的稳定性研究[D].长沙:中南大学,2005.