甘油缩丙酮的合成研究
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摘要
以甘油与丙酮为原料,以氨基磺酸为催化剂,合成甘油缩丙酮。考察了原料物质的量比、反应时间和催化剂用量等因素对产品收率的影响。最佳工艺条件为:甘油用量为7 mL(约0.1 mol),n(丙酮)∶n(甘油)=4.0,氨基磺酸用量为甘油质量的4%,石油醚与甘油体积相同,回流反应4.5 h。该条件下,产品收率可高于86%。
The glycerol acetonide was synthesized from glycerol and acetone, with sulfamic acid as the catalyst. The influences of the molar ratio of raw materials, the reaction time, and the catalyst dosage on product yield were investigated.The optimum technological conditions were as follows: the glycerol dosage was 7 mL(approximately equal to 0.1 mol), the molar ratio of acetone to glycerol was 4.0, the dosage of sulfamic acid was 4% of the glycerin quantity, the volume of petroleum ether was the same as glycerin′s volume, and the reflux reaction time was 4.5 h. Under above conditions, the product yield could be higher than 86%.
The glycerol acetonide was synthesized from glycerol and acetone, with sulfamic acid as the catalyst. The influences of the molar ratio of raw materials, the reaction time, and the catalyst dosage on product yield were investigated.The optimum technological conditions were as follows: the glycerol dosage was 7 mL(approximately equal to 0.1 mol), the molar ratio of acetone to glycerol was 4.0, the dosage of sulfamic acid was 4% of the glycerin quantity, the volume of petroleum ether was the same as glycerin′s volume, and the reflux reaction time was 4.5 h. Under above conditions, the product yield could be higher than 86%.
引文
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[2]刘芸双,傅伟昌.响应面法优化丙酮缩甘油合成工艺的研究[J].应用化工, 2015,44(3):445-449.
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[4]曹晶晶,刘景亮,范慧.丙酮缩甘油的制备[J].高校化学工程学报, 2015, 29(4):948-954.
[5]任立国,张晓丽,高文艺.二氧化硅负载磷钨酸催化甘油与丙酮的缩合反应[J].辽宁石油化工大学学报, 2011, 31(4):9-13.
[6]黄文恒,刘旭浩.利用固体催化剂制备丙酮缩甘油的工艺研究[J].广州化工, 2017, 45(3):39-41.
[7]于朝生,林韡,郑晓峰,等.自制氨基磺酸催化合成2-苯基苯并咪唑[J].化学工业与工程, 2008, 25(5):419-423.
[2]刘芸双,傅伟昌.响应面法优化丙酮缩甘油合成工艺的研究[J].应用化工, 2015,44(3):445-449.
[3]石祖芸,徐敬柱,洪朝锽,等.高纯度单硬脂酸甘油酯合成研究[J].化学反应工程与工艺, 1995(2):208-212.
[4]曹晶晶,刘景亮,范慧.丙酮缩甘油的制备[J].高校化学工程学报, 2015, 29(4):948-954.
[5]任立国,张晓丽,高文艺.二氧化硅负载磷钨酸催化甘油与丙酮的缩合反应[J].辽宁石油化工大学学报, 2011, 31(4):9-13.
[6]黄文恒,刘旭浩.利用固体催化剂制备丙酮缩甘油的工艺研究[J].广州化工, 2017, 45(3):39-41.
[7]于朝生,林韡,郑晓峰,等.自制氨基磺酸催化合成2-苯基苯并咪唑[J].化学工业与工程, 2008, 25(5):419-423.