管式反应器连续化合成3,5,6-三氯吡啶-2-醇钠工艺研究
|
摘要
以2,3,5,6-四氯吡啶为原料,采用管式反应器在水中与氢氧化钠水解合成3,5,6-三氯吡啶-2-醇钠,并对工艺进行了优化,四氯吡啶与2.2倍氢氧化钠在4倍溶剂水用量下,停留时间8 min,在140℃下连续反应,四氯吡啶转化率100%,产物收率98.0%。
This research is carried out on the preparation of 3,5,6-trichloropyridin-2-ol sodium with tetrachloropyridine,sodium hydroxide and water,by adopting a tubular reactor,and the process is optimized. The conversion of tetrachloropyridine was 100% and the yield of 3,5,6-trichloropyridin-2-ol sodium was 98.0% when the reaction temperature is 140℃,and the reaction mixture is allowed to remain in the reaction zone for a period of 8 minutes,use 2.2 mol sodium hydroxide and 4 times the mass of water, based on tetrachloropyridine.
This research is carried out on the preparation of 3,5,6-trichloropyridin-2-ol sodium with tetrachloropyridine,sodium hydroxide and water,by adopting a tubular reactor,and the process is optimized. The conversion of tetrachloropyridine was 100% and the yield of 3,5,6-trichloropyridin-2-ol sodium was 98.0% when the reaction temperature is 140℃,and the reaction mixture is allowed to remain in the reaction zone for a period of 8 minutes,use 2.2 mol sodium hydroxide and 4 times the mass of water, based on tetrachloropyridine.
引文
[1]王红明,李健,葛九敢,等.水相法合成毒死蜱的清洁工艺改进[J].现代农药, 2012(6):15-18.
[2]徐振元.毒死蜱合成研究[J].农药,1998(1):15-17.
[3]许龙,陈敏.甲基毒死蜱水相法合成路线的开发[J].化学工程与装备,2018(3):17-20.
[4]赵丹凤.3,5,6-三氯吡啶-2-醇钠的合成研究[D].河北工业大学, 2011.
[5]李培国,张柏青.3,5,6-三氯吡啶-2-醇钠的合成[J].浙江化工,2004,35(3):16-18.
[6]张未星,刘延娜,章灵均.3,5,6-三氯吡啶-2-醇钠的合成[J].浙江化工,2008, 39(9):13-15.
[7]王同涛,张瑞生,刘自友,等.农药中间体3,5,6一三氯吡啶-2-醇钠的合成[J].农药科学与管理,2009,30(7):31-34.
[8]方红新,张涛,王晓亭.一种3,5,6-三氯吡啶-2-醇钠的新的合成工艺[P]. CN:104177290A,2014.
[9]刘宁,崔洪友,姚德,等.3,5,6-三氯吡啶-2-醇钠在超(近)临界水中的稳定性[J].过程工程学报,2008,8(2):290-294.
[10]刘宁,崔洪友,姚德.2,3,5,6-四氯吡啶加压水解制备3,5,6-三氯吡啶-2-醇钠[J].农药,2008,47(1):31-33.
[11]马成亮,崔洪友.2,3,5,6-四氯吡啶在乙二醇中水解动力学[J].农药,2009,48(11):800-802.
[12]朱伟,肖国民.3,5,6-三氯吡啶-2-酚的合成[J].精细与专用化学品,2005, 13(18):26.
[13]张柏青,季旻,许清国,等.三氯吡啶醇钠的合成研究[J].杭州化工,2004,34(1):21-22.
[14]王旭艳,刘明.2,3,5,6-四氯吡啶工艺及市场分析[J].山东工业技术,2016(3):66.
[15]刘善和,梁锡臣,吴李瑞,等. 3,5,6-三氯吡啶-2-醇钠的合成工艺[J].安徽化工,2016, 42(2):35-37.
[2]徐振元.毒死蜱合成研究[J].农药,1998(1):15-17.
[3]许龙,陈敏.甲基毒死蜱水相法合成路线的开发[J].化学工程与装备,2018(3):17-20.
[4]赵丹凤.3,5,6-三氯吡啶-2-醇钠的合成研究[D].河北工业大学, 2011.
[5]李培国,张柏青.3,5,6-三氯吡啶-2-醇钠的合成[J].浙江化工,2004,35(3):16-18.
[6]张未星,刘延娜,章灵均.3,5,6-三氯吡啶-2-醇钠的合成[J].浙江化工,2008, 39(9):13-15.
[7]王同涛,张瑞生,刘自友,等.农药中间体3,5,6一三氯吡啶-2-醇钠的合成[J].农药科学与管理,2009,30(7):31-34.
[8]方红新,张涛,王晓亭.一种3,5,6-三氯吡啶-2-醇钠的新的合成工艺[P]. CN:104177290A,2014.
[9]刘宁,崔洪友,姚德,等.3,5,6-三氯吡啶-2-醇钠在超(近)临界水中的稳定性[J].过程工程学报,2008,8(2):290-294.
[10]刘宁,崔洪友,姚德.2,3,5,6-四氯吡啶加压水解制备3,5,6-三氯吡啶-2-醇钠[J].农药,2008,47(1):31-33.
[11]马成亮,崔洪友.2,3,5,6-四氯吡啶在乙二醇中水解动力学[J].农药,2009,48(11):800-802.
[12]朱伟,肖国民.3,5,6-三氯吡啶-2-酚的合成[J].精细与专用化学品,2005, 13(18):26.
[13]张柏青,季旻,许清国,等.三氯吡啶醇钠的合成研究[J].杭州化工,2004,34(1):21-22.
[14]王旭艳,刘明.2,3,5,6-四氯吡啶工艺及市场分析[J].山东工业技术,2016(3):66.
[15]刘善和,梁锡臣,吴李瑞,等. 3,5,6-三氯吡啶-2-醇钠的合成工艺[J].安徽化工,2016, 42(2):35-37.