[1]吴 霞,单玉华,任海永,等.2,4-二氯苯氧乙酸合成清洁技术研究[J].常州大学学报(自然科学版),2012,(01):10-13.
　WU Xia,SHAN Yu-hua,REN Hai-yong,et al.Development of a Clean Technique for the Synthesis of 2,4-Dichlorophenoxyacetic Acid[J].Journal of Changzhou University(Natural Science Edition),2012,(01):10-13.
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2,4-二氯苯氧乙酸合成清洁技术研究()
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常州大学学报(自然科学版)[ISSN:2095-0411/CN:32-1822/N]

卷:
期数:
2012年01期
页码:
10-13
栏目:
出版日期:
2012-01-01

文章信息/Info

Title:
Development of a Clean Technique for the Synthesis of 2,4-Dichlorophenoxyacetic Acid
作者:
吴 霞; 单玉华; 任海永; 鲁墨弘; 李明时
常州大学 江苏省精细石油化工重点实验室,江苏 常州 213164
Author(s):
WU Xia; SHAN Yu-hua; REN Hai-yong;  LU Mo-hong;  LI Ming-shi
Jiangsu Key Laboratory of Fine Petrochemical Engineering, Changzhou University, Changzhou 213164, China
关键词:
2; 4-二氯苯氧乙酸;  催化剂;  氯代;  苯氧乙酸;  合成
Keywords:
2; 4-dichlorophenoxyacetic acid;  catalysts;  chlorination;  phenoxyacetic acid;  synthesis
分类号:
TQ 245.24
文献标志码:
A
摘要:
以苯氧乙酸和氯气为原料,经催化氯化合成2,4-二氯苯氧乙酸(2,4-D)。对氯化催化剂进行了考察,对反应溶剂进行了筛选,并对反应条件进行了优化,以开发高效、环保的2,4-D合成新技术。结果表明:磷钨酸铋(BPW)是较好的催化剂,1,2-二氯乙烷是合适的溶剂; 优化的反应条件为:122.5 g 苯氧乙酸为原料、1.08 g BPW为催化剂,180 g1,2-二氯乙烷作为溶剂,50 ℃以50 g·h-1通入氯气,待2,4-D含量达到最高后停止通入氯气,能得到含量在98.4%(HPLC)、产率91.1%的外观为白色晶体2,4-D产品。用高压液相色谱(HPLC)对产品进行定量分析,通过FT-IR和NMR对产品结构进行确认。
Abstract:
2,4-Dichlorophenoxyacetic acid(2,4-D)was prepared by catalytic chlorination of phenoxyacetic acid with chlorine. Catalysts investigation, solvents screening, and reaction conditions optimization were carried out to develop a high yield and environmental-friendly process for 2,4-D production. The results show that: BiPW12O40(BPW)is a good catalyst and 1,2-dichloroethane is a suitable solvent for this reaction.Under the optimal reaction conditions(122.5 g phenoxyacetic acid, 0.72 g BPW, 180 g 1,2- dichloroethane, 40 g ·h-1, 50 ℃), 91.14% of 2,4-D(white crystalline)can be obtained with a purity of 98.37%(HPLC). The 2,4-D product was quantified by HPLC and confirmed by FT-IR and NMR.

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备注/Memo

备注/Memo:
作者简介:吴霞(1985—),女,江苏扬州人,硕士生; 通讯联系人:单玉华。
更新日期/Last Update: 2012-01-01