CN1194259A - 一种高纯度2.4-二氯苯氧乙酸的制备方法 - Google Patents

一种高纯度2.4-二氯苯氧乙酸的制备方法 Download PDF

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CN1194259A
CN1194259A CN97104606A CN97104606A CN1194259A CN 1194259 A CN1194259 A CN 1194259A CN 97104606 A CN97104606 A CN 97104606A CN 97104606 A CN97104606 A CN 97104606A CN 1194259 A CN1194259 A CN 1194259A
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purity
acid
dichlorophenoxyacetic acid
preparing high
sodium
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CN1076014C (zh
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阎学锦
王振江
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JIAMUSI PESTICIDE PLANT
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JIAMUSI PESTICIDE PLANT
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Abstract

本发明公开了一种用作高效除草剂和植物生长调节剂的农药,高纯度2.4-二氯苯氧乙酸的制备方法,它是在传统的基础上,采用低温合成,水相纯化的方法。本发明具有方法简单、收率高、产品质量好的特点。

Description

一种高纯度2.4-二氯苯氧乙酸的制备方法
本发明是关于农药的生产方法,更具体地说,本发明是关于用作高效除草剂和植物生长调节剂的农药高纯度2.4-二氯苯氧乙酸的制备方法。
目前,生产2.4-二氯苯氧乙酸的方法有水蒸汽蒸馏,三氯苯萃取和后氯化方法,不足之处是合成温度高、收率低、产品质量差,且“三废”不好控制。
本发明的目的是克服上述现有技术中的不足之处,提供一种方法简单,纯度高质量好的制备方法。
本发明的目的可通过下述技术方案予以实现:其制备方法是,先将先苯酚溶化,然后在温度80-110℃下进行氯化,生成二氯酚。氯乙酸和纯碱反应,转变为氯乙酸钠;然后,将二氯酚与烧碱反应,生成二氯酚钠,二氯酚钠同氯乙酸钠在温度90-95℃间进行缩合反应,生成2.4-二氯苯氧乙酸的钠盐。再将此钠盐在PH值9-10之间进行水相纯化,降低其酚的含量,直至达到规定标准。纯化后的钠盐再与盐酸进行酸化反应,转变成2.4-二氯苯氧乙酸。此酸经过吸滤,使氯化物含量合格后,进行离心分离,干燥后,包装成为正品。
本发明与现有技术相比有如下积极效果:
1、产品纯度高。
2、缩合反应温度低。
3、得率高。
下面是本发明的最佳实施例:苯酚在溶化池内溶解后,进入氯化塔,通入氯气进行氯化反应,生成二氯酚。氯乙酸和纯碱在中和釜内进行中和,产生氯乙酸钠;二氯酸和烧碱在缩合釜内反应,生成酚钠盐,然后,在温度90-95℃之间,同氯乙酸进行反应,生成2.4-二氯苯氧乙酸的钠盐。此钠盐在PH值9-10之间,水相纯化6-8小时。纯化后的钠盐进入酸化釜,同盐酸进行酸化反应,生成2.4-二氯苯氧乙酸。待氯化物含量合格后,进行离心,干燥、包装后,做为成品。

Claims (1)

1、本发明属于用作高效除草剂和植物生长调节剂的农药,高纯度2.4-二氯苯氧乙酸的制备方法,其特征在于:缩合反应温度控制在90-95℃之间;以水做为介质,来纯化产品中的异构物和其它杂质。
CN97104606A 1997-03-25 1997-03-25 一种高纯度2,4-二氯苯氧乙酸的制备方法 Expired - Fee Related CN1076014C (zh)

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CN97104606A CN1076014C (zh) 1997-03-25 1997-03-25 一种高纯度2,4-二氯苯氧乙酸的制备方法

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CN97104606A CN1076014C (zh) 1997-03-25 1997-03-25 一种高纯度2,4-二氯苯氧乙酸的制备方法

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CN1194259A true CN1194259A (zh) 1998-09-30
CN1076014C CN1076014C (zh) 2001-12-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101112194B (zh) * 2007-07-04 2011-12-21 常其钊 杀灭薇甘菊的药物及其制备方法和应用
CN103351296A (zh) * 2013-07-23 2013-10-16 山东科源化工有限公司 一种高纯度2,4-d的制备方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1147348A (en) * 1978-09-19 1983-05-31 Willem Eveleens Process for the preparation of optically active 2-phenoxy propionic acids and herbicidal preparations containing such acids
DE2903343A1 (de) * 1979-01-29 1980-07-31 Berlin Chemie Veb Verfahren zur herstellung von bis-p-chlorphenoxyessigsaeure
CN1006463B (zh) * 1985-08-22 1990-01-17 吴振久 苯(氯代苯)氧基乙酸的合成

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101112194B (zh) * 2007-07-04 2011-12-21 常其钊 杀灭薇甘菊的药物及其制备方法和应用
CN103351296A (zh) * 2013-07-23 2013-10-16 山东科源化工有限公司 一种高纯度2,4-d的制备方法

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