CN107382843A - 一种3,6‑二氯吡啶甲酸钾的合成工艺 - Google Patents

一种3,6‑二氯吡啶甲酸钾的合成工艺 Download PDF

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Publication number
CN107382843A
CN107382843A CN201710604301.9A CN201710604301A CN107382843A CN 107382843 A CN107382843 A CN 107382843A CN 201710604301 A CN201710604301 A CN 201710604301A CN 107382843 A CN107382843 A CN 107382843A
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potassium
lontrel
solution
potassium hydroxide
synthesis technique
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徐颖华
刘伟
李惠跃
张彦祥
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Lianyungang Avilive Chemical Co Ltd
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Lianyungang Avilive Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
    • C07D213/79—Acids; Esters
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
    • C07D213/79—Acids; Esters
    • C07D213/803—Processes of preparation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Pyridine Compounds (AREA)

Abstract

一种3,6‑二氯吡啶甲酸钾的合成工艺,步骤如下：(1)以氢氧化钾和3,4,5,6‑四氯吡啶甲酸为原料，在水溶液中电解反应转化成3,6‑二氯吡啶甲酸钾+氢氧化钾+氯化钾的水溶液；(2)然后用车间上的3,6‑二氯吡啶甲酸中和溶液中的氢氧化钾得到3,6‑二氯吡啶甲酸钾+氯化钾溶液；(3)将上述溶液浓缩到含3,6‑二氯吡啶甲酸钾的溶液即为产品；本发明优点是：30％3,6‑二氯吡啶甲酸钾水剂为高效除草剂，在农田中使用量非常小，因此掺入的氯化钾没有影响，该工艺的优点是可以免去原工艺需要酸化结晶，然后重新加氢氧化钾配置成30％3,6‑二氯吡啶甲酸钾水剂的优点，这不仅能节约大量盐酸，还可以减少大量含盐废水。

Description

一种3,6-二氯吡啶甲酸钾的合成工艺
技术领域
本发明涉及化工技术领域，具体涉及一种3,6-二氯吡啶甲酸钾的合成工艺。
背景技术
吡啶类化合物2,3,5,6-四氯吡啶是一种非常重要的农药中间体,可以用来制备各种很有潜力的杀虫剂和除草剂。目前最常见的合成方法是以五氯吡啶为原料,通过脱氯还原反应而生成；3,6-二氯吡啶甲酸钾水剂为高效除草剂，目前的合成工艺需要酸化结晶，容易产生大量含盐废水。
发明内容
为解决上述技术问题，本发明本发明采用如下技术方案：
一种3,6-二氯吡啶甲酸钾的合成工艺,步骤如下：
(1)以氢氧化钾和3,4,5,6-四氯吡啶甲酸为原料，首先在水溶液中电解反应转化成3,6-二氯吡啶甲酸钾+氢氧化钾+氯化钾的水溶液；
(2)然后用车间上的3,6-二氯吡啶甲酸中和溶液中的氢氧化钾得到3,6-二氯吡啶甲酸钾+氯化钾溶液；
(3)将上述溶液浓缩到含3,6-二氯吡啶甲酸钾的溶液即为产品，该产品可以直接作为原料使用。
优选地，所述步骤(3)中浓缩液中3,6-二氯吡啶甲酸钾的含量最少为30％。
本发明优点是：30％3,6-二氯吡啶甲酸钾水剂为高效除草剂，在农田中使用量非常小，因此掺入的氯化钾没有影响，该工艺的优点是可以免去原工艺需要酸化结晶，然后重新加氢氧化钾配置成30％3,6-二氯吡啶甲酸钾水剂的优点，这不仅能节约大量盐酸，还可以减少大量含盐废水。
具体实施方式
一种3,6-二氯吡啶甲酸钾的合成工艺,步骤如下：
(1)以氢氧化钾和3,4,5,6-四氯吡啶甲酸为原料，首先在水溶液中电解反应转化成3,6-二氯吡啶甲酸钾+氢氧化钾+氯化钾的水溶液；
(2)然后用车间上的3,6-二氯吡啶甲酸中和溶液中的氢氧化钾得到3,6-二氯吡啶甲酸钾+氯化钾溶液；
(3)将上述溶液浓缩到含3,6-二氯吡啶甲酸钾30％的溶液即为产品，该产品可以直接作为原料使用。
下面以具体实施例来说明本技术方案的实施。
实施例一：
一种3,6-二氯吡啶甲酸钾的合成工艺，以氢氧化钾和3,4,5,6-四氯吡啶甲酸为原料，首先在水溶液中电解反应转化成3,6-二氯吡啶甲酸钾+氢氧化钾+氯化钾的水溶液，然后用另外车间上的3,6-二氯吡啶甲酸中和溶液中的氢氧化钾得到3,6-二氯吡啶甲酸钾+氯化钾溶液，将上述溶液浓缩到含3,6-二氯吡啶甲酸钾30％的溶液即为产品。该产品可以直接作为30％3,6-二氯吡啶甲酸钾水剂的原料使用；因为30％3,6-二氯吡啶甲酸钾水剂为高效除草剂，在农田中使用量非常小，因此掺入的氯化钾没有影响。
上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。

Claims (2)

1.一种3,6-二氯吡啶甲酸钾的合成工艺,其特征在于步骤如下：
(1)以氢氧化钾和3,4,5,6-四氯吡啶甲酸为原料，首先在水溶液中电解反应转化成3,6-二氯吡啶甲酸钾+氢氧化钾+氯化钾的水溶液；
(2)然后用车间上的3,6-二氯吡啶甲酸中和溶液中的氢氧化钾得到3,6-二氯吡啶甲酸钾+氯化钾溶液；
(3)将上述溶液浓缩到含3,6-二氯吡啶甲酸钾的溶液即为产品，该产品可以直接作为原料使用。
2.根据权利要求1所述的一种3,6-二氯吡啶甲酸钾的合成工艺，其特征在于：所述步骤(3)中浓缩液中3,6-二氯吡啶甲酸钾的含量最少为30％。
CN201710604301.9A 2017-07-24 2017-07-24 一种3,6‑二氯吡啶甲酸钾的合成工艺 Pending CN107382843A (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4217185A (en) * 1979-07-02 1980-08-12 The Dow Chemical Company Electrolytic production of certain trichloropicolinic acids and/or 3,6-dichloropicolinic acid
EP0209611A1 (en) * 1985-07-18 1987-01-28 The Dow Chemical Company Electrolytic cell comprising stainless steel anode and a process for preparing polychloropicolinate anions
CN101235512A (zh) * 2007-11-16 2008-08-06 利尔化学股份有限公司 3,6-二氯吡啶甲酸的电解合成方法
CN103603006A (zh) * 2013-09-29 2014-02-26 杭州赛龙化工有限公司 一种3,6-二氯吡啶甲酸的电解合成工艺

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4217185A (en) * 1979-07-02 1980-08-12 The Dow Chemical Company Electrolytic production of certain trichloropicolinic acids and/or 3,6-dichloropicolinic acid
EP0209611A1 (en) * 1985-07-18 1987-01-28 The Dow Chemical Company Electrolytic cell comprising stainless steel anode and a process for preparing polychloropicolinate anions
CN101235512A (zh) * 2007-11-16 2008-08-06 利尔化学股份有限公司 3,6-二氯吡啶甲酸的电解合成方法
CN103603006A (zh) * 2013-09-29 2014-02-26 杭州赛龙化工有限公司 一种3,6-二氯吡啶甲酸的电解合成工艺

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Application publication date: 20171124