CN106748980A - 一种二氯吡啶生产工艺 - Google Patents

一种二氯吡啶生产工艺 Download PDF

Info

Publication number
CN106748980A
CN106748980A CN201510807194.0A CN201510807194A CN106748980A CN 106748980 A CN106748980 A CN 106748980A CN 201510807194 A CN201510807194 A CN 201510807194A CN 106748980 A CN106748980 A CN 106748980A
Authority
CN
China
Prior art keywords
reaction
aminopyridines
chlorination
diazo
carries out
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510807194.0A
Other languages
English (en)
Inventor
胡江海
张晓磊
于飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningxia Jihua Environmental Safety Technology Co Ltd
Original Assignee
Ningxia Jihua Environmental Safety Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningxia Jihua Environmental Safety Technology Co Ltd filed Critical Ningxia Jihua Environmental Safety Technology Co Ltd
Priority to CN201510807194.0A priority Critical patent/CN106748980A/zh
Publication of CN106748980A publication Critical patent/CN106748980A/zh
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D213/00Heterocyclic 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
    • C07D213/02Heterocyclic 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
    • C07D213/04Heterocyclic 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
    • C07D213/60Heterocyclic 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
    • C07D213/61Halogen atoms or nitro radicals

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pyridine Compounds (AREA)

Abstract

二氯吡啶是化工中的重要原材料。二氯吡啶生产工艺流程为:⑴氯化反应;将3-氨基吡啶加入到氯化釜中,加入一定量的双氧水,其夹套通入冷冻盐水降温至10℃,然后缓慢滴加盐酸进行氯化反应,控制反应温度为25℃,反应压力为常压,氯化反应结束后,得到2-氯-3-氨基吡啶。⑵重氮化反应;将2-氯-3-氨基吡啶转入至重氮化釜中,其夹套通入冷冻盐水降温至-5℃,然后缓慢滴加亚硝酸钠溶液进行重氮化反应,控制反应温度为5℃,反应压力为常压。重氮化反应结束后得到2-氯-3氨基吡啶重氮盐。(3)后处理;将粗品转入至萃取釜中,加入一定量的液碱进行中和,再加入氯仿进行萃取分离,水相经过滤回收氯化亚铜后进入污水处理。

Description

一种二氯吡啶生产工艺
反应原理及反应方程式
反应原理:以3-氨基吡啶、盐酸、双氧水、亚硝酸钠等为原料,经氯化、重氮化、分解等过程制得本品。
主要化学反应方程式:
⑴ 氯化反应(以3-氨基吡啶计,转化率为95%)
⑵ 重氮化反应(以2-氯-3-氨基吡啶计,转化率为94%)
副反应:
⑶ 分解反应(以2-氯-3-氨基吡啶重氮盐计,转化率为95%)
工艺流程简述:
⑴氯化反应
将3-氨基吡啶加入到氯化釜中,加入一定量的双氧水,其夹套通入冷冻盐水降温至10℃,然后缓慢滴加盐酸进行氯化反应,控制反应温度为25℃,反应压力为常压,氯化反应结束后,得到2-氯-3-氨基吡啶。
⑵重氮化反应
将2-氯-3-氨基吡啶转入至重氮化釜中,其夹套通入冷冻盐水降温至-5℃,然后缓慢滴加亚硝酸钠溶液进行重氮化反应,控制反应温度为5℃,反应压力为常压。重氮化反应结束后得到2-氯-3 氨基吡啶重氮盐。
⑷ 分解反应
将2-氯-3 氨基吡啶重氮盐转入至分解反应釜中,夹套中通入冷冻盐水降温至-10℃,加入一定量的催化剂(氯化亚铜)进行分解反应,控制反应温度为0℃,反应压力为常压,分解反应结束后得到粗品。反应过程中生成的氮气高空排放。
⑷后处理
将粗品转入至萃取釜中,加入一定量的液碱进行中和,再加入氯仿进行萃取分离,水相经过滤回收氯化亚铜后进入污水处理。有机相转入至蒸馏釜
中,于60℃减压蒸馏采用二级盐冷回收三氯甲烷(回用)后,于100℃减压蒸馏得到2,3-二氯吡啶粗品,残渣委托处理。粗品最后加入甲醇进行精制、冷却结晶、离心过滤、干燥得到产品。离心过滤滤液于64.8℃常压蒸馏甲醇回用,残渣委托处理。
本产品总收率约为82.9%。本项目采用二级盐水冷凝,冷冻盐水温度为-20℃,冷凝器面积均为10m2。氯仿(沸点61.3℃)、甲醇(沸点64.8℃)的冷凝效率为96%、96%。

Claims (2)

1.一种二氯吡啶生产工艺。
2.本发明生产涉及的原材料及配比。
CN201510807194.0A 2015-11-22 2015-11-22 一种二氯吡啶生产工艺 Pending CN106748980A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510807194.0A CN106748980A (zh) 2015-11-22 2015-11-22 一种二氯吡啶生产工艺

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510807194.0A CN106748980A (zh) 2015-11-22 2015-11-22 一种二氯吡啶生产工艺

Publications (1)

Publication Number Publication Date
CN106748980A true CN106748980A (zh) 2017-05-31

Family

ID=58886625

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510807194.0A Pending CN106748980A (zh) 2015-11-22 2015-11-22 一种二氯吡啶生产工艺

Country Status (1)

Country Link
CN (1) CN106748980A (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107954913A (zh) * 2017-12-21 2018-04-24 山东天信化工有限公司 一种卤代含氮不饱和环烃的制备方法
CN113292486A (zh) * 2021-06-08 2021-08-24 安徽星宇化工有限公司 一锅法2,3-二氯吡啶合成方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1807414A (zh) * 2006-02-06 2006-07-26 南京广通医药化工有限责任公司 一种2,3-二氯吡啶的合成方法
CN102086174A (zh) * 2011-03-07 2011-06-08 南京广通医药化工有限责任公司 2,3-二氯吡啶的生产方法
CN103570609A (zh) * 2013-10-28 2014-02-12 南通天泽化工有限公司 一种2,3-二氯吡啶的制备方法
CN104926715A (zh) * 2015-06-03 2015-09-23 安徽绩溪县徽煌化工有限公司 一种2,3-二氯吡啶的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1807414A (zh) * 2006-02-06 2006-07-26 南京广通医药化工有限责任公司 一种2,3-二氯吡啶的合成方法
CN102086174A (zh) * 2011-03-07 2011-06-08 南京广通医药化工有限责任公司 2,3-二氯吡啶的生产方法
CN103570609A (zh) * 2013-10-28 2014-02-12 南通天泽化工有限公司 一种2,3-二氯吡啶的制备方法
CN104926715A (zh) * 2015-06-03 2015-09-23 安徽绩溪县徽煌化工有限公司 一种2,3-二氯吡啶的制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107954913A (zh) * 2017-12-21 2018-04-24 山东天信化工有限公司 一种卤代含氮不饱和环烃的制备方法
CN113292486A (zh) * 2021-06-08 2021-08-24 安徽星宇化工有限公司 一锅法2,3-二氯吡啶合成方法

Similar Documents

Publication Publication Date Title
WO2017181759A1 (zh) 一种利用含锂废液制备无水氯化锂的方法
CN106748980A (zh) 一种二氯吡啶生产工艺
CN103896808A (zh) 一种制备偶氮二异丁腈的方法
EP2323990B1 (en) Methods for the production of 2-halo-4-nitroimidazole and intermediates thereof
CN107556214A (zh) 一种对氰基苯甲酸的制备方法
CN106608858A (zh) 一种硫噻唑生产工艺
CN101723883A (zh) 一种羟尼酮的制备方法
CN103351291B (zh) 一种天然根皮苷半合成制备根皮素工艺
CN103508974A (zh) 一种处理邻磺酰胺苯甲酸甲酯结晶母液的方法
CN105153251B (zh) 一种单糖甲苷的苄基化方法
CN104860843B (zh) 一种丙酮连氮的合成方法
CN104892405B (zh) 一种烯酮废水中提取对氯苯甲酸的方法
CN108440348A (zh) 一种als生产工艺
CN102924255A (zh) 一种液相氧化制备9-芴酮的方法
CN105315197A (zh) 2-氯-5-吡啶甲醛的制造方法
CN112225720A (zh) 一种噻吩-2-乙酰氯的生产方法
CN105985275B (zh) 一种依泽替米贝及其中间体的制备方法
CN111892488A (zh) 一种高效合成2,6-二氯-3-氟苯乙酮的方法
CN105899482B (zh) 六氯丙酮的制造方法
CN108530370A (zh) 一种一锅法合成轮环藤宁的方法
CN108383720A (zh) 一种邻取代苯甲酸间位氯化方法
CN104230747B (zh) 一种不对称芳香偶氮化合物的制备方法
CN101125815B (zh) 一种6-氯-6-氧代己酸乙酯的化学合成方法
CN101367849B (zh) 三氯蔗糖-2,3,6,3',4'-五乙酸酯的制备方法
CN110845337B (zh) 一种合成2-溴-4-氟-5-氨基-苯乙酸乙酯的方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170531

WD01 Invention patent application deemed withdrawn after publication