CN104016905A - 一种2-乙烯基吡啶的制备方法 - Google Patents

一种2-乙烯基吡啶的制备方法 Download PDF

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Publication number
CN104016905A
CN104016905A CN201410257602.5A CN201410257602A CN104016905A CN 104016905 A CN104016905 A CN 104016905A CN 201410257602 A CN201410257602 A CN 201410257602A CN 104016905 A CN104016905 A CN 104016905A
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China
Prior art keywords
vinylpyridine
formaldehyde
picoline
vinyl pyridine
preparation
Prior art date
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Pending
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CN201410257602.5A
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English (en)
Inventor
吕荣明
杨亮鸿
蔺继朋
蔺军虎
兰其盈
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Jiangsu Ya Tai Chemical Co Ltd
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Jiangsu Ya Tai Chemical Co Ltd
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Priority to CN201410257602.5A priority Critical patent/CN104016905A/zh
Publication of CN104016905A publication Critical patent/CN104016905A/zh
Pending legal-status Critical Current

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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
    • C07D213/06—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 containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/16—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 containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
    • 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
    • C07D213/06—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 containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/127—Preparation from compounds containing pyridine rings

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

Abstract

2-乙烯基吡啶制备主要原料是2-甲基吡啶及甲醛，其合成工艺有两大类，“两步法”及“一步法”生产工艺。其合成路线是2-甲基吡啶、甲醛缩合生产羟乙基吡啶，羟乙基吡啶在一定温度及催化剂作用下脱水生成2-乙烯基吡啶。本发明为“一步法”生产工艺，采用2-甲基吡啶及甲醛为原料在一定温度及酸催化剂作用下一步生成2-乙烯基吡啶，其工艺流程简单，收率高，原辅料消耗及能耗均优于“两步法”。

Description

一种2-乙烯基吡啶的制备方法
技术领域
本发明涉及化工生产技术领域，具体地说是一种2-乙烯基吡啶的制备方法。
背景技术
2-乙烯基吡啶除了用来合成广泛应用的丁吡(丁苯吡)胶乳外，还用于其它高分子材料改性、离子交换树脂、印染助剂、药剂合成等，主要生产国有日本、美国、印度、中国等。目前国内2-乙烯基吡啶均为“两步法”合成工艺，该工艺在我国已很成熟，淄博张店东方化学已有专利报道，其合成路线是2-甲基吡啶、甲醛缩合生产羟乙基吡啶，羟乙基吡啶在一定温度及催化剂作用下脱水生成2-乙烯基吡啶，然而该工艺路线复杂、能耗大，同时产生大量废渣及废碱液，严重不利于当前环保要求和企业生产效率。
发明内容
本发明的目的是为了克服现有技术的不足，采用“一步法”合成2-乙烯基吡啶，其工艺简单，收率高，原辅料消耗及能耗低等特点。
根据本发明示例的一种2-乙烯基吡啶的制备方法是指：
将2-甲基吡啶和甲醛在强酸和烯烃阻聚剂的存在下在管道反应器中反应2～10分钟，一步高收率的得到2-乙烯基吡啶。其具体特征在于：
a)2-甲基吡啶与甲醛的摩尔比为1.5～3.5∶1。
b)合成2-乙烯基吡啶催化剂为强酸，如硫酸或磷酸。
c)合成2-乙烯基吡啶催化剂用量为甲醛的5～10％。
d)合成2-乙烯基吡啶的反应温度为160～240℃，反应压力为3～10Mpa，反应时间2～10分钟。
具体实施方式
下面采用一个实施例来进一步阐明本发明：
将2-甲基吡啶6750克/小时流经一管道，甲醛900克、水1500克和硫酸205克组成的混合物(2-甲基吡啶∶甲醛∶硫酸＝2.5∶1∶0.07)以2605克/小时流经另一管道，同时进入容积为1000毫升的管道式反应器，温度控制在230℃，压力7.0Mpa，停留时间5分钟，由此每小时得到的反应物包含4200克未反应的2-甲基吡啶，2560克2-乙烯基吡和40克羟乙基吡啶。2-甲基吡啶的收率以转化的2-甲基吡啶计算约89％。单程收率是33％，2-甲基吡啶的单程转化率37％。
上述具体实施实例是对本发明的进一步描述，不能理解为对本发明保护范围的限制，本发明不限于上述实施实例。

Claims (4)

1.一种2-乙烯基吡啶的制备方法，其特征在于，将2-甲基吡啶和甲醛在强酸和烯烃阻聚剂的存在下在管道反应器中反应2～10分钟，一步高收率的得到2-乙烯基吡啶。
2.根据权利要求书1所述的一种2-乙烯基吡啶的制备方法，其特征在于：2-甲基吡啶与甲醛的摩尔比为1.5～3.5∶1。
3.根据权利要求书1所述的一种2-乙烯基吡啶的制备方法，其特征在于：所述强酸的用量为甲醛的5～10％。
4.根据权利要求书1所述的一种2-乙烯基吡啶的制备方法，其特征在于：合成2-乙烯基吡啶的反应温度为160～240℃，反应压力为3～10Mpa，反应时间2～10分钟。
CN201410257602.5A 2014-06-06 2014-06-06 一种2-乙烯基吡啶的制备方法 Pending CN104016905A (zh)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105175319A (zh) * 2015-10-15 2015-12-23 江苏宝众宝达药业有限公司 一种盐酸倍他司汀的制备方法
CN111995566A (zh) * 2019-12-19 2020-11-27 上海中西三维药业有限公司 一种2-羟乙基吡啶的合成方法
CN112028817A (zh) * 2019-12-18 2020-12-04 上海中西三维药业有限公司 一种2-乙烯基吡啶的制备方法
CN112108177A (zh) * 2020-09-11 2020-12-22 北京弗莱明科技有限公司 一种乙烯基氮苯的制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2512660A (en) * 1946-03-07 1950-06-27 Phillips Petroleum Co Production of pyridine derivative
US6727365B1 (en) * 2002-10-31 2004-04-27 Shivanand Janardan Kulkarni Process for the preparation of vinylpyridine from picoline over modified zeolites
CN102675192A (zh) * 2011-03-09 2012-09-19 淄博张店东方化学股份有限公司 2-乙烯基吡啶生产过程中的连续缩合工艺

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2512660A (en) * 1946-03-07 1950-06-27 Phillips Petroleum Co Production of pyridine derivative
US6727365B1 (en) * 2002-10-31 2004-04-27 Shivanand Janardan Kulkarni Process for the preparation of vinylpyridine from picoline over modified zeolites
CN102675192A (zh) * 2011-03-09 2012-09-19 淄博张店东方化学股份有限公司 2-乙烯基吡啶生产过程中的连续缩合工艺

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105175319A (zh) * 2015-10-15 2015-12-23 江苏宝众宝达药业有限公司 一种盐酸倍他司汀的制备方法
CN112028817A (zh) * 2019-12-18 2020-12-04 上海中西三维药业有限公司 一种2-乙烯基吡啶的制备方法
CN112028817B (zh) * 2019-12-18 2023-10-03 上海中西三维药业有限公司 一种2-乙烯基吡啶的制备方法
CN111995566A (zh) * 2019-12-19 2020-11-27 上海中西三维药业有限公司 一种2-羟乙基吡啶的合成方法
CN111995566B (zh) * 2019-12-19 2023-12-26 上海中西三维药业有限公司 一种2-羟乙基吡啶的合成方法
CN112108177A (zh) * 2020-09-11 2020-12-22 北京弗莱明科技有限公司 一种乙烯基氮苯的制备方法

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Application publication date: 20140903