CN106699641A - 一种4-乙烯基吡啶生产工艺 - Google Patents

一种4-乙烯基吡啶生产工艺 Download PDF

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Publication number
CN106699641A
CN106699641A CN201510774383.2A CN201510774383A CN106699641A CN 106699641 A CN106699641 A CN 106699641A CN 201510774383 A CN201510774383 A CN 201510774383A CN 106699641 A CN106699641 A CN 106699641A
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Prior art keywords
vinylpyridine
kettle
recycling
paraformaldehyde
crude product
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CN201510774383.2A
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English (en)
Inventor
胡江海
张晓磊
于飞
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Ningxia Jihua Environmental Safety Technology Co Ltd
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Ningxia Jihua Environmental Safety Technology Co Ltd
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Application filed by Ningxia Jihua Environmental Safety Technology Co Ltd filed Critical Ningxia Jihua Environmental Safety Technology Co Ltd
Priority to CN201510774383.2A priority Critical patent/CN106699641A/zh
Publication of CN106699641A publication Critical patent/CN106699641A/zh
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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
    • C07D213/127—Preparation from compounds containing pyridine rings

Abstract

4-乙烯基吡啶是一种重要的化工产品。4-乙烯基吡啶生产流程：4-羟乙基吡啶合成在合成釜中加入定量的4-甲基吡啶和多聚甲醛，在常压和温度105-110℃条件下进行反应45-70h，转化率40-60%，合成粗品先进入回收釜，开启回收釜夹套蒸汽加热，控制温度在114-116℃下冷凝回收套用，生成的2-羟乙基吡啶去粗品釜，未反应的2-甲基吡啶和多聚甲醛抽回缩合釜回收套用，直至反应效率达到95%。

Description

一种 4- 乙烯基吡啶生产工艺
4- 乙烯基吡啶反应机理
①聚合反应
反应式：
物料名称：4-甲基吡啶多聚甲醛 4-羟乙基吡啶
分子量：93.13 30（n） 123.13
②脱水反应
反应式：
物料名称：4-羟乙基吡啶 4-乙烯基吡啶水
分子量： 123.13 105.13 18.0
③副反应：4-乙烯基吡啶在加热条件下会发生缩聚反应，生成聚4-乙烯基吡啶，通过加入一定量的阻聚剂对叔丁基邻苯二酚（TBC）抑制其发生聚合反应。涉及的副反应方程式为：
反应式：
物料名称： 4-乙烯基吡啶聚4-乙烯基吡啶
分子量： n105.13 105.13n
（1）4-羟乙基吡啶合成
在合成釜中加入定量的4-甲基吡啶和多聚甲醛，在常压和温度105-110℃条件下进行反应45-70h，转化率40-60%，合成粗品先进入回收釜，开启回收釜夹套蒸汽加热，控制温度在114-116℃下冷凝回收套用，生成的2-羟乙基吡啶去粗品釜，未反应的2-甲基吡啶和多聚甲醛抽回缩合釜回收套用，直至反应效率达到95%。2-羟乙基吡啶回收过程会挥发产生2-甲基吡啶和2-羟乙基吡啶，经三级循环水冷凝和冷盐水深度冷凝液化后储存于尾气回收罐，剩余不凝气体经活性炭吸附装置处理
（2）脱水反应
脱水釜中加入脱水剂NaOH、阻聚剂TBC及水，搅拌并逐渐升温至180℃，滴加（4）-羟乙基吡啶，在脱水剂NaOH条件下，2-羟乙基吡啶脱水生成2-乙烯基吡啶和水，阻聚剂TBC防止（4）-羟乙基吡啶自聚反应，脱水反应效率按80%计算，釜液主要为 2-乙烯基吡啶及2-羟乙基吡啶混合液，经三级循环水冷凝和冷盐水深度冷凝液化后去精馏釜。
（3）精蒸
釜液在精馏釜内首先经过100℃减压蒸馏将废水蒸馏出，再经过117℃减压蒸馏将2-羟乙基吡啶蒸出收集，最后经过170℃减压蒸馏2-乙烯基吡啶蒸出制得成品。
粗品回收及产品接收过程中挥发物料经三级循环水冷凝、冷盐水深度冷凝后储存于回收罐套用
4 、主要原材料消耗情况
（4）-乙烯基吡啶生产原料为（4）-甲基吡啶、多聚甲醛、氢氧化钠、对叔丁基邻苯二酚（TBC）。
表2.3-10项目主要原料用量情况表
序号 原料名称 年用量（t） 纯度 工艺过程中作用
1 2-甲基吡啶 1300.0 含量≥99.5%，水分≤0.5% 反应物
2 4-甲基吡啶 650.0 含量≥99.5%，水分≤0.5% 反应物
3 多聚甲醛 600.0 含量≥99%，水分≤0.5% 反应物
4 氢氧化钠 300 含量≥99.0%，水分≤1.0% 脱水剂
5 对叔丁基邻苯二酚 150 含量≥97.0% ，水分≤3% 阻聚剂
6 水 450 --- 溶剂

Claims (2)

1.一种4-乙烯基吡啶生产工艺。
2.4-乙烯基吡啶生产过程原料配比及成分。
CN201510774383.2A 2015-11-14 2015-11-14 一种4-乙烯基吡啶生产工艺 Pending CN106699641A (zh)

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CN201510774383.2A CN106699641A (zh) 2015-11-14 2015-11-14 一种4-乙烯基吡啶生产工艺

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS535170A (en) * 1976-07-05 1978-01-18 Koei Chemical Co Treatment of methylol alkyl pyridines reactive solution
JPS53144577A (en) * 1977-05-18 1978-12-15 Koei Chemical Co Method of recovering vinylpyridine
CN102863375A (zh) * 2011-07-03 2013-01-09 沙文茜 合成制备2-乙烯基吡啶的方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS535170A (en) * 1976-07-05 1978-01-18 Koei Chemical Co Treatment of methylol alkyl pyridines reactive solution
JPS53144577A (en) * 1977-05-18 1978-12-15 Koei Chemical Co Method of recovering vinylpyridine
CN102863375A (zh) * 2011-07-03 2013-01-09 沙文茜 合成制备2-乙烯基吡啶的方法

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