CN106748977A - 一种乙烯基吡啶生产工艺 - Google Patents
一种乙烯基吡啶生产工艺 Download PDFInfo
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- CN106748977A CN106748977A CN201510805067.7A CN201510805067A CN106748977A CN 106748977 A CN106748977 A CN 106748977A CN 201510805067 A CN201510805067 A CN 201510805067A CN 106748977 A CN106748977 A CN 106748977A
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- CN
- China
- Prior art keywords
- vinylpyridine
- production technology
- ethoxy
- kettle
- pyridine
- 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.)
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Classifications
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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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
乙烯基吡啶是一种重要的化工产品。生产流程：（1）2-羟乙基吡啶合成；（2）脱水反应；（3）精蒸。
Description
乙烯基吡啶工艺流程
1、反应机理
（1）2-乙烯基吡啶
①聚合反应
物料名称：2-甲基吡啶多聚甲醛 2-羟乙基吡啶
分子量：
93.13 30（n） 123.13
②脱水反应
物料名称：2-羟乙基吡啶
2-乙烯基吡啶水
分子量：
123.13 105.13 18.0
③副反应：2-乙烯基吡啶在加热条件下会发生缩聚反应，生成聚2-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：
物料名称： 2-乙烯基吡啶聚2-乙烯基吡啶
分子量：
n105.13 105.13n
（1）2-羟乙基吡啶合成
在合成釜中加入定量的2-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2-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2-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
2（4）-乙烯基吡啶生产原料为2-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)
1.一种乙烯基吡啶生产工艺。
2.乙烯基吡啶生产涉及的原料成分及配比。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510805067.7A CN106748977A (zh) | 2015-11-21 | 2015-11-21 | 一种乙烯基吡啶生产工艺 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510805067.7A CN106748977A (zh) | 2015-11-21 | 2015-11-21 | 一种乙烯基吡啶生产工艺 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106748977A true CN106748977A (zh) | 2017-05-31 |
Family
ID=58915856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510805067.7A Pending CN106748977A (zh) | 2015-11-21 | 2015-11-21 | 一种乙烯基吡啶生产工艺 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106748977A (zh) |
-
2015
- 2015-11-21 CN CN201510805067.7A patent/CN106748977A/zh active Pending
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Application publication date: 20170531 |