CN103709087B - 一种α-吡咯烷酮的制备方法 - Google Patents

一种α-吡咯烷酮的制备方法 Download PDF

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CN103709087B
CN103709087B CN201310632185.3A CN201310632185A CN103709087B CN 103709087 B CN103709087 B CN 103709087B CN 201310632185 A CN201310632185 A CN 201310632185A CN 103709087 B CN103709087 B CN 103709087B
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pyrrolidone
alpha
waste residue
production process
acid
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CN103709087A (zh
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张恒家
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Jiaozuo Zhongwei Special Products Pharmaceutical Co ltd
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JIAOZUO ZHONGWEI SPECIAL PRODUCTS PHARMACEUTICAL CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
    • C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member 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
    • C07D207/24—Oxygen or sulfur atoms
    • C07D207/26—2-Pyrrolidones
    • C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
    • C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
    • C07D201/16—Separation or purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pyrrole Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

本发明公开了一种α-吡咯烷酮的制备方法，包括以下步骤：将N-乙烯基吡咯烷酮生产过程中产生的废渣粉碎，放入釜中加上述废渣重量1-1.2倍的水，在50-60℃下加热搅拌，至固体废渣不再溶解为止，过滤，水溶液蒸馏后得部分α<b>-</b>吡咯烷酮纯品；将上述过滤后得到的水的不溶物加入其重量0.5-15%的催化剂进行搅拌，加热至100-150℃，生成<b>α-</b>吡咯烷酮粗品；然后对粗品进行减压蒸馏，得到α-吡咯烷酮纯品。本发明利用N-乙烯基吡咯烷酮生产过程中产生的废渣，使废渣减量化和增值化；所述的催化剂用量小，价格低，使其成本大幅度降低；催化剂直接和反应液一起反应，不需要人工填装和更换，节省时间；本发明生产条件温和、安全，通过此工艺的生产过程后，N-乙烯基吡咯烷酮生产过程中产生的废液量可以降低65%，实现了废品物资的减量化和增值化。

Description

一种α-吡咯烷酮的制备方法
技术领域
本发明主要涉及一种α-吡咯烷酮的制备方法，属于化工领域。
背景技术
α-吡咯烷酮是一种十分有用的溶剂和医药中间体，性质活泼，为无色或微黄色澄清液体，有微氨味，25℃以下为无色结晶。熔点24.6℃，沸点245℃，能与水、醇、醚、氯仿等混溶，难溶于石油醚。由其衍生可以制备多种物质，比如：用于合成尼龙4、N-乙烯基吡咯烷酮、聚酰胺纤维等。
分子式：C4H7NO
分子量：85.11
分子结构式：
国内生产α-吡咯烷酮一般是采用γ-丁内酯作原料，已经有较成熟的工艺，其衍生物之一的N-乙烯基吡咯烷酮在蒸馏后有12-15%的蒸馏残渣，属三废中的废渣。
发明内容
本发明目的就是为了提供一种α-吡咯烷酮的制备方法。
本发明是通过以下技术方案实现的：
一种α-吡咯烷酮的制备方法，包括以下步骤：
将N-乙烯基吡咯烷酮生产过程中产生的废渣粉碎，放入釜中加上述废渣重量1-1.2倍的水，在50-60℃下加热搅拌，至固体废渣不再溶解为止，过滤，水溶液蒸馏后后得部分α-吡咯烷酮纯品；
将上述过滤后得到的水的不溶物加入其重量0.5-15%的催化剂进行搅拌，加热至100-150℃，生成α-吡咯烷酮粗品；然后对粗品进行减压蒸馏，得到α-吡咯烷酮纯品。
一种α-吡咯烷酮的制备方法，所述的催化剂为无机和有机酸类组合物溶液，比如硼酸、苯甲酸、萘硫酸、琥珀酸、磷苯二甲酸、对苯二酸、枸橼酸中的任意两种或两种以上。
一种α-吡咯烷酮的制备方法，N-乙烯基吡咯烷酮生产过程中产生的废渣中主要成分及含量为：主要有未反应的α-吡咯烷酮（约占10-15%）；未蒸出的N-乙烯基吡咯烷酮（约占3-5%），α-吡咯烷酮多聚体（约占20-35%），N,N’-二吡咯烷酮乙缩醛（30-40%），其它副产物（5-35%）。
本发明的优点是：
本发明利用N-乙烯基吡咯烷酮生产过程中产生的废渣，使废渣减量化和增值化；所述的催化剂用量小，价格低，使其成本大幅度降低；催化剂直接和反应液一起反应，不需要人工填装和更换，节省时间；本发明生产条件温和、安全，通过此工艺的生产过程后，N-乙烯基吡咯烷酮生产过程中产生的废液量可以降低65%，实现了废品物资的减量化和增值化。
具体实施方式
实施例1
一种α-吡咯烷酮的制备方法，包括以下步骤：
将N-乙烯基吡咯烷酮生产过程中产生的废渣粉碎，放入釜中加上述废渣重量1倍的水，在60℃下加热搅拌，至固体废渣不再溶解为止，过滤，水溶液蒸馏后后得部分α-吡咯烷酮纯品,蒸馏废液进行循环使用，反应的残渣装桶，交由有处理资质的单位处理；
将上述过滤后得到的水的不溶物加入其重量2%的催化剂进行搅拌，加热至150℃，生成α-吡咯烷酮粗品；然后对粗品进行减压蒸馏，得到α-吡咯烷酮纯品。
一种α-吡咯烷酮的制备方法，所述的催化剂为无机和有机酸类组合物溶液，比如硼酸、苯甲酸、萘硫酸、琥珀酸、磷苯二甲酸、对苯二酸、枸橼酸中的任意两种或两种以上。

Claims (1)

1.一种α-吡咯烷酮的制备方法，其特征在于包括以下步骤：
将N-乙烯基吡咯烷酮生产过程中产生的废渣粉碎，放入釜中加上述废渣重量1-1.2倍的水，在50-60℃下加热搅拌，至固体废渣不再溶解为止，过滤，水溶液蒸馏后得部分α-吡咯烷酮纯品；
将上述过滤后得到的水的不溶物加入其重量0.5-15%的催化剂进行搅拌，加热至100-150℃，生成α-吡咯烷酮粗品；然后对粗品进行减压蒸馏，得到α-吡咯烷酮纯品；
所述的催化剂为无机和有机酸类组合物溶液，为硼酸、苯甲酸、萘硫酸、琥珀酸、邻苯二甲酸、对苯二酸、枸橼酸中的任意两种或两种以上；
所述的N-乙烯基吡咯烷酮生产过程中产生的废渣中主要成分及含量为：主要有未反应的α-吡咯烷酮，占10-15%；未蒸出的N-乙烯基吡咯烷酮，占3-5%，α-吡咯烷酮多聚体，占20-35%；N,N’-二吡咯烷酮乙缩醛，占30-40%，其它副产物，占5-35%。
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CN106166559B (zh) * 2016-06-13 2018-08-21 焦作中维特品药业有限公司 一种nvp生产中残渣物质处理回收的方法
CN106432027A (zh) * 2016-06-13 2017-02-22 焦作中维特品药业有限公司 一种2‑吡咯烷酮的纯化方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4264501A (en) * 1977-05-06 1981-04-28 Stamicarbon, B.V. Process for the recovery of pyrrolidone-2
CN1095373A (zh) * 1993-05-22 1994-11-23 秦应胜 N-甲基吡咯烷酮回收方法
CN1551868A (zh) * 2001-09-07 2004-12-01 �����ɷ� 2-吡咯烷酮的制备方法
CN103003238A (zh) * 2010-05-19 2013-03-27 生物琥珀酸有限公司 吡咯烷酮的制备方法
CN103025712A (zh) * 2010-05-19 2013-04-03 生物琥珀酸有限公司 吡咯烷酮的制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4264501A (en) * 1977-05-06 1981-04-28 Stamicarbon, B.V. Process for the recovery of pyrrolidone-2
CN1095373A (zh) * 1993-05-22 1994-11-23 秦应胜 N-甲基吡咯烷酮回收方法
CN1551868A (zh) * 2001-09-07 2004-12-01 �����ɷ� 2-吡咯烷酮的制备方法
CN103003238A (zh) * 2010-05-19 2013-03-27 生物琥珀酸有限公司 吡咯烷酮的制备方法
CN103025712A (zh) * 2010-05-19 2013-04-03 生物琥珀酸有限公司 吡咯烷酮的制备方法

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