CN1109013C - 氯代苯酐异构体的分离方法 - Google Patents

氯代苯酐异构体的分离方法 Download PDF

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Publication number
CN1109013C
CN1109013C CN96122195A CN96122195A CN1109013C CN 1109013 C CN1109013 C CN 1109013C CN 96122195 A CN96122195 A CN 96122195A CN 96122195 A CN96122195 A CN 96122195A CN 1109013 C CN1109013 C CN 1109013C
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chloro
benzoic anhydride
isomers
benzoic
anhydride
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CN1186063A (zh
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丁孟贤
张劲
杨正华
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JILIN HIPOLYKING POLYIMIDE MATERIAL CO., LTD.
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Changchun Institute of Applied Chemistry of CAS
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Abstract

本发明属于氯代苯酐异构体的分离。在压力范围为6-100KPa，相应温度为180-215℃，以20块以上的理论塔板可以由混合氯代苯酐蒸馏获得95%以上高纯度的3-氯代苯酐和4-氯代苯酐。

Description

氯代苯酐异构体的分离方法
本发明属于氯代苯酐异构体的分离方法。
氯代苯酐是聚酰亚胺的重要原料，用它可以合成多种单体二酐，也可用来直接合成聚酰亚胺。此外氯代苯酐还是染料中间体、药物的原料。在现有的合成路线中，以邻二甲苯为原料，氯代后再以空气氧化为氯代苯酐的方法最为经济。但目前尚未找到选择性足够高的方法，以获得单一的3-氯代邻二甲苯或4-氯代邻二甲苯。以上述的方法，中国专利92104637·5，获得的氯代邻二甲苯为二种异构体的混合物，3-位和4-位氯代的异构体的比例约为45∶55。二者的沸点仅相差1-2℃，难以分离。4-氯代苯酐的沸点为298℃，3-氯代苯酐的沸点尚未见报道。由混合的氯代苯酐分离二种异构体的方法也未见报道。
本发明的目的是提供一种蒸馏分离高纯度3-氯代苯酐和4-氯代苯酐的方法。
本发明包括在压力范围为6-100KPa，相应温度为180-325℃，蒸馏分离出95％以上高纯度的3-氯代苯酐和4-氯代苯酐的方法。
如上所述，目前尚无从混合氯代苯酐中分离出二个异构体的方法报道。蒸馏法与其它方法如重结晶法比较，则是化学工业最易接受、最经济又适于大规模生产的方法。
实施例1：
将500克氯代苯酐在常压(99KPa)下，通过一根约有25块理论塔板的分馏柱进行蒸馏、各馏分情况如下表：
  馏份温度(℃) 1          2         3         4         5         6＜290      290-292   292-296   296-299   296-306   306-325
 苯酐3-氯代苯酐4-氯代苯酐重量(克) 含水分的   0.17％    0.03％    0.09％    0.33％    0.01％馏头部分   0.43％    15.25％   17.82％   35.08％   97.67％99.39％   84.72％   82.09％   64.60％   2.32％21.4       122.5     97.5      60.2      55.0      101.8
纯度由气相色谱测定，混合氯代苯酐的组分为：苯酐：0.12％，3-氯代苯酐：40.78％，4-氯代苯酐：59.14％。蒸馏后残液33.5克。
实施例2：
以1000公斤混合氯代苯酐，通过理论塔板为45块的蒸馏塔，在12.5KPa压强下进行蒸馏，在208-212℃获得4-氯代苯酐608公斤，纯度为98.5％；在216-221℃获得3-氯代苯酐278公斤，纯度为98.3％。

Claims (1)

1.一种氯代苯酐异构体的分离方法，是在压力范围6-100Kpa，相应温度为180-325℃下蒸馏分离，其特征在于采用3-氯代苯酐和4-氯代苯酐异构体为原料，该过程在一个蒸馏塔中完成，得到纯度为95％以上的3-氯代苯酐和4-氯代苯酐。
CN96122195A 1996-12-25 1996-12-25 氯代苯酐异构体的分离方法 Expired - Lifetime CN1109013C (zh)

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CN1109013C true CN1109013C (zh) 2003-05-21

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260168B (zh) * 2011-05-10 2013-11-27 柯美达（北京）科技有限公司 单氯代邻苯二甲酸的分离方法和产品
CN103819435A (zh) * 2014-02-17 2014-05-28 扬州大学 一种从单氯代苯酐异构体混合物中分离3-氯代苯酐的方法
CN105646419B (zh) * 2016-03-23 2017-11-03 天津大学 一种结晶提纯3‑氯代苯酐的方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB869297A (en) * 1957-09-19 1961-05-31 Yawata Iron & Steel Co Continuous purification of crude maleic anhydride
EP0719757A1 (de) * 1995-01-02 1996-07-03 Basf Aktiengesellschaft Verfahren zur Herstellung von 3-Chlorphthalsäureanhydrid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB869297A (en) * 1957-09-19 1961-05-31 Yawata Iron & Steel Co Continuous purification of crude maleic anhydride
EP0719757A1 (de) * 1995-01-02 1996-07-03 Basf Aktiengesellschaft Verfahren zur Herstellung von 3-Chlorphthalsäureanhydrid

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