CN1160346C - 氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法 - Google Patents
氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法 Download PDFInfo
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- CN1160346C CN1160346C CNB011102047A CN01110204A CN1160346C CN 1160346 C CN1160346 C CN 1160346C CN B011102047 A CNB011102047 A CN B011102047A CN 01110204 A CN01110204 A CN 01110204A CN 1160346 C CN1160346 C CN 1160346C
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- OLENANGIJWDOPG-UHFFFAOYSA-N (2-chlorobenzoyl) 2-chlorobenzoate Chemical compound ClC1=CC=CC=C1C(=O)OC(=O)C1=CC=CC=C1Cl OLENANGIJWDOPG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- BKFXSOCDAQACQM-UHFFFAOYSA-N 3-chlorophthalic acid Chemical compound OC(=O)C1=CC=CC(Cl)=C1C(O)=O BKFXSOCDAQACQM-UHFFFAOYSA-N 0.000 title claims abstract description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012043 crude product Substances 0.000 claims abstract description 13
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- NVLHGZIXTRYOKT-UHFFFAOYSA-N 1-chloro-2,3-dimethylbenzene Chemical group CC1=CC=CC(Cl)=C1C NVLHGZIXTRYOKT-UHFFFAOYSA-N 0.000 claims description 9
- 238000002203 pretreatment Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- UERPUZBSSSAZJE-UHFFFAOYSA-N 3-chlorophthalic anhydride Chemical class ClC1=CC=CC2=C1C(=O)OC2=O UERPUZBSSSAZJE-UHFFFAOYSA-N 0.000 abstract 1
- -1 4-chlorobenzene anhydride Chemical class 0.000 abstract 1
- 238000010533 azeotropic distillation Methods 0.000 abstract 1
- 238000003672 processing method Methods 0.000 abstract 1
- 239000008096 xylene Substances 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000003472 neutralizing effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- NIHKFGMYMWGERR-UHFFFAOYSA-N (3-chlorobenzoyl) 3-chlorobenzoate Chemical compound ClC1=CC=CC(C(=O)OC(=O)C=2C=C(Cl)C=CC=2)=C1 NIHKFGMYMWGERR-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- MWUSAETYTBNPDG-UHFFFAOYSA-N (4-chlorobenzoyl) 4-chlorobenzoate Chemical compound C1=CC(Cl)=CC=C1C(=O)OC(=O)C1=CC=C(Cl)C=C1 MWUSAETYTBNPDG-UHFFFAOYSA-N 0.000 description 1
- BOCJQSFSGAZAPQ-UHFFFAOYSA-N 1-chloroanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2Cl BOCJQSFSGAZAPQ-UHFFFAOYSA-N 0.000 description 1
- HNQLMBJUMVLFCF-UHFFFAOYSA-N 4-chloro-1,2-dimethylbenzene Chemical group CC1=CC=C(Cl)C=C1C HNQLMBJUMVLFCF-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- FRCLEVMOUWRROF-UHFFFAOYSA-N ClC1=C(C(C(=O)O)=CC=C1)C(=O)O.ClC1=C(C(=O)OC(C2=C(C=CC=C2)Cl)=O)C=CC=C1 Chemical compound ClC1=C(C(C(=O)O)=CC=C1)C(=O)O.ClC1=C(C(=O)OC(C2=C(C=CC=C2)Cl)=O)C=CC=C1 FRCLEVMOUWRROF-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明属于氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法。该方法是使用一种带水剂兼溶剂又与水不相溶的物质：甲苯、二甲苯、氯苯或氯代邻二甲苯和粗产物混合加热，利用共沸蒸馏将粗产物中所含的水分和盐酸带出，在分水器中分层后将带水剂循环使用；当水分和盐酸带尽后，将含有少量溶剂的残留物料打入异构体精馏釜，就可以进行3-氯代苯酐和4-氯代苯酐异构体的分离。
Description
本发明属于氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法。
氯代苯酐是合成高性能高分子材料聚酰亚胺、燃料中间体氯代蒽醌及农药和药物的重要原料。氯代邻二甲苯经气相或液相氧化可以得到氯代苯酐。单氯代邻二甲苯存在3-氯代邻二甲苯和4-氯代邻二甲苯两个异构体，这两个异构体因为沸点太接近而难以用精馏方法分离，而氧化后的3-氯代苯酐和4-氯代苯酐两者的异构体的沸点有20-30℃之差，可以用精馏方法分离(中国专利：96122195.x)。气相氧化产物中由于深度氧化而产生氯化氢和水及二氧化碳，氯化氢和水在冷却后形成盐酸。氯代苯酐在水分存在下水解得到的氯代邻苯二甲酸，液相氧化的产物就是氯代邻苯二甲酸，由于氯的活化，氯代邻苯二甲酸的酸性也很强。因此将这些粗产物精馏时都会对设备造成严重的腐蚀。
本发明的目的是提供一种氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法，该方法使氯代苯酐及氯代邻苯二甲酸粗产物精馏时避免酸性物质对设备腐蚀的前处理方法。
本发明是将氯代苯酐或氯代邻苯二甲酸粗产物和一种带水剂兼溶剂又与水不相溶的物质：甲苯、二甲苯、氯苯或氯代邻二甲苯混合加热，粗产物中所含的水分和盐酸及加热氯代邻苯二甲酸脱水形成的水由带水剂带出，在分水器中分层后将带水剂循环使用；氯代苯酐则溶于兼带水剂的溶剂中，当水分和盐酸带尽后，剩下的就是没有腐蚀性的氯代苯酐溶液，将剩余的带水剂兼溶剂尽量蒸出后将含有少量溶剂的残留物料打入异构体精馏釜，就可以进行3-氯代苯酐和4-氯代苯酐异构体的分离；本发明中带水剂兼溶剂与氯代苯酐或氯代邻苯二甲酸粗产物的重量比为0.2-2倍；带水剂兼溶剂的馏出温度为共沸物的沸点到带水剂的沸点，当沸点达到带水剂的沸点时，物料中的水分就已基本除尽。
实施例1
将粗氯代苯酐500kg和1000kg甲苯在3000L预处理釜中搅拌加热，甲苯和水的共沸物在90℃开始蒸出，馏液在分水器中分层后将处于上层的甲苯放回釜中，下层酸水放出中和处理后排放，到馏出物的沸点达到110℃，馏出的甲苯中不再含水，然后将釜中的甲苯尽量蒸出后，再将残留的含少量甲苯的氯代苯酐打到精馏釜中进行异构体分离。
实施例2
将粗氯代苯酐1000kg和500kg二甲苯在3000L预处理釜中搅拌加热，共沸物在95℃开始蒸出，馏液在分水器中分层后将处于上层的邻二甲苯放回釜中，下层酸水放出中和处理后排放，到馏出物的沸点达到144℃，馏出的邻二甲苯不再含水时将釜中的邻二甲苯尽量蒸出后，再将残留的含少量邻二甲苯的氯代苯酐打到精馏釜中进行异构体分离。
实施例3
将粗氯代邻苯二甲酸1000kg和700kg氯苯在3000L预处理釜中搅拌加热，共沸物在90℃开始蒸出，馏液在分水器中分层后将处于下层的氯苯放回釜中，上层酸水放出中和处理后排放，到馏出物的沸点达到190℃后，蒸出的氯代邻二甲苯中不再含水时将釜中的氯代邻二甲苯蒸出，再将残留的含少量氯代邻二甲苯的氯代苯酐打到精馏釜中进行异构体分离。
实施例4
将粗氯代苯酐1000kg和200kg氯代邻二甲苯在3000L预处理釜中搅拌加热，共沸物在98℃开始蒸出，馏液在分水器中分层后将处于下层的氯代邻二甲苯放回釜中，上层酸水放出中和处理后排放，到馏出物的沸点达到131℃后，蒸出的氯苯中不再含水时将釜中的氯苯蒸出，再将残留的含少量氯苯的氯代苯酐打到精馏釜中进行异构体分离。
Claims (1)
1.一种氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法，其特征在于用甲苯、二甲苯、氯苯或氯代邻二甲苯为带水剂兼溶剂与氯代苯酐及氯代邻苯二甲酸粗产物的重量比为0.2-2∶1的比例在预处理釜中加热搅拌，将存在和产生的水分和盐酸带出，经分层后，带水剂兼溶剂返回釜中重复使用，直到蒸出的带水剂兼溶剂中不再含有水分，再将釜中的带水剂兼溶剂蒸出。
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| Application Number | Priority Date | Filing Date | Title |
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| CNB011102047A CN1160346C (zh) | 2001-04-02 | 2001-04-02 | 氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法 |
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| CNB011102047A CN1160346C (zh) | 2001-04-02 | 2001-04-02 | 氯代苯酐及氯代邻苯二甲酸粗产物的精馏前处理方法 |
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| Publication Number | Publication Date |
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| CN1318543A CN1318543A (zh) | 2001-10-24 |
| CN1160346C true CN1160346C (zh) | 2004-08-04 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6670487B1 (en) * | 2002-06-18 | 2003-12-30 | General Electric Company | Method for removing impurities from oxidation products |
| 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 |
| 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 |
| CN114621170B (zh) * | 2022-03-16 | 2023-07-11 | 万华化学集团股份有限公司 | 一种纯化氯代邻二甲苯气相氧化产物中4-氯代苯酐和3-氯代苯酐的方法 |
| CN114656351B (zh) * | 2022-05-24 | 2022-08-26 | 河北海力香料股份有限公司 | 一种4-氯代邻苯二甲酸或其单钠盐生产废水的处理方法 |
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2001
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