CN100506789C - 离析的3,4-二氨基苯磺酸的制备方法 - Google Patents
离析的3,4-二氨基苯磺酸的制备方法 Download PDFInfo
- Publication number
- CN100506789C CN100506789C CNB031589995A CN03158999A CN100506789C CN 100506789 C CN100506789 C CN 100506789C CN B031589995 A CNB031589995 A CN B031589995A CN 03158999 A CN03158999 A CN 03158999A CN 100506789 C CN100506789 C CN 100506789C
- Authority
- CN
- China
- Prior art keywords
- acid
- sulfuric acid
- orthaminic
- product
- diaminobenzene
- 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.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
Abstract
Description
反应条件 | 原料 | 产物(单磺酸) | 次要产物(二磺酸) |
6小时/135℃ | 7.2 | 90.95 | 1.9 |
9小时/135℃ | 6.1 | 92.05 | 1.8 |
+3小时/138℃ | 5.7 | 92.37 | 1.9 |
+3小时/138℃ | 3.6 | 94.50 | 1.95 |
反应条件 | 原料 | 产物 | 次要产物 |
8小时/138℃ | 2.8 | 95.4 | 1.7 |
分离后产物 | 0.6 | 98.8 | 0.6 |
反应条件 | 原料 | 产物(3,4-二氨基苯磺酸) | 次要产物(二磺酸) |
6小时/138℃ | 4.1 | 91.2 | 2.1 |
随后加入发烟硫酸和3小时/135℃ | 3.1 | 91.9 | 4.0 |
分离的产物 | 0.4 | 98.0 | 1.6 |
反应条件 | 原料 | 产物(3,4-二氨基苯磺酸) | 次要产物(二磺酸) |
8小时/145℃ | 1.9 | 94.3 | 3.8 |
分离的产物 | 1.1 | 98.3 | 0.6 |
反应条件:温度 | 原料 | 产物(3,4-二氨基苯磺酸) |
1小时/80℃ | 96.2 | 2.4 |
2小时/80℃ | 96.1 | 3.3 |
2小时/90℃ | 88.9 | 7.1 |
2小时/100℃ | 83.6 | 12.1 |
2小时/110℃ | 71.6 | 24.8 |
2小时/120℃ | 51.3 | 41.7 |
2小时/130℃ | 15.0 | 84.0 |
2小时/140℃ | 5.5 | 93.3 |
反应条件:时间[小时] | 原料 | 产物(3,4-二氨基苯磺酸) | 次要产物(二磺酸) |
2 | 27.2 | 69.2 | 3.8 |
4 | 14.0 | 81.9 | 4.2 |
5 | 10.5 | 86.7 | 2.8 |
6 | 8.3 | 88.8 | 2.9 |
8 | 6.6 | 90.6 | 2.8 |
10 | 5.3 | 92.2 | 2.6 |
12 | 6.4 | 91.1 | 2.5 |
14 | 5.3 | 92.7 | 2.3 |
16 | 4.9 | 93.9 | 2.3 |
Claims (9)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10243028A DE10243028A1 (de) | 2002-09-17 | 2002-09-17 | Verfahren zur Herstellung isolierter 3,4-Diaminobenzolsulfonsäure |
DE10243028.4 | 2002-09-17 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1486977A CN1486977A (zh) | 2004-04-07 |
CN100506789C true CN100506789C (zh) | 2009-07-01 |
Family
ID=31896075
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB031589995A Expired - Lifetime CN100506789C (zh) | 2002-09-17 | 2003-09-17 | 离析的3,4-二氨基苯磺酸的制备方法 |
Country Status (5)
Country | Link |
---|---|
US (1) | US6787666B2 (zh) |
EP (1) | EP1400507B1 (zh) |
CN (1) | CN100506789C (zh) |
DE (1) | DE10243028A1 (zh) |
ES (1) | ES2398647T3 (zh) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100386312C (zh) * | 2006-07-18 | 2008-05-07 | 上海世景国际贸易有限公司 | 2,4-二氨基苯磺酸及其盐的合成方法 |
EP2457886B1 (en) * | 2010-11-29 | 2014-04-02 | Corning Incorporated | Sulfonation in continuous-flow microreactors |
CN102516137A (zh) * | 2011-12-08 | 2012-06-27 | 江苏远征化工有限公司 | 2,4-二氨基苯磺酸及其盐的生产方法 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2131367C3 (de) * | 1971-06-24 | 1979-10-11 | Hoechst Ag, 6000 Frankfurt | Verfahren zur Herstellung von Benzimidazolonen-(2) |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5748961A (en) * | 1980-09-05 | 1982-03-20 | Sumitomo Chem Co Ltd | Preparation of 2,4-diaminobenzenesulfonic acid |
DE3114829A1 (de) * | 1981-04-11 | 1982-11-04 | Bayer Ag, 5090 Leverkusen | Verfahren zur herstellung von aromatischen aminosulfonsaeuren |
US4808342A (en) * | 1986-04-09 | 1989-02-28 | Ciba-Geigy Corporation | Production of sulfonated amines |
DE3723801A1 (de) * | 1987-07-18 | 1989-01-26 | Bayer Ag | Verfahren zur herstellung von aminoaryl-sulfonsaeuren |
DE4203072C1 (zh) * | 1992-02-04 | 1992-11-12 | Merck Patent Gmbh, 6100 Darmstadt, De | |
DE10030663A1 (de) * | 2000-06-23 | 2002-01-10 | Merck Patent Gmbh | UV-B-Filter |
DE10030664A1 (de) * | 2000-06-23 | 2002-01-10 | Merck Patent Gmbh | Verfahren zur Herstellung von UV-Filter-Substanzen |
-
2002
- 2002-09-17 DE DE10243028A patent/DE10243028A1/de not_active Withdrawn
-
2003
- 2003-09-04 EP EP03019620A patent/EP1400507B1/de not_active Expired - Lifetime
- 2003-09-04 ES ES03019620T patent/ES2398647T3/es not_active Expired - Lifetime
- 2003-09-16 US US10/663,827 patent/US6787666B2/en not_active Expired - Lifetime
- 2003-09-17 CN CNB031589995A patent/CN100506789C/zh not_active Expired - Lifetime
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2131367C3 (de) * | 1971-06-24 | 1979-10-11 | Hoechst Ag, 6000 Frankfurt | Verfahren zur Herstellung von Benzimidazolonen-(2) |
Also Published As
Publication number | Publication date |
---|---|
EP1400507A1 (de) | 2004-03-24 |
CN1486977A (zh) | 2004-04-07 |
EP1400507B1 (de) | 2012-12-26 |
US20040059126A1 (en) | 2004-03-25 |
ES2398647T3 (es) | 2013-03-20 |
US6787666B2 (en) | 2004-09-07 |
DE10243028A1 (de) | 2004-03-25 |
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