CN1623981A - Process for purifying 2,5 diamino phenyl-1,3-disulfonic acid - Google Patents
Process for purifying 2,5 diamino phenyl-1,3-disulfonic acid Download PDFInfo
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- CN1623981A CN1623981A CN 200310109031 CN200310109031A CN1623981A CN 1623981 A CN1623981 A CN 1623981A CN 200310109031 CN200310109031 CN 200310109031 CN 200310109031 A CN200310109031 A CN 200310109031A CN 1623981 A CN1623981 A CN 1623981A
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- diamino
- phenyl
- acid
- disulfonic acid
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Abstract
A process for purifying 2,5-diaminophenyl-1,3-disulfonic acid includes such steps as mixing it with water, alcohol solvent and inorganic acid, adding activated carbon, heating, reflux for decoloring, filtering for removing activated carbon, vacuum distilling crystallizing, filtering and drying. Its advantage is high purity (99% or more).
Description
Technical field
The present invention relates to a kind of 2,5-diamino-phenyl-1, the purification process of 3-disulfonic acid.
Background technology
2,5-diamino-phenyl-1,3-disulfonic acid are a kind of important organic intermediates, especially can be used as new dye synthetic intermediate, have wide practical use.
In the prior art, 2,5-diamino-phenyl-1, the synthetic route of 3-disulfonic acid is raw material usually with the Ursol D, and heating condition down carries out sulfonation reaction with oleum, synthesize obtain 2,5-diamino-phenyl-1,3-disulfonic acid crude product is the semisolid of taupe, is difficult to direct use, and purification effect is undesirable.
JP 04-193,858 (1992) disclose a kind of purification process: 2,5-diamino-phenyl-1,3-disulfonic acid dissolving crude product is in water-sodium hydroxide solution, stir adding Glacial acetic acid down, separate out crystallization, through separating, drying obtains 2 of purifying, 5-diamino-phenyl-1,3-disulfonic acid.Though the content of this method organic impurity can reduce, introduced a large amount of inorganic salt sodium-acetates, the content by the ignition test inorganic salt has reduced the purity of purified product up to about 20%, and industrial value is very low.
Summary of the invention
It is a kind of 2 that the technical problem that the present invention solves provides, 5-diamino-phenyl-1, and the purification process of 3-disulfonic acid, lower to overcome in the prior art purified product purity, purifying can be introduced other impurity simultaneously and cause the low-down deficiency of industrial value.
Technical scheme of the present invention:
Purification process of the present invention may further comprise the steps: with 2,5-diamino-phenyl-1,3-disulfonic acid crude product and water, alcoholic solvent, mineral acid mixed dissolution add gac again, the reflux decolouring, filtered while hot is removed gac, filtrate decompression distillation removed desolvates, the crystallization of separating out after filtration, drying, obtain purified product 2,5-diamino-phenyl-1, the 3-disulfonic acid.
Used in the present invention 2,5-diamino-phenyl-1, the purity of 3-disulfonic acid crude product is 50-98% (weight), can be by JP 04-193,858 (1992), prepare by sulfonation by Ursol D and oleum, the present invention repeats no more.
Alcoholic solvent used in the present invention is C
1-C
4Unit alcohol, one or more in particular methanol, ethanol, propyl alcohol, Virahol, the butanols.
Mineral acid used in the present invention is one or more in sulfuric acid, hydrochloric acid, the nitric acid, preferred hydrochloric acid.
The present invention is with 2,5-diamino-phenyl-1, and 3-disulfonic acid crude product and water, alcoholic solvent, mineral acid carry out mixed dissolution, and its ratio of components is 1.0: 3.0-10.0: 0.5-2.0: 0.5-2.0 (mass ratio).
The present invention carries out reflux decolour with gac, and return time was controlled at 20-40 minute, and the add-on of gac is 2,5-diamino-phenyl-1, and 3-disulfonic acid crude product: gac=1.0: 0.01-0.1 (mass ratio), the fineness of gac is the 200-400 order.
Purification process equipment of the present invention is simple, the operating process controllability is strong, and stable in properties is fit to large-scale industrial production; The product purity that obtains with purification process of the present invention reaches more than 99%, productive rate 80-95%.
Embodiment
The invention will be further described below by embodiment, but embodiment does not limit protection scope of the present invention.
Embodiment 1
Having heating, thermometer, mechanical stirring, in the reaction unit of reflux exchanger, add 2 respectively, 5-diamino-phenyl-1,3-disulfonic acid crude product (purity 65%) 100g, water 500g, methyl alcohol 100g, hydrochloric acid 100g, stirring at room was mixed 15 minutes, add gac 5g (300 order), be heated to backflow in the time of stirring, kept 30 minutes, filtered while hot is removed gac, filtrate decompression distillation is separated out whitely 2,5-diamino-phenyl-1,3-disulfonic acid crystallization 52.0g, purity 99.3% (HPLC), ignition residue 0.01%, yield 80.0%.
Embodiment 2
Having heating, thermometer, mechanical stirring, in the reaction unit of reflux exchanger, add 2 respectively, 5-diamino-phenyl-1,3-disulfonic acid crude product (purity 80%) 1000g, water 5000g, ethanol 600g, hydrochloric acid 600g, stirring at room is mixed, add gac 80g (300 order), be heated to backflow, kept 40 minutes, filtered while hot is removed gac, filtrate decompression distillation is separated out whitely 2,5-diamino-phenyl-1,3-disulfonic acid crystallization 680g, purity 99.5% (HPLC), ignition residue 0.01%, yield 85.0%
Embodiment 3
Having heating, thermometer, mechanical stirring, in the reaction unit of reflux exchanger, add 2 respectively, 5-diamino-phenyl-1,3-disulfonic acid crude product (purity 95%) 1000g, water 6000g, ethanol 500g, hydrochloric acid 500g, stirring at room is mixed, add gac 100g (400 order), be heated to backflow, kept 40 minutes, filtered while hot is removed gac, filtrate decompression distillation is separated out whitely 2,5-diamino-phenyl-1,3-disulfonic acid crystallization 874g, purity 99.3% (HPLC), ignition residue 0.01%, yield 92.0%.
Claims (9)
1. one kind 2,5-diamino-phenyl-1, the purification process of 3-disulfonic acid is characterized in that comprising the steps:
2,5-diamino-phenyl-1,3-disulfonic acid crude product mixes with water, alcoholic solvent, mineral acid, adds gac, reflux decolouring removes by filter gac, the filtrate decompression distillation is removed desolvates, the crystallization of separating out after filtration, drying, obtain 2 of purifying, 5-diamino-phenyl-1,3-disulfonic acid.
2. method according to claim 1, it is characterized in that said 2,5-diamino-phenyl-1, the purity of 3-disulfonic acid crude product is 50-98% (weight).
3. method according to claim 1 is characterized in that said alcoholic solvent is C
1-C
4Unit alcohol.
4. method according to claim 3 is characterized in that said alcoholic solvent is one or more in methyl alcohol, ethanol, propyl alcohol, Virahol, the butanols.
5. method according to claim 1 is characterized in that said mineral acid is one or more in sulfuric acid, hydrochloric acid, the nitric acid.
6. method according to claim 5 is characterized in that said mineral acid is a hydrochloric acid.
7. method according to claim 1 is characterized in that said gac fineness is the 200-400 order.
8. method according to claim 1 is characterized in that the said reflux decolour time is 20-40 minute.
9. according to each described method of claim 1-8, it is characterized in that said ratio of components is 2,5-diamino-phenyl-1,3-disulfonic acid crude product: water: alcoholic solvent: mineral acid: gac=1.0: 3.0-10.0: 0.5-2.0: 0.5-2.0: 0.01-0.1 (mass ratio).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101090312A CN1308296C (en) | 2003-12-03 | 2003-12-03 | Process for purifying 2,5 diamino phenyl-1,3-disulfonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101090312A CN1308296C (en) | 2003-12-03 | 2003-12-03 | Process for purifying 2,5 diamino phenyl-1,3-disulfonic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1623981A true CN1623981A (en) | 2005-06-08 |
| CN1308296C CN1308296C (en) | 2007-04-04 |
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ID=34758816
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003101090312A Expired - Fee Related CN1308296C (en) | 2003-12-03 | 2003-12-03 | Process for purifying 2,5 diamino phenyl-1,3-disulfonic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104487417A (en) * | 2012-09-28 | 2015-04-01 | 湖南阿斯达生化科技有限公司 | Method for preparing methanedisulfonic acid |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0623167B2 (en) * | 1990-11-27 | 1994-03-30 | 株式会社デハラファイン研究所 | Method for producing 1,4-diaminobenzene-2,6-disulphonic acid and purification method thereof |
| JPH068273B2 (en) * | 1990-11-27 | 1994-02-02 | 株式会社デハラファイン研究所 | Production method and purification method of 1,4-diaminobenzenesulfonic acid |
| CN1066446A (en) * | 1991-05-08 | 1992-11-25 | 陈文友 | The synthetic method of ORTHO AMINO PHENOL SULPHONIC |
-
2003
- 2003-12-03 CN CNB2003101090312A patent/CN1308296C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104487417A (en) * | 2012-09-28 | 2015-04-01 | 湖南阿斯达生化科技有限公司 | Method for preparing methanedisulfonic acid |
| CN104487417B (en) * | 2012-09-28 | 2018-06-01 | 湖南阿斯达生化科技有限公司 | A kind of preparation method of methylene-disulfonic acid |
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| Publication number | Publication date |
|---|---|
| CN1308296C (en) | 2007-04-04 |
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Granted publication date: 20070404 Termination date: 20101203 |