CN103121683A - Easy separation method of benzene sulfonate and carbonate mixture - Google Patents
Easy separation method of benzene sulfonate and carbonate mixture Download PDFInfo
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- CN103121683A CN103121683A CN2012105112343A CN201210511234A CN103121683A CN 103121683 A CN103121683 A CN 103121683A CN 2012105112343 A CN2012105112343 A CN 2012105112343A CN 201210511234 A CN201210511234 A CN 201210511234A CN 103121683 A CN103121683 A CN 103121683A
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- carbonate
- benzene sulfonate
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- acid
- acid root
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Abstract
The invention relates to an easy separation method of a benzene sulfonate and carbonate mixture. The mixture can be separated through the method comprising the following steps of: selectively extracting benzene sulfonate or substituted benzene sulfonate which is contained in the mixture by using a right amount of mixed solvents, and filtering and recovering residual solids, namely carbonate or (and) bicarbonate; acidifying a benzene sulfonate or substituted benzene sulfonate extracting solution by adding inorganic acid; separating out inorganic acid salt, filtering, and separating; and concentrating benzene sulfonic acid or substituted benzene sulfonic acid which is contained in a mother solution to be dry, and recovering.
Description
Technical field
The present invention is the easy separation method of a kind of benzene sulfonate and carbonate mixture, is specifically related to separation and the recovery technology of industrial production mixture.
Background technology
Acid group in benzene sulfonate and substituted benzene sulfonate is a kind of good leavings group, and this class ester more easily carries out nucleophilic substitution reaction than alcohol, replaces alcohol that nucleophilic substitution reaction occurs so often alcohol is converted into the ester of Phenylsulfonic acid or substituted benzenesulfonic acid.In the reaction of this class, some reaction need add in the excess carbon hydrochlorate and the Phenylsulfonic acid or the substituted benzenesulfonic acid that generate, this industrial can produce a large amount of Phenylsulfonic acids or substituted benzenesulfonic acid salt and carbonate or (with) mixture of supercarbonate.Cationic benzene sulfonate of the same race and carbonate, the solubleness in organic solvent is all less, and the solubleness in water is all larger, is difficult to use the single solvent separated and dissolved.In a certain proportion of water and organic solvent composition, the difference in solubility of these two kinds of salt is larger, can utilize difference in solubility to realize separating.
Summary of the invention
The object of the present invention is to provide a kind of benzene sulfonate or substituted benzenesulfonic acid and carbonate or (with) the easy isolation technique of bicarbonate mixture, it can be applicable to separation and the recovery of this salt mixture of industrial realization.
Technical scheme of the present invention is as follows:
The benzene sulfonate that the present invention relates to and the positively charged ion in carbonate can be NH
4 +, Na
+Or K
+The benzene sulfonate negatively charged ion can be Phenylsulfonic acid root, tosic acid root, o-toluene sulfonic acid root, p-chlorobenzenesulfonic acid root, adjacent chlorobenzenesulfonic acid root, to bromo-benzene sulfonic acid root, adjacent bromo-benzene sulfonic acid root, p-nitrophenyl sulfonate radical or o-nitrobenzene sulfonic acid root; Anion, carbonate can be carbonate or (with) bicarbonate radical.
Said mixture can separate like this and reclaim: benzene sulfonate or substituted benzenesulfonic acid salt and carbonate or (with) add the appropriate combination solvent appropriate in bicarbonate mixture, fully stir under proper temperature and extract, filter out insoluble solids be carbonate or (with) supercarbonate; Extracting solution is separated out solid and is inorganic acid salt with suitable mineral acid acidifying, filtration, and mother liquor is concentrated into to do and namely gets Phenylsulfonic acid or substituted benzenesulfonic acid.
The appropriate combination solvent refers to the composition of water and some organic solvent, and organic solvent can select herein: acetone, butanone, tetrahydrofuran (THF), acetonitrile etc.; The content of above-mentioned organic solvent in water can be: 1%-is saturated.
Appropriate solvent refers to that the ratio of solvent and solid mixture is: 1-50.
Proper temperature refers to room temperature to the boiling temperature of solvent, is generally 20-50 ℃.
Mineral acid can select hydrochloric acid, Hydrogen bromide, sulfuric acid, phosphoric acid.
Embodiment
Following specific embodiment is used for further illustrating the present invention.
The typical separate of mixture and recovery embodiment:
Example 1
Get 10g mixture (containing tosic acid potassium 55.5%, salt of wormwood 18.2%, saleratus 26.4%), add 50ml 70% acetone, fully stir, suction filtration, dry salt of wormwood and the saleratus mixture 4.3g of getting, roasting gets salt of wormwood 3.4 g; Filtrate is stirred the lower concentrated hydrochloric acid that drips, and is acidified to the pH=5 left and right, and the solid that filtration is separated out is dried to get Repone K 2.0g; Filtrate is concentrated into dried solid, and solid is dried to get tosic acid 5.0 g.
Example 2
Get 10g mixture (paratoluenesulfonic acid sodium salt and sodium carbonate each 50%), add 60ml 80% acetonitrile, fully stir, suction filtration, dry sodium carbonate 4.8g; Filtrate is stirred the lower vitriol oil that drips, and is acidified to the pH=5 left and right, and the solid that filtration is separated out is dried to get sodium sulfate 1.8g; Filtrate is concentrated into dried solid, and solid is dried to get tosic acid 4.3 g.
Example 3
Get 10g mixture (paratoluenesulfonic acid ammonium salt and volatile salt each 50%), add 40ml 70% tetrahydrofuran (THF), fully stir, suction filtration, dry volatile salt 4.8g; Filtrate is stirred the lower concentrated hydrochloric acid that drips, and is acidified to the pH=5 left and right, and the solid that filtration is separated out is dried to get ammonium chloride 1.4g; Filtrate is concentrated into dried solid, and solid is dried to get tosic acid 4.4 g.
Other mixture is with reference to the aforesaid method Separation and Recovery.
Claims (2)
1. a benzene sulfonate and carbonate mixture, it is composed as follows:
Positively charged ion in benzene sulfonate and carbonate can be NH
4 +, Na
+Or K
+
The benzene sulfonate negatively charged ion can be Phenylsulfonic acid root, tosic acid root, o-toluene sulfonic acid root, p-chlorobenzenesulfonic acid root, adjacent chlorobenzenesulfonic acid root, to bromo-benzene sulfonic acid root, adjacent bromo-benzene sulfonic acid root, p-nitrophenyl sulfonate radical or o-nitrobenzene sulfonic acid root;
Anion, carbonate can be carbonate or (with) bicarbonate radical.
2. said mixture can come Separation and Recovery like this: benzene sulfonate or substituted benzenesulfonic acid salt and carbonate or (with) add the appropriate combination solvent appropriate in bicarbonate mixture, fully stir under proper temperature and extract, filter out insoluble solids be carbonate or (with) supercarbonate; Extracting solution is separated out solid and is inorganic acid salt with suitable mineral acid acidifying, filtration, and mother liquor is concentrated into to do and namely gets Phenylsulfonic acid or substituted benzenesulfonic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210511234.3A CN103121683B (en) | 2012-12-04 | 2012-12-04 | Easy separation method of benzene sulfonate and carbonate mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210511234.3A CN103121683B (en) | 2012-12-04 | 2012-12-04 | Easy separation method of benzene sulfonate and carbonate mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103121683A true CN103121683A (en) | 2013-05-29 |
| CN103121683B CN103121683B (en) | 2014-12-31 |
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| CN201210511234.3A Active CN103121683B (en) | 2012-12-04 | 2012-12-04 | Easy separation method of benzene sulfonate and carbonate mixture |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112874A (en) * | 2013-03-04 | 2013-05-22 | 京博农化科技股份有限公司 | Separating and recovering process for solid wastes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709056A (en) * | 2009-11-13 | 2010-05-19 | 天津理工大学 | 2-[5-(2-oxyphenyl)-1,3,4-thiadiazole-2-thioether]-1-acetophenone compound |
| CN102584765A (en) * | 2012-01-18 | 2012-07-18 | 云南大学 | Synthetic method of liquid phase combination of hydroxyisoflavone compound |
-
2012
- 2012-12-04 CN CN201210511234.3A patent/CN103121683B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709056A (en) * | 2009-11-13 | 2010-05-19 | 天津理工大学 | 2-[5-(2-oxyphenyl)-1,3,4-thiadiazole-2-thioether]-1-acetophenone compound |
| CN102584765A (en) * | 2012-01-18 | 2012-07-18 | 云南大学 | Synthetic method of liquid phase combination of hydroxyisoflavone compound |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112874A (en) * | 2013-03-04 | 2013-05-22 | 京博农化科技股份有限公司 | Separating and recovering process for solid wastes |
| CN103112874B (en) * | 2013-03-04 | 2014-08-27 | 京博农化科技股份有限公司 | Separating and recovering process for solid wastes |
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| Publication number | Publication date |
|---|---|
| CN103121683B (en) | 2014-12-31 |
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