CN108003069A - A kind of preparation method of sulfosuccinic acid - Google Patents
A kind of preparation method of sulfosuccinic acid Download PDFInfo
- Publication number
- CN108003069A CN108003069A CN201711282096.5A CN201711282096A CN108003069A CN 108003069 A CN108003069 A CN 108003069A CN 201711282096 A CN201711282096 A CN 201711282096A CN 108003069 A CN108003069 A CN 108003069A
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- CN
- China
- Prior art keywords
- sulfosuccinic acid
- solution
- sodium
- acid
- sulfosuccinic
- 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.)
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- 0 *S(C(C*1)C(O)=O)(=*=C1O)=O Chemical compound *S(C(C*1)C(O)=O)(=*=C1O)=O 0.000 description 1
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
- C07C303/22—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 from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
-
- 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
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pyrrole Compounds (AREA)
Abstract
The present invention discloses a kind of preparation method of sulfosuccinic acid, it is characterised in that：By maleic anhydride in 70 90 DEG C of preheatings, 1.1 1.7 equivalent solution of sodium bisulfite are slowly added into pre- hot system；Finish, continue to stir 2 10h at 70 90 DEG C；Gained reaction solution is sulfosuccinic acid sodium solution；Into above-mentioned solution plus water is formulated as 5% 30% sulfosuccinic acid sodium solution and prepares sulfosuccinic acid by strong-acid ion exchange resin.The advantage of the invention is that：The sulfosuccinic acid product of sodium ion solubility ＜ 0.05% can be obtained by the above method.The route raw material is simple, synthetic route advantages of simple, reaction conversion ratio are high, cost substantially reduces, and whole synthetic route is environmentally protective, is adapted to industrialized production.
Description
Technical field
The present invention relates to the preparation of compound, especially a kind of preparation method of sulfosuccinic acid.
Background technology
Sulfosuccinic acid is a kind of additive for being used to electroplate, its traditional synthetic method is same using maleic acid or fumaric acid
Sulphite, inclined dithionite react to obtain sulfosuccinic acid sodium salt, are then removed with organic acid displacement method, inorganic acid displacement method
Sulfosuccinic acid is obtained after salt.This method conversion ratio when preparing sulfosuccinic acid sodium salt is not high, is not suitable for industrialization production.System
It is incomplete there are desalination during standby sulfosuccinic acid, the problems such as yield is low, poor product quality.Whole process route cost is higher and grasps
Make relatively complicated, while there are the problems such as poor product quality.Therefore, a high conversion rate is invented, cost is low, quality is high, operation
Simple process route is very important, and the present invention can preferably resolve this problem.
The content of the invention
The purpose of the present invention is solution sulfosuccinic acid preparation process conversion ratio bottom, of high cost, of poor quality and desalinating process
The problems such as complicated.The present invention provides that a kind of easy to operate, quality is high and the synthetic method of lower-cost sulfosuccinic acid, is adapted to
Industrialization production.
The technical scheme is that：A kind of preparation method of sulfosuccinic acid, maleic anhydride is pre- in 70-90 DEG C
Heat, 1.1-1.7 equivalent solution of sodium bisulfite is slowly added into pre- hot system.Finish, continue to stir 2-10h at 70-90 DEG C.
Gained reaction solution is sulfosuccinic acid sodium solution.Into above-mentioned solution plus water is formulated as the sulfosuccinic acid sodium solution of 5%-30%
Sulfosuccinic acid is prepared by strong-acid ion exchange resin.
Reaction equation：
The advantage of the invention is that：The sulfosuccinic acid that sodium ion solubility ＜ 0.05% can be obtained by the above method produces
Product.The route raw material is simple, synthetic route advantages of simple, reaction conversion ratio are high, cost substantially reduces, and whole synthetic route is green
Colour circle is protected, and is adapted to industrialized production.
Embodiment
Embodiment 1：
By maleic anhydride：Sodium hydrogensulfite 1:1.2 (molar ratio) ratios feed intake.
Cis-butenedioic anhydride (98.0g) is added in 1000ml three-necked bottles.Temperature control is slowly added to solution of sodium bisulfite to 80 DEG C
(125.0g sodium hydrogensulfites are dissolved in 450g water).Finish, continue to stir 5h at 80 DEG C.Reaction terminates, and adds into reaction solution
1500ml water is configured to 10% or so sulfosuccinic acid sodium solution, and above-mentioned solution is passed into the ion exchange column of diameter 50mm
In, which is filled with the storng-acid cation exchange resin (model that capacity is 1L：DOW Chemical 650C (H)).When ion is handed over
Start to collect product when changing the pH of the liquid of column lower curtate outflow less than 1, the product being collected into is sulfosuccinic aqueous acid.Pass through
Na ion concentration is detected below 0.05%, product yield 84%.
Embodiment 2：
By maleic anhydride：Sodium hydrogensulfite 1:1.4 (molar ratio) ratios feed intake.
Cis-butenedioic anhydride (98.0g) is added in 1000ml three-necked bottles.Temperature control is slowly added to solution of sodium bisulfite to 80 DEG C
(146.0g sodium hydrogensulfites are dissolved in 500g water).Finish, continue to stir 5h at 80 DEG C.Reaction terminates, and adds into reaction solution
1450ml water is configured to 10% or so sulfosuccinic acid sodium solution, and above-mentioned solution is passed into the ion exchange column of diameter 50mm
In, which is filled with the storng-acid cation exchange resin (model that capacity is 1L：DOW Chemical 650C (H)).When ion is handed over
Start to collect product when changing the pH of the liquid of column lower curtate outflow less than 1, the product being collected into is sulfosuccinic aqueous acid.Pass through
Na ion concentration is detected below 0.05%, product yield 85%.
Embodiment 3：
By maleic anhydride：Sodium hydrogensulfite 1:1.6 (molar ratio) ratios feed intake.
Cis-butenedioic anhydride (98.0g) is added in 1000ml three-necked bottles.Temperature control is slowly added to solution of sodium bisulfite to 80 DEG C
(167.0g sodium hydrogensulfites are dissolved in 600g water).Finish, continue to stir 5h at 80 DEG C.Reaction terminates, and adds into reaction solution
1350ml water is configured to 10% or so sulfosuccinic acid sodium solution, and above-mentioned solution is passed into the ion exchange column of diameter 50mm
In, which is filled with the storng-acid cation exchange resin (model that capacity is 1L：DOW Chemical 650C (H)).When ion is handed over
Start to collect product when changing the pH of the liquid of column lower curtate outflow less than 1, it is sulfosuccinic aqueous acid to be collected into product.Pass through inspection
Na ion concentration is surveyed below 0.05%, product yield 86%.
Claims (1)
- A kind of 1. preparation method of sulfosuccinic acid, it is characterised in that：By maleic anhydride in 70-90 DEG C of preheating, to preheating 1.1-1.7 equivalent solution of sodium bisulfite is slowly added in system；Finish, continue to stir 2-10h at 70-90 DEG C；Gained reacts Liquid is sulfosuccinic acid sodium solution；The sulfosuccinic acid sodium solution for adding water to be formulated as 5%-30% into above-mentioned solution passes through strong acid Property ion exchange resin prepares sulfosuccinic acid；Reaction equation：
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711282096.5A CN108003069A (en) | 2017-12-07 | 2017-12-07 | A kind of preparation method of sulfosuccinic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711282096.5A CN108003069A (en) | 2017-12-07 | 2017-12-07 | A kind of preparation method of sulfosuccinic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108003069A true CN108003069A (en) | 2018-05-08 |
Family
ID=62057198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711282096.5A Withdrawn CN108003069A (en) | 2017-12-07 | 2017-12-07 | A kind of preparation method of sulfosuccinic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108003069A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5698626A (en) * | 1996-12-18 | 1997-12-16 | Witco Corporation | Functional group terminated polymers containing sulfonate group via polymerization of sulfonated monomers |
| JP2010064987A (en) * | 2008-09-11 | 2010-03-25 | Adeka Corp | Method for producing sulfosuccinic acid or its salt |
| CN104140388A (en) * | 2013-05-08 | 2014-11-12 | 天津希恩思生化科技有限公司 | Compound N-hydroxyl sulfo succinimide sodium and preparation method thereof |
-
2017
- 2017-12-07 CN CN201711282096.5A patent/CN108003069A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5698626A (en) * | 1996-12-18 | 1997-12-16 | Witco Corporation | Functional group terminated polymers containing sulfonate group via polymerization of sulfonated monomers |
| JP2010064987A (en) * | 2008-09-11 | 2010-03-25 | Adeka Corp | Method for producing sulfosuccinic acid or its salt |
| CN104140388A (en) * | 2013-05-08 | 2014-11-12 | 天津希恩思生化科技有限公司 | Compound N-hydroxyl sulfo succinimide sodium and preparation method thereof |
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| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180508 |