CN101607926A - Remove the method for sodium sulfate and sodium-chlor from sodium lauryl sulphate - Google Patents
Remove the method for sodium sulfate and sodium-chlor from sodium lauryl sulphate Download PDFInfo
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- CN101607926A CN101607926A CNA2009101620208A CN200910162020A CN101607926A CN 101607926 A CN101607926 A CN 101607926A CN A2009101620208 A CNA2009101620208 A CN A2009101620208A CN 200910162020 A CN200910162020 A CN 200910162020A CN 101607926 A CN101607926 A CN 101607926A
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Abstract
The present invention relates to a kind of method, may further comprise the steps: a) thick SDS is dissolved in the solvent of the alcohol-water of ethanol content between 15-35%, makes solution from technical grade sodium lauryl sulphate acquisition pharmaceutical grade sodium lauryl sulphate; B) described solution is cooled to 0-5 ℃; C) filter described solution; D) filtrate of concentrated gained is to remove all solvents.The present invention utilizes the otherwise impact of alcoholic acid existence to SDS and sodium sulfate and sodium-chlor solubleness, can effectively remove sodium sulfate contained among the SDS and sodium chloride as impurity, has compared with prior art reduced the content of ionogen impurity.
Description
Technical field
The present invention relates to the pharmaceutical auxiliary agent production field, relate more specifically to the PURIFICATION OF SODIUM LAURYL SULFATE method.
Background technology
Sodium lauryl sulphate (SDS) is as typical anion surfactant, have effects such as emulsification, decontamination, dispersion, wetting and foaming, in the medicament manufacturing, be widely used as emulsifying agent, stain remover, dispersion agent, wetting agent, pore forming material, be used for film-making agent, granule, capsule, ointment, drug shampoo, skin cleaner etc.Impurities is generally the homologue of dodecyl sulfate, responseless pure and mild ionogen (as sodium sulfate, sodium-chlor).Sulfuric acid content among the pharmaceutical grade SDS reaches 8% at present, and sodium chloride content reaches 4%.These electrolytical existence then can make the micelle-forming concentration c.m.c of SDS greatly reduce, and are the aggregation number increases of micelle, and it is big that micelle becomes.
From SDS, remove rather difficulty of sodium sulfate and sodium-chlor.In the water recrystallization method,, be difficult to sodium sulfate and sodium-chlor are removed substantially because SDS, sodium sulfate and the solubleness of sodium-chlor in water are more or less the same (under 20 ℃, SDS is about 10, and sodium sulfate is 19.5, and sodium-chlor is 22).In the ether crystallization process, because three's solubleness is all very little, the efficient of purification is not high yet.
Therefore, this area needs a kind of method of removing sodium sulfate and sodium-chlor effectively from SDS.
Summary of the invention
Therefore the present invention proposes a kind of method from technical grade sodium lauryl sulphate removal sodium sulfate and sodium chloride as impurity, to overcome sodium sulfate and sodium chloride content problem of higher among the existing pharmaceutical grade SDS.
Method of the present invention may further comprise the steps: a) thick SDS is dissolved in the solvent of the alcohol-water of ethanol content between 15-35%, makes solution; B) described solution is cooled to 0-5 ℃; C) filter described solution; D) filtrate of concentrated gained is to remove all solvents.
The present invention utilizes the otherwise impact of alcoholic acid existence to SDS and sodium sulfate and sodium-chlor solubleness, can effectively remove sodium sulfate contained among the SDS and sodium chloride as impurity, has compared with prior art reduced the content of ionogen impurity.
Embodiment
The contriver finds that under study for action the solubleness of SDS in a certain proportion of ethanol-water mixed solvent is greater than the solubleness in water.If Xiang Shuizhong introduces ethanol, then the solubleness of sodium sulfate and sodium-chlor then reduces greatly.And under 0-5 ℃ temperature, the solubleness of these two kinds of salt in this mixed solvent then more reduces.Table 1 shows SDS solubility property in alcohol-water under 25 ℃.
The solvability of table 1.SDS in SDS (1)-ethanol (2)-water (3) system
As can be seen from Table 1, under 25 ℃, when ethanol content was between 4-40wt% in the ethanol-water mixture, the solubleness of SDS was greater than the solubleness in water; When ethanol content was between 14-35%, solubleness significantly increased; When ethanol content is between 20-30%, solubleness the best of SDS.In contrast, when ethanol content was between 15-35%, the solubleness of sodium sulfate and sodium-chlor then reduced greatly.
The present invention just is being based on above-mentioned discovery and is proposing a kind of method of isolating sodium sulfate and sodium-chlor from SDS.
Find that by test in order fully to remove sodium sulfate and sodium-chlor, the alcoholic acid ratio in ethanol-water system can not be too high.If ethanol content is higher than 35%, though electrolytical solubleness may further reduce, the solubility property of SDS does not reach predetermined value, and crystalline rate is not ideal.On the contrary, about 16% if ethanol content is lower than, then electrolytical solubleness can not be dropped to the ideal value because water content is too high.
Find that by test take all factors into consideration ethanol to SDS and the influence of electrolytical solvability, the weight ratio of ethanol and water suits between 15-35%, preferably between 20-30%.
In the method for the invention, the SDS crude product at room temperature is dissolved in the adequate amount of ethanol-water mixed solvent of suitable proportion, slowly cools to 0-5 ℃ then, and crystallization goes out the ionogen of indissoluble under this temperature.
Generally speaking, need not by crystallisation by cooling, when crude product is dissolved in the solvent, promptly some ionogen is separated because of being insoluble to solvent.Can remove this part ionogen (sodium sulfate and sodium-chlor) by at room temperature filtering.
As preferably, solution can be cooled to 0-5 ℃, so that electrolytical solubleness further reduces, thereby can from solution, separate out.
The contriver finds that if solution is slowly cooled off, for example reduced to 0-5 ℃ from room temperature in 3-5 hour, then being mixed in electrolytical SDS can be still less.
For SDS can not separated out from solution because of decrease of temperature, should make for SDS solution unsaturated.But must be noted that this and do not mean that degree of unsaturation is high more good more, otherwise if strength of solution is rare excessively, ionogen can not fully therefrom be separated out.Therefore, suitable way is to make that the pure SDS in the solution of dissolving back is lower than its saturation capacity slightly.The add-on of general SDS is not less than 80% of its saturation capacity, is preferably 85-95%, and for example about 87%, 90% and 93%.
Use method of the present invention can obtain to have the medicinal sodium lauryl sulphate of low sodium sulfate and sodium chloride content than prior art.
Exemplify explanation method of the present invention with specific embodiment below, these embodiment should not be construed as the restriction to the inventive method.
Embodiment
35g technical grade SDS is dissolved in 70g to be contained in the 30% alcoholic acid alcohol-water solvent.Stir 30min, filter to remove insolubles.3 hours times solution is dropped to 0-1 ℃, and keep 30min.Filtration obtains powder.Powder and above-mentioned insolubles are merged, weigh after the drying, 3.2g.This powder of calcination, imponderability reduces.Concentrating under reduced pressure filtrate becomes pulpous state up to filtrate.Drying dewaters in 80 ℃ vacuum drying oven at last, obtains finished product 30.7g.Detecting its sodium sulphate content is 2.1%, and sodium chloride content is 1.1%.
Below with reference to exemplary embodiments embodiments of the present invention are described, but these embodiments only are for exemplary purposes rather than limit the present invention.It should be understood that those skilled in the art can be under the prerequisite that does not deviate from scope and spirit of the present invention, change and revise for embodiment.Similarly, except above-mentioned embodiment, can also find many embodiments in the appended claims.
Claims (5)
1. method of removing sodium sulfate and sodium-chlor from SDS may further comprise the steps:
A) thick SDS is dissolved in the solvent of the alcohol-water of ethanol content between 15-35%, makes solution;
B) described solution is cooled to 0-5 ℃;
C) filter described solution;
D) filtrate of concentrated gained is to remove all solvents.
2. method according to claim 1, wherein, an additional filtration step before step b).
3. method according to claim 1, wherein, the content of ethanol in described solvent is between 20-30%.
4. method according to claim 1 and 2, wherein, in step a), thick SDS makes unsaturated solution, and its saturation ratio is 85-95%.
5. method according to claim 1 wherein, in step b), was reduced to 0-5 ℃ from room temperature with solution in 3-5 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200910162020 CN101607926B (en) | 2009-08-07 | 2009-08-07 | Method for removing sodium sulfate and sodium chloride from lauryl sodium sulfate |
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| CN 200910162020 CN101607926B (en) | 2009-08-07 | 2009-08-07 | Method for removing sodium sulfate and sodium chloride from lauryl sodium sulfate |
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| CN101607926A true CN101607926A (en) | 2009-12-23 |
| CN101607926B CN101607926B (en) | 2013-02-27 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183393A (en) * | 2011-03-07 | 2011-09-14 | 中国海洋大学 | Soil extracting and measuring method of anion surfactant |
| CN103111228A (en) * | 2013-01-28 | 2013-05-22 | 深圳市美凯特科技有限公司 | Mixed solvent for refining surface active agent and purification method thereof |
| CN107501137A (en) * | 2017-08-29 | 2017-12-22 | 东明俱进化工有限公司 | The purifying technique and its equipment of a kind of lithium dodecyl sulfate |
| CN108546240A (en) * | 2018-04-11 | 2018-09-18 | 上海奥威日化有限公司 | It is used to prepare the K12 precursor compositions of K12 dried objects |
| CN114044526A (en) * | 2021-12-10 | 2022-02-15 | 郑州中科新兴产业技术研究院 | Separation method of mixed salt containing sodium sulfate and sodium chloride |
| CN114773236A (en) * | 2022-06-16 | 2022-07-22 | 泽升科技(广州)有限公司 | Method for purifying industrial sodium dodecyl sulfate |
-
2009
- 2009-08-07 CN CN 200910162020 patent/CN101607926B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183393A (en) * | 2011-03-07 | 2011-09-14 | 中国海洋大学 | Soil extracting and measuring method of anion surfactant |
| CN103111228A (en) * | 2013-01-28 | 2013-05-22 | 深圳市美凯特科技有限公司 | Mixed solvent for refining surface active agent and purification method thereof |
| WO2014114031A1 (en) * | 2013-01-28 | 2014-07-31 | 深圳市美凯特科技有限公司 | Mixed solvent for refining surfactants and surfactant purification method |
| CN107501137A (en) * | 2017-08-29 | 2017-12-22 | 东明俱进化工有限公司 | The purifying technique and its equipment of a kind of lithium dodecyl sulfate |
| CN107501137B (en) * | 2017-08-29 | 2023-09-05 | 东明俱进化工有限公司 | Purification process and equipment for lithium dodecyl sulfate |
| CN108546240A (en) * | 2018-04-11 | 2018-09-18 | 上海奥威日化有限公司 | It is used to prepare the K12 precursor compositions of K12 dried objects |
| CN114044526A (en) * | 2021-12-10 | 2022-02-15 | 郑州中科新兴产业技术研究院 | Separation method of mixed salt containing sodium sulfate and sodium chloride |
| CN114773236A (en) * | 2022-06-16 | 2022-07-22 | 泽升科技(广州)有限公司 | Method for purifying industrial sodium dodecyl sulfate |
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| CN101607926B (en) | 2013-02-27 |
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Application publication date: 20091223 Assignee: Hunan Xiangyikang Pharmaceutical Co., Ltd. Assignor: Hunan Er-Kang Pharmaceutical Co., Ltd. Contract record no.: 2014430000029 Denomination of invention: Method for removing sodium sulfate and sodium chloride from lauryl sodium sulfate Granted publication date: 20130227 License type: Exclusive License Record date: 20140411 |
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