CN101607926B - Method for removing sodium sulfate and sodium chloride from lauryl sodium sulfate - Google Patents
Method for removing sodium sulfate and sodium chloride from lauryl sodium sulfate Download PDFInfo
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Abstract
The invention relates to a method for obtaining pharmaceutical-grade lauryl sodium sulfate from industrial-grade lauryl sodium sulfate, which comprises the following steps of: (a) dissolving crude SDS into an ethanol-water solvent with ethanol content within 15-35 percent to prepare solution; (b) cooling the solution to 0-5 DEG C; (c) filtering the solution; and (d) concentrating the obtained solution so as to remove all solvents. The method utilizes the adverse impact on the solubility of SDS, sodium sulfate and sodium chloride due to the existence of ethanol, and can effectively remove sodium sulfate and sodium chloride impurities contained in the SDS and reduce the content of electrolyte impurities compared with the prior art.
Description
Technical field
The present invention relates to the pharmaceutical auxiliary agent production field, relate more specifically to the method for purification of sodium lauryl sulphate.
Background technology
Sodium lauryl sulphate (SDS) is as typical anion surfactant, have the 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 (such 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 large that micelle becomes.
From SDS, remove rather difficulty of sodium sulfate and sodium-chlor.In the water recrystallization method, 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), be difficult to sodium sulfate and sodium-chlor are removed substantially.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 effectively removing sodium sulfate and sodium-chlor from SDS.
Summary of the invention
Therefore the present invention proposes a kind of method of removing sodium sulfate and sodium chloride as impurity from the technical grade sodium lauryl sulphate, to overcome sodium sulfate and the higher problem of sodium chloride content 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 existence of ethanol to the otherwise impact of 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 under study for action, and 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 was between 20-30%, the solubleness of SDS was best.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 by test, in order fully to remove sodium sulfate and sodium-chlor, the ratio of the ethanol in ethanol-water system can not be too high.If ethanol content is higher than 35%, although electrolytical solubleness may further reduce, the solubility property of SDS does not reach predetermined value, and crystalline rate is not ideal.On the contrary, if ethanol content is lower than approximately 16%, then electrolytical solubleness can not be dropped to desirable value because water content is too high.
Find by test, consider ethanol to SDS and the impact 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 an amount of ethanol-water mixed solvent of suitable proportion, then slowly cools to 0-5 ℃, 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, namely some ionogen is separated because 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.
If contriver's discovery with the solution Slow cooling, for example was down to 0-5 ℃ from room temperature in 3-5 hour, then being mixed in electrolytical SDS can be still less.
In order to make the decline that SDS can Yin Wendu and from solution, separate out, should make for SDS solution unsaturated.But must be noted that this and do not mean that degree of unsaturation is more high better, otherwise if strength of solution is excessively rare, ionogen can not fully therefrom be separated out.Therefore, suitable way is, so that the pure SDS in the solution is lower than its saturation capacity slightly after the dissolving.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 than prior art the medicinal sodium lauryl sulphate of low sodium sulfate and sodium chloride content.
The below exemplifies explanation method of the present invention with specific embodiment, and these embodiment should not be construed as the restriction to the inventive method.
Embodiment
35g technical grade SDS is dissolved in the alcohol-water solvent that 70g contains 30% ethanol.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, get 3.2g.This powder of calcination, imponderability reduces.Concentrating under reduced pressure filtrate is until filtrate becomes pulpous state.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 sodium lauryl sulphate may further comprise the steps:
A) thick sodium lauryl sulphate is dissolved in the solvent of the alcohol-water of ethanol content between 15-35wt%, 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 is wherein, at step b) an additional filtration step before.
3. method according to claim 1, wherein, the content of ethanol in described solvent is between 20-30wt%.
4. method according to claim 1 and 2, wherein, step a) in, thick sodium lauryl sulphate is made unsaturated solution, its saturation ratio is 85-95%.
5. method according to claim 1, wherein, at step b) in, solution was down to 0-5 ℃ from room temperature in 3-5 hour.
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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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| CN101607926B true CN101607926B (en) | 2013-02-27 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102183393A (en) * | 2011-03-07 | 2011-09-14 | 中国海洋大学 | Soil extracting and measuring method of anion surfactant |
| CN103111228B (en) * | 2013-01-28 | 2015-09-09 | 深圳市美凯特科技有限公司 | A kind of mixed solvent for finished surface activating agent and purification process thereof |
| 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 |
| CN108546240B (en) * | 2018-04-11 | 2020-12-25 | 上海奥威日化有限公司 | K12 precursor composition for preparing K12 dry product |
| 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 |
| CN114773236B (en) * | 2022-06-16 | 2022-09-09 | 泽升科技(广州)有限公司 | Method for purifying industrial sodium dodecyl sulfate |
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2009
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Non-Patent Citations (5)
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| Dreggr EE,ect.Sodium Alcohol Sulfates Properties Involving Surface Activity.《Industrial and Engineering Chemistry》.1964,第7卷(第6期),610-617. * |
| Huang Zhi,ect.The Effect of Mixed Cationic- Anionic Surfactants on the Cloud Point of Nonionic Surfactant.《Journal of colloid and lnterface Science》.1990,第138卷(第2期),19-23. * |
| 方弈文.十二烷基硫酸钠的纯化.《汕头大学学报》.1996,第11卷(第1期),18-23. * |
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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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