CN106977428B - Improve the method for preparing lauryl sodium sulfate - Google Patents
Improve the method for preparing lauryl sodium sulfate Download PDFInfo
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- CN106977428B CN106977428B CN201710159294.6A CN201710159294A CN106977428B CN 106977428 B CN106977428 B CN 106977428B CN 201710159294 A CN201710159294 A CN 201710159294A CN 106977428 B CN106977428 B CN 106977428B
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- China
- Prior art keywords
- sodium sulfate
- lauryl sodium
- sulfamic acid
- acidic ion
- ion liquid
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- 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
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The present invention relates to a kind of preparation methods of nontoxic, widely used fatty alcohol sulfate salt form anion surfactant.The present invention directly uses sulfamic acid and laruyl alcohol for raw material, and preparation lauryl sodium sulfate is stirred to react under the catalysis of acidic ion liquid and urea.That the present invention provides a kind of reaction conditions is mild, product surface it is active it is high, inorganic salt content is low, simple and safe operation, the method for the high synthesis lauryl sodium sulfate of yield.
Description
Technical field
The present invention relates to a kind of nontoxic, widely used fatty alcohol sulfate salt form anionic surfaces in organic chemistry filed
The preparation method of activating agent more particularly to a kind of lauryl sodium sulfate novel preparation method.
Background technology
Lauryl sodium sulfate is nontoxic as one kind, uses extensive fatty alcohol sulfate salt form anion surface active
Agent, detergency are better than sodium alkyl sulfonate and sodium alkyl benzene sulfonate, are the main actives in washing powder.Dodecyl sulphate
Sodium usually by generating lauryl alcohol sulfuric ester after laruyl alcohol and chlorosulfonic acid effect, is made by alkali neutralization.However chlorosulfonic acid is liquid
Body is easy smoke in air, has acrid odors, special means of transport is needed in transport, and its steam is easy to viscous
Film and respiratory tract generate stimulation and cause damages, and have very strong corrosivity, strong and stimulating, and meet water decomposition and release a large amount of
Heat, the HCl severe corrosion to equipment of generation, big inconvenience and danger are caused to operating process.Sulfamic acid is colourless, tasteless
Nontoxic solid powdery again, it is non-volatile, it is minimum to human toxicity, replace chlorosulfonic acid that can reduce operation using sulfamic acid
The damage to equipment of danger and reaction process, effectively improve safety.
It is raw material the present invention provides a kind of sulfamic acid, acidic ion liquid and urea are catalyst, synthesize dodecane
The method of base sodium sulphate.The present invention is mild with reaction condition, the active high inorganic salt content of product surface is low, safe operation letter
Just, the advantages that yield is high.
Invention content
It is raw material the object of the present invention is to provide a kind of sulfamic acid, acidic ion liquid and urea are catalyst, reaction
The method of the preparation lauryl sodium sulfate of mild condition.
Technical solution of the present invention is as follows：
The present invention directly uses sulfamic acid and laruyl alcohol under the catalysis of acidic ion liquid and urea, is stirred to react system
Standby lauryl sodium sulfate.The reaction equation of the present invention is as follows：
The method that the present invention prepares lauryl sodium sulfate, steps are as follows：
1) laruyl alcohol and sulfamic acid are added into reaction bulb, while the acidic ion liquid of catalytic amount is added and urea is
Catalyst；Wherein laruyl alcohol and sulfamic acid molar ratio are 1: 0.56~1.22, sulfamic acid and acidic ion liquid molar ratio
It is 1: 0.08~0.2,80~100 DEG C to be stirred to react 2~4 hours.
2) it dries after completion of the reaction, white lauryl sodium sulfate is obtained after absolute ethyl alcohol washing, chloroform.
The preferred laruyl alcohol of the step 1) and sulfamic acid molar ratio are 1: 0.56；
The preferred reaction condition of the step 1) is to be stirred to react 4 hours at 100 DEG C.
Preferably, the step 1) catalyst is acidic ion liquid 1- butyl-pyridinium disulfates, and mole percent is
8.38mol%.
That the present invention provides a kind of reaction conditions is mild, product surface it is active it is high, inorganic salt content is low, safe operation letter
Just, the method for the high preparation lauryl sodium sulfate of yield.
Specific implementation mode
The preparation of embodiment 1, lauryl sodium sulfate, structural formula are as follows：
Raw material laruyl alcohol 6.64g and sulfamic acid 1.94g is added in 100ml round-bottomed flasks, makes original under agitation
Material dissolving, is added 1- butyl-pyridiniums disulfate ([BPy] HSO later4) (structural formula is：) acidic ion liquid
0.3884g and urea 0.48g is stirred to react 4h as catalyst at 90 DEG C.It uses at 30%NaOH solution after completion of the reaction
Reason is washed, after chloroform with absolute ethyl alcohol after dry to neutrality, obtains white powder lauryl sodium sulfate sterling 3.69g,
It is 64.0% to detach yield, and fusing point is 183-185 DEG C.
The identification of lauryl sodium sulfate：
Infrared spectrogram IR (KBr) v/cm-1：2957,2919,2851,1249,1205,830.
Product is identified consistent with document report.
Embodiment 2
Raw material laruyl alcohol 6.64g and sulfamic acid 1.94g is added in 100ml round-bottomed flasks, makes original under agitation
Material dissolving, is added 1- butyl-pyridiniums disulfate ([BPy] HSO later4) (structural formula is：) acidic ion liquid
0.3884g and urea 0.48g is stirred to react 2h as catalyst at 95 DEG C.It uses at 30%NaOH solution after completion of the reaction
Reason is washed, after chloroform with absolute ethyl alcohol after dry to neutrality, obtains white powder lauryl sodium sulfate sterling 4.56g,
It is 79.1% to detach yield, and fusing point is 183-185 DEG C.
Product is identified consistent with document report.
Embodiment 3
Raw material laruyl alcohol 6.64g and sulfamic acid 1.94g is added in 100ml round-bottomed flasks, makes original under agitation
Material dissolving, is added 1- butyl-pyridiniums disulfate ([BPy] HSO later4) (structural formula is：) acidic ion liquid
0.3884g and urea 0.48g is stirred to react 4h as catalyst at 100 DEG C.It uses at 30%NaOH solution after completion of the reaction
Reason is washed, after chloroform with absolute ethyl alcohol after dry to neutrality, obtains white powder lauryl sodium sulfate sterling 5.30g,
It is 91.9% to detach yield, and fusing point is 183-185 DEG C.
Product is identified consistent with document report.
According to the disclosure of the present invention, those skilled in the art can apply the present invention to greatest extent.Therefore,
Above-mentioned preferred embodiment is merely illustrative of, rather than is limited the scope of the invention in any way.
Claims (1)
1. the preparation method of lauryl sodium sulfate, it is characterised in that using sulfamic acid as raw material, acidic ion liquid and urea
For catalyst, lauryl sodium sulfate is directly prepared, is as follows：
Laruyl alcohol and sulfamic acid are added in round-bottomed flask, makes dissolution of raw material, laruyl alcohol and sulfamic acid under agitation
Molar ratio is 1: 0.56~1.22, and acidic ion liquid 1- butyl-pyridiniums disulfate and the urea conduct of catalytic amount are added later
Catalyst, it is 1: 0.08~0.2 to make the molar ratio of sulfamic acid and acidic ion liquid, it is stirred to react 2 at 90~100 DEG C~
4h；30%NaOH solution treatments are used to be washed, after chloroform, obtained white with absolute ethyl alcohol after dry to neutrality after completion of the reaction
Color powder lauryl sodium sulfate sterling, structural formula are
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710159294.6A CN106977428B (en) | 2017-03-17 | 2017-03-17 | Improve the method for preparing lauryl sodium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710159294.6A CN106977428B (en) | 2017-03-17 | 2017-03-17 | Improve the method for preparing lauryl sodium sulfate |
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| CN106977428A CN106977428A (en) | 2017-07-25 |
| CN106977428B true CN106977428B (en) | 2018-08-21 |
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| CN201710159294.6A Expired - Fee Related CN106977428B (en) | 2017-03-17 | 2017-03-17 | Improve the method for preparing lauryl sodium sulfate |
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| CN112675061A (en) * | 2021-01-29 | 2021-04-20 | 广东丽臣奥威实业有限公司 | Production method of composition of sodium lauryl sulfate and fluorine-containing sodium lauryl sulfate |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS56133256A (en) * | 1980-03-24 | 1981-10-19 | Nippon Shokubai Kagaku Kogyo Co Ltd | Production of high-purity higher secondary alcohol ethoxy sulfate |
| JP2000169520A (en) * | 1998-10-01 | 2000-06-20 | Dai Ichi Kogyo Seiyaku Co Ltd | Novel decomposable reactive emulsifier and method for modifying polymer therewith |
| JP2000319305A (en) * | 1999-05-12 | 2000-11-21 | Dai Ichi Kogyo Seiyaku Co Ltd | New decomposable reactive emulsifier, and modification of polymer using the same |
| US6479546B1 (en) * | 2000-07-26 | 2002-11-12 | The Regents Of The University Of California | Allosteric inhibitors of lipoxygenase |
| CN101235001A (en) * | 2007-12-21 | 2008-08-06 | 王伟松 | Synthetic method of fatty alcohol sulfate |
| WO2014086908A1 (en) * | 2012-12-07 | 2014-06-12 | Shell Internationale Research Maatschappij B.V. | Process for preparing alkoxylated alcohols |
| CN103058894A (en) * | 2013-01-07 | 2013-04-24 | 东明俱进化工有限公司 | Production method of high-purity sodium dodecyl sulfate |
| CN104892467A (en) * | 2015-06-16 | 2015-09-09 | 眉山华瑞科技开发有限责任公司 | Synthetic method for alcohol ether sulfate salt foaming agent |
| CN105732442B (en) * | 2016-01-27 | 2017-11-03 | 江苏苏博特新材料股份有限公司 | Oligomeric-type surfactant, its preparation method and application |
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Granted publication date: 20180821 Termination date: 20190317 |