CN106977428A - Improve the method for preparing lauryl sodium sulfate - Google Patents
Improve the method for preparing lauryl sodium sulfate Download PDFInfo
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- CN106977428A CN106977428A CN201710159294.6A CN201710159294A CN106977428A CN 106977428 A CN106977428 A CN 106977428A CN 201710159294 A CN201710159294 A CN 201710159294A CN 106977428 A CN106977428 A CN 106977428A
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- sodium sulfate
- lauryl sodium
- sulfamic acid
- preparation
- acidic ion
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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 nontoxic, widely used fatty alcohol sulfate salt form anion surfactant preparation method.The present invention directly uses sulfamic acid and laruyl alcohol for raw material, and stirring reaction prepares lauryl sodium sulfate under the catalysis of acidic ion liquid and urea.The invention provides a kind of reaction condition is gentle, the active high, inorganic salt content of product surface 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 surface 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 as one kind it is nontoxic, use extensive fatty alcohol sulfate salt form anion surface active
Agent, its detergency is better than sodium alkyl sulfonate and sodium alkyl benzene sulfonate, is the main active in washing powder.Dodecyl sulphate
Sodium generally generates lauryl alcohol sulfuric ester after laruyl alcohol and chlorosulfonic acid effect, neutralizes and is made by alkali.But chlorosulfonic acid is liquid
Body, in atmosphere easy smoke, with acrid odors, needs special means of transport in transport, and its steam is easily to viscous
Film and respiratory tract produce stimulation and caused harm, and with very strong corrosivity, strong and stimulating, and meet water decomposition and release substantial amounts of
Heat, the HCl of generation is serious to equipment corrosion, and very big inconvenient and danger is caused to operating process.Sulfamic acid is colourless, tasteless
Nontoxic solid powdery, non-volatile again, minimum to human toxicity, replaces chlorosulfonic acid just to reduce operation using sulfamic acid
The infringement to equipment of danger and course of reaction, effectively improve security.
It is raw material the 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 has that reaction condition is gentle, the active high inorganic salt content of product surface is low, safe operation letter
Just, the advantages of yield is high.
The content of the invention
It is raw material it is an object of the invention 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, stirring reaction 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, step is as follows：
1) laruyl alcohol and sulfamic acid are added into reaction bulb, while the acidic ion liquid and urea that add catalytic amount are
Catalyst；Wherein laruyl alcohol and sulfamic acid mol ratio are 1: 0.56~1.22, sulfamic acid and acidic ion liquid mol ratio
For 1: 0.08~0.2,80~100 DEG C of stirring reactions 2~4 hours.
2) dry after completion of the reaction, white lauryl sodium sulfate is obtained after absolute ethyl alcohol washing, chloroform.
The step 1) preferred laruyl alcohol and sulfamic acid mol ratio be 1: 0.56；
The step 1) preferred reaction condition is stirring reaction 4 hours at 100 DEG C.
It is preferred that, the step 1) catalyst is acidic ion liquid 1- butyl-pyridinium disulfates, mole percent is
8.38mol%.
The invention provides a kind of reaction condition is gentle, the active high, inorganic salt content of product surface is low, safe operation letter
Just, the method for the high preparation lauryl sodium sulfate of yield.
Embodiment
The preparation of embodiment 1, lauryl sodium sulfate, structural formula is as follows：
Raw material laruyl alcohol 6.64g and sulfamic acid 1.94g is added in 100ml round-bottomed flasks, original is made under agitation
Material dissolving, adds 1- butyl-pyridiniums disulfate ([BPy] HSO afterwards4) (structural formula is：) acidic ion liquid
0.3884g and urea 0.48g is as catalyst, the stirring reaction 4h at 90 DEG C.After completion of the reaction with 30%NaOH solution
Reason after drying, is washed, after chloroform with absolute ethyl alcohol, obtains white powder lauryl sodium sulfate sterling 3.69g to neutrality,
It is 64.0% to separate 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, original is made under agitation
Material dissolving, adds 1- butyl-pyridiniums disulfate ([BPy] HSO afterwards4) (structural formula is：) acidic ion liquid
0.3884g and urea 0.48g is as catalyst, the stirring reaction 2h at 95 DEG C.After completion of the reaction with 30%NaOH solution
Reason after drying, is washed, after chloroform with absolute ethyl alcohol, obtains white powder lauryl sodium sulfate sterling 4.56g to neutrality,
It is 79.1% to separate 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, original is made under agitation
Material dissolving, adds 1- butyl-pyridiniums disulfate ([BPy] HSO afterwards4) (structural formula is：) acidic ion liquid
0.3884g and urea 0.48g is as catalyst, the stirring reaction 4h at 100 DEG C.After completion of the reaction with 30%NaOH solution
Reason after drying, is washed, after chloroform with absolute ethyl alcohol, obtains white powder lauryl sodium sulfate sterling 5.30g to neutrality,
It is 91.9% to separate 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 be to greatest extent using the present invention.Therefore,
Above-mentioned preferred embodiment is merely illustrative of, rather than limits the scope of the present invention in any way.
Claims (5)
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 comprised the following steps that：
Laruyl alcohol and sulfamic acid are added in round-bottomed flask, dissolution of raw material, laruyl alcohol and sulfamic acid are made under agitation
Mol ratio is 1: 0.56~1.22, and the acidic ion liquid and urea of catalytic amount are added afterwards as catalyst, makes sulfamic acid
Mol ratio with acidic ion liquid is 1: 0.08~0.2,2~4h of stirring reaction at 90~100 DEG C.Use after completion of the reaction
30%NaOH solution is handled to neutrality, after drying, is washed with absolute ethyl alcohol, after chloroform, is obtained white powder dodecyl sulphur
Sour sodium.
。
2. such as the preparation method of claim 1 lauryl sodium sulfate, it is characterised in that sulfamic acid and acidic ion liquid
Mol ratio be 1: 0.08~0.2.
3. the preparation method of lauryl sodium sulfate as claimed in claim 1, it is characterised in that the presence of acidic ionic liquid catalyst
Agent is 1- butyl-pyridinium disulfates.
4. the preparation method of lauryl sodium sulfate as claimed in claim 1, it is characterised in that the reaction condition is 90~100
2~4h of stirring reaction at DEG C.
5. such as the preparation method of claim lauryl sodium sulfate, it is characterised in that the lauryl sodium sulfate needs to carry out
Purification process.
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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
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| CN106977428A true CN106977428A (en) | 2017-07-25 |
| CN106977428B CN106977428B (en) | 2018-08-21 |
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| Application Number | Title | Priority Date | Filing Date |
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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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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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 |
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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 |
| EP0990465A2 (en) * | 1998-10-01 | 2000-04-05 | Dai-Ichi Kogyo Seiyaku Co., Ltd. | Decomposition type reactive emulsifier and polymer-modifying method using the same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN106977428B (en) | 2018-08-21 |
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