CN103058894A - Production method of high-purity sodium dodecyl sulfate - Google Patents
Production method of high-purity sodium dodecyl sulfate Download PDFInfo
- Publication number
- CN103058894A CN103058894A CN2013100046299A CN201310004629A CN103058894A CN 103058894 A CN103058894 A CN 103058894A CN 2013100046299 A CN2013100046299 A CN 2013100046299A CN 201310004629 A CN201310004629 A CN 201310004629A CN 103058894 A CN103058894 A CN 103058894A
- Authority
- CN
- China
- Prior art keywords
- sodium lauryl
- lauryl sulphate
- production method
- sodium dodecyl
- dodecyl sulfate
- 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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- 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
-
- 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
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Abstract
The invention belongs to the field of sodium dodecyl sulfate, and especially relates to a production method of sodium dodecyl sulfate. The sodium dodecyl sulfate production method is characterized in comprising the steps that: (1) sulfonation and neutralization are carried out, wherein a sulfonating agent is added into lauryl alcohol, such that a sulfate is produced through a sulfonation reaction; sulfate is subjected to a neutralization reaction with sodium hydroxide, such that liquid sodium dodecyl sulfate is produced; (2) concentration is carried out; (3) drying is carried out, wherein the concentrated solid material is dried, and a drying temperature is 40-100 DEG C; and (4) crushing, molding, and packaging are carried out, wherein the dried solid material is crushed, molded, and packaged, such that products are obtained. The method provided by the invention has the advantages that: with the method, a production process route of sodium dodecyl sulfate used in a conventional daily use material is broken through. The product purity is up to 97% or even higher than 99%. The product can be used in biological pharmacy and chemical reagent production.
Description
(1) technical field
The invention belongs to the sodium lauryl sulphate field, particularly a kind of production method of high purity sodium lauryl sulphate.
(2) background technology
Present industrialized sodium lauryl sulphate belongs to the daily necessities raw material, because conventional operational path adopts mixed fatty alcohol (take carbon 12-14 alcohol as main) sulfonation, neutralization, sedimentation, spraying drying, because raw materials used and production technique is limit, its product purity is low, foreign matter content is high, impurity mainly is homologue, sodium sulfate, sodium-chlor and the unreacted Fatty Alcohol(C12-C14 and C12-C18) of sodium lauryl sulphate, has restricted the use range of product.
(3) summary of the invention
The invention provides a kind of production method for preparing simple high purity sodium lauryl sulphate.
The present invention is achieved through the following technical solutions:
A kind of production method of high purity sodium lauryl sulphate, its special character is: may further comprise the steps:
(1) sulfonation, neutralization: add sulphonating agent generation sulfonation reaction in the lauryl alcohol and generate sulfuric ester, sulfuric ester is sent out into neutralization reaction with sodium hydroxide and is obtained the liquid sodium lauryl sulphate;
(2) concentrated: with the concentrated solid substances that obtains being crystal paillette shape of liquid sodium lauryl sulphate;
(3) drying: the solid substances after concentrated is carried out drying, and drying temperature is 40 ℃-100 ℃, obtains work in-process;
(4) pulverizing, moulding, packing: will be packaged to be product after work in-process pulverizing, the moulding.
Corresponding chemical equation is:
The production method of high purity sodium lauryl sulphate of the present invention, the sodium lauryl sulphate mass percentage concentration is 10-38% in the middle liquid sodium lauryl sulphate of step (1), sulphonating agent is chlorsulfonic acid or sulphur trioxide.
The production method of high purity sodium lauryl sulphate of the present invention, the mass percentage concentration of sodium lauryl sulphate is 60-85% in the middle solid substances of step (2), the weight water content of solid substances is 15-40%.
The production method of high purity sodium lauryl sulphate of the present invention, the sodium lauryl sulphate mass percentage concentration is higher than 97% in the middle product of step (4).
Beneficial effect of the present invention: production method of the present invention has broken through conventional daily raw material sodium lauryl sulphate production process route, adopt lauryl alcohol (having another name called lauryl alcohol) through steps such as sulfonation, neutralization, concentrated, crystallization and purification, solid-liquid separation, fragmentation, cryodryings, its product purity is up to more than 97% even 99%, product is as a kind of novel anion surfactant, can be used for bio-pharmaceuticals, chemical reagent production, and three-waste free discharge, environmental protection and energy saving in the production process.
(4) embodiment
Embodiment 1:
The production method of present embodiment high purity sodium lauryl sulphate the steps include:
(1) sulfonation, neutralization: generate sulfuric ester (CH with adding 116.52kg chlorsulfonic acid liquid generation sulfonation reaction in the 190.18kg lauryl alcohol (mass percentage concentration is 98.1%)
3(CH
2)
11OSO
3H), sulfuric ester and 118kg mass percentage concentration are that 34% NaOH sends out into neutralization reaction and obtains the liquid sodium lauryl sulphate, and the mass percentage concentration of sodium lauryl sulphate is 38%, 177kg in this liquid sodium lauryl sulphate after measured;
(2) concentrated, crystallization and purification, solid-liquid separation: the liquid sodium lauryl sulphate is concentrated, separates out the solid substances that 295kg is crystal paillette shape, and the massfraction that sodium lauryl sulphate accounts for solid substances is 60%, and the weight water content of this solid substances is 39%;
(3) cryodrying: the solid substances after concentrated is carried out drying at 100 ℃, obtain work in-process;
(4) pulverizing, moulding, packing: with work in-process pulverizing, moulding (outward appearance is the crystal sheet), be packaged to be the 178.79kg product, product purity is 99%.
Its reaction formula is:
Embodiment 2:
The production method of present embodiment high purity sodium lauryl sulphate the steps include:
(1) sulfonation, neutralization: add 82.5kg sulfur trioxide gas generation sulfonation reaction in the 188.26kg lauryl alcohol (mass percentage concentration is 99%) and generate sulfuric ester (CH
3(CH
2)
11OSO
3H), sulfuric ester and 200kg mass percentage concentration are that 20% NaOH sends out into neutralization reaction and obtains the liquid sodium lauryl sulphate, and the mass percentage concentration of sodium lauryl sulphate is 10%, 42.48kg in this liquid sodium lauryl sulphate after measured;
(2) concentrated, crystallization and purification, solid-liquid separation: the liquid sodium lauryl sulphate is concentrated, separates out the solid substances that 49.97kg is crystal paillette shape, the massfraction that sodium lauryl sulphate accounts for solid substances is 85%, and the weight water content of this solid substances is 13.1%;
(3) cryodrying: the solid substances after concentrated is carried out drying at 40 ℃, obtain work in-process;
(4) pulverizing, moulding, packing: the pulverizing of this product, moulding are packaged to be the 43.74kg product after (outward appearance is powdery), and product purity is 97.1%.
Its reaction formula is:
Embodiment 3:
The production method of present embodiment high purity sodium lauryl sulphate the steps include:
(1) sulfonation, neutralization: add 96kg sulfur trioxide gas generation sulfonation reaction in the 187.32kg lauryl alcohol (mass percentage concentration is 99.5%) and generate sulfuric ester (CH
3(CH
2)
11OSO
3H), sulfuric ester and 150kg mass percentage concentration are that 27% NaOH sends out into neutralization reaction and obtains the liquid sodium lauryl sulphate, and the mass percentage concentration of sodium lauryl sulphate is 19%, 80.54kg in this liquid sodium lauryl sulphate after measured;
(2) concentrated, crystallization and purification, solid-liquid separation: the liquid sodium lauryl sulphate is concentrated, separates out the solid substances that 111.86kg is crystal paillette shape, the massfraction that sodium lauryl sulphate accounts for solid substances is 72%, and the weight water content of this solid substances is 27.5%;
(3) cryodrying: the solid substances after concentrated is carried out drying at 70 ℃;
(4) pulverizing, moulding, packing: dried solid substances pulverizing, moulding (outward appearance is spherical or needle-like) are packaged to be the 80.94kg product, and product purity is 99.5%.
Its reaction formula is:
Production method of the present invention has removed that traditional processing technology prepares sodium lauryl sulphate and the inorganic salt that generate, the composition of unreacted Fatty Alcohol(C12-C14 and C12-C18), and inner quality is not destroyed, and makes the sodium lauryl sulphate that high purity is applicable to bio-pharmaceuticals and chemical reagent-grade.Purity by method preparing product of the present invention is higher than 97%, has effectively promoted quality product, has expanded the range of application of SDS product, makes it to enter high-technology field; Three-waste free discharge, environmental protection and energy saving.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equal variation.In every case be not break away from the technical solution of the present invention content, according to technical spirit of the present invention any simple modification equivalent variations that above embodiment does still belonged to the technical solution of the present invention protection domain with remodeling.
Claims (4)
1. the production method of a high purity sodium lauryl sulphate is characterized in that: may further comprise the steps:
(1) sulfonation, neutralization: add sulphonating agent generation sulfonation reaction in the lauryl alcohol and generate sulfuric ester, sulfuric ester is sent out into neutralization reaction with sodium hydroxide and is obtained the liquid sodium lauryl sulphate;
(2) concentrated: with the concentrated solid substances that obtains being crystal paillette shape of liquid sodium lauryl sulphate;
(3) drying: the solid substances after concentrated is carried out drying, and drying temperature is 40 ℃-100 ℃, obtains work in-process;
(4) pulverizing, moulding, packing: will be packaged to be product after the pulverizing of this product, the moulding.
2. the production method of high purity sodium lauryl sulphate according to claim 1 is characterized in that: in the step (1) in the liquid sodium lauryl sulphate sodium lauryl sulphate mass percentage concentration be 10-38%, sulphonating agent is chlorsulfonic acid or sulphur trioxide.
3. the production method of high purity sodium lauryl sulphate according to claim 1 is characterized in that: in the step (2) in the solid substances mass percentage concentration of sodium lauryl sulphate be 60-85%, the weight water content of solid substances is 15-40%.
4. the production method of high purity sodium lauryl sulphate according to claim 1 is characterized in that: in the step (4) in the product sodium lauryl sulphate mass percentage concentration be higher than 97%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100046299A CN103058894A (en) | 2013-01-07 | 2013-01-07 | Production method of high-purity sodium dodecyl sulfate |
| PCT/CN2013/001337 WO2014106312A1 (en) | 2013-01-07 | 2013-11-05 | Method for producing high-purity sodium dodecyl sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100046299A CN103058894A (en) | 2013-01-07 | 2013-01-07 | Production method of high-purity sodium dodecyl sulfate |
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|---|---|
| CN103058894A true CN103058894A (en) | 2013-04-24 |
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| CN2013100046299A Pending CN103058894A (en) | 2013-01-07 | 2013-01-07 | Production method of high-purity sodium dodecyl sulfate |
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| WO (1) | WO2014106312A1 (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804461A (en) * | 2014-02-17 | 2014-05-21 | 浙江大学 | Preparation method of tea saponin sulfate surfactant and product thereof |
| CN106977428A (en) * | 2017-03-17 | 2017-07-25 | 内蒙古工业大学 | Improve the method for preparing lauryl sodium sulfate |
| 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 |
| CN107602423A (en) * | 2017-08-29 | 2018-01-19 | 东明俱进化工有限公司 | A kind of production technology and its device of powdered bay alcohol sulfuric ester sylvite |
| CN107602431A (en) * | 2017-09-12 | 2018-01-19 | 广东丽臣奥威实业有限公司 | A kind of high concentration lauryl sodium sulfate liquid and preparation method thereof |
| 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 |
| CN110590610A (en) * | 2019-06-17 | 2019-12-20 | 中轻化工绍兴有限公司 | Preparation method of high-quality sodium alkyl sulfate |
| CN112500320A (en) * | 2020-12-16 | 2021-03-16 | 江苏优扬药业有限公司 | Preparation device and method of pharmaceutical adjuvant sodium dodecyl sulfate |
| CN114786727A (en) * | 2019-12-27 | 2022-07-22 | 中外制药株式会社 | Method for screening, evaluating or producing sodium lauryl sulfate or pharmaceutical preparation containing the same as raw material |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278958A (en) * | 2015-05-18 | 2017-01-04 | 上海紫源制药有限公司 | A kind of synthetic method of sodium tetradecyl sulfate |
| CN106278961A (en) * | 2015-05-18 | 2017-01-04 | 上海紫源制药有限公司 | A kind of synthetic method of sodium tetradecyl sulfate |
Citations (6)
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|---|---|---|---|---|
| US4322367A (en) * | 1979-11-26 | 1982-03-30 | Colgate-Palmolive Company | Deoiling of aqueous solutions of sodium lauryl sulfate |
| CN1082456A (en) * | 1992-05-28 | 1994-02-23 | 国际壳牌研究有限公司 | The preparation method who contains the surfactant composition of secondary alkyl sulfate |
| CN1222142A (en) * | 1996-04-16 | 1999-07-07 | 普罗格特-甘布尔公司 | Process for mfg. sulphates of longer chain branched alkanols and alkoxylated alkanols |
| JP2000136398A (en) * | 1998-11-02 | 2000-05-16 | Lion Corp | Manufacture of anionic surfactant |
| RU2271351C1 (en) * | 2004-09-24 | 2006-03-10 | ГОУ ВПО Белгородский государственный университет | Method for preparing sodium lauryl sulfate |
| CN101235001A (en) * | 2007-12-21 | 2008-08-06 | 王伟松 | Method for synthesizing aliphatic alcohol sulfate |
-
2013
- 2013-01-07 CN CN2013100046299A patent/CN103058894A/en active Pending
- 2013-11-05 WO PCT/CN2013/001337 patent/WO2014106312A1/en active Application Filing
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4322367A (en) * | 1979-11-26 | 1982-03-30 | Colgate-Palmolive Company | Deoiling of aqueous solutions of sodium lauryl sulfate |
| CN1082456A (en) * | 1992-05-28 | 1994-02-23 | 国际壳牌研究有限公司 | The preparation method who contains the surfactant composition of secondary alkyl sulfate |
| CN1222142A (en) * | 1996-04-16 | 1999-07-07 | 普罗格特-甘布尔公司 | Process for mfg. sulphates of longer chain branched alkanols and alkoxylated alkanols |
| JP2000136398A (en) * | 1998-11-02 | 2000-05-16 | Lion Corp | Manufacture of anionic surfactant |
| RU2271351C1 (en) * | 2004-09-24 | 2006-03-10 | ГОУ ВПО Белгородский государственный университет | Method for preparing sodium lauryl sulfate |
| CN101235001A (en) * | 2007-12-21 | 2008-08-06 | 王伟松 | Method for synthesizing aliphatic alcohol sulfate |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804461A (en) * | 2014-02-17 | 2014-05-21 | 浙江大学 | Preparation method of tea saponin sulfate surfactant and product thereof |
| CN103804461B (en) * | 2014-02-17 | 2016-01-06 | 浙江大学 | The preparation method of tea saponin sulfuric acid ester surfactant and product |
| CN106977428A (en) * | 2017-03-17 | 2017-07-25 | 内蒙古工业大学 | Improve the method for preparing lauryl sodium sulfate |
| 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 |
| CN107602423A (en) * | 2017-08-29 | 2018-01-19 | 东明俱进化工有限公司 | A kind of production technology and its device of powdered bay alcohol sulfuric ester sylvite |
| 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 |
| CN107602431A (en) * | 2017-09-12 | 2018-01-19 | 广东丽臣奥威实业有限公司 | A kind of high concentration lauryl sodium sulfate liquid and preparation method thereof |
| 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 |
| CN110590610A (en) * | 2019-06-17 | 2019-12-20 | 中轻化工绍兴有限公司 | Preparation method of high-quality sodium alkyl sulfate |
| CN114786727A (en) * | 2019-12-27 | 2022-07-22 | 中外制药株式会社 | Method for screening, evaluating or producing sodium lauryl sulfate or pharmaceutical preparation containing the same as raw material |
| CN112500320A (en) * | 2020-12-16 | 2021-03-16 | 江苏优扬药业有限公司 | Preparation device and method of pharmaceutical adjuvant sodium dodecyl sulfate |
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| Publication number | Publication date |
|---|---|
| WO2014106312A1 (en) | 2014-07-10 |
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Application publication date: 20130424 |