Method of preparing alpha-sulphonic acid fatty acid ester

A technology of sulfonic acid fatty acid ester and fatty acid ester, which is applied in the fields of sulfonic acid preparation and organic chemistry, can solve problems such as difficulty in removing heat in time, high reaction temperature, and long reaction time, and achieve short reaction residence time and high reaction time. The effect of low temperature and stable product quality

Inactive Publication Date: 2009-08-19
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to propose a kind of α-sulfonic acid in view of the disadvantages of strong exothermic reaction in the prior art, difficult to control, difficult to remove heat in time, long reaction time, high reaction temperature and low safety. The preparation method of fatty acid ester

Method used

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  • Method of preparing alpha-sulphonic acid fatty acid ester
  • Method of preparing alpha-sulphonic acid fatty acid ester
  • Method of preparing alpha-sulphonic acid fatty acid ester

Examples

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Effect test

Embodiment 1

[0038] 98% concentrated sulfuric acid (storage tank 1) and preheated palm oil fatty acid methyl ester (storage tank 2) are injected into the temperature control unit with the flow rate of 0.71ml / min and 4.29ml / min by high-pressure pumps 3 and 4 respectively. In a rectangular cross-toed glass microstructure reactor 5 with a channel width of 0.05mm, a depth of 0.15mm, and a length of 40mm at 65°C, the residence time is 3.6ms, and after mixing, it enters a polytetrafluoroethylene microchannel reactor with an inner diameter of 2mm 6. Adjust the residence time of the reactants in the microchannel reactor to 3min, and then enter the polytetrafluoroethylene microchannel reactor 7 with an inner diameter of 2mm at a temperature controlled at 85°C to adjust the residence time of the reactants in the microchannel reactor The time was 2.5 minutes, and the reaction product (storage tank 10) was collected, and the sulfonation rate of the reaction was calculated by extraction method to be 74....

Embodiment 2

[0040] Free SO 3 Content is the oleum (storage tank 1) of 50% and the palm oil fatty acid methyl ester (storage tank 2) that preheated, inject into with the flow rate of 1.53ml / min, 3.47ml / min by high-pressure pump 3,4 respectively The temperature is controlled at 80°C in a rectangular cross-toed glass microstructure reactor 5 with a channel width of 0.05 mm, a depth of 0.15 mm, and a length of 40 mm. The residence time is 3.6 ms. After mixing, it enters a polytetrafluoroethylene microchannel with an inner diameter of 2 mm. Reactor 6, adjust the residence time of the reactant in the microchannel reactor to be 2min, then enter the polytetrafluoroethylene microchannel reactor 7 with an inner diameter of 2mm at 90°C and control the temperature of the reactant in the microchannel reactor The residence time is 5min, and the reaction product (storage tank 10) is collected to obtain a sulfonation rate of 98.8%, and the free fatty acid methyl ester content in the sulfonation product i...

Embodiment 3

[0042] With 99% chlorosulfonic acid (storage tank 1) and the palm oil fatty acid methyl ester (storage tank 2) of preheating, inject to temperature with the flow rate of 1.11ml / min, 1.89ml / min by high-pressure pump 3,4 respectively Controlled at 85°C in a stainless steel slit cross-toed microstructure reactor 5 with a channel width of 0.04mm, a depth of 0.15mm, and a length of 25mm, the residence time is 3.0ms, and after mixing, it enters a stainless steel microchannel reactor with an inner diameter of 1.2mm 6. Adjust the residence time of the reactant in the microchannel reactor to be 0.8min, and then enter the polytetrafluoroethylene microchannel reactor 7 with an inner diameter of 2mm at a temperature of 85°C to adjust the reactant's residence time in the microchannel reactor. The residence time was 1.3 min, and the reaction product was collected (storage tank 10). The sulfonation rate of the reaction was 95.3%, and the free fatty acid methyl ester content in the sulfonation...

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Abstract

The invention relates to a method for preparing alpha-sulfonic fatty acid ester by sulfonating fatty acid ester, comprising the following steps: injecting the fatty acid ester and a sulfonating agent into a micro-structural reactor (5) and a reactor (6) inside diameter of which is a micro passage respectively, mixing and sulfonating the fatty acid ester and the sulfonating agent, controlling the reaction temperature between 50 and 100 DEG C, and controlling the reaction materials to stay for 1ms to 1s in the micro-structural reactor (5) and stay for 0.5 to 30 minutes in the micro-passage reactor (6); and then injecting the reaction materials into a micro-passage reactor (7), aging the reaction materials at a reaction temperature between 50 and 100 DEG C, and controlling the reaction materials to stay for 0.5 to 30 minutes in the micro-passage reactor to obtain the alpha-sulfonic fatty acid ester. In the method, the novel micro-structural reactor is adopted, the defect of difficult control due to strong reaction heat release in the prior art is overcome, the materials can be mixed evenly, the released reaction heat can be removed in time, the reaction time can be controlled accurately, and the method has the advantages of good sulfonating efficiency, simple and safe operation and good product quality.

Description

technical field [0001] The invention belongs to the field of surfactants, and relates to a method for preparing alpha-sulfonic fatty acid esters by sulfonation of fatty acid esters. Background technique [0002] Fatty Acid Methyl Ester Sulphonates (MES for short) is an excellent anionic surfactant, mainly used to replace sodium tripolyphosphate and sodium alkylbenzene sulfonate, known as the third-generation detergent active agent things. The detergency of MES is best with C14MES, and the detergency of C14, C16, and C18MES is better than sodium dodecylbenzenesulfonate (LAS) and fatty alcohol sulfate (AS). The foaming performance of MES is equivalent to that of LAS, among them, the foaming performance of C16 MES is better, and the foaming performance of C18MES is medium. Compared with the existing washing powder, it has the advantages of environmental protection, good washing effect, no embrittlement and cracking of washed fabrics, and the like. In addition, MES is mild in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/17C07C303/06C07C303/08
Inventor 张利雄许鹏飞姚建峰谢天明徐南平
Owner NANJING UNIV OF TECH
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