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Production method for extracting VE and sterol from soybean oil deodorized distillate by using enzyme-chemistry combined technology

A deodorizing distillate and production method technology, applied in the field of sterol and VE extraction, can solve the problems of incomplete alcoholysis, no alcoholysis of sterol esters, and enzyme cost problems, and achieve favorable recovery and utilization, mild reaction conditions, Improve the effect of high energy consumption

Inactive Publication Date: 2017-09-29
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many other patents and articles describing the enzyme-catalyzed reaction of vegetable oil deodorization distillate, but the enzymatic process is still rarely used in industrial production. Alcoholysis of glycerides and sterol esters in deodorized distillates
[0007] In summary, the process of purifying vitamin E from vegetable oil deodorization distillates by using strong acid and strong base can complete the reaction of esterification and alcoholysis, so the yields of sterols and methyl esters are high, but there are complicated procedures, The product quality is not good, a large amount of waste water is produced, labor intensity is high, etc.
The process of purifying vitamin E from vegetable oil deodorized distillates by enzymatic method has the advantages of mild reaction conditions, no waste water, and high-quality products. However, the alcoholysis of triglycerides and sterol esters in the deodorized distillate is not complete. , leading to subsequent separation difficulties, the yields of methyl esters and sterols also decreased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] To 100 g of vegetable oil deodorization effluent (purchased from Nantong Cargill Grain and Oil Co., Ltd.), 10 mL of methanol was added, 5 g of immobilized lipase Novozym435 was added, the temperature was controlled at 40° C., and the reaction was stopped after stirring for 1 h. Recover the immobilized lipase by filtration, add 50ML methanol after desolvation under reduced pressure or normal pressure, add dropwise 1ML sodium methoxide, and stir at 70°C for 2h to complete the transesterification reaction. After the reaction is completed, add an appropriate amount of sulfuric acid for neutralization, wash the feed solution to neutrality at 2°C / hr, freeze to 10°C, crystallize for 8 hours, and filter to obtain the filter cake crude sterol and filtrate. The filtrate is subjected to distillation, in which the methyl ester fraction is collected at 150°C-240°C, and the VE fraction is collected at 240-280°C. The operating pressure is 1-50Pa.

Embodiment 2

[0025] Add 150ml of methanol to 500g of vegetable oil deodorization effluent (purchased from Nantong Cargill Grain and Oil Co., Ltd.), add 2.5g of immobilized lipase Novozym 435, control the temperature at 50°C, stir for 5 hours and then stop the reaction. Recover the immobilized lipase by filtration, add 40ML methanol after desolvation under reduced pressure or normal pressure, add dropwise 5ML sodium methoxide, and stir at 70°C for 2h to complete the transesterification reaction. After the reaction is completed, add an appropriate amount of sulfuric acid for neutralization, wash the feed solution to neutrality with water, freeze to 5°C at 2°C / hr, crystallize for 8h, and filter to obtain the crude sterol and filtrate of the filter cake. The filtrate is subjected to distillation, in which the methyl ester fraction is collected at 150°C-240°C, and the VE fraction is collected at 240-280°C. The operating pressure is 1-50Pa.

Embodiment 3

[0027] Add 1000g vegetable oil deodorization effluent (purchased from Nantong Cargill Grain and Oil Co., Ltd.), add 500ML methanol, add 100g immobilized lipase Lipozyme RM IM, control the temperature at 20°C, stir for 3 hours, then stop the reaction. Recover the immobilized lipase by filtration, add 200ML methanol after precipitation under reduced pressure or normal pressure, add dropwise 30ML sodium methoxide, and stir at 60°C for 2 hours to complete the transesterification reaction. After the reaction is completed, add an appropriate amount of sulfuric acid for neutralization, wash the feed solution to neutrality at 2°C / hr, freeze to 15°C, crystallize for 10h, and filter to obtain the crude sterol and filtrate of the filter cake. The filtrate is subjected to distillation, in which the methyl ester fraction is collected at 150°C-240°C, and the VE fraction is collected at 240-280°C. The operating pressure is 1-50Pa.

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Abstract

The invention provides a production method for extracting VE and sterol from a soybean oil deodorized distillate by using an enzyme-chemistry combined technology. The method comprises the steps of firstly, converting fatty acids in the deodorized distillate into fatty acid methyl ester by using immobilized lipase as a catalyst, then, carrying out an ester exchange reaction on the material by using sodium methylate as a catalyst so as to convert glyceryl esters and sterol esters in the deodorized distillate into fatty acid methyl ester, glycerine and sterol, carrying out water washing to remove the glycerine, carrying out cooling, crystallizing and filtrating so as to obtain crude sterol, and carrying out distillation, thereby obtaining the fatty acid methyl ester and the VE. According to the method, the esterification reaction is carried out by replacing strong acid with the lipase, the fatty acids in the deodorized distillate are converted into the fatty acid methyl ester under mild conditions, no wastewater is generated, the operation is simple, no environmental pollution is caused, industrialization is easy to achieve, the yield of the fatty acid methyl ester and the sterol is remarkably increased; and through an enzyme method and a chemical method, the VE with relatively high purity and the crude sterol are finally obtained.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, in particular to a production method for extracting VE and sterols from soybean oil deodorized distillate by using enzyme-chemical combined technology. Background technique [0002] Natural VE has important physiological functions such as anti-free radicals, anti-oxidation, anti-aging, and improving immunity, and natural VE is superior to synthetic VE in terms of physiological activity and safety. It is a non-toxic and efficient natural antioxidant and is currently widely used Used in oil, food, cosmetics, medicine and other industrial products. [0003] Vegetable oil and its processing by-products are the most abundant sources of phytosterols, mainly including campesterol, stigmasterol and sitosterol, which are widely used in food, medicine, cosmetics, animal growth agents and paper processing, printing, textiles and other fields, especially It is very common as a food additive in ...

Claims

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Application Information

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IPC IPC(8): C07C69/003C07C67/02C07D311/72C07J9/00C12P7/64
CPCC07C67/02C07D311/72C07J9/00C12P7/6436C07C69/003
Inventor 王升帆许新德邵斌张莉华郑建永汪钊
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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