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Preparation method for conjugated alkyl linoleate

The technology of conjugated linoleic acid alkyl ester and conjugated linoleic acid alkyl ester is applied in the field of separation and preparation of chemical raw materials, and can solve the problems of high content of trans isomer, difficulty in applying solvent, large discharge of three wastes, etc. Achieve the effect of increasing content, reducing saponification and reducing mass transfer resistance

Inactive Publication Date: 2017-04-19
武汉藤欣生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2) High content of trans isomer
3) The alkali consumption is large, and the solvent application is difficult
The conjugation reaction needs to be catalyzed by a large amount of base in an organic solvent, resulting in a large discharge of three wastes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]1) Take 500.0 g of methyl linoleate (derived from safflower seed oil) with a methyl linoleate content of 82.0%, add 20.0 g of potassium methylate under the protection of nitrogen, and stir the reaction for 4 hours at 120° C. Structured reaction to obtain the crude product of conjugated methyl linoleate, the content of unconverted methyl linoleate was 0.65% by sampling;

[0037] 2) After cooling down to 80°C, add 85% food-grade phosphoric acid to acidify the pH value to 7-8, then add 25g of diatomaceous earth, stir at 80°C for 0.5h, filter while hot, and separate the filter residue and filtrate;

[0038] 3) Wash the filtrate with hot water at 80°C for 1-2 times to neutrality, remove the water layer, dry the oil layer, add 25.0g of activated carbon, and decolorize at 100°C for 0.5h under vacuum conditions;

[0039] 4) Filtrate while hot to obtain the decolorized and purified filtrate, and finally carry out molecular distillation on the filtrate at 140°C to 150°C and 1Pa to...

Embodiment 2

[0042] 1) Take 500.0 g of ethyl linoleate (derived from sunflower oil) with an ethyl linoleate content of 85.0%, add 20.0 g of potassium ethoxide under the protection of nitrogen, and stir at 110°C for 5 hours for solvent-free isomerization reaction to obtain the crude product of conjugated ethyl linoleate, and the content of unconverted ethyl linoleate was detected by sampling as 0.8%;

[0043] 2) After cooling down to 70°C, add 85% food-grade phosphoric acid to adjust the pH value to 7-8, then add 10g of diatomaceous earth, stir at 70°C for 0.5h, filter while hot, and separate the filter residue and filtrate;

[0044] 3) Wash the filtrate with hot water at 70°C for 1-2 times to neutrality, remove the water layer, dry the oil layer, add 5g of activated carbon, and decolorize at 90°C for 45 minutes under vacuum conditions;

[0045] 4) Filtrate while hot to obtain the decolorized and purified filtrate, and finally carry out molecular distillation on the filtrate at 150°C to 160...

Embodiment 3

[0048] 1) Take 500.0 g of ethyl linoleate (derived from corn oil) with an ethyl linoleate content of 90.0%, add 30.0 g of sodium ethoxide under the protection of nitrogen, and stir at 100°C for 6 hours to carry out a solvent-free isomerization reaction , the crude product of conjugated ethyl linoleate was obtained, and the content of unconverted ethyl linoleate was detected by sampling as 0.2%;

[0049] 2) After cooling down to 60°C, add 85% food-grade phosphoric acid to adjust the pH value to 7-8, then add 10g clay, stir at 60°C for 1 hour, filter while hot, and separate the filter residue and filtrate;

[0050] 3) Wash the filtrate with hot water at 60°C for 1-2 times to neutrality, remove the water layer, dry the oil layer, add 40.0g of activated carbon, and decolorize at 110°C under vacuum for 1 hour;

[0051] 4) Filtrate while hot to obtain the decolorized and purified filtrate, and finally perform molecular distillation on the filtrate at 140°C to 150°C and 1Pa to 5Pa to...

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Abstract

The invention discloses a preparation method for conjugated alkyl linoleate. The preparation method comprises the following steps: subjecting alkyl linoleate and an alkaline catalyst to a solvent-free isomerization reaction at 100 DEG C to 140 DEG C, wherein the reaction time is 2 h to 6 h; carrying out acidification until the pH value of an obtained solution is 7 to 8, and carrying out filtration and separation so as to obtain filter residue and a filtrate; and subjecting the filtrate to washing, then carrying out decolorization and purification, and removing a solvent so as to obtain the conjugated alkyl linoleate. According to the invention, the alkyl linoleate is selected as a raw material; the alkaline catalyst consumption is reduced; and a direct solvent-free reaction is adopted. Meanwhile, the preparation method provided by the invention adopts a lower reaction temperature and can meet the content requirement of the conjugated alkyl linoleate, so energy and raw materials are further saved. In addition, the preparation method adopts vegetable oil with rich alkyl linoleate, enriches raw material sources, and reduces the dependence on safflower oil, thereby effectively reducing production cost and achieving strong practicability.

Description

technical field [0001] The invention relates to the field of separation and preparation of chemical raw materials, in particular to a preparation method of conjugated linoleic acid and its alkyl ester. Background technique [0002] Conjugated linoleic acid (CLA) is a general term for a series of positional isomers and spatial isomers of linoleic acid (LA) with double bonds at carbon 9, 11 or 10, 12. Studies have shown that CLA has physiological functions such as lowering cholesterol, improving immune function, inhibiting tumors, and resisting atherosclerosis. At the same time, related literature reports that CLA can inhibit the synthesis of fat in adipose tissue and enhance the decomposition of fat, reducing body fat, especially abdominal fat. Therefore, unlike other long-chain saturated fatty acids, conjugated linoleic acid can be absorbed by the human body as a special functional fatty acid, and promote fat decomposition by changing the way of lipid metabolism, so as to a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/333C07C69/587
CPCC07C67/333C07C69/587
Inventor 周小波
Owner 武汉藤欣生物工程有限公司
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