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Method for synthesizing citric acid glyceride by immobilized lipase catalysis in rotatory evaporator

A technology of glyceryl citrate and immobilized lipase, which is applied in the field of synthesis of glyceryl citrate, can solve the problems of cumbersome steps and difficult separation, and achieve the effect of strong specificity, easy removal and less by-products

Inactive Publication Date: 2009-10-21
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the second technology to produce glyceryl citrate has higher catalytic efficiency, but the steps are cumbersome, and it is easy to form impurity glyceryl acetate, which belongs to the same surfactant as glyceryl citrate, which has similar properties and is not easy to separate

Method used

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  • Method for synthesizing citric acid glyceride by immobilized lipase catalysis in rotatory evaporator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.1921g (0.001mol) of citric acid and 0.7171g (0.002mol) of monoglyceride, 10mL of anhydrous isopropanol into a round bottom flask, and heat to 40°C. After the substrate was fully dissolved, 900 mg of immobilized Rhizomucor miehei lipase Lipozyme RM IM was added, and the round-bottomed flask was placed in a rotary evaporator to react at 45°C with a rotation speed of 120 rpm and a vacuum of 0.1 MPa for 40 h. After the reaction was finished, sampling and analysis showed that the conversion rate of citric acid reached more than 70%. The organic solvent was removed by distillation under reduced pressure, the rotation speed was 120 rpm, the vacuum degree was 0.1 MPa, and the temperature was 75° C. to obtain glycerol citrate. After analysis, the acid value of the product is 90-100 mgKOH / g, and the saponification value is 260-265 mgKOH / g.

Embodiment 2

[0022] Add 0.1921g of citric acid and 0.3586g of monoglyceride, 5mL of anhydrous isoamyl alcohol into a round bottom flask, and heat to 40°C. After the substrate was fully dissolved, 550 mg of immobilized Rhizomucor miehei lipase Lipozyme RM IM was added, and the round-bottomed flask was placed in a rotary evaporator, and reacted at 45°C with a rotation speed of 120 rpm and a vacuum of 0.1 MPa for 40 h. After the reaction was finished, sampling and analysis showed that the conversion rate of citric acid reached more than 70%. The organic solvent was removed by distillation under reduced pressure, the rotation speed was 120 rpm, the vacuum degree was 0.1 MPa, and the temperature was 75°C. After vacuum distillation, filter while hot to remove unreacted suspended solids in the oil phase, 95% (w / w) of which is unesterified citric acid. Wash the oil phase with an equal volume of water at a temperature of 50° C., centrifuge to collect the oil phase, and repeat 3 times. After the o...

Embodiment 3

[0024] Add 0.1921g of citric acid and 0.3586g of monoglyceride, 5mL of anhydrous tert-amyl alcohol into a round bottom flask, and heat to 40°C. After the substrate was fully dissolved, 550 mg of immobilized Candida antarctica lipase Novozym 435 was added, and the round-bottomed flask was placed in a rotary evaporator, and reacted at 50°C with a rotation speed of 120 rpm and a vacuum of 0.1 MPa for 30 h. After the reaction was finished, sampling and analysis showed that the conversion rate of citric acid reached more than 70%. The organic solvent was removed by distillation under reduced pressure, the rotation speed was 120 rpm, the vacuum degree was 0.1 MPa, and the temperature was 85°C. After vacuum distillation, filter while hot to remove unreacted suspended solids in the oil phase, 95% (w / w) is unesterified citric acid. Wash the oil phase with an equal volume of water at a temperature of 50° C., centrifuge to collect the oil phase, and repeat 3 times. After the oil phase ...

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Abstract

A method for synthesizing citric acid glyceride by immobilized lipase catalysis in a rotatory evaporator is disclosed, belonging to the technical field of the synthesis of citric acid glyceride. In the invention, monoglyceride and citric acid are used as reaction substrates, organic solvents like anhydrous isopropanol, anhydrous isoamylol or anhydrous tertiary amyl alcohol are used as reaction media, the immobilized lipase is used as a catalyst, and esterification reaction is carried out in the rotatory evaporator to obtain the product of the citric acid glyceride. The invention, which takes the rotatory evaporator as the reactor, can facilitate the substrates to contact with the catalyst sufficiently. The inventive method has the characteristics of mild conditions, strong specificity, less number of byproducts, high conversion rate and the like.

Description

technical field [0001] The invention discloses a method for synthesizing glyceryl citrate catalyzed by immobilized lipase with a rotary evaporator, which belongs to the technical field of glyceryl citrate synthesis. Background technique [0002] Glyceryl citrate is an esterification product of glycerin, fatty acid and citric acid, which has an amphiphilic molecular structure and belongs to anionic surfactants. Due to its non-toxic, easy biodegradation and good surface activity, glyceryl citrate is widely used in food, medicine, cosmetics, detergents and other fields. [0003] Glyceryl citrate is a new type of surfactant developed in the past ten years in China. Its production method is mainly chemical method: ①Using acetic acid as the reaction medium, adding 0.1% to 1% (w / w) catalyst, such as acid , alkali or metal oxides, etc., directly catalyze the esterification reaction of citric acid and monoglyceride or diglyceride. ②Use acetic anhydride and citric acid to prepare ci...

Claims

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Application Information

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IPC IPC(8): C12P7/64
Inventor 单良金青哲刘元法吴晓娟王兴国潘秋琴黄健花宋志华
Owner JIANGNAN UNIV
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