A continuous circulation preparation method and product of high-purity lactulose solution

A technology for the cyclic preparation of lactulose, applied in the preparation of sugar derivatives, chemical instruments and methods, disaccharides, etc., can solve the problems of many by-products, difficult to realize industrial production, complicated separation and purification, etc., and achieve simplified production process, Improve production efficiency and overcome the effect of low yield

Active Publication Date: 2020-10-30
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the problems existing in the existing lactulose preparation process such as long reaction time, many by-products, low conversion rate, complicated separation and purification, and difficulty in realizing industrialized production, the purpose of the present invention is to provide an efficient and environmentally friendly lactose isomerization method A method for chemically preparing high-purity lactulose solution to fill the gap in the field of isomerization of sodium metaaluminate / sodium hydroxide catalytic system in China to prepare lactulose, and at the same time make up for and overcome the deficiencies in the current technology of chemical isomerization for the preparation of lactulose

Method used

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  • A continuous circulation preparation method and product of high-purity lactulose solution

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Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1: Preparation of high-purity lactulose syrup.

[0039] Under the condition of mechanical stirring, add 20kg food-grade lactose and 3kg sodium metaaluminate as the lactose substrate into 100L deionized water and dissolve, then add sodium hydroxide, and adjust the pH value of the system to 11.5, and then The reaction was stirred under low temperature for 2 hours. After the reaction was completed, the system was cooled to room temperature to obtain isomerized lactulose syrup. As determined by HPLC, the conversion rate of lactulose was 66%, and the mass concentration of lactulose was 135g / L.

[0040] Under the condition of mechanical stirring, 6 mol / L hydrochloric acid solution was added dropwise to the above-mentioned isomerized lactulose syrup to adjust the pH value of the system to 6.5 to form a mixed solution containing lactulose and flocculation precipitation system.

[0041]Add 100L of deionized water to the above mixed solution, and mechanically stir the...

Embodiment 2

[0046] Example 2: Preparation of crystalline lactulose.

[0047] Under the condition of mechanical stirring, 35kg of food-grade lactose and 8kg of sodium metaaluminate as the lactose substrate were added to 100L of deionized water and dissolved, then sodium hydroxide was added, and the pH value of the system was adjusted to 12.0, and then heated at 60°C The reaction was stirred under low temperature for 1 h, and after the reaction was completed, the system was cooled to room temperature to obtain isomerized lactulose syrup. As determined by HPLC, the conversion rate of lactulose was 85%, and the mass concentration of lactulose was 298g / L.

[0048] Under the condition of mechanical stirring, 10 mol / L sulfuric acid was added dropwise to the above-mentioned isomerized lactulose syrup, and the pH value of the system was adjusted to 5.0 to form a mixed solution containing lactulose and flocculation precipitation system.

[0049] Add 200L of deionized water to the above mixed solut...

Embodiment 3

[0054] Embodiment 3: Preparation of high-purity lactulose powder.

[0055] Under the condition of mechanical stirring, add 50kg food grade lactose and 24kg sodium metaaluminate as the lactose substrate into 100L deionized water and dissolve, then add sodium hydroxide, and adjust the pH value of the system to 12.5, and then The reaction was stirred under low pressure for 30 minutes. After the reaction was completed, the system was cooled to room temperature to obtain isomerized lactulose syrup. As determined by HPLC, the conversion rate of lactulose was 72%, and the mass concentration of lactulose was 360 g / L.

[0056] Under mechanical stirring conditions, 10 mol / L hydrochloric acid was added dropwise to the above-mentioned isomerized lactulose syrup, and the pH value of the system was adjusted to 4.5 to form a mixed solution containing lactulose and a flocculation precipitation system.

[0057] Add 300L of deionized water to the above mixed solution, and mechanically stir the...

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Abstract

A method for preparing high-purity lactulose by efficient removal of sodium meta-aluminate, pertaining to the technical field of oligosaccharide preparation. The method comprises preparing a high-purity lactulose syrup and a product thereof by pretreatment of a syrup, removal of a catalyst, removal of a monosaccharide and a salt, and posttreatment of the syrup. The efficient removal and recycling of the catalyst sodium meta-aluminate is realized. In the final product, Al residue is < 10 ppm (with respect to lactulose) and the purity of lactulose is > 95%. The preparation process meets resource-saving and environmentally-friendly production requirements, and facilitates clean, efficient, and environmentally-friendly industrial production of high-purity lactulose.

Description

technical field [0001] The invention belongs to the technical field of oligosaccharide preparation, and relates to a continuous circulation preparation method of a high-purity lactulose solution and a product thereof. Background technique [0002] Lactulose (also known as lactulose or isomerized lactose, molecular formula: C 12 h 22 o 11 ; Molecular weight: 342.30Da; Chemical name: 4-O-β-D-galactopyranosyl-D-fructose) is a bifidobacterium promoting factor with low calorie, high safety, good stability, and wide application wide advantages. Japan approved lactulose as "food for specified health uses" (FOSHU: food for specified health uses) in 1996, and more than 100 countries in the world have approved it to enter the pharmacopoeia. Lactulose has a wide range of applications. In addition to medicine, health products, food additives and animal feed, it can also be used as a functional factor in infant milk powder. In recent years, with the sharp increase in people's demand...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H3/04C07H1/00C07H1/06B01J23/04
CPCB01J23/04C07H1/00C07H1/06C07H3/04Y02P20/584
Inventor 杨瑞金汪明明华霄张文斌赵伟
Owner JIANGNAN UNIV
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