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Continuous cyclic preparation method of high-purity lactulose solution and product thereof

A technology for cyclic preparation of lactulose, which is applied in the preparation of sugar derivatives, chemical instruments and methods, disaccharides, etc., can solve the problems of many by-products, complicated separation and purification, and difficulty in industrialized production, so as to improve production efficiency, The effect of overcoming the low yield and simplifying the production process

Active Publication Date: 2018-06-12
JIANGNAN UNIV
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  • Summary
  • 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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  • Continuous cyclic preparation method of high-purity lactulose solution and product thereof

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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

The invention belongs to the technical field of oligosaccharide preparation, and relates to a continuous cyclic preparation method of a high-purity lactulose solution and a product thereof. Specifically speaking, the preparation method comprises the following steps: (1) performing lactulose isomerisation; (2) performing acidity adjustment; (3) diluting, dispersing and separating; (4) purifying clear lactulose liquid; (5) performing cyclic utilization of a catalyst. Through the preparation method, high-concentration lactulose solution and a subsequent product thereof can be prepared. Accordingto the continuous cyclic preparation method of the high-purity lactulose solution and the product thereof, sodium metaaluminate / an alkaline matter is taken as an alkaline complexing catalyst for the first time in China, and the conversion rate and lactulose concentration achieved by preparing the lactulose by taking the sodium metaaluminate / an alkaline matter as the alkaline complexing catalyst are far higher than those achieved by adopting a boracic acid / sodium hydroxide system; repeated cyclic use of a sodium metaaluminate catalyst is realized; the defect that precipitate wraps the lactuloseis overcome. The preparation method provided by the invention meets resource-saving and environment-friendly production requirements, and provides beneficial experience and reference for promoting clean, high-efficiency and environment-friendly lactulose industrial production.

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 Applications(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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