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Method for crystallizing psicose from ethanol solution

A technology of allulose and ethanol solution, which is applied in the direction of chemical instruments and methods, monosaccharides, sugar derivatives, etc., can solve the problems of easy deliquescence, poor product phase, and difficult crystallization of allulose, and achieve crystallization Uniform crystal form, simple and easy drying, and easy solid-liquid separation

Inactive Publication Date: 2019-05-14
JILIN COFCO BIOCHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, allulose is difficult to crystallize, spray drying is easy to deliquescence, and the product is not good. Therefore, the development of a suitable crystallization process is very important for the development of the allulose industry.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 20L of the purified allulose solution, concentrate under reduced pressure to a specific gravity of 1.20 (2L in volume), heat the concentrated solution to 65°C, add 1L of absolute ethanol, concentrate under reduced pressure at 60°C to make the ethanol take away the allulose Water in the solution to obtain a concentrated solution with a specific gravity of 1.20 (volume 2L), add 6L of absolute ethanol, heat to 60°C, allulose is completely dissolved, slowly cool down, about every 2°C / h, precipitate crystals and continue Slowly lower the temperature to 40°C to obtain a mixed solution containing allulose crystals. Filter through a 100-mesh filter cloth, heat and dry the solid under vacuum at 50°C, with a vacuum degree of 0.10 MPa, and obtain 400 g of crystals; the permeate is concentrated to 1.5 L, and the temperature is lowered twice to crystallize. Repeat the above crystallization process, and the crystals are dried and recovered. The filtrate and the next batch Merge ...

Embodiment 2

[0037] Take 40L of purified allulose solution, concentrate under reduced pressure to a specific gravity of 1.20 (volume 2L), heat the concentrated solution to 80°C, add 0.4L of absolute ethanol, and concentrate under reduced pressure at 65°C to allow the ethanol to take away the allulone Water in the sugar solution, to obtain a concentrated solution with a specific gravity of 1.30 (volume 1.5L), add 15L of absolute ethanol, heat to 30°C, allulose is completely dissolved, and slowly cool down, about every 0.5°C / h, crystals are precipitated Afterwards, continue to slowly lower the temperature to 10° C. to obtain a mixed solution containing allulose crystals. Filter through a 60-mesh filter cloth, heat and dry the solid under vacuum at 40°C, with a vacuum degree of 0.10 MPa, to obtain 300 g of crystals; the permeate was concentrated to 1.2 L, and crystallized by cooling twice, and the above crystallization process was repeated, and the crystals were dried and recovered. Merge app...

Embodiment 3

[0039] Take 10L of purified allulose solution, concentrate under reduced pressure to a specific gravity of 1.10 (volume 1.0L), heat the concentrated solution to 30°C, add 1.5L of absolute ethanol, and concentrate under reduced pressure at 70°C to make the ethanol take away allulose Water in the ketose solution to obtain a concentrated solution with a specific gravity of 1.25 (volume 0.5L), add 2.5L of absolute ethanol, heat to 80°C, allulose is completely dissolved, and slowly cool down, about every 10°C / h, After the crystals were precipitated, the temperature continued to be slowly lowered to 30° C. to obtain a mixed solution containing allulose crystals. Filter through a 500-mesh filter cloth, heat and dry the solid under vacuum at 60°C, with a vacuum degree of 0.090 MPa, to obtain 80 g of crystals; the permeate was concentrated to 0.4 L, and crystallized by cooling twice, and the above crystallization process was repeated, and the crystals were dried and recovered. Merge ap...

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Abstract

The invention provides a method for crystallizing psicose from an ethanol solution. The method comprises the steps that a purified psicose solution is taken, and decompression concentration is carriedout to obtain a solution I; the concentrated solution I is heated, absolute ethyl alcohol is added, decompression concentration is carried out again, so that ethyl alcohol takes away the moisture inthe psicose solution to become an ethanol solution II of the psicose; the absolute ethyl alcohol is added into the concentrated solution II, heating is carried out until the psicose is completely dissolved, slow cooling is carried out, after crystals are separated out, slow cooling is carried out until crystals are no longer added, and a mixed liquor III is obtained; solid-liquid separation is carried out to on the mixed liquor III to obtain a solid IV and a clear liquid V; decompression drying is carried out on the solid IV to obtain psicose crystals; the clear liquid V continues to be concentrated, the above steps are repeated, and crystallization is carried out to obtain remaining psicose crystals. The method for crystallizing psicose from the ethanol solution has the advantages that through the cooling crystallization of the psicose in the ethanol solution, one-time crystallization ratio is high, the crystal forms of crystallization are uniform, the drying preservation and transportation are easy, the preparation process is safe and reliable, the process is simplified, the conventional operability of equipment is strong, and the material consumption is low.

Description

technical field [0001] The invention relates to a method for crystallizing psicose from ethanol solution, belonging to the technical field of biochemical separation. Background technique [0002] With the global spread of chronic diseases such as obesity, diabetes, and "three highs", the "healthy intake" of sugar in the diet has become a new health issue. Among them, the development and application of low-calorie sweeteners is one of the most effective ways one. [0003] Allulose (D-psicose, Psi) is the epimer of D-fructose (D-fructose, Fru) C-3, the sweetness is equivalent to 70% of sucrose, the heat is equivalent to 0.3% of sucrose, and the volume characteristics And the taste is similar to sucrose, it can be used as a substitute for sucrose in the food and pharmaceutical industry. Compared with high fructose syrup, which has the risk of causing obesity and diabetes, allulose has the effect of controlling obesity and diabetes, can significantly inhibit weight gain and ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H3/02
Inventor 佟毅吕哲郭元亨丁子元王小艳李皓然刘颖慰陈博
Owner JILIN COFCO BIOCHEM
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