Method of separating and purifying sucrose-6-acetate mother liquor by salt fractionation

A technology for purifying sucralose and sucralose is applied in the field of separation and purification of sucralose-6-acetate waste mother liquor, and can solve the problem of difficulty in effectively realizing recrystallization, high impurity content, and sucralose-6-acetate. It is difficult to obtain good results in the separation and purification of the ester mother liquor, so as to achieve the effects of improving treatment and utilization effects, improving economic benefits and reducing pressure

Active Publication Date: 2015-04-15
TECHNO (FUJIAN) FOOD INGREDIENTS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the polarity of many impurities such as sucralose-6-acetate, sucralose-6-acetate, and sucralose-6-acetate in the mother liquor of sucralose-6-acetate It is not much different from sucralose-6-acetate, and at the same time, due to the high content of impurities, it is difficult to effectively achieve recrystallization only by extraction
For this reason, the separation and purification of sucralose-6-acetate mother liquor in the prior art is also difficult to obtain good results

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In this embodiment, a method for separating and purifying sucralose-6-acetate mother liquor, the steps are as follows:

[0019] (1) Add 33.66g of sodium sulfate to 500ml of sucralose-6-acetate mother liquor with a specific gravity of 1.122g / ml (the content of sucralose-6-acetate is 5wt%), and at a temperature of 50°C React on a magnetic stirrer for 0.8h, stop stirring when turbidity occurs in the solution, cool at room temperature until sedimentation and stratification, and obtain 300ml of an upper layer solution containing sucralose-6-acetate;

[0020] (2) Add ethyl acetate to the upper layer solution for extraction, and extract three times, the amount of ethyl acetate extracted each time is 300ml, after concentration, sucralose-6-acetate concentrate is obtained;

[0021] (3) Add 200ml of water to the sucralose-6-acetate concentrate to dissolve it, then add 4.49g of activated carbon and stir at 60°C for 0.5h to decolorize, filter and crystallize at 12°C for 10h, 18 g ...

Embodiment 2

[0023] In this embodiment, a method for separating and purifying sucralose-6-acetate mother liquor, the steps are as follows:

[0024] (1) Add 60.90 g of ammonium sulfate to 500 ml of sucralose-6-acetate mother liquor with a specific gravity of 1.218 g / ml (the content of sucralose-6-acetate is 8 wt%), React on a magnetic stirrer for 0.5h, stop stirring when turbidity appears in the solution, cool at room temperature until sedimentation and stratification, and obtain 350ml of an upper layer solution containing sucralose-6-acetate;

[0025] (2) Add ethyl acetate to the upper layer solution for extraction, and extract three times, the amount of ethyl acetate extracted each time is 350ml, after concentration, sucralose-6-acetate concentrate is obtained;

[0026] (3) Add 250ml of water to the sucralose-6-acetate concentrate to dissolve it, then add 6.09g of activated carbon and stir at 65°C for 1h to decolorize, filter and crystallize at 10°C for 20h to obtain 30 g of white crysta...

Embodiment 3

[0028] In this embodiment, a method for separating and purifying sucralose-6-acetate mother liquor, the steps are as follows:

[0029] (1) Add 80.76 g of trisodium citrate to 500 ml of sucralose-6-acetate mother liquor with a specific gravity of 1.346 g / ml (the content of sucralose-6-acetate is 10 wt %), React on a magnetic stirrer at high temperature for 1 hour, stop stirring when turbidity occurs in the solution, cool at room temperature until sedimentation and layering, and obtain 350 ml of an upper layer solution containing sucralose-6-acetate;

[0030] (2) Add ethyl acetate to the upper layer solution for extraction, and extract three times, the amount of ethyl acetate extracted each time is 325ml, after concentration, sucralose-6-acetate concentrate is obtained;

[0031] (3) Add 300ml of water to the sucralose-6-acetate concentrate to dissolve it, then add 8.07g of activated carbon and stir at 70°C for 1h to decolorize, filter and crystallize at 15°C for 24h to obtain 4...

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Abstract

The invention discloses a method of separating and purifying sucrose-6-acetate mother liquor by salt fractionation. A sucrose-6-acetate crystal is obtained by salt fractionation, extracting, decoloration, filtering and crystallizing. The method is simple, quick and efficient; and by utilizing the method, not only the purifying effect obviously is improved, and the product yield and economic benefit are improved, so that actual production requirements are goodly met, but also the environment pressure is reduced, and a new path is provided for the treatment of industrial production waste water.

Description

technical field [0001] The invention relates to the technical field of chemical production waste treatment, in particular to a method for separating and purifying waste sucralose-6-acetate mother liquor produced in the sucralose production process. Background technique [0002] Sucralose (chemically named 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose) is the only functional new sweetener based on sucrose, sweet The sugar content can reach 600 times that of sucrose. It has the characteristics of no energy, high sweetness, pure sweet taste, high safety, anti-caries, and wide application range. The preparation of sucralose uses sucrose as a raw material, and the intermediate sucralose-6-acetate obtained through acylation and chlorination reactions must be recrystallized to remove impurities before the next step of the reaction can be carried out. The recrystallization process must produce mother liquor while obtaining crystals. In actual production, about 10-20 tons of was...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/06
Inventor 崔灿陈子昂陆夏莲佘觉民
Owner TECHNO (FUJIAN) FOOD INGREDIENTS CO LTD
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