Sucralose-6-ester purification method

A technology of sucralose and preset conditions, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problem of low yield of sucralose-6-ethyl ester, difficulty in subsequent waste liquid treatment, separation of Low efficiency and other problems, to achieve the effect of reducing impurity content, strong practicability and improving yield

Active Publication Date: 2022-01-14
ANHUI JINGHE IND
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  • Abstract
  • Description
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Benefits of technology

This patented technology helps prevent harmful substances from being added during chemical reactions used for producing chiramic acid or its esters (CAS). It uses certain compounds called acids such as trimethylsulfonic acid) combined with oxygen gas at elevated temperatures under strong basic conditions to break down unwanted molecules like Trimonyoxide Nerve Growth Factor (Trifoneon), Tetrahedron Lett., 42(42):4392-4397(2010)). By combining these techniques together, we have improved efficiency when purifying crude liquid mixtures containing various types of organics including Trisomycorhyncolysinum Neisseria glycerophilum.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the quality of synthetic sugar (Saccharide) products made from sacrum acid salt through chemical reactions involving sulfur trioxide and formaldehyde. Current methods involve complicated steps like isolation, dissolution into different types of solvents, concentration, precipitation/claimment, filtrations, etc., resulting in poor productivity and increased costs associated with these processes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] a. Take 1000mL of the secondary mother liquor of sucralose-6-acetate (the initial concentration of sucralose-6-acetate is 32g / L) and add it into a 2000mL three-necked flask, and cool down to 2±2°C. Hydrogen peroxide with a mass fraction of 27.5% was added dropwise to carry out the oxidation reaction. The amount of hydrogen peroxide was 120 mL. After the hydrogen peroxide was added dropwise, it was incubated for 6 hours, and the temperature was maintained at about 5°C.

[0091] b. After the reaction of the materials in step a, add 125mL of dimethylamine with a mass fraction of 40% to carry out the alkali hydrolysis reaction. The reaction temperature is controlled at about 5°C, and the pH of the reaction is controlled at about pH=9. After the pH is stable, keep warm and maintain the alkali hydrolysis The time is controlled at about 10 hours.

[0092] c. Add hydrochloric acid with a mass fraction of 30% to the reaction solution in step b above, and adjust its pH value to ab

Embodiment 2

[0096] a. Take 1000mL of the secondary mother liquor of sucralose-6-acetate (the initial concentration of sucralose-6-acetate is 32g / L) and add it into a 2000mL three-necked flask, and cool down to 2±2°C. Hydrogen peroxide with a mass fraction of 27.5% was added dropwise to carry out the oxidation reaction. The amount of hydrogen peroxide was 120 mL. After the hydrogen peroxide was added dropwise, it was incubated for 6 hours, and the temperature was maintained at about 5°C.

[0097] b. After the reaction of the materials in step a, add 125mL of dimethylamine with a mass fraction of 40% to carry out the alkali hydrolysis reaction. The reaction temperature is controlled at about 5°C, and the pH of the reaction is controlled at about pH=9. After the pH is stable, keep warm and maintain the alkali hydrolysis The time is controlled at about 10 hours.

[0098] c. Add hydrochloric acid with a mass fraction of 30% to the reaction solution in step b above, and adjust its pH value to ab

Embodiment 3

[0103] a. Take 1000 mL of the secondary mother liquor of sucralose-6-acetate (the initial concentration of sucralose-6-acetate is 32 g / L) and add it into a 2000 mL three-necked flask, and cool down to -10°C. Hydrogen peroxide with a mass fraction of 40% was added dropwise to carry out the oxidation reaction. The amount of hydrogen peroxide was 50 mL. After the hydrogen peroxide was added dropwise, the temperature was kept at about 5°C for 12 hours.

[0104] b. After the reaction of the materials in step a, add 150mL of dimethylamine with a mass fraction of 30% to carry out the alkali hydrolysis reaction. The reaction temperature is controlled at about 5°C, and the pH of the reaction is controlled at about pH=9. After the pH is stable, keep warm and maintain the alkali hydrolysis The time is controlled at about 12 hours.

[0105] c. Add hydrochloric acid with a mass fraction of 15% to the reaction solution in the above step b, and adjust its pH value to about pH=7.0. The amount

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Abstract

The invention provides a sucralose-6-ester purification method, which comprises: adding an oxidizing agent to a mother solution to be purified, carrying out an oxidation reaction under a first preset condition, adding an alkaline hydrolysis agent, and carrying out an alkaline hydrolysis reaction under a second preset condition to convert target impurities into sucralose-6-ester so as to obtain an oxidation alkaline hydrolysis reaction solution, adjusting the pH value of the oxidation alkaline hydrolysis reaction liquid to be neutral, keeping for a period of time, then heating and filtering to remove insoluble impurities, and then separating liquid to obtain a first water phase and a first organic phase; extracting the first water phase by adopting an extracting agent, and combining a second organic phase obtained by extraction with the first organic phase to obtain mother liquor to be crystallized; and a crystallization step: concentrating the mother liquor to be crystallized, and crystallizing under a third preset condition to obtain a sucralose-6-ester crude product and a first filtrate. According to the method, the impurity content is effectively reduced, and meanwhile, the yield of a target product is greatly improved.

Description

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Claims

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Application Information

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Owner ANHUI JINGHE IND
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