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Method for purifying sucralose-6-ethyl ester

A technology of sucralose and purification method, which is applied in the field of sugar industry, and can solve problems affecting the quality of sucralose products, production and environmental burden, and increasing the amount of solvent used

Active Publication Date: 2021-09-07
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has been found in production that after white oil extraction, a small amount of white oil will remain in the sucralose-6-ethyl ester refined product processed in the above method, which affects the quality of subsequent sucralose products. Therefore, it is necessary to The fine sucralose-6-ethyl ester was recrystallized multiple times to remove traces of white oil
Thus, due to the trace amount of white oil introduced by the extraction in the chlorination process, the amount of solvent used in the purification process of the sucralose-6-ethyl ester product has increased, and it has caused a certain burden and impact on production and the environment
[0004] At present, there are few reports about the method for removing white oil from sucralose-6-ethyl ester products. The visible reports on the purification of sucralose-6-ethyl ester, such as CN101328195, CN101709069, etc., usually only use esters, etc. Solvents purify sucralose-6-ethyl ester by crystallization, such as commonly used ethyl acetate, butyl acetate, etc., the inclusion of white oil is always unavoidable in effect

Method used

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  • Method for purifying sucralose-6-ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Add 1 t of sucralose-6-ethyl ester mother liquor with a water content of 30% into the mixing kettle E-1, heat and boil at 40°C, specifically, add water with a mass of 90% of the mother liquor at a stirring rate of 300r / min, Stir well. After stirring for 0.5h, it is separated by the solid-liquid separator H-1, and the solid is returned to the mixing kettle E-1, and the mother liquor enters the liquid phase separator E-2 to stand still; after the mother liquor is left standing in the liquid phase separator E-2 The brown tar in the lower phase is discharged, and the upper phase enters the upper edge of the extraction tower E-3; the extractant cyclopentane enters from the lower edge of the extraction tower E-3, the ratio of the two is 1:0.5, and the temperature is 30 ° C. Extraction, after the extraction is completed, the sucralose-6-ethyl ester aqueous solution without white oil is extracted from the bottom of the tower, and the alkane mixed liquid is extracted from the to...

Embodiment 2

[0066] Add 2t sucralose-6-ethyl ester mother liquor with a water content of 40% into mixing kettle E-1, heat and boil at 90°C, add water with 80% mother liquor mass at a stirring speed of 400r / min, and stir thoroughly. After stirring for 0.5h, it is separated by the solid-liquid separator H-1, and the solid is returned to the mixing kettle E-1, and the mother liquor enters the liquid phase separator E-2 to stand still; after the mother liquor is left standing in the liquid phase separator E-2 The brown tar in the lower phase is discharged, and the upper phase enters the upper edge of the extraction tower E-3; the extractant cyclohexane enters from the lower edge of the extraction tower, the ratio of the two is 1:0.6, and the extraction is carried out at a temperature of 25 ° C. After the extraction is completed, the tower The sucralose-6-ethyl ester aqueous solution without white oil is extracted from the bottom, and the alkane mixed liquid is extracted from the top of the towe...

Embodiment 3

[0070] Add the 3t sucralose-6-ethyl ester mother liquor with a water content of 50% into the mixing kettle E-1, heat and boil at 55°C, add water with a mass of 65% of the mother liquor at a stirring speed of 250r / min, and stir thoroughly. After stirring for 1.5h, it is separated by the solid-liquid separator H-1, and the solid is returned to the mixing kettle E-1, and the mother liquor enters the liquid phase separator E-2 to stand still; The brown tar in the lower phase is discharged, and the upper phase enters the upper edge of the extraction tower E-3; the extractant isoheptane enters from the lower edge of the extraction tower, the ratio of the two is 1:0.8, and the extraction is carried out at a temperature of 40 ° C. After the extraction is completed, the tower The sucralose-6-ethyl ester aqueous solution without white oil is extracted from the bottom, and the alkane mixed liquid is extracted from the top of the tower; the extraction liquid from the bottom of the extracti...

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Abstract

The invention discloses a sucralose-6-ethyl ester purification method which comprises the following steps: a secondary water boiling step: taking sucralose-6-ethyl ester mother liquor subjected to water boiling and negative pressure treatment, adding a preset proportion of water into the sucralose-6-ethyl ester mother liquor, fully stirring and heating for water boiling, and after stirring and water boiling for a preset time, filtering to obtain a filtrate; carrying out solid-liquid separation to obtain a secondary water boiling mother solution in which sucralose-6-ethyl ester is dissolved; a phase separation extraction step: standing the secondary water boiling mother liquor for phase separation, taking an upper phase after phase separation, extracting by using an alkane extraction agent at a preset temperature, and removing residual white oil in the upper phase; a recrystallization purification step: evaporating the lower effluent obtained after extraction to obtain a solid, and purifying the solid through recrystallization to obtain sucralose-6-ethyl ester; and a recycling step: separating the extracted upper-layer effluent, recycling the alkane extraction agent, and recycling the alkane extraction agent to the split-phase extraction step for use. The method is simple, efficient and low in cost, trace white oil can be effectively removed, and the purity of sucralose-6-ethyl ester is improved.

Description

technical field [0001] The invention relates to the technical field of sugar industry, in particular to a method for purifying sucralose-6-ethyl ester. Background technique [0002] In the sucralose production process, the chlorinated neutralization solution obtained in the chlorination section contains impurities such as trichloroethane and dimethylformamide (DMF), which need to be extracted and removed with white oil. White oil is a mixture of liquid hydrocarbons, mainly a mixture of saturated naphthenes and saturated paraffins, obtained from petroleum refining, or obtained from crude oil by normal pressure and vacuum fractionation, solvent extraction, dewaxing, and hydrofining. Industrial standards such as "NB / SH / T 0006-2017 Industrial White Oil". [0003] In the traditional process, the product of sucralose-6-ethyl ester in the high-temperature chlorination section of sucralose needs to be boiled once after the white oil is extracted, and a small amount of residual tric...

Claims

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Application Information

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IPC IPC(8): C07H13/04C07H1/06
CPCC07H13/04C07H1/06C07H3/04
Inventor 郑学连王东陈永乐
Owner ANHUI JINGHE IND
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