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A kind of sucralose-6-ethyl ester purification method

A technology of sucralose and purification method, which is applied in the field of sugar industry, can solve the problems of affecting the quality of sucralose products, increasing the amount of solvent used, production and environmental burden, etc., achieve high industrial application value, and reduce the amount of solvent used , the effect of reducing the number of crystallization

Active Publication Date: 2022-07-26
ANHUI JINHE IND CO LTD
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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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  • A kind of sucralose-6-ethyl ester purification method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] 1t sucralose-6-ethyl ester mother liquor with a water content of 30% was added to the mixing kettle E-1, and boiled at 40°C, specifically, adding 90% of the mother liquor quality water at a stirring speed of 300r / min, Stir well. After stirring for 0.5h, it is separated by the solid-liquid separator H-1, the solid is returned to the mixing kettle E-1, and the mother liquor enters the liquid phase separator E-2 to stand; The brown tar in the lower phase is removed, and the upper phase enters the upper edge of the extraction tower E-3; the extraction agent 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 top of the tower; the extracted liquid from the bottom of the extraction tower enters the e...

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 a mass of 80% of the mother liquor at a stirring speed of 400r / min, and stir well. After stirring for 0.5h, it is separated by the solid-liquid separator H-1, the solid is returned to the mixing kettle E-1, and the mother liquor enters the liquid phase separator E-2 to stand; The brown tar in the lower phase is removed, and the upper phase enters the upper edge of the extraction tower E-3; the extraction agent cyclohexane enters from the lower edge of the extraction tower, and the ratio of the two is 1:0.6. 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 extracted liquid from the bottom of the extraction tower enters the evaporator E-4 for evaporation, and the obtained solid is passed through ethyl acetate twice. Cooling a...

Embodiment 3

[0070] The 3t sucralose-6-ethyl ester mother liquor with a water content of 50% was added to the mixing kettle E-1, heated and boiled at 55°C, and 65% of the mother liquor mass was added at a stirring rate of 250r / min, and stirred thoroughly. After stirring for 1.5h, it is separated by solid-liquid separator H-1, the solid is returned to mixing kettle E-1, and the mother liquor enters liquid phase separator E-2 to stand; The brown tar in the lower phase is removed, and the upper phase enters the upper edge of the extraction tower E-3; the extraction agent isoheptane enters from the lower edge of the extraction tower, and the ratio of the two is 1:0.8. 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 extracted liquid from the bottom of the extraction tower enters the evaporator E-4 for evaporation, and the obtained solid is passed through ethyl acetate twice. Cool...

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Abstract

The invention discloses a method for purifying sucralose-6-ethyl ester. The method comprises: a secondary boiling step: taking a boiled and negative-pressure-treated mother liquor of sucralose-6-ethyl ester; ‑Adding a predetermined proportion of water to the ethyl ester mother liquor, fully stirring and heating it for boiling, stirring and boiling for a preset time, and then solid-liquid separation to obtain a secondary boiling mother liquor in which sucralose‑6‑ethyl ester is dissolved; phase-separated extraction step : the secondary boiled mother liquor is left to stand for phase separation, the upper phase after the phase separation is taken, and the alkane extractant is used for extraction at a preset temperature to remove the residual white oil in the upper phase; recrystallization and purification step: extracting the obtained The lower layer effluent obtained is evaporated to obtain a solid, and the solid is purified by recrystallization to obtain sucralose-6-ethyl ester; recovery and circulation step: the upper layer effluent after extraction is separated, and the alkane extractant is recovered and recycled to the phase-separating extraction step use. The method is simple, efficient, and low in cost, can effectively remove trace amounts of white oil, and improve the purity of sucralose-6-ethyl ester.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/04C07H1/06
CPCC07H13/04C07H1/06
Inventor 郑学连王东陈永乐
Owner ANHUI JINHE IND CO LTD
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