Method for separating solvents after chlorination and neutralization reaction of sucralose

A technology of sucralose and separation method, which is applied in chemical instruments and methods, esterified saccharides, sugar derivatives, etc., can solve the problems of low equipment utilization efficiency, complicated operation process, DMF loss, etc., and avoid decomposition and coking. , The method and process are simple, and the effect of clean production is good

Active Publication Date: 2019-01-11
ANHUI JINGHE IND
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AI Technical Summary

Problems solved by technology

In the chlorination section of the sucralose production process, trichloroethane and DMF are widely used as solvents. With the increase of production, the usage of trichloroethane and DMF also increases, and solvents are bound to exist in the current production process. The problem of recovery, the current process is after the chlorination and neutralization step, the ammonium chloride salt is removed by filtration, and then the filtrate is directly taken in the still to take the method of jacket heating water to distill and recover the solvent. The disadvantage of this process is that it will cause The decomposition of DMF will cause the loss of DMF and the decomposition and coking of sucralose-6-ethyl ester. In order to completely recover the solvent, it is necessary to add a large amount of pure water to remove the azeotropic solvent during the distillation process. The operation process is complicated and time-consuming Long, low equipment utilization efficiency, and a large amount of DMF-containing wastewater that is difficult to treat

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  • Method for separating solvents after chlorination and neutralization reaction of sucralose

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Embodiment 1

[0019] Such as figure 1 As shown, a method for separating the solvent after the chlorination and neutralization reaction of sucralose provided by the present invention comprises the following steps:

[0020] a. Freeze and cool 8000L neutralizing solution containing sucralose-6-ethyl ester, trichloroethane, DMF, ammonium chloride and some impurities to 0°C, and filter the neutralizing solution through a filter press, and the filtrate enters first Put it in the neutralization liquid tank, then pump it into the extraction kettle, add 3600L10# industrial white oil under the stirring condition, stir for 1 hour and let it stand for stratification;

[0021] b. Put about 500kg of oil in the lower layer extracted and separated into a heat preservation kettle, add 2000L of water, heat to 60°C under normal pressure and cook for 1 hour, add 50kg of activated carbon to decolorize, filter through a filter press to remove activated carbon and some impurities, and the filtrate Enter the crys...

Embodiment 2

[0028] a. Freeze 8000L of neutralizing solution containing sucralose-6-ethyl ester, trichloroethane, DMF, ammonium chloride and some impurities to 5°C, filter the neutralizing solution through a filter press, and the filtrate enters the medium and liquid tank, and then pumped into the extraction kettle, stirring and adding 3400L10# industrial white oil, stirring for 1 hour and then standing for stratification.

[0029] b. Remove the solvent from the upper layer, put about 500kg of oily matter in the lower layer into a heat preservation kettle, add 2000L of water, heat to 60°C under normal pressure, cook for 1 hour, add 50kg of activated carbon for decolorization, and filter through a filter press to remove activated carbon and some impurities , the filtrate enters the crystallization kettle, add 1500L ethyl acetate under stirring and cool down to 5°C, then continue to stir for 3 hours to crystallize the crude product of sucralose-6-ethyl ester, which can be refined to obtain th...

Embodiment 3

[0035] a. Freeze 4000L of neutralizing solution containing sucralose-6-ethyl ester, trichloroethane, DMF, ammonium chloride and some impurities to 5°C, filter the neutralizing solution through a filter press, and the filtrate enters the medium and liquid tank, then pumped into the extraction kettle, stirring and adding 1800L10# industrial white oil, stirring for 1 hour and then standing for stratification.

[0036] b. Remove the solvent from the upper layer, put about 250kg of oil in the lower layer into a heat preservation kettle, add 1000L of water, heat to 60°C under normal pressure and cook for 1 hour, add 25kg of activated carbon for decolorization, and filter through a filter press to remove activated carbon and some impurities , the filtrate enters the crystallization kettle, add 750L of ethyl acetate under stirring and cool down to 0°C, then continue to stir for 3 hours to crystallize the crude product of sucralose-6-ethyl ester, which can be refined to obtain the fine ...

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Abstract

The invention relates to a method for separating solvents after a chlorination and neutralization reaction of sucralose. The method comprises the following steps: filtering a neutralized solution obtained after chlorination and neutralization, pumping the filtered neutralized solution into an extraction kettle, adding 10# industrial oil used as an extractant to extract the solvent trichloroethaneand DMF and make the solvents enter a supernatant, carrying out secondary reduced-pressure rectification on the supernatant, respectively separating the trichloroethane and DMF by using a boiling point difference, decolorizing high-boiling point industrial oil obtained after the secondary rectification with activated carbon to make the decolorized high-boiling point industrial oil directly reused,and directly reusing the trichloroethane and DMF obtained after the two-stage rectification in chlorination; and directly adding water to obtained lower oil to dissolve the lower oil, decolorizing and filtering the obtained solution, adding ethyl acetate, and performing freezing crystallization to obtain crude sucralose-6-acetate. The method has the advantages of simplicity, avoiding of the process of adding water to carry away the solvents during solvent recovery in traditional processes, reduction of the solvent recovery difficulty, improvement of the solvent recovery efficiency, energy consumption saving, great reduction of the production cost, and reduction of pollution.

Description

technical field [0001] The invention belongs to the production method of sucralose in the technical field of chemical industry, and in particular relates to a method for separating solvent after chlorination and neutralization reaction of sucralose. Background technique [0002] Sucralose is a fresh sweetener, its sweetness is 600-800 times that of sucrose, and its sweetness is similar to that of sucrose. Sucralose is not absorbed by the human body, has no bioaccumulation, and has high safety. The sucrose industry developed rapidly, the number of production enterprises gradually increased, and the output continued to increase. In the chlorination section of the sucralose production process, trichloroethane and DMF are widely used as solvents. With the increase of production, the usage of trichloroethane and DMF also increases, and solvents are bound to exist in the current production process. The problem of recovery, the current process is after the chlorination and neutral...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/02C07H13/04C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H5/02C07H13/04
Inventor 张正颂赵金刚孙多龙
Owner ANHUI JINGHE IND
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