CN104387427A

CN104387427A - Method for producing sucralose

Info

Publication number: CN104387427A
Application number: CN201410592960.1A
Authority: CN
Inventors: 程光锦; 郑学连
Original assignee: Anhui Jinhe Industrial Co Ltd
Current assignee: Anhui Jinhe Industrial Co Ltd
Priority date: 2014-10-30
Filing date: 2014-10-30
Publication date: 2015-03-04

Abstract

The invention relates to the field of food additives and relates to a method for producing sucralose. The method comprises the following steps: a, carrying out a chlorination reaction on sucrose 6-acetate generated through esterification reaction; b, neutralizing the reacting liquid after chlorination is completed; c, desolventizing the neutralized liquid; and d, hydrolyzing the desolventized liquid to obtain a crude liquid of sucralose. The method has the advantages that sucrose 6-acetate is not purified and a sodium hydroxide solution is directly added dropwise to react to generate the target product sucralose after chlorination and neutralization; besides, the sucrose 6-acetate can react to generate sucralose, about 13 percent of byproducts in chlorination can be converted into the target product sucralose. According to the novel process, the conversion rate is increased by about 10 percent, environmental pollution caused by separation purification of intermediates after chlorination and neutralization can be reduced.

Description

A kind of production method of Sucralose

Technical field:

The present invention relates to foodstuff additive field, particularly a kind of production method of Sucralose.

Background technology:

Sucralose traditional processing technology, as shown in Figure 1, through step of esterification generation in early stage sucrose 6-ethyl ester, after superchlorination, neutralization reaction step, extracting and separating purification is carried out to the Sucralose 6-ethyl ester that reaction generates, then after hydrolysing step, obtains crude product Sucralose.A large amount of sewage can be produced in the process of extracting and separating purification Sucralose 6-ethyl ester, lose moiety intermediate simultaneously, not only contaminate environment and productive rate but also low.

Summary of the invention

Object of the present invention is exactly to solve during Sucralose produces, the lower and problem of environmental pollution that brings thus of the Sucralose transformation efficiency caused because of the separating-purifying of intermediate, the production method of a kind of Sucralose provided.

Technology technical scheme of the present invention is as follows:

A production method for Sucralose, through step of esterification generation in early stage sucrose 6-ethyl ester, is characterized in that comprising the following steps:

The sucrose 6-ethyl ester that a, esterification generate, be added drop-wise at 0 DEG C ~ 5 DEG C the Vilsmeier reagent prepared and carry out low temperature chlorination reaction, after low temperature chlorination terminates, half an hour is stirred under normal temperature, be warmed up to about 50 degree again, be incubated one hour again, be then incubated one hour respectively at 75 degree, 85 degree, 95 degree, 105 degree, 110 degree of two to three hours of insulation;

B, chlorination terminate, and cool to about 10 degree, add ammonia neutralization to pH value 9.5, then stir half hour, then with hydrochloric acid, pH value is adjusted to 7-7.5, and neutral temperature controls at≤20 DEG C;

Proceed to precipitation still after c, neutralizer press filtration desalination, decompression sloughs trichloroethane and DMF, precipitation temperature 50 C ~ 60 DEG C;

D, precipitation liquid proceed to hydrolysis kettle, cool to 20 DEG C, with the pH value to 12 of alkali regulator solution, maintain still temperature stirring reaction 5 hours, sampling detects, when area ratio≤0.5% of trichloro-cane-6-ethyl ester, with hydrochloric acid, pH value is adjusted to 6.8 ~ 7.0 again, stir 10 minutes after adjustment puts in place, repetition measurement PH=6.8 ~ 7.0, namely obtain Sucralose crude product liquid.

Advantage of the present invention

1) after adopting the present invention, the step of former technique separation trichloro-cane-6-ethyl ester is omitted, and therefore saves relevant extraction agent consumption, decreases operator simultaneously, reduce labor cost because operation steps reduces.

2), after adopting existing Process, producing total yield obviously increases, and yield is increased to present 41% by original 31%.Because part intermediate by-products is converted into product (old technique extraction loss moiety intermediate), therefore while yield improves, also reduce the processing cost of later stage to by product and the pollution to environment.

Accompanying drawing illustrates:

fig. 1 is traditionalsucralose traditional processing technology schema;

Fig. 2 is Sucralose traditional processing technology figure of the present invention.

Embodiment:

Embodiment 1:

A, in chlorination tank, add 3000L trichloroethane, open stirring chuck and lead to salt solution, then at the solid phosgene slowly dropping into 800KG, feed temperature controls below 20 DEG C, finish molten clear after, be cooled to 0 DEG C, add catalyzer 1kg, stir and start to drip esterifying liquid 1200L after 15 minutes, maintain temperature of charge 0 DEG C ~ 5 DEG C, and tiny structure, after low temperature chlorination terminates, under normal temperature, stir half an hour, be warmed up to about 50 degree again, be incubated one hour again, be then incubated one hour respectively at 75 degree, 85 degree, 95 degree, 105 degree, 110 degree of two to three hours of insulation.

B, chlorination terminate, and cool to about 10 degree, and add ammonia neutralization to pH value 9.5, then stir half hour, then with hydrochloric acid, pH value is adjusted to 7-7.5, neutral temperature controls at≤20 DEG C.

Proceed to precipitation still after c, neutralizer press filtration desalination, decompression sloughs trichloroethane and DMF, precipitation temperature 50 C ~ 60 DEG C, material thickness after precipitation, adds 900L about 50 DEG C of hot water wherein or applies mechanically water;

D, precipitation liquid proceed to hydrolysis kettle, cool to 20 DEG C, with the pH value to 12 of sheet alkali regulator solution, maintain still temperature stirring reaction 5 hours, sampling detects, and when area ratio≤0.5% of trichloro-cane-6-ethyl ester, then with 30% hydrochloric acid, pH value is adjusted to 6.8 ~ 7.0, stir 10 minutes repetition measurement PH=6.8 ~ 7.0 after adjustment puts in place, namely obtain Sucralose crude product liquid.Again through extract assorted, extract, dry to obtain Sucralose sterling 124KG.

Advantage of the present invention: new production technique be in chlorination and after Sucralose 6-ethyl ester is not purified and does not directly drip sodium hydroxide solution reaction and generate target product Sucralose, the benefit of this novel process generates Sucralose except Sucralose 6-ethyl ester can react, and the by product of chlorination reaction about 13% can be made in addition to be converted into target product Sucralose.Therefore novel process had both improve the transformation efficiency of about 10%, decreased because of in chlorination and the separating-purifying of rear center body and the environmental pollution that causes simultaneously.

Implementation column 2:

A, in chlorination tank, add 2700L trichloroethane, open stirring chuck and lead to salt solution, then at the solid phosgene slowly dropping into 540KG, feed temperature controls below 20 DEG C, finish molten clear after, be cooled to 0 DEG C, add catalyzer 1kg, stir and start to drip esterifying liquid 800L after 15 minutes, maintain temperature of charge 0 DEG C ~ 5 DEG C, and tiny structure, after low temperature chlorination terminates, under normal temperature, stir half an hour, then be warmed up to about 50 degree, be incubated one hour again, then at 75 degree, 85 degree, 95 degree, 105 degree are incubated one hour respectively, 110 degree of two to three hours of insulation.

B, chlorination terminate, and cool to about 10 degree, add ammonia neutralization to pH value 9.5, then stir half hour.With hydrochloric acid, pH value is adjusted to 7---7.5 again.Neutral temperature controls at≤20 DEG C

Proceed to precipitation still after c, neutralizer press filtration desalination, decompression sloughs trichloroethane and DMF, precipitation temperature 50 C ~ 60 DEG C, material thickness after precipitation, adds 600L about 50 DEG C of hot water wherein or applies mechanically water;

D, precipitation liquid proceed to hydrolysis kettle, cool to 20 DEG C, with the pH value to 12 of sheet alkali regulator solution, maintain still temperature stirring reaction 5 hours, sampling detects, and when area ratio≤0.5% of trichloro-cane-6-ethyl ester, then with 30% hydrochloric acid, pH value is adjusted to 6.8 ~ 7.0, adjustment puts in place to pester and mixes 10 minutes repetition measurement PH=6.8 ~ 7.0, namely obtains Sucralose crude product liquid.Through extract assorted, extract, dry to obtain Sucralose sterling 82.3KG.

Claims

1. a production method for Sucralose, through step of esterification generation in early stage sucrose 6-ethyl ester, is characterized in that comprising the following steps:

A, chlorinating step: the sucrose 6-ethyl ester generated through esterification, be added drop-wise at 0 DEG C ~ 5 DEG C the Vilsmeier reagent prepared and carry out chlorination reaction, after being added dropwise to complete, half an hour is stirred under normal temperature, be warmed up to 50 degree, be incubated 1 hour, be then incubated 1 hour respectively at 75 degree, 85 degree, 95 degree, 105 degree, finally at 110 degree of insulation 2-3 hour;

B, neutralization procedure: chlorinating step terminates, cool to 10 degree by chlorination reaction liquid, adds ammonia neutralization to pH value 9.5, then stir half hour, then with hydrochloric acid, pH value is adjusted to 7-7.5, and neutral temperature controls at≤20 DEG C;

C, precipitation step: after the neutralizer press filtration desalination that neutralization procedure obtains, proceed to precipitation still, decompression sloughs trichloroethane and DMF, precipitation temperature 50 C ~ 60 DEG C;

D, hydrolysing step: the precipitation liquid that precipitation step obtains proceeds to hydrolysis kettle, cool to 20 DEG C, with the pH value to 12 of alkali regulator solution, maintain still temperature stirring reaction 5 hours, sampling detects, when area ratio≤0.5% of trichloro-cane-6-ethyl ester, with hydrochloric acid, pH value is adjusted to 6.8 ~ 7.0 again, stir 10 minutes after adjustment puts in place, repetition measurement PH=6.8 ~ 7.0, namely obtain Sucralose crude product liquid.