Recrystallization method of sucrose-6-acetate and applications thereof

An acetate and recrystallization technology, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve problems such as increased environmental pressure, increased side reactions, and complicated treatment processes, and achieve the reduction of chlorinated reagents consumption, overcoming carbonization, and simple operation

Active Publication Date: 2017-07-14
ZHEJIANG NHU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current sucralose synthesis process generally does not crystallize sucrose-6-acetate, but directly adds the esterification reaction mixture solution to the next step reaction. Such a process will not only bring the by-products of the esterification step into the next step. One-step process increases side reactions, consumes more chlorination reagents, and produces some impurities that cannot be reused, resulting in carbonization of sugar in the chlorination step, increasing costs and increasing environmental pressure
[0004] CN103554196A discloses that adding petroleum ether under the condition of ultrasonic flow at a specific temperature can make the crystallization of sucrose-6-acetate relatively regular, and then use ethyl acetate to recrystallize sucrose-6-acetate, but sucrose-6-acetate The solubility of acetate in ethyl acetate is very small, and the pretreatment process is relatively complicated, which is not conducive to industrial production
[0005] CN103936799A discloses removing solvent water and dimethylformamide at the end of esterification reaction, adding a mixed solvent of acetone and methanol to carry out the recrystallization of sucrose-6-acetate, the method needs DMF to be evaporated to dryness before crystallization, and there is no Given the purity of the final product and the benefits of crystallization
[0006] There are not many other reports on the recrystallization technology of sucrose-6-acetate, and most of these recrystallization methods will introduce more toxic solvents, or cause solvent residues, which will affect the yield of the next chlorination process or trichloride. Sugar product quality

Method used

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  • Recrystallization method of sucrose-6-acetate and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 500g of sucrose and 2L of DMF solution into a 5L four-neck flask, install a stirring paddle, a thermometer and a condenser tube with a water separator. Heat to 60°C, wait for the sucrose to dissolve, add 375g of dibutyltin oxide and 1.5L of cyclohexane, heat to 90-95°C to reflux and separate water, after 5 hours of reaction, cool to 5°C, add 157.5g of acetic anhydride dropwise After half an hour, it was warmed up to room temperature, continued to stir for 4 hours, added 150mL of water, stirred for half an hour and then distilled under reduced pressure to remove water, cyclohexane and most of the DMF to obtain 700g of the reaction mixture, which was analyzed by high performance liquid phase, the result See Table 1.

[0029] Weigh 20 g of the above mixture, heat it to 45°C, add 10 mL of acetonitrile and 5 mL of diethyl ether while stirring at a speed of 450 rpm, and after the concentrate is completely dissolved, cool down slowly and a white precipitate appears. Stand...

Embodiment 2

[0031] Add 500g of sucrose and 2L of DMF solution into a 5L four-neck flask, install a stirring paddle, a thermometer, and a condenser tube with a water separator. Heat to 60°C, wait for the sucrose to dissolve, add 375g of dibutyltin oxide and 1.5L of cyclohexane, heat to 90-95°C to reflux and separate water, after 5 hours of reaction, cool to 5°C, add 157.5g of acetic anhydride dropwise After half an hour, it was warmed up to room temperature, continued to stir for 4h, added 150mL of water, stirred for half an hour and then distilled under reduced pressure to remove water, cyclohexane and most of the DMF to obtain 700g of the reaction mixture.

[0032] Weigh 50 g of the above mixture, heat it to 40°C, add 15 mL of propionitrile and 7.5 mL of ether while stirring at a speed of 500 rpm, and after the concentrate is completely dissolved, cool down slowly and a white precipitate appears. Stand at -5°C to 0°C for 2h, filter, and dry to obtain 35.29g of white powdery crystals. Th...

Embodiment 3

[0034] Add 500g of sucrose and 2L of DMF solution into a 5L four-neck flask, install a stirring paddle, a thermometer, and a condenser tube with a water separator. Heat to 60°C, wait for the sucrose to dissolve, add 375g of dibutyltin oxide and 1.5L of cyclohexane, heat to 90-95°C to reflux and separate water, after 5 hours of reaction, cool to 5°C, add 157.5g of acetic anhydride dropwise After half an hour, it was warmed up to room temperature, continued to stir for 4h, added 150mL of water, stirred for half an hour and then distilled under reduced pressure to remove water, cyclohexane and most of the DMF to obtain 700g of the reaction mixture.

[0035] Weigh 50g of the above mixture, heat it to 45°C, add 40mL of butyronitrile and 8mL of diethyl ether while stirring at a speed of 500 rpm, and after the concentrate is completely dissolved, slowly cool down and white precipitate appears. Stand still at -5°C to 0°C for 1.5h, filter, and dry to obtain 35.66g of white powdery crys...

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Abstract

The invention discloses a recrystallization method of sucrose-6-acetate, and applications thereof. The recrystallization method comprise following steps: a solvent is added into a sucrose-6-acetate mixture obtained via sucrose esterification; and stirring, dissolving, filtering, and drying are carried out so as to obtain sucrose-6-acetate, wherein the solvent is a mixture of a nitrile solvent and an ether solvent. The recrystallization method is capable of increasing sucrose-6-acetate purity, and reducing adverse influences on subsequent chlorination.

Description

technical field [0001] The invention relates to a sucralose production process, in particular to a sucrose-6-acetate recrystallization method and application thereof. Background technique [0002] Sucralose (chemically named 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose) is the only functional new sweetener based on sucrose, sweet The concentration can reach 600 times that of sucrose, and it has the characteristics of no energy, high sweetness, pure sweetness, high safety, anti-caries, and wide application range. Sucrose-6-acetate is the product of the first step of esterification reaction in the synthesis process of sucralose. It is a very important intermediate, and its quality is directly related to the chlorination yield in the next step, thus affecting the trichloro Quality and yield of sucrose products. [0003] The current sucralose synthesis process generally does not crystallize sucrose-6-acetate, but directly adds the esterification reaction mixture solution t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H5/02C07H1/06C07H1/00
CPCC07H1/00C07H1/06C07H5/02C07H13/06
Inventor 盛毓张永辉石清爱郑思敏周有桂
Owner ZHEJIANG NHU CO LTD
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