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Preparation method of dibutyltin oxide catalyzed sucrose-6-acetate single solvent

A technology of dibutyltin oxide and acetate, applied in the preparation of sugar derivatives, chemical instruments and methods, esterification of saccharides, etc., can solve the problems of large resource consumption, complicated operation steps, etc., and achieve high yield , The operability is strong, the method is simple effect

Inactive Publication Date: 2017-08-04
林洪
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the cyclohexane phase to the catalyst available for the reaction, the operation steps are cumbersome and the resource consumption is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: Single-solvent preparation of sucrose-6-acetate catalyzed by dibutyltin oxide

[0031] In a 1L reactor with a vacuum fractionation device, 25.67 grams (0.075mol) of sucrose and 550 grams of DMF were added, followed by 21.66 grams (0.087mol) of dibutyltin oxide catalyst, and then 1 drop of acetic acid (0.020 ml, 0.003mol), heated up to 60~70℃ under vacuum, separated water with DMF azeotrope, gradually dissolved sucrose and catalyst, dissolved after half an hour, and obtained a clear condensation reaction solution after 3~4 hours. The condensation reaction solution was diluted with 22 g of cyclohexane, cooled to 2-3°C, and 9.22 g (0.090 mol) of acetic anhydride was added dropwise to react for 90 minutes, and then heated to room temperature for 1 hour to obtain a light yellow esterification reaction solution.

[0032] After the esterification reaction is over, start to extract the catalyst. Add 7ml of water to the esterification reaction solution, then add 150m...

Embodiment 2

[0034] Embodiment 2: the method for neutralizing dibutyltin oxide by heating and alkali washing

[0035] Add 30 ml of 10% sodium hydroxide aqueous solvent with a volume mass concentration to the cyclohexane extract phase obtained in Example 1, stir and heat to control the temperature of 55~65°C for alkali washing and neutralization, and keep it at 55~65°C for 20 Minutes, the lower alkaline water phase is separated, and the cyclohexane phase after neutralization contains recovered dibutyltin oxide and a small amount of diacetyldistannoxane, which is poured into the condensation reactor under heat to be used for the next batch of condensation reaction .

Embodiment 3

[0036] Example 3: Single-solvent preparation of recovered dibutyltin oxide catalyzed sucrose-6-acetate

[0037]In a 1L reactor with a vacuum fractionation device (pre-filled with cyclohexane solution containing recovered dibutyltin oxide and a trace of diacetyldistannoxane), 25.67 g (0.075 mol) of sucrose and 550 gram of DMF, distill cyclohexane under a slight vacuum first, then increase the vacuum degree, raise the temperature to 60~70°C, separate the water with DMF azeotropically, the sucrose and the catalyst gradually dissolve, and dissolve after half an hour, 3~ After 4 hours, a clear condensation reaction solution was obtained. The condensation reaction solution was diluted with 22 g of cyclohexane, cooled to 2-3°C, and 9.22 g (0.090 mol) of acetic anhydride was added dropwise to react for 90 minutes, and then heated to room temperature for 1 hour to obtain a light yellow esterification reaction solution. The catalyst in the esterification reaction solution was extracted...

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PUM

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Abstract

The invention relates to a preparation method of dibutyltin oxide catalyzed sucrose-6-acetate. The preparation method is characterized by including: using dibutyltin oxide as the catalyst and trace diacetyl distannoxane as the cosolvent to prepare the sucrose-6-acetate single solvent in a single DMF solvent, and using a simple heating, alkali washing and neutralizing method to recycle the dibutyltin oxide. The preparation method has the advantages that the method is high in sucrose-6-acetate yield, low in resource consumption and high in operability in industrial production, the prepared sucrose-6-acetate is good in quality, and the catalyst recycling method is simple.

Description

technical field [0001] The invention relates to a preparation method of sucrose-6-acetate. Background technique [0002] Sucralose is currently the only natural modified artificial sweetener derived from sucrose, which is 600 times sweeter than sucrose. Sucralose not only has high sweetness, but also has a pure taste. Its sweetness is similar to that of sucrose, and it is safe to eat. It has become the mainstream sweetener in the food industry and other industries, with a large market capacity. [0003] The current preparation methods of sucralose basically start from sucrose and obtain the final product through sucrose-6-acetate. The preparation of sucrose-6-acetate intermediate is a key process for the preparation of sucralose. [0004] In order to increase the yield of sucrose-6-acetate and catalyze the selective esterification of the 6-position hydroxyl of sucrose, the 6-position of sucrose must be activated first. [0005] Patents such as US5034551 have disclosed the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/04C07H1/00
CPCY02P20/584C07H13/04C07H1/00
Inventor 林洪
Owner 林洪
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