Preparation method of sucrose-6-ester

A technology of sucrose and tin esters, which is applied in the field of preparation of sucrose-6-esters, achieving the effects of strong selectivity, improved conversion degree, and low energy consumption

Pending Publication Date: 2021-01-12
ANHUI JINGHE IND
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Atomization drying technology is a process that is completed in a short period of time. A technical problem in the esterification dehydration reaction is how to quickly take away the generated water to avoid the reverse reaction and reduce the occurrence of side reactions.

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  • Preparation method of sucrose-6-ester

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preparation example Construction

[0053] The application provides a preparation method of sucrose-6-ester, the preparation method comprising: the step of preparing a reaction solution: heating and dissolving sucrose and an organotin compound in a polar aprotic solvent, and adding a nonpolar solution thereto, The reaction solution is obtained; the atomization step: the reaction solution is atomized to form small droplets; the dehydration step: the small droplets are fully mixed and contacted with the gasified dehydration medium, so that the small droplets undergo a dehydration reaction, thereby generating an organic compound containing sucrose. An intermediate mixture of small droplets of tin ester; separation step: separating the intermediate mixture to obtain a sucrose organotin ester solution and a dehydrated gas-liquid mixture; circulation step: reclaiming and recycling the sucrose organotin ester solution obtained in the separation step to Atomization step and dehydration step several times; and esterificat...

Embodiment 1

[0097] Dissolve 1,000 grams of sucrose and 2,000 grams of 1,3-diacetoxy-1,1,3,3-tetra-(butyl)distannoxane in 10L of polar aprotic solvent DMF, add 1L later Cyclohexane, a non-polar solvent, forms a reaction solution of sucrose and organotin compounds.

[0098] The specific process parameters of this embodiment are as follows: the atomization dehydration reactor is a low-temperature vacuum spray dryer, model: JOYN-1000T; feed liquid injection volume: 10mL / min; atomization nozzle diameter: 0.5mm; reaction solution at 80°C Bottom feeding; vaporizer nitrogen gas injection volume: 2000mL / min; temperature 120°C; system pressure in the atomization dehydration reactor 50KPa.

[0099] After a reaction, the solution received by the liquid outlet is light amber, which is the sucrose organotin ester solution, and a part of the solution received is subjected to a secondary atomization step and a dehydration step, that is, a secondary esterification reaction; the other part Acylation exper...

Embodiment 2

[0104] Dissolve 1,000 grams of sucrose and 2,000 grams of 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl) distannoxane in 10 L of polar aprotic solvent DMF, add 1 L later Cyclohexane, a non-polar solvent, forms a reaction solution of sucrose and organotin compounds.

[0105] The specific process parameters of this embodiment are as follows: the atomization dehydration reactor is a low-temperature vacuum spray dryer, model: JOYN-1000T; injection volume: 10mL / min; atomization nozzle diameter: 0.5mm; The gas injection volume of the vaporizer after cyclohexane gasification is 2000mL / min; the temperature is 90°C; the system pressure in the atomization dehydration reactor is 50KPa.

[0106] Atomization dehydration is done and follow-up acylation treatment is identical with embodiment 1, and the sucrose-6-acetate solution that obtains is analyzed by HPLC, and analysis result (in parentheses is normalization result) is as follows:

[0107] The HPLC analysis result of the sucrose-6-acetate ...

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Abstract

The invention provides a preparation method of sucrose 6 ester. The preparation method comprises the following steps: preparing a reaction solution of sucrose and an organic tin compound; atomizing the reaction solution to form small liquid drops; fully mixing and contacting the droplets with a gasified dehydration medium, and carrying out dehydration reaction on the droplets so as to generate anintermediate mixture containing the sucrose organic tin ester droplets; separating the intermediate mixture to obtain a sucrose organic tin ester solution and a dehydrated gas-liquid mixture; recovering the sucrose organic tin ester solution obtained in the separation step and circulating the sucrose organic tin ester solution to the atomization step and the dehydration step for multiple times; and carrying out acylation reaction on the sucrose organic tin ester solution and organic anhydride to generate sucrose 6 ester. According to the method, rapid and efficient dehydration of the esterification reaction can be realized in an extremely short time, the sucrose organic tin ester intermediate is efficiently prepared, decomposition of carbohydrates and side reactions in the system are reduced to a great extent, the energy consumption is low, the product yield is high, the selectivity is high, and the sucrose reaction degree is more thorough.

Description

technical field [0001] The invention belongs to the technical field of chemical manufacturing, and in particular relates to a preparation method of sucrose-6-ester. Background technique [0002] Sucrose-6-ester is an important chemical product and intermediate, such as sucrose-6-acetate is an important intermediate for the synthesis of sucralose (Wu Hongying, School of Chemical Engineering and Biological Engineering, Zhejiang University, Wu Hongying, etc. Sweetener The latest progress in the synthesis of sucralose[J].Chemical Progress, 2016,35(1):227-238.), many sucrose-6-fatty acid esters are important food additives and chemicals. [0003] At present, the industry usually adopts the single-group protection method to synthesize sucrose-6-ester. The synthesis process is generally to dissolve the organotin compound and sucrose in a polar solvent, and azeotropically dehydrate through a non-polar solvent (Chinese patent CN1210286) or a single The polar solvent is directly dist...

Claims

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Application Information

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IPC IPC(8): C07H13/04C07H13/02C07H1/00
CPCC07H13/04C07H13/02C07H1/00B01J19/002B01J19/26B01J2204/002B01J2219/00245
Inventor 姜维强夏家信张正颂杨志健陈永乐
Owner ANHUI JINGHE IND
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