Method for removing acetic acid in sucrose-6-acetate solution and application thereof

A technology of acetate and sucrose, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of high price, large quantity, and high manufacturing cost of sucralose, and achieve good fluidity and continuous operation simple effect

Active Publication Date: 2018-10-19
SHANDONG NHU FINE CHEM SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the functionalized DSDA is easy to precipitate in the system, the whole treatment process must be operated at about 60°C, otherwise, it will cause too much loss of expensive organotin, which will lead to high manufacturing cost of sucralose ; At the same time, the treatment process will eventually produce a large amount of sodium acetate dilute salt wastewater, which will bring greater pressure to environmental protection

Method used

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  • Method for removing acetic acid in sucrose-6-acetate solution and application thereof
  • Method for removing acetic acid in sucrose-6-acetate solution and application thereof
  • Method for removing acetic acid in sucrose-6-acetate solution and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: Using a packed tower to remove acetic acid, the packing is BX packing

[0046] Turn on the electric heating cable to preheat the packed tower. When the temperature of the heating cable rises to about 75°C, turn on the vacuum system to maintain the absolute pressure at the top of the tower at 4.5kPa, and pass 65°C DMF steam into the packed tower. The prepared sucrose-6-acetate DMF solution (the composition of the raw material liquid is shown in the table below) is passed into the position near the top of the side wall, and the top and bottom of the tower are continuously collected from the top and bottom of the tower (or called tower Kettle) liquid, keep the feed ratio of DMF vapor to sucrose-6-acetate DMF solution at 3:1 (by weight) and flow rates of 3Kg / h and 1Kg / h respectively; after 8 hours of continuous operation, it corresponds to each kilogram As far as the feed liquid of the sucrose-6-acetate DMF solution is concerned, 0.95 kg of column bottom solution is...

Embodiment 2

[0051] Example 2: Using a packed tower to remove acetic acid, the packing is BX packing

[0052] Turn on the electric heating cable to preheat the packed tower. When the temperature of the heating cable rises to about 85°C, turn on the vacuum system to maintain the absolute pressure at the top of the tower at 5.0kPa, and pass 75°C DMF steam into the packed tower. The prepared sucrose-6-acetate DMF solution (the composition of the raw material liquid is shown in the table below) is passed through the side wall near the top, and the top and bottom liquids are continuously collected from the top and bottom of the tower. DMF vapor and The feed flow rate of the sucrose-6-acetate DMF solution is 4Kg / h and 1Kg / h respectively; after 6.5 hours of continuous operation, 1.2Kg per kilogram of sucrose-6-acetate DMF solution is produced. Bottom solution. The components of the top and bottom liquids were measured separately.

[0053] The composition of the raw material liquid, the top of the to...

Embodiment 3

[0057] Example 3: Use a packed tower to remove acetic acid, the packing is Raschig ring

[0058] Turn on the electric heating cable to preheat the packed tower. When the temperature of the heating cable rises to about 75°C, turn on the vacuum system to maintain the absolute pressure at the top of the tower at 4.5kPa, and pass 65°C DMF steam into the packed tower. The prepared sucrose-6-acetate DMF solution (the composition of the raw materials is shown in the table below) is passed through the side wall near the top, and the top and bottom liquids are continuously collected from the top and bottom of the tower to keep the DMF vapor and The feed flow rate of the sucrose-6-acetate DMF solution is 4Kg / h and 1Kg / h respectively; after 5.5 hours of continuous operation, 1.1Kg per kilogram of sucrose-6-acetate DMF solution is produced. Bottom solution. The components of the top and bottom liquids were measured separately.

[0059] The composition of the raw material liquid, the top of t...

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Abstract

The invention discloses a method for removing acetic acid in a sucrose-6-acetate solution and application thereof. The method comprises the following steps: under a certain residence time condition, in tower equipment for removing acetic acid, vapor formed by tertiary amide of certain temperature is in contact with the sucrose-6-acetate solution containing acetic acid in a continuous countercurrent manner, thereby achieving the purpose of removing the acetic acid from the sucrose-6-acetate solution. The method provided by the invention can be applied to the synthesis of sucrose-6-acetate and sucralose, has the advantages of simple process, high acetic acid removal rate, no damage to a sucrose-6-acetate product, continuity and the like, and is very suitable for industrial production.

Description

Technical field [0001] The invention relates to an improved method for synthesizing sucrose-6-acetate. The prepared sucrose-6-acetate can be used to prepare high-grade sweetener sucralose, which belongs to the field of fine chemicals. Background technique [0002] Sucralose (4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose, referred to as sucralose) is a high-strength food sweetener, The sweetness is 600 times that of sucrose, and it is safe, stable, and not absorbed by the body. It was successfully synthesized by Tate&Lyte in 1976 and successfully put into the market in 1988. It is currently approved for production and use in many countries around the world; among them, sucrose-6-acetate is the most important reaction material for the synthesis of sucralose: under heating conditions, sucrose- The sucralose intermediate can be prepared by the chlorination reaction of 6-acetate; the sucralose intermediate can then be saponified to finally prepare sucralose. [0003] At present, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H13/06
CPCC07H1/06C07H13/06
Inventor 周有桂杨征宇甄岳仁张雷杨应阔李瑞田杨运晗刘钢严荣伟
Owner SHANDONG NHU FINE CHEM SCI & TECH CO LTD
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