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Method for continuously preparing sucrose-6-acetic ester

A technology of acetate and sucrose, which is applied in the field of preparing sucrose-6-acetate, can solve the problems of low utilization rate of equipment and achieve the effects of high utilization rate of equipment, simple and practical process, and high mass transfer efficiency

Inactive Publication Date: 2012-05-30
GUANGXI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the concentration of sucrose in the solution is generally 10-20%, a very large reaction equipment can only obtain a very small amount of product intermittently, and the utilization rate of the equipment is very low

Method used

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  • Method for continuously preparing sucrose-6-acetic ester
  • Method for continuously preparing sucrose-6-acetic ester
  • Method for continuously preparing sucrose-6-acetic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of a regular structure catalyst (see figure 1 ), mix the catalyst carrier, oxide, compounding agent, water and adhesive in parts by weight of 60: 20: 2: 15: 3 to form a certain plasticity mud:

[0033] The catalyst carrier is a mixture of one or more of diatomaceous earth, carboxymethyl cellulose, colloidal alumina and silica gel, preferably a mixture of one or two of diatomaceous earth and silica gel.

[0034] The oxide is TiO 2 , ZrO 2 , Fe 2 o 3 and Al 2 o 3 One or a mixture of several substances, preferably TiO 2 and Al 2 o 3 one or a mixture of both.

[0035] The compounding agent is a mixture of one or more substances in magnesium stearate, graphite, paraffin wax, talcum powder and EDTA, preferably one or two mixtures of magnesium stearate and graphite.

[0036] The adhesive is one or a mixture of polyvinyl alcohol, starch and water glass; preferably one or two mixtures of polyvinyl alcohol and water glass.

[0037] A hollow dodecagonal temp...

Embodiment 2

[0042] A kind of preparation of sucrose-6-acetate (see figure 2 ), add 10kg of sucrose, 35L of N,N-dimethylformamide (DMF), and 15L of ethyl acetate into the batching tank, heat up and stir evenly, and control the temperature at 80°C. Use a metering pump to continuously pump into the regular structure reactor at a flow rate of 16L / h. The total volume of the reactor is 32L, and the material flow rate per unit time and unit area is 8L / h·M 2 The calculated total surface area of ​​the catalyst is about 2M 2 , The residence time of the material in the reactor is about 2.0h, and the outlet sampling analysis shows that the yield of sucrose-6-acetate is 69.6%.

Embodiment 3

[0044] A kind of preparation of sucrose-6-acetate (see figure 2 ), add 10kg of sucrose, 35L of DMF, and 15L of ethyl acetate into the batching tank, heat up and stir evenly, and control the temperature at 80°C. Use a metering pump to continuously pour into the structured structure reactor at a flow rate of 13L / h. The total volume of the reactor is 32L, and the material flow rate per unit time and unit area is 6.5L / h·M 2 The calculated total surface area of ​​the catalyst is about 2M 2 , The residence time of the material in the reactor is about 2.5h, and the outlet sampling analysis shows that the yield of sucrose-6-acetate is 77.4%.

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Abstract

The invention relates to a method for continuously preparing sucrose-6-acetic ester by utilizing a monolithic reactor. The method comprises the following steps of: A, preparing a monolithic catalyst, namely mixing a catalyst carrier, an oxide, an ingredient, water and an adhesive to form plastic mud, extruding and cutting to manufacture a framework material with the length of 0.5 to 1m, putting the framework material into an oven for drying, cooling, putting the cooled framework material into lanthanide-containing sulfuric acid solution for soaking, taking the soaked framework material out, naturally airing, and drying and roasting to prepare the monolithic catalyst; and B, preparing the sucrose-6-acetic ester, namely adding sucrose, dimethyl formamide (DMF) and ethyl acetate into a material-mixing tank, uniformly mixing, heating to the temperature of between 70 and 90 DEG C, and throwing the materials in the material-mixing tank into the monolithic reactor, which contains the monolithic catalyst prepared in the step A, wherein the effluent of the reactor is sucrose-6-acetic ester solution. In the method, batch production is improved into continuous production, the process is simple and practical, the equipment utilization rate is high and the production time is shortened.

Description

technical field [0001] The invention relates to a method for preparing sucrose-6-acetate, in particular to a method for continuously preparing sucrose-6-acetate using a regular structure reactor. Background technique [0002] Sucralose-6-acetate is an intermediate for the synthesis of sucralose. The production process for the synthesis of sucralose by the general single-base protection method is: sucrose→sucrose-6-acetate→sucralose-6-acetate→ Sucralose. [0003] There are many traditional methods for preparing sucrose-6-acetate, such as: [0004] 1. The sucrose reported in U.S. Patent US 4,889,928, US 5,449,772, European Patent EP 0515145, and Chinese Patent CN 1526716A is dissolved in N, N-dimethylformamide solvent, under acidic conditions, and the original Trimethyl acetate reaction, preparation of sucrose-6-acetate through hydrolysis and transfer; [0005] 2. The sucrose reported in Chinese patent CN 1528772A, US patent US 5,023,329, and US 4,950,746 is dissolved in N,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06B01J31/26C07H1/00B01J35/02B01J27/053B01J35/00
Inventor 周小柳
Owner GUANGXI UNIVERSITY OF TECHNOLOGY