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Synthesis of trichloio-sugar

A technology of sucralose and synthesis process, which is applied in the direction of sugar derivatives, sugar derivatives, chemical instruments and methods, etc. It can solve the problems of short life, easy deactivation, poor catalyst stability, etc., and achieve low production cost and high catalytic activity. High, simple process effect

Inactive Publication Date: 2007-09-05
淄博联技甜味剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are disadvantages such as poor catalyst stability, short service life, and easy deactivation.

Method used

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  • Synthesis of trichloio-sugar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] SO 4 2- / TiO 2 / C 4+ Catalyst preparation

[0021] Add 20g TiCl to a 1000ml round bottom flask 4 Hydrolyze with dilute ammonia water until the solution is alkaline, and obtain white metatitanic acid precipitate. After standing for 24 hours, separate and remove the supernatant, wash the precipitate until there is no chloride ion, dry it at 110°C, grind it into powder, and pass through a 120-mesh sieve to obtain white powder TiO 2 . Dissolve cerium sulfate in 500mmol / L sulfuric acid solution to form a 1mol / L (molar concentration of cerium) solution, and sieve the white powder TiO 2 Soak in it for 14h, filter with suction, dry the solid in an oven at 110°C, and roast in a muffle furnace to obtain about 25g of rare earth solid superacid catalyst SO 4 2- / TiO 2 / C 4+ .

Embodiment 2

[0023] For the synthesis of sucrose-6-acetate, the molar ratio of sucrose to acetic anhydride is 1:0.9; the catalyst is 2% of the weight of sucrose.

[0024] Add 50g (0.146mol) sucrose, 350g N,N-dimethylformamide, entrainer cyclohexane 100g, acetic anhydride 13.4g in the 1000ml three-necked flask equipped with magnetic stirrer, water separator, reflux condenser (0.131mol), 1g catalyst SO 4 2- / TiO 2 / C 4+, stirred and heated to 85°C for 5 hours, cooled to normal temperature, filtered to recover the catalyst, and recovered N,N-dimethylformamide under reduced pressure to obtain 62g of syrup, which contained 80.1% of sucrose-6-acetate as measured by HPLC , sucrose diacetate was 5.2%, and residual sucrose was 10.5%.

Embodiment 3

[0026] For the synthesis of sucrose-6-acetate, the molar ratio of sucrose to acetic anhydride is 1:1; the catalyst is 2% of the weight of sucrose.

[0027] Add 50g (0.146mol) sucrose, 350g N, N-dimethylformamide, entrainer cyclohexane 100g, acetic anhydride 14.9g in the 1000ml three-necked flask equipped with magnetic stirrer, water separator, reflux condenser (0.146mol), 1g catalyst SO 4 2- / TiO 2 / C 4+ , stirred and heated to 85°C for 5 hours, cooled to normal temperature, recovered the catalyst by filtration, and recovered N,N-dimethylformamide under reduced pressure to obtain 64g of syrup, which contained 84.1% of sucrose-6-acetate as measured by HPLC , sucrose diacetate was 6.2%, and residual sucrose was 4.1%.

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Abstract

A process for synthesizing trichlorosucrose from sucrose includes such steps as adding sucrose, azeotropic agnet, solid catalyst and acetic anhydride to the organic solvent of N-amide compound, reacting at 70-95 deg.C to generate sucrose-6-acetate, chorinating, and alcoholyzing.

Description

technical field [0001] The invention relates to a synthesis process of sweetener-sucralose. Background technique [0002] Sucralose, the chemical name is 4,1',6'-trichloro-4,1',6'trideoxygalactose, and its structural formula is: [0003] [0004] The sweetness of sucralose is pure, very similar to natural sucrose; the sweetness is 600-650 times that of natural sucrose; it does not participate in human metabolism and has no calories; it has good thermal stability and no measurable loss; its anti-acid hydrolysis stability is higher than 10 times sucrose; high safety, it is the most perfect and competitive non-nutritive, high-sweetness sweetener developed by humans so far. At present, it has been approved as a food sweetener by more than 20 countries. [0005] The synthesis of sucralose can be divided into sucrose route and raffinose route according to the synthetic raw materials. Synthesizing sucralose from raffinose has a short route and a simple process, but the source...

Claims

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Application Information

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IPC IPC(8): C07H5/02
Inventor 黄云芳崔国臣王讯
Owner 淄博联技甜味剂有限公司
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