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Crystallization method for synthesizing sucrose-6-acetate from sucrose and ortho-acetate

A technology of orthoacetate and acetate, which is applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve problems such as difficult suction filtration and drying, complicated and cumbersome operation, poor crystal shape, etc., to achieve The effect of reducing the requirement of ambient temperature, simple operation steps and mild operating conditions

Active Publication Date: 2017-05-31
JK SUCRALOSE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Both the methods of Gong Fuchun and Li Can require at least two vacuum distillations and ultrasonic flow-controlled crystallization. The operation is complicated and cumbersome, and many instruments and drugs are required; The time is long, and the viscosity is too high during the crystallization operation, the fluidity is poor, and it is not easy to stir to affect the uniform growth and crystallization speed of the crystal; in addition, sucrose-6-acetate is very soluble in water, which will lead to serious loss of sucrose-6-acetate
It was found through experiments that the crystals obtained by Lin Furong's method were not in good shape, and only viscous sugar or lumps could be obtained, which were difficult to filter and dry

Method used

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  • Crystallization method for synthesizing sucrose-6-acetate from sucrose and ortho-acetate
  • Crystallization method for synthesizing sucrose-6-acetate from sucrose and ortho-acetate
  • Crystallization method for synthesizing sucrose-6-acetate from sucrose and ortho-acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Take 50 mL of the synthesis solution of sucrose-6-acetate synthesized according to the above method, add 25 mL of ethyl acetate, heat and rotary steam at 55 ° C, -0.1 Mpa for 30 min until the volume of the mixture is 20 mL.

[0048] Add 2mL of ethyl acetate at 30°C, add glacial acetic acid dropwise under continuous stirring until the pH value of the solution reaches 2.6, then add about 20mL of glacial acetic acid dropwise; stir for about 25min to form a large number of white crystals, and filter under reduced pressure to obtain sucrose-6-acetic acid 10.4 g of ester primary crystals.

[0049] Take the primary crystals and place them in a beaker, slowly add isopropanol, and keep stirring until the sucrose-6-acetate crystals are completely dissolved, then add about 0.1g of sucrose-6-acetate primary crystals to make the sucrose-6-acetate -Acetate was recrystallized and precipitated, stood still for 30 minutes, filtered out the sucrose-6-acetate crystals, washed the crystals...

Embodiment 2

[0061] Take 50 mL of the sucrose-6-acetate mixture synthesized according to the above method, add 25 mL of methanol, 50 ° C, -0.1 Mpa, and rotary steam for 30 min until the volume of the mixture is 18 mL.

[0062] Add 2 mL of ethyl acetate at 30°C, add glacial acetic acid dropwise under constant stirring until the pH value of the solution reaches 2.6, then add about 20 mL of glacial acetic acid dropwise; stir for about 25 minutes to form a large number of white crystals, crystallize completely after 30 minutes, and filter under reduced pressure to obtain sucrose - 10.7 g of primary crystallization of 6-acetate.

[0063] Put the primary crystals in a beaker, slowly add isopropanol, and keep stirring until the sucrose-6-acetate crystals are completely dissolved, then add about 0.2g of sucrose-6-acetate primary crystals in batches to make the sucrose-6-acetate 6-Acetate was recrystallized and precipitated, stood still for 30 minutes, filtered out the crystals, washed twice with 3...

Embodiment 3

[0065] Take 50 mL of the synthesis solution of sucrose-6-acetate synthesized according to the above method, add 25 mL of ethyl acetate, heat and rotary steam at 53 ° C, -0.09 Mpa for 30 min until the volume of the mixture is 19 mL.

[0066] Add 2mL of ethyl acetate at 30°C, add glacial acetic acid dropwise under continuous stirring until the pH value of the solution reaches 2.6, then add about 20mL of glacial acetic acid dropwise; stir for about 25min to form a large number of white crystals, and filter under reduced pressure to obtain sucrose-6-acetic acid 10.6g of ester primary crystallization.

[0067] Take the primary crystals and place them in a beaker, slowly add isopropanol, and keep stirring until the sucrose-6-acetate crystals are completely dissolved, then add about 0.2g of sucrose-6-acetate primary crystals to make the sucrose-6-acetate -Acetate recrystallization precipitated, stood still for 30min, filtered out sucrose-6-acetate crystals, then washed the crystals t...

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Abstract

The invention discloses a crystallization method for synthesizing sucrose-6-acetate from sucrose and ortho-acetate. The crystallization method comprises the following steps: putting an appropriate amount of a synthetic solution of the sucrose-6-acetate into a round-bottom flask, and adding a low-boiling organic solvent of which the volume is 0.4 to 0.5 time of that of the synthetic solution; carrying out rotary evaporation, and concentrating the volume of the synthetic solution, thus obtaining a concentrated solution of the sucrose-6-acetate; transferring the concentrated solution into a beaker, and cooling to room temperature; dropwise adding glacial acetic acid in the concentrated solution until the pH (Potential of Hydrogen) value is 2.5, continuously stirring for 25 to 35 minutes under 25 to 30 DEG C and at the speed of 100 r / min, and stopping stirring when much white crystalline precipitation is formed; standing for 30 minutes until complete crystallization of the white crystalline precipitation, and carrying out suction filtration, thus obtaining a primary crystallization product of the sucrose-6-acetate; putting a certain mass of the primary crystallization product in the beaker under the room temperature, forming a saturated solution by adding isopropanol of which the mass is 1.5 to 2.5 times of that of the primary crystallization product, then adding a small amount of the primary crystallization product until completely separating out the sucrose-6-acetate, and carrying out vacuum drying under 40 to 45 DEG C, thus obtaining the sucrose-6-acetate.

Description

technical field [0001] The invention relates to the crystallization field of sucrose-6-acetate in the field of food additives, in particular to a crystallization method for synthesizing sucrose-6-acetate from sucrose and orthoacetate. Background technique [0002] Sucralose, chemically named 4,1,6'-trichloro-4,1',6'-trideoxygalactose, is a new type of sweetener. After more than ten years of toxicity tests and biochemical performance tests, it has been proved that it is non-toxic, safe and reliable, does not participate in metabolism in the human body, and is not absorbed by the human body. It is an ideal sweet substitute for obesity, cardiovascular disease and diabetes patients. In its industrial preparation process, the intermediate sucrose-6-acetate is firstly obtained. [0003] Sucrose-6-acetate (sucrose 6'-acetate), the carbon-oxygen 6-membered ring connected to the ester group at the 6-position is a chair-shaped sucrose ester, and its molecular formula is C 14 h 24 o...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/06
CPCC07H1/06C07H13/06
Inventor 姚志湘文毅粟晖刘柳劳巾婷
Owner JK SUCRALOSE
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