Novel method for separating and purifying sucralose-6-ethyl ester

A technology for purifying sucralose and sucralose, which is applied in the direction of chemical instruments and methods, esterified saccharides, sugar derivatives, etc., can solve problems such as increased production costs, incomplete extraction, and material loss, so as to reduce the cost of products Loss, increase of extraction rate, effect of reducing loss

Inactive Publication Date: 2010-05-19
ZHEJIANG UNIV OF TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Multiple extractions are required, the amount of organic solvent is large, and because the density of ethyl acetate or butyl acetate in the organic phase is similar to that of water, both the organic phase and the water phase are dark brown, and the separation is not obvious, which may easily lead to incomplete extraction or partial material loss , the extraction rate is not high, and the extraction rate is generally about 90%; and in the whole production process, there is a lot of ethyl acetate lost due to entrainment, which correspondingly increases the production cost, pollutes the environment, and seriously harms the operators. At the same time, the equipment occupies a large area, the operation can only be operated intermittently, the labor intensity of the workers is high, and the working environment is not friendly.
There is no report on the separation and purification of sucralose-6-ethyl ester using an annular gap centrifugal extractor

Method used

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  • Novel method for separating and purifying sucralose-6-ethyl ester
  • Novel method for separating and purifying sucralose-6-ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 100mL of the aqueous solution containing sucralose-6-ethyl ester and other by-products prepared by the above method, and use three Φ20 annular gap centrifugal extractors to form a series countercurrent extraction process (see the attached figure 1 ), the extraction solvent is 80mL of fresh ethyl acetate, the flow control of the aqueous solution is 2L / h, the operating flow ratio (organic phase / water phase) is controlled to be 0.8: 1, the rotating speed is 1800r / min, and the ethyl acetate extract is concentrated to dryness Obtain 42.5g content and be 52% syrup-like substance (containing 22.1g sucralose-6-ethyl ester), use 30mL of 1% diethyl ether (volume ratio) water crystallization to obtain sucralose 6-ethyl ester crude product, gained crude product with 35mL Recrystallized from a mixed solvent of ethyl acetate and water (ethyl acetate:water=1:0.5) with a content of more than 98% of sucralose-6-ethyl ester (the yield of separation and purification was 46.2%).

Embodiment 2

[0024] Take 100mL of the aqueous solution containing sucralose-6-ethyl ester and other by-products prepared by the above method, and use 4 sets of Φ20 ring-gap centrifugal extractors to form a series countercurrent extraction process. The extraction solvent is 150mL of fresh ethyl acetate. The flow control is 3L / h, the operating flow ratio (organic phase / water phase) is controlled to be 1.5: 1, and the rotating speed is 1800r / min, and the ethyl acetate extract is concentrated to dryness to obtain 43.1g content of 52.5% syrupy substance (containing 22.6g sucralose-6-ethyl ester), crystallized with 30mL of 2% diethyl ether (volume ratio) water to obtain the crude product of sucralose-6-ethyl ester, and the resulting crude product was recrystallized with a mixed solvent of 35mL ethyl acetate and water ( Ethyl acetate: water = 1:0.5) with a content of more than 98% of sucralose-6-ethyl ester (separation and purification yield of 49.2%).

Embodiment 3

[0026] Take 100 mL of the aqueous solution containing sucralose-6-ethyl ester and other by-products prepared by the above method, and use 3 sets of Φ20 annular gap centrifugal extractors to form a series countercurrent extraction process. The extraction solvent is 100 mL of fresh ethyl acetate, and the aqueous solution The flow control is 4L / h, the operating flow ratio (organic phase / water phase) is controlled to be 1: 1, and the rotating speed is 1800r / min, and the ethyl acetate extract is concentrated to dryness to obtain 42.8g content of 52.5% syrupy substance (containing 22.5g sucralose-6-ethyl ester), crystallized with 35mL of water containing 1% ether to obtain the crude product, and the resulting crude product was recrystallized with a mixed solvent of 30mL ethyl acetate and water (ethyl acetate: water = 1: 0.6) content More than 98% of sucralose-6-ethyl ester (separation and purification yield is 48.2%).

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Abstract

The invention discloses a novel method for separating and purifying sucralose-6-ethyl ester, which is realized in a way that: preparing a water solution from crude sucralose-6-ethyl ester obtained by chlorinating sucrose-6-ester; constituting a serial counter-current extraction process by utilizing a plurality of annular space type centrifugal extractors, and separating and extracting by using ethyl acetate or butyl acetate as the extraction solvent; condensing the extract to be dry; and crystallizing and recrystallizing to obtain the sucralose-6-ethyl ester crystal. The invention carries out the continuous extraction by using the annular space type centrifugal extractors, thereby greatly reducing the use amount of the organic solvent for extraction and also reducing the loss of the organic solvent and the environmental pollution. The extraction rate of the product is enhanced from 90% to 98%, thereby obviously reducing the product loss in the separation process. Meanwhile, the technique can obviously reduce the labor intensity of the operational workers and improve the working environment of the workers.

Description

(1) Technical field [0001] The invention relates to a new method for separating and purifying the key intermediate sucralose-6-ethyl ester of food sweetener sucralose. (2) Background technology [0002] Sucralose, chemical name: 4,1′,6′-trichloro-4,1′,6′-trideoxygalactose; English name: 4,1′,6′-trichloro-4,1′ , 6′-trideoxygalactosucrose; CAS accession number: 56038-13-2, molecular formula: C 12 h 19 Cl 3 o 8 , molecular weight 396.01. [0003] Molecular formula: [0004] [0005] Sucralose is a white powder product that is easily soluble in water (solubility 28.2g, 20°C). Its sweetness is 600 times that of sucrose, and its sweetness is pure. The sweetness characteristic curve almost overlaps with sucrose. Sucralose is a non-nutritive strong sweetener, which is hardly absorbed in the human body and has zero calorie value. Sucralose is stable in nature, and its crystalline product is also stable for 4 years under dry conditions at 20°C. In aqueous solution, within t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 陈志卫苏为科李坚军陈炯明张春雷吕斌
Owner ZHEJIANG UNIV OF TECH
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