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Method for extracting sucralose-6-ethyl ester from tar

A technology for sucralose and tar, which is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., to achieve the effects of simple and feasible process, cheap and easy-to-obtain raw materials, and cost reduction

Inactive Publication Date: 2019-05-21
刘静
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, strong alkaline sodium hydroxide cannot be used, because too strong alkalinity can quickly decompose sucralose-6-ethyl ester, and even decompose sucralose itself

Method used

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  • Method for extracting sucralose-6-ethyl ester from tar
  • Method for extracting sucralose-6-ethyl ester from tar
  • Method for extracting sucralose-6-ethyl ester from tar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] S1 gel breaking

[0065] Add 1005.00g tar (sucralose content 12.52g / L, sucralose-6-ethyl ester content 92.48g / L) into a 2000mL four-neck flask, start stirring, and slowly add 33.17g calcium hydroxide powder below room temperature ( Analytical pure), feed liquid pH=9.

[0066] After reacting for 12.5 hours, sampling analysis showed that the content of sucralose was 23.49g / L, and the content of sucralose-6-ethyl ester became 166.55g / L.

[0067] Continue to slowly add 19.78g of calcium hydroxide powder, the pH value of the feed liquid becomes 13, after stirring for 1 hour, add hydrochloric acid dropwise to adjust the pH value of the feed liquid to 7, sampling analysis shows that the content of sucralose is 12.71g / L, sucralose-6- The ethyl ester content became 8.61 g / L. Excessive pH caused the decomposition of sucralose-6-ethyl ester and the experiment failed.

Embodiment 2

[0069] S1 gel breaking

[0070] Add 1501.50g tar (sucralose content 21.04g / L, sucralose-6-ethyl ester content 101.64g / L) into a 2000mL four-neck flask, start stirring, and slowly add 50.50g calcium hydroxide powder below room temperature ( Analytical pure), pH=9, the material liquid is dark brown. After reacting for 24 hours, hydrochloric acid was added dropwise to adjust the pH value of the feed solution to 6.

[0071] Sampling and analysis showed that the content of sucralose was 30.23g / L, and the content of sucralose-6-ethyl ester was 153.89g / L.

[0072] S2 Hydrating Ester

[0073] Transfer the feed liquid after the gel breaking reaction into a 5000mL pear-shaped separatory funnel, add 800g tap water and 800g ethyl acetate, oscillate and let stand to separate layers.

[0074] The lower layer is the ethyl acetate layer, which is the heavy ester phase (ethyl acetate dissolves sugars and has a high density, so it is in the lower layer). The upper layer is the water layer, ...

Embodiment 3

[0086] S1 gel breaking

[0087] Add 1503.0g tar (sucralose content 17.69g / L, sucralose-6-ethyl ester content 109.70g / L) into a 2000mL four-necked flask, start stirring, and slowly add 56.78g ammonia water (analytical pure) below room temperature , pH=9, the feed liquid is dark brown. After reacting for 24 hours, hydrochloric acid was added dropwise to adjust the pH value of the feed solution to 7.

[0088] Sampling and analysis showed that the content of sucralose was 20.14g / L, and the content of sucralose-6-ethyl ester was 138.36g / L.

[0089] S2 Hydrating Ester

[0090] Transfer the material liquid after the gel breaking reaction of S1 into a 5000mL pear-shaped separatory funnel, add 1000g tap water and 1500g ethyl acetate, oscillate evenly and let stand to separate layers.

[0091] The lower layer is the ethyl acetate layer, which is the heavy ester phase (ethyl acetate dissolves sugars and has a relatively high density, so it is in the lower layer). The upper layer is t...

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Abstract

The invention discloses a method for extracting sucralose-6-ethyl ester from tar and belongs to the technical field of compound extraction. Sucralose-6-ethyl ester is extracted from tar through the steps of gel breaking, water replenishing and ester replenishing, aqueous phase extraction, water washing of a heavy ester phase, concentration, cooling, crystallization and the like, and a sucralose-6-ethyl ester solid crystal is directly obtained. The method is simple in process, can well meet actual production requirements, can effectively utilize tar, improves the overall yield of sucralose, reduces pollution control cost and difficulty, and has important economic benefits and environmental protection benefits.

Description

technical field [0001] The invention belongs to the technical field of compound extraction, in particular to a method for extracting sucralose-6-ethyl ester from tar. Background technique [0002] Sucralose (CAS No.: 56038-13-2) is a new type of sweetener with high sweetness (about 600 times that of sucrose), easily soluble in water, low in calories, high in safety, and almost No absorption and other advantages, the market prospect is very broad. At present, the method of industrially synthesizing sucralose is as follows: using sucrose as raw material, sucrose is subjected to esterification reaction to obtain sucrose-6-ethyl ester, and then chlorinated sucrose-6-ethyl ester to obtain sucralose-6-ethyl ester , and finally deesterify sucralose-6-ethyl ester to obtain sucralose. [0003] In the industrial production process of sucralose using the organotin method, the yield of sucralose-6-ethyl ester was estimated to be 66% after the chlorination step, while the yield of sucr...

Claims

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Application Information

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IPC IPC(8): C07H13/04C07H1/06
Inventor 刘静
Owner 刘静
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