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Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester

A dibutyltin oxide and treatment method technology, applied in the direction of chemical instruments and methods, esterified saccharides, tin organic compounds, etc., can solve problems such as dust interference, difficulty in vacuum dehydration, and existing safety, so as to avoid hazards and Potential safety hazards, suitable for industrial production, not easy to damage and lose effects

Active Publication Date: 2016-05-25
ZHEJIANG NHU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Existing production technology all adopts vacuum drying to the dibutyltin oxide containing water obtained in the dibutyltin oxide recycling method, because the existence of water has obvious negative impact on the preparation of sucrose-6-ester by organotin method
However, dibutyltin oxide is a white powder, flammable and highly toxic, which makes it very difficult to vacuum dehydrate. It is easy to cause dust interference during the transfer process, which is labor intensive and has potential safety hazards in the drying process.

Method used

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  • Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester
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  • Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Weigh 90g of sucrose, 72g of dibutyltin oxide into a 1000ml three-neck flask, add 550ml of N,N-dimethylformamide, 225ml of cyclohexane, heat up to reflux, keep warm at 83-85°C and reflux to separate water 3h. The temperature was lowered to 10°C and 29.63 g of acetic anhydride was added dropwise, and the reaction was stirred for 1.5 h.

[0034] (2) 50ml of water was added, and 300ml of cyclohexane was added to extract the organotin in the reaction solution. Separation, the upper layer is a cyclohexane solution containing DSDA, and the lower layer is extracted with 300ml*2 cyclohexane to extract the remaining organotin. Concentrate the lower layer at no more than 80°C to remove water, cyclohexane and most of DMF. After detection by high performance liquid chromatography, 1.2% of sucrose remains, and the yield of sucrose-6-ethyl ester is 89.7%.

[0035](3) Combine the cyclohexane extracts, concentrate under reduced pressure until the concentrate is 260 to 350 g, and ...

Embodiment 2

[0038] In step (4) of Example 1, dibutyltin oxide containing water was azeotropically dried with DMF-free cyclohexane with water. Repeat Example 1 to obtain hydrated dibutyltin oxide. The specific operation is as follows: add 225ml of cyclohexane, heat up to reflux, keep warm and reflux to separate water for 4 hours, and the obtained dibutyltin oxide cyclohexane liquid has a water content of about 2.28% (w / w) as determined by the Karl Fischer method.

Embodiment 3

[0040] The dibutyltin oxide cyclohexane solution obtained in Example 1 was used to prepare sucrose-6-ethyl ester, and the operating conditions were repeated in Example 1. The dibutyltin oxide cyclohexane solution obtained in this experiment was again prepared under the same conditions to prepare sucrose-6-ethyl ester. The relevant dibutyl tin oxide recovery that the experiment of dibutyl tin oxide recycling obtains like this, the yield of sucrose-6-ethyl ester and the data such as number of times of applying mechanically are summarized in the following table. The weight of dibutyltin oxide is obtained by subtracting the weight of cyclohexane from the weight of dibutyltin oxide cyclohexane.

[0041]

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Abstract

The invention discloses a treatment method of dibutyltin oxide and application of the treatment method to synthesis of cane sugar-6-ethyl ester. The treatment method comprises the steps of adding the water-containing dibutyltin oxide to nonpolar solvent containing DMF, and heating the mixture for azeotropic water removal, so that low-water-content dibutyltin oxide is obtained after the process is ended. The mass percentage of water in the low-water-content dibutyltin oxide is 0.6% and below. The treatment method is safe, easy to operate and good in dehydration effect, the dibutyltin oxide is not prone to damage and loss in the recycling process, the recycling rate is high, purity is high, the method can be directly applied to production of cane sugar-6-ethyl ester, meanwhile, harm and potential safety hazards caused to human bodies and the environment in the dibutyltin oxide shifting process are avoided, and the treatment method is quite suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for recovering and reusing dibutyltin oxide in a sucrose-6-ethyl ester reaction mixture. The sucrose-6-ethyl ester reaction mixture contains sucrose-6-ethyl ester, 1,3-diacyloxy- 1,1,3,3-Tetrabutyldistannoxane (DSDA), cyclohexane and DMF, recovered dibutyltin oxide for the preparation of sucrose-6-ethyl ester. Background technique [0002] Sucralose is a high-intensity sweetener used in many foods and beverages. It is obtained by replacing the 4, 1', 6' three hydroxyl groups in the sucrose molecule with three chlorine atoms. In the method of synthesizing sucralose from sucrose, the most mature method is to convert sucrose into sucrose-6-ester, such as sucrose-6-ethyl ester, and then convert it into sucralose through chlorination, deacylation and other processes , and finally the sucralose is purified and separated. Among the methods for synthesizing sucrose-6-ethyl ester, the most suitable for industrialization are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22C07H1/06C07H1/00C07H13/06
CPCC07F7/2224C07F7/2296C07H1/00C07H1/06C07H13/06
Inventor 王晓军车来宾王昌泽晏文武曹家明
Owner ZHEJIANG NHU CO LTD
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