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Method of recycling and reusing of dibutyltin oxide in process of cane sugars manufacturing cane suger-6-ethyl ester

A technology of dibutyltin oxide and sucrose, which is applied in the preparation of sugar derivatives, chemical instruments and methods, esterified saccharides, etc., can solve the problems of hidden danger, flammability, high toxicity, inconvenience in production, etc., and reduce production costs. , the effect of eliminating safety hazards

Inactive Publication Date: 2013-06-05
LIYANG WEIXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the reaction between dibutyltin oxide and sucrose is a reflux water extraction process, dibutyl tin oxide containing water will affect the reaction time and reaction speed, so it is generally believed that if the added dibutyl tin oxide contains water, the reaction will not be easy Realize, therefore existing production technology all needs to be dried through the wet dibutyl tin oxide that obtains in the recycling method of dibutyl tin oxide, and dibutyl tin oxide is a kind of white powder, insoluble in water, And it is flammable and highly toxic, making it very difficult to dehydrate and dry, causing great inconvenience to production, and there are safety hazards in the dehydration and drying process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0023] (1) Preparation of sucrose-6-ethyl ester from sucrose

[0024] Weigh 72g of sucrose, 58g of dibutyltin oxide (dry) into a flask, add 280ml of organic solvent dimethylformamide, 120ml of cyclohexane, heat up to 85°C and start to reflux, keep warm at 87°C-90°C and collect water for 6 hour, lower the temperature to 0°C, add 23ml of acetic anhydride dropwise, and stir for 1 hour; add 15ml of water, and stir for 1 hour; add 250ml of cyclohexane to extract dibutyltin oxide, and the upper layer is cyclohexane containing dibutyltin oxide solution, and the lower layer was concentrated to remove water and dimethylformamide to obtain sucrose-6-ethyl ester (purity 87.77%).

[0025] (2) Recovery of cyclohexane solution containing dibutyltin oxide

[0026] (a) Warm up 102.55g of sodium hydroxide solution with a mass concentration of 10% to 90°C-95°C, heat and stir at a stirring speed of 60-70rpm, and extract the cyclohexane solution containing dibutyltin oxide obtained from the abov...

Embodiment 1

[0030] Weigh 72g of sucrose, put 65g of dibutyltin oxide (moisture content 10%) recovered by the method of Preparation Example 1 into a flask, add 280ml of organic solvent dimethylformamide, 120ml of cyclohexane, and heat up to 85°C Start to reflux, keep warm at 87°C-90°C for reflux to collect water for 6 hours, cool down to 0°C, add 23ml of acetic anhydride dropwise, stir for 1 hour; add 15ml of water, stir for 1 hour; add 250ml of cyclohexane to extract dibutyltin oxide,

[0031] The upper layer is a cyclohexane solution containing dibutyltin oxide, and the lower layer is concentrated to remove water and dimethylformamide to obtain sucrose-6-ethyl ester (purity: 86.85%).

Embodiment 2

[0033] Weigh 180kg of sucrose, put 160kg of dibutyltin oxide (moisture content 10%) recovered by the method of Preparation Example 1 into a flask, add 500L of organic solvent dimethylformamide, heat up to 300L of cyclohexane, and start at 83°C Reflux, keep warm at 87°C-90°C for reflux water collection for 12 hours, cool down to 0°C, add 57.5L of acetic anhydride dropwise, stir for 1 hour; add 37.5L of water, stir for 1 hour; add 500L of cyclohexane to extract dibutyltin oxide , the upper layer is a cyclohexane solution containing dibutyltin oxide, and the lower layer is concentrated to remove water and dimethylformamide to obtain sucrose-6-ethyl ester (purity 88.06%).

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PUM

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Abstract

The invention relates to a method of recycling and reusing of dibutyltin oxide in the process of cane sugars manufacturing cane suger-6-ethyl ester. The method of recycling and reusing of the dibutyltin oxide in the process of the cane sugars manufacturing the cane suger-6-ethyl ester comprises the following steps: (1), carrying out the cane sugars manufacturing the cane suger-6-ethyl ester; (2), recycling cyclochexane liquor which contains the dibutyltin oxide; (3), using the recycled and obtained dibutyltin oxide with a moisture percentage of 10%-20% for the step (1) of manufacturing the cane suger-6-ethyl ester. The method of recycling and reusing of the dibutyltin oxide in the process of the cane sugars manufacturing the cane suger-6-ethyl ester is concise, operation is easy, and the obtained dibutyltin oxide which contains water can be directly used for manufacturing the cane suger-6-ethyl ester again. A step of drying the dibutyltin oxide can be saved. Under conditions of not affecting yields generally, production cost is reduced. Safe hidden dangers which exist in the process of drying and dewatering the dibutyltin oxide are completely prevented. The method of recycling and reusing of the dibutyltin oxide in process of the cane sugars manufacturing the cane suger-6-ethyl ester can be suitable for industrial production.

Description

technical field [0001] The invention relates to the field of synthesis of sucralose intermediates, in particular to a method for recovering and reusing dibutyltin oxide in the process of preparing sucrose-6-ethyl ester from sucrose. Background technique [0002] Sucralose is a kind of chlorinated sucrose. It is a new type of sweetener. Its sweetness is 600 times that of sucrose. It does not participate in human metabolism. It has high safety and strong ability to resist acid hydrolysis. Many advantages make it a market Preferred product. Sucralose esterification reaction is currently mature with triethyl orthoacetate esterification method, dibutyltin oxidation method and acetic anhydride esterification method, among which some raw materials and organic solvents can be recovered by dibutyltin oxide plus acetic anhydride esterification method Reuse, and the recovery rate is very high, greatly reducing the cost. Because the reaction between dibutyltin oxide and sucrose is a r...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/00C07F7/22
Inventor 李挺山丁红辉蒋朝明
Owner LIYANG WEIXIN CHEM
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