Preparation method of dibutyltin oxide and its application in the synthesis of sucralose

A technology of dibutyltin oxide and dibutyltin dichloride, which is applied in the field of preparation of organic tin substances, can solve the problems of serious adsorption, side reactions, poor temperature and salt resistance, etc.

Active Publication Date: 2019-02-22
启东市强强贸易有限公司
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0005] Dibutyltin dichloride reacts with alkali to produce dibutyltin oxide. Since the dibutyltin oxide produced by the reaction is hydrophobic and there are side reactions in the reaction process, an inert organic solvent is used in the traditional process to help the reaction complete , but the product will be mixed with a small amount of solvent after washing, which will affect the product quality
[0006] In addition, in the prior art, surfactants are added to improve the side reactions produced during the reaction between dibutyltin dichloride and alkali, but the existing surfactants have problems such as serious adsorption, poor temperature and salt resistance, etc.
[0007] Therefore, the present invention provides a kind of preparation method of dibutyl tin oxide, improves the side reaction that produces in dibutyl tin dichloride and alkali reaction process by preparing suitable surfactant, overcomes the existence of adsorption, poor temperature resistance and salt resistance And other issues

Method used

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  • Preparation method of dibutyltin oxide and its application in the synthesis of sucralose

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preparation example Construction

[0036] The invention provides the preparation method of dibutyltin oxide, at least comprises the following steps:

[0037] (1) Synthesis of tetrabutyltin: add magnesium powder, composite solvent and n-butyl chloride to the reactor, heat up to reflux reaction for 0.5h, slowly add dropwise the mixed solution of n-butyl chloride and tin tetrachloride, reflux reaction for 3h, Cool to room temperature, add 10% hydrochloric acid aqueous solution, stir evenly, separate the organic layer, and concentrate the organic layer under reduced pressure to obtain a colorless liquid tetrabutyltin;

[0038] (2) Synthesis of dibutyltin dichloride: add tetrabutyltin and catalyst in the reactor in step (1), replace with nitrogen 3 times, slowly add tin tetrachloride dropwise, control the temperature in the reaction system to be less than 80°C, After the dropwise addition, keep warm at 65°C for 1h, raise the temperature to 136°C, keep warm for 3h, cool to room temperature, add 10% hydrochloric acid ...

Embodiment approach

[0055] In one embodiment, the Gemini cationic surfactant is prepared by reacting tertiary amines, concentrated hydrochloric acid and epichlorohydrin; the tertiary amines include dodecyldimethyl tertiary amine, dodecylphenylbutyl One or more of tertiary amines.

[0056] In one embodiment, the preparation method of described Gemini cationic surfactant comprises the following steps:

[0057] (1) Add tertiary amine and concentrated hydrochloric acid into the reactor in a molar ratio and slowly heat up to 60°C, keep the temperature for 5 hours, and cool to obtain tertiary amine hydrochloride;

[0058] (2) Add tertiary amine hydrochloride, tertiary amine, epichlorohydrin and n-propanol into the reactor, heat up to 65° C., keep the reaction for 8 hours, and concentrate under reduced pressure to obtain Gemini cationic surfactant.

[0059] In one embodiment, the molar ratio of the tertiary amine to the epichlorohydrin in the Gemini cationic surfactant is (1-1.3):1.

[0060] In one em...

Embodiment 1

[0079] The preparation method of dibutyl tin oxide at least comprises the following steps:

[0080] (1) Synthesis of tetrabutyltin: add magnesium powder, composite solvent and n-butyl chloride to the reactor, heat up to reflux reaction for 0.5h, slowly add dropwise the mixed solution of n-butyl chloride and tin tetrachloride, reflux reaction for 3h, Cool to room temperature, add 10% hydrochloric acid aqueous solution, stir evenly, separate the organic layer, and concentrate the organic layer under reduced pressure to obtain a colorless liquid tetrabutyltin;

[0081] (2) Synthesis of dibutyltin dichloride: add tetrabutyltin and catalyst in the reactor in step (1), replace with nitrogen 3 times, slowly add tin tetrachloride dropwise, control the temperature in the reaction system to be less than 80°C, After the dropwise addition, keep warm at 65°C for 1h, raise the temperature to 136°C, keep warm for 3h, cool to room temperature, add 10% hydrochloric acid aqueous solution, filte...

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Abstract

The invention provides a preparation method of dibutyltin oxide and application thereof to sucralose synthesis. The preparation method of the dibutyltin oxide comprises the following steps of (1) synthesizing tetrabutyl tin; (2) synthesizing dibutyltin dichloride; and (3) synthesizing dibutyltin oxide, wherein a surfactant in the step (3) is a Gemini cationic surfactant, and the dibutyltin oxide is applied to the field of sucralose synthesis.

Description

technical field [0001] The invention relates to a preparation method of organotin substances, in particular, the invention relates to a preparation method of dibutyltin oxide and its application in the synthesis of sucralose. Background technique [0002] At present, the methods for producing organotin at home and abroad mainly include the Grignard method, the Wutz method, the alkyl aluminum method and the direct iodine method. The Grignard method is mostly used in European and American countries. The alkyl aluminum method is also used in East Germany. The direct iodine method is widely used in Japan. The advantage of the Grignard method is that it can control the composition of the product at any time, but there are many steps, and the Grignard reaction is an exothermic reaction, and the boiling point of the solvent is very low, so the temperature and reaction speed must be carefully controlled to avoid explosions; although the iodine method has fewer steps than the Grigna...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22C07H5/02C07H1/00
CPCC07F7/2224C07H1/00C07H5/02
Inventor 杨学强张建根俞永峰黄海娟顾周全
Owner 启东市强强贸易有限公司
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