A kind of preparation method of dibutyltin oxide

A technology of dibutyltin oxide and dibutyltin dichloride, which is applied in the field of preparation of dibutyltin oxide, can solve problems such as coating defects with poor catalytic effect, inability to apply electrophoretic paint, and large product particles

Active Publication Date: 2019-02-22
启东市强强贸易有限公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production and preparation method of dibutyl tin oxide is prepared by directly dropping dibutyl tin dichloride into lye after liquefaction. The produced product has large particles, uneven particles, and many impurities in the product. It is widely used in the coating industry. It is prone to disadvantages such as poor catalytic effect and obvious coating defects, which make it unable to be used in electrophoretic paint
[0004] Tetrabutyltin is a key intermediate in the production of dibutyltin oxide. Generally, ether is used as a solvent to synthesize tetrabutyltin by the traditional Grignard method. This method has flammable and explosive hazards and certain operational difficulties. Replacing ether with a high boiling point solvent can To achieve a better effect; control the reaction ratio of tetrabutyltin and tin tetrachloride and the appropriate reaction conditions, can synthesize a product with a main content of dibutyltin dichloride exceeding 90%, and the product is distilled to remove butyl trichloride After tin chloride, dibutyl tin dichloride boutique with a main content greater than 98.5% can be obtained; dibutyl tin dichloride reacts with alkali to produce dibutyl tin oxide, because the dibutyl tin oxide produced by the reaction has Hydrophobic, and there are side reactions in the reaction process. In the traditional process, an inert organic solvent is used to help complete the reaction, but the product will be mixed with a small amount of solvent after washing, which will affect the product quality.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of dibutyltin oxide
  • A kind of preparation method of dibutyltin oxide

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] The invention provides a kind of preparation method of dibutyl tin oxide, at least comprise the following steps:

[0033](1) Synthesis of tetrabutyltin: add magnesium powder, composite solvent and n-butyl chloride to the reactor, heat up to reflux for 0.5-1h, slowly add the mixed solution of n-butyl chloride and tin tetrachloride, and reflux for 3h , cooled to room temperature, adding an aqueous hydrochloric acid solution with a mass fraction of 10%, and stirring evenly, separating the organic layer, and concentrating the organic layer under reduced pressure to obtain a colorless liquid tetrabutyltin;

[0034] (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 60-70°C for 1h, raise the temperature to 135-138°C, keep warm for 3-4h, cool to room t...

Embodiment 1

[0070] The preparation method of dibutyl tin oxide comprises the following steps:

[0071] (1) Synthesis of tetrabutyltin: add magnesium powder, composite solvent and n-butyl chloride in 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;

[0072] (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, filter, separa...

Embodiment 2

[0084] The preparation method of dibutyl tin oxide comprises the following steps:

[0085] (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;

[0086] (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, filter, separa...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a preparation method of dibutyltin oxide. The dibutyltin oxide is at least prepared by (1), synthesis of tetrabutyl tin; (2), synthesis of dibutyl stannous chloride; (3), synthesis of dibutyltin oxide, wherein catalyst used in step (2) is composite of modified nano-crystalline cellulose and aluminium chloride. The dibutyltin oxide is applied to electric paint and electrophoretic paint fields.

Description

technical field [0001] The invention relates to a method for preparing an organotin substance, in particular, the invention relates to a method for preparing dibutyltin oxide. 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 Grignard method , but it must be recovered according to...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22C09D5/44
CPCC07F7/2224C09D5/448
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap