Preparation method of monobutyltin oxide

A technology of monobutyltin oxide and monobutyltin trichloride, which is applied in the field of preparation of monobutyltin oxide, and can solve problems affecting the purity and production efficiency of monobutyltin oxide products

Active Publication Date: 2017-07-25
启东市强强贸易有限公司
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  • Abstract
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Problems solved by technology

[0004] At present, the synthesis method of monobutyl tin oxide is usually to separate monobutyl tin trichloride and dibutyl tin dichloride according to the difference of boiling point after tetrabutyl tin and tin tetrachloride are reacted, under alkaline conditions The monobutyltin trichloride aqueous solution is converted into monobutyltin oxide product by following steps, and then washed with water, centrifuged, and dried to produce, the monobutyltin oxide prepared by this method sticks during the production process, which affects the monobutyltin oxide product. Product purity and production efficiency of tin oxide

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  • Preparation method of monobutyltin oxide

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[0029] The invention provides a kind of preparation method of monobutyl tin oxide, comprises the following steps:

[0030] (1) Add tetrabutyltin into the reactor, stir evenly, slowly add tin tetrachloride dropwise, after the dropwise addition, stir for 30min, raise the temperature to 140°C, keep warm for 4-8h, and after the reaction is over, monobutyl trichloride is obtained. A mixed solution of tin chloride and dibutyl tin dichloride;

[0031] (2) The mixed solution of monobutyl tin trichloride and dibutyl tin dichloride is heated up to 95-100° C., and the boiling points of the two substances in the mixture are different, and monobutyl tin trichloride, dibutyl tin trichloride, Dibutyltin dichloride, collect monobutyltin trichloride;

[0032] (3) Add monobutyl tin trichloride, surfactant, organic solvent collected in step (2) to the reactor, after stirring evenly, slowly add sodium hydroxide solution dropwise, after dropwise, be warming up to 90 ℃, heat preservation reaction...

Embodiment 1

[0069] The preparation method of described monobutyl tin oxide comprises the following steps:

[0070] (1) Add tetrabutyltin into the reactor, stir evenly, slowly add tin tetrachloride dropwise, after the dropwise addition, stir for 30min, heat up to 140°C, keep warm for 6h, and the reaction is over to obtain monobutyltin trichloride A mixed solution of tin and dibutyltin dichloride;

[0071] (2) Warm up the mixed solution of monobutyltin trichloride and dibutyltin dichloride to 98°C, the boiling points of the two substances in the mixture are different, and the monobutyltin trichloride, dibutyltin trichloride and dibutyltin trichloride are successively distilled. Base tin dichloride, collect monobutyl tin trichloride;

[0072] (3) Add monobutyl tin trichloride, surfactant, organic solvent collected in step (2) to the reactor, after stirring evenly, slowly add sodium hydroxide solution dropwise, after dropwise, be warming up to 90 ℃, keep warm for 4 hours, cool down to room ...

Embodiment 2

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

[0085] (1) Add tetrabutyltin into the reactor, stir evenly, slowly add tin tetrachloride dropwise, after the dropwise addition, stir for 30min, heat up to 140°C, keep warm for 6h, and the reaction is over to obtain monobutyltin trichloride A mixed solution of tin and dibutyltin dichloride;

[0086] (2) Warm up the mixed solution of monobutyltin trichloride and dibutyltin dichloride to 98°C, the boiling points of the two substances in the mixture are different, and the monobutyltin trichloride, dibutyltin trichloride and dibutyltin trichloride are successively distilled. Base tin dichloride, collect monobutyl tin trichloride;

[0087] (3) Add monobutyl tin trichloride, surfactant, organic solvent collected in step (2) to the reactor, after stirring evenly, slowly add sodium hydroxide solution dropwise, after dropwise, be warming up to 90 ℃, keep warm for 4 hours, cool down to room ...

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Abstract

The invention provides a preparation method of monobutyltin oxide. The method includes the steps of firstly, adding tetrabutyl tin into a reactor, evenly stirring, slowly dropwise adding tin tetrachloride, then stirring for 30 minutes, heating to 140 DEG C, and performing heat-preservation reaction for 4-8 hours to obtain the mixed solution of monobutyltin trichloride and dibutyltin dichloride; secondly, heating the mixed solution of the monobutyltin trichloride and the dibutyltin dichloride to 95-100 DEG C, and collecting the monobutyltin trichloride; thirdly, adding the monobutyltin trichloride collected in the second step, surfactant and an organic solvent into a reactor, evenly stirring, slowly dropwise adding a sodium hydroxide solution, then heating to 90 DEG C, performing heat-preservation reaction for 3.5-4 hours, cooling to room temperature, filtering to obtain crude monobutyltin oxide, washing the crude monobutyltin oxide until the crude monobutyltin oxide is neutral, and performing reduced-pressure drying at 80 DEG C for 12 hours to obtain the monobutyltin oxide, wherein the surfactant is chitosan modified imidazoline ampholytic surfactant and quaternized polyvinyl alcohol.

Description

technical field [0001] The invention relates to the field of preparation of organotin heat stabilizers, in particular, the invention relates to a preparation method of monobutyltin oxide. Background technique [0002] Organotin is widely used as stabilizer of PVC, polyurethane foaming agent and bactericide, material protection agent, animal insect repellant, etc. Organotin is decomposed into harmless divalent inorganic tin in the environment, unlike tin , Lead as left residual poison, endanger the environment. [0003] Monobutyl tin oxide is mainly used as a catalyst for the production of saturated polyester resins such as powder coatings, coil (steel) coatings, and insulating varnishes, as a catalyst for the production of unsaturated polyester resins; as a raw material for plastic stabilizers, organic tin intermediates, Esterification catalyst, electrophoretic electrodeposition coating catalyst. [0004] At present, the synthesis method of monobutyl tin oxide is usually t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
CPCC07F7/2224
Inventor 杨学强张建根顾周全胡为莉
Owner 启东市强强贸易有限公司
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