Preparation method of tributyltin chloride

A technology of tributyltin chloride and monobutyltin trichloride, which is applied in the field of preparation of high-purity tributyltin chloride, can solve the difficulties of separation of dibutyltin dichloride, low main content and labor Occupational health hazards and other problems, to achieve the effects of easy control of feeding and reaction conditions, simple preparation process, and high purity

Inactive Publication Date: 2020-03-06
云南锡业锡化工材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing problems mainly include the low main content of the product (≥95%), it is difficult to meet the requirements for the use of pharmaceutical intermediates, the separation of dibutyl tin dichloride is difficult during the production process, and the occupational health hazards to employees are large during the operation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of tributyl tin chloride, the steps are as follows:

[0025] (1) According to tetrabutyltin analysis result and quality calculation tin tetrachloride charging amount, prepare tin tetrachloride and tetrabutyltin as 1:1 by the amount ratio of substance;

[0026] (2) Add tetrabutyltin into the jacketed enamel reaction kettle, start stirring and add chilled water, after cooling down to below 0°C, turn on the vacuum machine, pump the reaction kettle to the ultimate vacuum, and close the vacuum valve;

[0027] (3) Control the temperature in the reactor at -10°C to 0°C and continuously add tin tetrachloride dropwise, and keep the reaction for half an hour after the feeding is completed. The reaction equation is mainly as follows:

[0028] (C 4 h 9 ) 4 Sn+SnCl 4 →(C 4 h 9 ) 3 SnCl+C 4 h 9 SnCl 3 (A)

[0029] (C 4 h 9 ) 3 SnCl+C 4 h 9 SnCl 3 →2(C 4 h 9 ) 2 SnCl 2 (B)

[0030] (C 4 h 9 ) 3 SnCl+SnCl 4 →(C 4 h 9 ) 2 SnCl 2 +C 4...

Embodiment 2

[0036] (1) according to tetrabutyl tin analysis result and quality calculation tin tetrachloride charging amount, prepare tin tetrachloride and the mixture containing tetrabutyl tin for 1:1 by the amount ratio of substance, the described mixture containing tetrabutyl tin is tetrabutyl tin and tetrabutyl tin The mixture of tributyltin chloride, the mass ratio of tetrabutyltin and tributyltin chloride is tetrabutyltin≥80%, tributyltin chloride≤20%;

[0037] (2) Add the mixture of tetrabutyltin and tributyltin chloride into the enamel reaction kettle, start stirring and add chilled water, after cooling down to below 0°C, turn on the vacuum machine, pump the reaction kettle to the ultimate vacuum, and close the vacuum valve ;

[0038] (3) Control the temperature in the reaction kettle to continuously add tin tetrachloride dropwise at -10°C to 0°C, and keep the reaction for half an hour after the feeding is completed;

[0039] (4) After the reaction finishes, transfer the material...

Embodiment 3

[0043] This example is performed in a laboratory.

[0044] Weigh 500 grams of tetrabutyltin (the main content is 82.6%) and add it to the reaction flask, and cool it to below 0°C with an ice bath; weigh 310 grams of tin tetrachloride (the main content is 99.9%) and add it to the constant pressure funnel, and control the dropping The temperature is lower than 0°C and the tin tetrachloride is continuously added dropwise, and the reaction is carried out for half an hour after the addition is completed. Add 500 grams of distilled water to the reaction bottle, stir for half an hour and then pour into a separatory funnel for static phase separation. After the phase separation, the upper organic phase in the bottle is dried with a rotary evaporator to finally obtain 495 grams of tributyltin chloride product. The analysis results are as follows: Sn: 36.32%; Cl: 10.94%; tributyltin chloride 99.59%; monobutyltin trichloride 0.01%; dibutyltin dichloride 0.34%.

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PUM

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Abstract

The invention relates to a preparation method of tributyltin chloride. The preparation method includes: preparing tin tetrachloride and tetrabutyltin or a mixture containing tetrabutyltin according toa mole ratio of 1:1; adding the tetrabutyltin or the mixture containing tetrabutyltin into a reaction kettle, starting stirring, and adding chilled water, performing cooling to 0DEG C or below, vacuumizing the reaction kettle to ultimate vacuum, and closing a vacuum valve; continuously adding tin tetrachloride dropwise when the temperature in the reaction kettle is controlled ranging from -10DEGC to 0DEG C, keeping reaction for half an hour at the end of feeding, then transferring materials in the reaction kettle to a washing kettle, adding pure water, performing stirring, and conducting full standing; separating a monobutyltin trichloride aqueous solution at a lower layer in the washing kettle into a storage tank, leaving an upper layer organic phase in the washing kettle, controlling the temperature of the washing kettle at 90-110DEG C, and carrying out vacuum drying; and cooling the dried material to obtain a tributyltin chloride product. The process provided by the invention is simple and is easy to control, and the prepared product has high purity.

Description

technical field [0001] The invention belongs to the technical field of organotin preparation, and in particular relates to a preparation method of high-purity tributyltin chloride. Background technique [0002] Triorganotin compounds are an important series of organotin chemical products with the general formula R3SnX, which are widely used in agriculture, wood, shipbuilding and other industries. Among them, tributyltin chloride is widely used as an important intermediate in the synthesis of α, β-unsaturated methyl ketone and isoxazole because of its high biological activity. Algae agent, antifungal agent, etc. are used as fungicides in agriculture, as protective agents in wood, paper, textile, painting and other industries, and also as catalysts and pharmaceutical intermediates in polymerization reactions. [0003] The method for preparing tributyltin chloride in the prior art is to rearrange tetrabutyltin and tin tetrachloride to generate a mixture of monobutyltin trichlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
CPCC07F7/2208
Inventor 艾维华楚斌蒋学泉王丽媛高忠连姚俊江鑫
Owner 云南锡业锡化工材料有限责任公司
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