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Preparation method of granular dibutyltin oxide

A dibutyltin oxide, state technology, applied in the direction of tin organic compounds, can solve the problems of personnel and environmental hazards, small specific gravity, fine particle size, etc., and achieve the effects of low operating intensity, low cost, and large production capacity

Active Publication Date: 2012-11-14
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

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Problems solved by technology

In recent years, my country has begun to produce dibutyltin oxide on a large scale, but its appearance is in a powder state. Due to its small specific gravity and fine particle size, it is very easy to fly during use, causing harm to personnel and the environment.

Method used

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  • Preparation method of granular dibutyltin oxide

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Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: 5000kg concentration is that 20% sodium hydroxide, 85kg ammoniacal liquor and tensio-active agent 8.5kg add in the reactor, be warming up to 60 ℃ of initial reaction temperatures, then slowly add dropwise 3500kg dibutyl tin chloride, control The temperature is 60°C at the starting temperature of the alkaline hydrolysis reaction. After adding dibutyltin dichloride dropwise, control the temperature at 60-70°C and react for 2 hours to do one reaction. After the constant temperature is over, the brine is pumped away. Add 4000kg of hot water at 60°C, 200kg of ammonia water and 1kg of surfactant for the second reaction, control the temperature at 60-70°C for 2 hours, add 4000kg of hot water at 60°C, 80kg of ammonia water and 1kg of surfactant for the third reaction, and control the temperature at 60-70 °C for 2 hours. After the reaction, the dibutyltin oxide product was repeatedly washed three times with hot water at 60°C, centrifugally filtered, and dried in a...

Embodiment 2

[0017] Embodiment 2: 5200kg concentration is that 15% sodium hydroxide, 80kg ammoniacal liquor and 8kg tensio-active agent are added in the reactor, be warmed up to initial reaction temperature 55 ℃, then slowly dropwise add 2950kg dibutyl tin chloride, control temperature The initial temperature of alkaline hydrolysis reaction is 55°C. After adding dibutyltin dichloride dropwise, control the temperature at 60-70°C and react for 2.5 hours for one reaction. After the constant temperature is over, the brine is pumped away. Add 4000kg of hot water at 60°C, 180kg of ammonia water and 1kg of surfactant for the second reaction, and react at a temperature of 60-70°C for 2 hours. °C for 2 hours. After the reaction, the dibutyltin oxide product was repeatedly washed 4 times with hot water at 60°C, centrifugally filtered, and dried in a vacuum dryer at 80-90°C for 24 hours to obtain 2385kg of qualified dibutyltin oxide product. The obtained product quality: main content: 99.62%; Sn: 4...

Embodiment 3

[0018] Embodiment 3: 6660kg concentration is that 15% sodium hydroxide, 100kg ammoniacal liquor and 10kg tensio-active agent are added in the reactor, be warming up to initial reaction temperature 50 ℃, then slowly dropwise add 3500kg dibutyl tin chloride, control temperature The initial temperature of alkaline hydrolysis reaction is 50°C. After adding dibutyltin dichloride dropwise, control the temperature at 60-70°C and react for 2 hours to do one reaction. After the constant temperature is over, the brine is pumped away. Add 4000kg of hot water at 60°C, 150kg of ammonia water and 1kg of surfactant for the second reaction, and react at a temperature of 60-70°C for 1 hour. °C for 1 hour. After the reaction, the dibutyltin oxide product was repeatedly washed with hot water at 60°C for 3 times, centrifugally filtered, and dried in a vacuum dryer at 80-90°C for 24 hours to obtain 2842kg of qualified dibutyltin oxide product. The quality of the obtained product: main content: 9...

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Abstract

The invention relates to a preparation method of an organotin product, in particular to a preparation method of granular dibutyltin oxide, belonging to the field of the chemical engineer. The method comprises the following steps: adding sodium hydroxide solution, neutralizer and surfactant in a reaction tank, heating the mixture to the initial temperature of the alkaline hydrolysis reaction, then dropwise adding dibutyltin dichloride solution while controlling the adding speed to 15-25kg / min, then performing the alkaline hydrolysis reaction under the temperature of the alkaline hydrolysis reaction to obtain dibutyltin oxide and finally obtaining the pure white granular dibutyltin oxide through water washing, filtrating and vacuum drying. The invention is characterized by high efficiency, controllable reaction and high purity and yield, the prepared product is granular, the purity of the prepared dibutyltin oxide is not less than 99%, and the yield of dibutyltin oxide which is synthesized by adopting dibutyltin dichloride as starting raw material is not less than 98%.

Description

technical field [0001] The invention relates to a preparation method of an organotin product, in particular to a preparation method of granular dibutyltin oxide, which belongs to the field of chemical industry. Background technique [0002] Dibutyltin oxide is an important intermediate product in the synthesis of butyl series organotin plastic heat stabilizers. It is used in the production of dibutyltin laurate, dibutyltin maleate and monobutyltin maleate. Its quality is directly related to Affect the quality of stabilizer products. Dibutyltin oxide is a versatile product that is thermally stable and hydrolytically resistant as an esterification catalyst. The product is neutral and non-corrosive. As a polyurethane catalyst, it can form a stable dispersion system in water-based coatings. At the same time, it is also an intermediate raw material for the synthesis of polyvinyl chloride heat stabilizers, polyurethane catalysts, and organic silicon curing catalysts. [0003] my...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22
Inventor 蒋学泉郭应辉普俊勇姚俊罗家轩高忠连
Owner 云南锡业锡化工材料有限责任公司
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