Preparation method of high-purity dibutyltin oxide

A technology of dibutyltin oxide and dibutyltin chloride, which is applied in chemical instruments and methods, organic chemistry, tin organic compounds, etc., can solve the problems of aggravating water pollution and consuming water resources, so as to reduce water pollution, The effect of saving water resources and reducing the content of chloride ions

Inactive Publication Date: 2017-08-18
JIANGSU FEITUO INTERFACE ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to break through the bottleneck of this application, many companies reduce the chloride ion content by using a large amount of water washing in the centrifugation and water washing process. The chloride ion content in the best product index can only be reduced to 80-100ppm, while the process consumes water and The amount of waste water generated is dozens of times that of the finished product, which seriously consumes water resources and aggravates water pollution

Method used

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  • Preparation method of high-purity dibutyltin oxide
  • Preparation method of high-purity dibutyltin oxide

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Experimental program
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Effect test

Embodiment 1

[0021] 607.4kg of dibutyltin chloride is dissolved in 500kg of toluene, and is dropped into the solution containing 1600kg of 10% sodium hydroxide and 0.4kg of surfactant at a rate of 14kg / min, wherein the molecules of surfactant In the structural formula, m takes a value of 10, and n takes a value of 2. The temperature was controlled at 50°C, and the stirring reaction was continued for 2 hours after the dripping was completed;

[0022] The reaction solution after the stirring reaction was allowed to stand for 1.5 hours to separate layers, and the upper organic solvent layer was separated and collected for later use. Add 400kg of deionized water into the distiller, heat to 90°C, then add dropwise an organic solvent containing dibutyltin oxide, and distill to recover the toluene solvent. The remaining water phase after distillation was centrifuged and dried to prepare 495.2 kg of white dibutyltin oxide powder.

[0023] The productive rate of the present embodiment is 99.54%. ...

Embodiment 2

[0025] Dissolve 607.4kg of dibutyltin chloride in 800kg of toluene, drop in 2240kg of potassium hydroxide with a mass concentration of 10% at a rate of 14kg / min, control the temperature at 45°C, and continue to stir for 2.5 hours after the drop;

[0026] The reaction solution after the stirring reaction was left to stand for 2 hours and separated into layers, and the upper organic solvent layer was separated and collected for later use. Add 400kg of deionized water into the distiller, heat to 95°C, then add dropwise an organic solvent containing dibutyltin oxide, and distill to recover the toluene solvent. The remaining water phase after distillation was centrifuged and dried to prepare 493.4 kg of white dibutyltin oxide powder.

[0027] The productive rate of the present embodiment is 99.18%.

Embodiment 3

[0029] Dissolve 607.4kg of dibutyltin chloride in 650kg of cyclohexane, drop 1680kg of sodium hydroxide with a mass concentration of 10% at a rate of 15kg / min, control the temperature at 50°C, and continue to stir the reaction after dripping 3 Hour;

[0030] The reaction solution after the stirring reaction was left to stand for 2 hours and separated into layers, and the upper organic solvent layer was separated and collected for later use. Add 350 kg of deionized water into the distiller, heat to 95° C., then dropwise add an organic solvent containing dibutyltin oxide, and recover the cyclohexane solvent by distillation. The remaining water phase after distillation was centrifuged and dried to prepare 495.9 kg of white dibutyltin oxide powder.

[0031] The productive rate of the present embodiment is 99.48%.

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Abstract

The invention relates to a preparation method of high-purity dibutyltin oxide. The preparation method comprises the steps of carrying out synthetic reaction on the raw materials including dibutyltin oxide and alkali in a heterogeneous system of an organic solvent and a water solution, and finally carrying out centrifugation and drying, so as to obtain a dibutyltin oxide finished product. The product prepared by virtue of the preparation method is high in purity; the organic solvent and a surfactant are respectively used as a solvent and an extraction medium in a preparation process, and dibutyltin oxide particles generated by alkalization reaction are rapidly transferred into an organic phase by virtue of an absorption effect of the surfactant in the alkalization reaction process, so that the product is separated from water rich in chloride ions; the organic phase containing dibutyltin oxide is collected through layering separation, toluene is recycled through distillation, and then high-purity dibutyltin oxide is prepared; the content of the chloride ions in the product is effectively controlled to be less than or equal to 50ppm, so that the industrial water pollution is reduced.

Description

technical field [0001] The invention relates to a preparation method of dibutyl tin oxide, in particular to a preparation method of dibutyl tin oxide with high purity and low chloride ion content. Background technique [0002] Organotins are usually used in the production of polyurethane and other products, especially in polyurethane foam, coatings, elastomers, adhesives, resins and other industries. Dibutyltin oxide can be used as a catalyst, heat stabilizer and intermediate in many fields. Dibutyltin oxide is a near-neutral homogeneous surfactant with mild reaction conditions, high yield, fast reaction speed, high efficiency and non-toxicity, non-corrosive to the reaction vessel, and high stereo and regioselectivity It has good stability and hydrolysis resistance, and is an organotin surfactant with multiple industrial uses. Dibutyltin oxide can be used as a heat stabilizer in the production of polyvinyl chloride and organotin plastics. Secondly, dibutyltin oxide can al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
CPCC07F7/2224
Inventor 郑建周汉涛王昌如陈春雷
Owner JIANGSU FEITUO INTERFACE ENG TECH CO LTD
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