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Preparation process of dibutyltin oxide

A technology of dibutyltin oxide and dibutyltin chloride, which is applied in the fields of organic chemistry, tin organic compounds, chemical instruments and methods, etc., can solve problems such as complicated process, poor effect, and increased production cost, and achieve the goal of preparing The reaction process is simple, easy to wash and dry, and the effect of saving raw material costs

Inactive Publication Date: 2016-07-27
JIANGSU XINLU CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The domestic prior art discloses some researches on the preparation process of dibutyltin oxide, and the patent CN101665510A discloses a preparation method of dibutyltin oxide in a granular state, using dibutyltin chloride, sodium hydroxide solution, medium The method of preparing dibutyltin oxide as raw materials with an agent and a surfactant, the product is in a granular state, and the reaction is efficient and controllable; but the process is complex, with many steps and many additives used, thereby increasing the production cost, and the reaction additives remain In the product, no separation
[0005] Li Quan and others disclosed an improved process for the preparation of dibutyl tin oxide (improved preparation of dibutyl tin oxide, Li Quan et al., Yunnan Chemical Industry, Volume 29, No. 2, 2002): Tin, sodium hydroxide solution and ether are used as raw materials to prepare dibutyltin oxide. The synthesis process is simple and the operation is simple, but the ether used in the reaction has a low boiling point, the effect is not good, and the yield of the prepared product is low
Wu Liang disclosed a synthesis method of dibutyltin oxide (process improvement of the synthesis method of dibutyltin oxide, Wu Liang, Plastic Additives, No. 4, 2007): with sodium hydroxide, surfactant, solvent Prepare dibutyl tin oxide with dibutyl tin oxide as raw material, control the dropping rate, and keep warm for reaction. This process has few operation steps and controllable reaction, but the production cost of this reaction is high and the product purity is low
[0006] The problems of high cost, complex process, cumbersome operation, low yield and low product purity generally exist in the above technical research and industrial scale production of dibutyltin oxide.

Method used

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  • Preparation process of dibutyltin oxide
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Examples

Experimental program
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Effect test

Embodiment 1

[0028] 607.4g dibutyl tin chloride and 1.2g n-heptane are added in the reactor that thermometer and stirrer are housed, be warmed up to 60 ℃, then dropwise add 1600g mass concentration with the dropping rate of 14Kg / min in the reactor. 10% sodium hydroxide solution, about 2.5 hours to drop, after the drop, continue to stir and react at constant temperature for 1 hour;

[0029] The reaction solution after the stirring reaction was left to stand for stratification for 1.5 hours, and the supernatant was separated, and transferred to the secondary reactor, and then 80 g of 10% mass concentration was added dropwise to the secondary reactor at a rate of 14Kg / min. Sodium hydroxide solution, controlled reaction temperature 50 DEG C to react for 3 hours, after the reaction finished, the reaction solution in the secondary reactor was allowed to stand for stratification for 2 hours;

[0030] Transfer the upper layer solution in the secondary reactor to the distiller, distill out n-heptan...

Embodiment 2

[0032] 607.4g dibutyl tin chloride and 1.2g n-heptane are added in the reactor that thermometer and stirrer are housed, be warmed up to 60 ℃, dropwise with the dropping rate of 14Kg / min in the reactor then 1640g mass concentration is 10% sodium hydroxide solution, about 2.5 hours to drop, after the drop, continue to stir and react at constant temperature for 1 hour;

[0033] The reaction solution after the stirring reaction was left to stand for stratification for 1 hour, and the supernatant was separated, and transferred to the secondary reactor, and then 160 g of 10% mass concentration was added dropwise to the secondary reactor at a rate of 14Kg / min. Sodium hydroxide solution, controlled reaction temperature 50 DEG C to react for 3 hours, after the reaction finished, the reaction solution in the secondary reactor was allowed to stand for stratification for 2 hours;

[0034] Transfer the upper layer solution in the secondary reactor to the distiller, distill out n-heptane at...

Embodiment 3

[0036] Add 607.4g of dibutyltin chloride and 1g of n-heptane into a reactor equipped with a thermometer and a stirring device, raise the temperature to 60°C, and then dropwise add 1680g of 1680g with a mass concentration of 10 to the reactor at a rate of 14Kg / min. % sodium hydroxide solution, drop it in about 2.5 hours, after the drop, continue to stir and react at a constant temperature for 1 hour;

[0037] The reaction solution after the stirring reaction was left to stand for stratification for 2 hours, and the supernatant was separated, and transferred to the secondary reactor, and then 80 g of 10% mass concentration was added dropwise to the secondary reactor at a rate of 14Kg / min. Sodium hydroxide solution, controlled reaction temperature 50 DEG C to react for 3 hours, after the reaction finished, the reaction solution in the secondary reactor was allowed to stand for stratification for 2 hours;

[0038] Transfer the upper layer solution in the secondary reactor to the d...

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Abstract

The invention relates to a preparation process of dibutyltin oxide. According to the preparation process, dibutyltin chloride and sodium hydroxide are taken as raw materials and subjected to a synthesis reaction under the action of a surfactant, finally, centrifugal water washing, vacuum drying and smashing are performed, and a finished product, namely, dibutyltin oxide, is prepared; the surfactant used in the synthesis process is one of n-heptane, toluene and ethanol, and a sodium hydroxide solution is added twice in the reaction process. The preparation process of dibutyltin oxide has the advantages that the synthesis raw materials and the reaction process are simple, little waste is discharged, and the production cost is saved; the reaction is controllable, the operation is simple and convenient, the product purification process is simple, and the product is high in purity and good in color; the surfactant can be completely separated from the product and recycled; the conversion rate of the raw material dibutyltin chloride can reach 99.80%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a preparation process of dibutyltin oxide. 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. [0003] 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 also be used as an intermediate with exc...

Claims

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Application Information

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IPC IPC(8): C07F7/22
CPCC07F7/2224
Inventor 周汉涛郑建曹智娟周德龙
Owner JIANGSU XINLU CHEM NEW MATERIAL
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