Method of synthesizing tetraalkyltin

A technology of tetrabutyltin and chlorobutane, applied in the direction of tin organic compounds, etc., can solve the problems of affecting the Grignard conversion rate, low tetraalkyltin purity, unfavorable reaction control, etc., and achieves easy recovery, easy reaction control, Grignard effect. high conversion rate

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
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  • Application Information

AI Technical Summary

Problems solved by technology

However, tin tetrachloride is easy to react with metal magnesium to generate by-products, which affects the Grignard conversion rate and the direct yield of tin. Simultaneously, multiple exothermic reactions release a large amount of heat in a short period of time, which is not conducive to reaction control and has a greater potential safety hazard. many
The solvents used in the traditional two-step method are generally low-boiling-point solvents such as ether, tetrahydrofuran, and benzene. In industrial production, a large amount of Grignard reagents are synthesized, which is prone to accidents such as punching and burning. It is volatile and has a high risk of explosion. Poor safety, high harmfulness to human body, low recovery rate and other problems, the produced tetraalkyltin has low purity and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Add 400kg of magnesium and 3500kg of butyl ether into the reaction kettle, add part of the prepared Grignard reagent, start stirring, add 100kg of chlorobutane and heat to initiate the reaction, after the reaction is initiated, add 1400kg of chlorobutane dropwise under cooling water. During the reaction, the temperature is controlled at 60-70°C. After adding chlorobutane, react for 2 hours to complete the preparation of Grignard reagent. After the Grignard reagent was left to stand for 30 minutes, nitrogen was used to press the material into a closed metering tank for metering, and then nitrogen was used to press the material into the synthesis reaction kettle again, and the addition of tin tetrachloride was determined to be 1100kg according to the known weight and production requirements. The reaction temperature was controlled at 85° C. for 2 hours. Add 3500kg of water and 50kg of hydrochloric acid into the water washing kettle, add the reacted materials for washing,...

Embodiment 2

[0012] Add 350kg of magnesium and 3300kg of butyl ether into the reaction kettle, add part of the prepared Grignard reagent, start stirring, add 100kg of chlorobutane and heat to initiate the reaction, after the reaction is initiated, add 1200kg of chlorobutane dropwise under cooling water. During the reaction, the temperature is controlled at 60-70°C. After adding chlorobutane, react for 2 hours to complete the preparation of Grignard reagent. After the Grignard reagent was left to stand for 30 minutes, nitrogen was used to press the material into a closed metering tank for metering, and then nitrogen was used to press the material into the synthesis reaction kettle again, and the addition of tin tetrachloride was determined to be 1050kg according to the known weight and production requirements. The reaction temperature was controlled at 90° C. for 2 hours. Add 3500kg of water and 50kg of hydrochloric acid into the water washing kettle, add the reacted materials for washing,...

Embodiment 3

[0014] In a four-necked flask equipped with an electric stirrer, a thermometer, and a reflux tube, add 20.50g of magnesium chips, 220g of butyl ether, 20g of Grignard reagent, and 15g of chlorobutane, raise the temperature to 77°C to initiate the reaction, and add dropwise in the state of cooling water 77.5g of chlorobutane, the temperature is controlled at 60-70°C during the reaction process, after adding the chlorobutane, react for 2 hours to complete the preparation of the Grignard reagent. Slowly add 72 g of tin tetrachloride dropwise to the prepared Grignard reagent, control the reaction temperature at 85-95° C., and react for 2 hours. The reacted material was added to 140g of dilute hydrochloric acid solution for washing, and the temperature was controlled below 60°C, then stood for 15 minutes, the brine was separated, and butyl ether was distilled off under reduced pressure to obtain 85.16g of colorless transparent liquid with a yield of 98.12%. , The test results are: ...

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Abstract

The invention relates to a preparation method of an organotin product, in particular to a method of synthesizing tetraalkyltin through two-step method, belonging to the technical field of the chemical engineer. The method adopts a two-step method and the method comprises the following steps: firstly adopting metal magnesium, solvent and a small number of the prepared Grignard reagent to react andsynthesize Grignard reagent, and then dropwise adding stannic chloride to perform an alkylation reaction and obtain tetraalkyltin, wherein the added solvent is butyl ether solution, the Grignard reaction is performed at 55-75 DEG C for 2-4h under the nitrogen protective atmosphere, and the alkylation reaction is performed at 80-100 DEG C for 1-3h under the nitrogen protective atmosphere. Comparedwith the current one-step reaction, the method avoids the generation of the side reaction so that the Grignard exothermic reaction can be performed safely and stably and the reaction is easy to control. Compared with the traditional two-step method, the method solves the problems that the boiling point of the solvent is low, the solvent is volatilizable, the explosive risk is high, and the solvent is harmful to human body and the like.

Description

technical field [0001] The invention relates to a method for preparing an organotin product, in particular to a method for synthesizing tetraalkyltin in two steps, and belongs to the technical field of chemical industry. Background technique [0002] Organotin compounds are an important product of tin deep processing, with the characteristics of various varieties and wide applications, and it is the fastest growing field of tin consumption. Organotin products are mainly used in three aspects, that is, as insecticides and fungicides in agriculture, medicine, and textiles; as preservatives in forestry; and as heat stabilizers and catalysts in the plastic industry in chemical industry. There are usually one-step method and two-step method for the synthesis of tetraalkyltin by Grignard method. The one-step method is to first raise the temperature of metal magnesium chips, solvent and a small amount of Grignard reagent to the initial reaction temperature, and then dropwise add ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22
Inventor 普俊勇郭应辉高忠连刘路坷蒋学泉罗家轩
Owner 云南锡业锡化工材料有限责任公司
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