Tetrabutyl tin preparation method

Abstract

The invention discloses a modified synthesizing method of tetrabutyltin, which comprises the following steps: adding metal magnesium, ether solution and little synthesized Grignard reagent in the autoclave; heating to starting reacting temperature; dripping halogenated hydrocarbon and tin tetrachloride; controlling the temperature within alkylated reacting temperature. The invention possesses good security and reacting course, which is convenient to control dripping speed to receiving rate over 95%.

Description

technical field

[0001] The invention relates to the improvement of the tetrabutyltin preparation method, in particular to a tetrabutyltin preparation method with safe synthesis, controllable reaction, high yield and purity. Background technique

[0002] Organotin compounds and derivatives have a very wide range of uses and are an important chemical raw material. To synthesize organotin, the monomer tetrabutyltin must first be synthesized. Usually tetrabutyltin is synthesized by the following methods: Grignard method, Wutz method, alkylaluminum method, direct method, etc. Grignard method has been valued because of its many advantages. The synthesis of tetrabutyltin by Grignard method is usually carried out in two steps. Firstly, the ether solution of magnesium and halogenated hydrocarbon (such as chloroalkane or bromoalkane) is reacted to generate Grignard reagent, and then tin tetrachloride is added dropwise to In Grignard reagent, carry out alkylation reaction at 60-100°C ...

Examples

Embodiment 1

[0012] Embodiment 1: in the four-neck flask that electric stirrer, thermometer, reflux condenser and pressure dropping funnel are housed, add 23.3g (1mol) magnesium chip, 450ml butyl ether, the Grignard reagent that 20g has made, stir And be warmed up to 75 ℃; 92.6g (1mol) n-chlorobutane, 65.2g (0.25mol) tin tetrachloride are mixed, dropwise in the four-necked flask through the constant pressure funnel, and the dropping rate keeps certain reflux, controls The reaction temperature was 70-80°C, and the dropwise addition was completed in 85 minutes. Reflux and stir for 2.5 hours, and cool naturally. The reactant was hydrolyzed with dilute hydrochloric acid, stirred at below 40°C for 2 hours, and the organic phase was separated. The aqueous phase was extracted with 50ml of butyl ether and combined with the organic phase, and 81.3g (tetrabutyltin) of a colorless and transparent liquid was collected by distillation under reduced pressure at 142-145°C / 7mmHg. The yield (according to ...

Embodiment 2

[0013] Embodiment 2: as embodiment 1, when adding magnesium chips, butyl ether and a small amount of Grignard reagent, also add 450ml toluene; Add 900ml toluene in the n-chlorobutane that adds dropwise, tin tetrachloride mixed solution. Tetrabutyltin yield (according to SnCl 4 Total) is 96.93%, and the purity is 95.92%.

technical field

[0001] The invention relates to the improvement of the tetrabutyltin preparation method, in particular to a tetrabutyltin preparation method with safe synthesis, controllable reaction, high yield and purity. Background technique

[0002] Organotin compounds and derivatives have a very wide range of uses and are an important chemical raw material. To synthesize organotin, the monomer tetrabutyltin must first be synthesized. Usually tetrabutyltin is synthesized by the following methods: Grignard method, Wutz method, alkylaluminum method, direct method, etc. Grignard method has been valued because of its many advantages. The synthesis of tetrabutyltin by Grignard method is usually carried out in two steps. Firstly, the ether solution of magnesium and halogenated hydrocarbon (such as chloroalkane or bromoalkane) is reacted to generate Grignard reagent, and then tin tetrachloride is added dropwise to In Grignard reagent, carry out alkylation reaction at 60-100°C ...

Examples

Embodiment 1

[0012] Embodiment 1: in the four-neck flask that electric stirrer, thermometer, reflux condenser and pressure dropping funnel are housed, add 23.3g (1mol) magnesium chip, 450ml butyl ether, the Grignard reagent that 20g has made, stir And be warmed up to 75 ℃; 92.6g (1mol) n-chlorobutane, 65.2g (0.25mol) tin tetrachloride are mixed, dropwise in the four-necked flask through the constant pressure funnel, and the dropping rate keeps certain reflux, controls The reaction temperature was 70-80°C, and the dropwise addition was completed in 85 minutes. Reflux and stir for 2.5 hours, and cool naturally. The reactant was hydrolyzed with dilute hydrochloric acid, stirred at below 40°C for 2 hours, and the organic phase was separated. The aqueous phase was extracted with 50ml of butyl ether and combined with the organic phase, and 81.3g (tetrabutyltin) of a colorless and transparent liquid was collected by distillation under reduced pressure at 142-145°C / 7mmHg. The yield (according to ...

Embodiment 2

[0013] Embodiment 2: as embodiment 1, when adding magnesium chips, butyl ether and a small amount of Grignard reagent, also add 450ml toluene; Add 900ml toluene in the n-chlorobutane that adds dropwise, tin tetrachloride mixed solution. Tetrabutyltin yield (according to SnCl 4 Total) is 96.93%, and the purity is 95.92%.