Monobutyltin Oxide CAS 2273-43-0

(1) Add tetrabutyltin into the reactor, stir evenly, slowly add tin tetrachloride dropwise, after the dropwise addition, stir for 30min, heat up to 140°C, keep warm for 6h, and the reaction is over to obtain monobutyltin trichloride A mixed solution of tin and dibutyltin dichloride;

(2) Warm up the mixed solution of monobutyltin trichloride and dibutyltin dichloride to 98°C, the boiling points of the two substances in the mixture are different, and the monobutyltin trichloride, dibutyltin trichloride and dibutyltin trichloride are successively distilled. Base tin dichloride, collect monobutyl tin trichloride;

(3) Add monobutyl tin trichloride, surfactant, organic solvent collected in step (2) to the reactor, after stirring evenly, slowly add sodium hydroxide solution dropwise, after dropwise, be warming up to 90 ℃, heat preservation reaction for 4 hours, cool down to room temperature, filter to obtain the crude product of monobutyltin oxide, wash the crude product of butyl stannoic acid with water to neutrality, and dry under reduced pressure at 80 ℃ for 12 hours to obtain butyl stannoic acid;

Wherein, the surfactant is a chitosan modified imidazoline amphoteric surfactant and a quaternized polyvinyl alcohol; the mol ratio of tetrabutyltin to the tin tetrachloride in step (1) is 1:2 ; The weight ratio of monobutyl tin trichloride described in step (3) and described surfactant, described organic solvent is 1: 0.0024: 5; Said mono butyl tin trichloride in step (3) The weight ratio with the sodium hydroxide solution is 1:7; the concentration of the sodium hydroxide solution is 0.1mol/L; the organic solvent is n-octanol; the modified chitosan in the surfactant The weight ratio of the imidazoline amphoteric surfactant to the quaternized polyvinyl alcohol is 1:0.7.

(1) Control feeding: Weigh 5g NaOH into the reaction bottle and stir and dissolve with 200g water, use cooling water to control the temperature below 40°C, weigh 80g monobutyltin trichloride liquid into the constant pressure funnel, weigh 25g NaOH Dissolve in 50g of water and put it into the constant pressure funnel to slowly drop into the reaction flask, control the dropping temperature to be less than 30°C, and the pH of the dropping process is 8.0;

(2) Constant temperature reaction: After controlling the feeding, the liquid in the reaction vessel is heated to 50°C, and the constant temperature reaction is carried out for 1 hour to produce butylstannoic acid;

(3) Water washing: Suction filter the butyl stannoic acid obtained from the reaction with a Buchner funnel, transfer the filter cake to a 500ml beaker and add about 200ml water for washing, repeat twice and then suction filtration;

(4) Centrifugation: After passing the water washing, the butyl stannoic acid product is slowly transferred to a centrifuge for centrifugation;

(5) Drying: Collect and centrifuge the material and transfer it to the drying equipment for drying to obtain the butyl stannoic acid product.

The monobutyltin trichloride in the step (2) is a pure product of monobutyltin trichloride or a pure aqueous solution of monobutyltin trichloride.

The drying equipment in the step (5) is a vacuum drying oven or a vacuum rotary dryer.

Finally, 58.8g of butyl stannoic acid product was obtained, and the yield was 99.3%. The assay indicators are as follows: Sn: 55.56%; Cl: 0.4%; purity: 99.3%.