Beta-diketone organotin PVC heat stabilizer and preparation method thereof

[0019] Example 1

[0020] Pour nitrogen into an ultrasonic reaction vessel equipped with a stirring device, then add 300 mL of a dichloromethane solution containing 22.5 g (0.1 mol) of 1,3-diphenyl-1,3-propanedione, and add 100 mL of ammonia , Slowly add 300mL of methanol solution with 22.5g (0.1mol) of stannous chloride dihydrate dissolved in the ultrasonic reaction vessel at a reaction temperature of 25°C, and turn on the stirring device and ultrasonic generator during the dropping process. The set frequency is 20KHz. After the addition, the solution is clear at this time, stop stirring, keep the ultrasonic generator continuing to work, slowly reduce the temperature to 0℃, the reaction liquid is still, open the vent on the ultrasonic reaction vessel, and keep The introduced nitrogen is discharged from the exhaust hole, and the nitrogen is discharged from the ultrasonic reaction vessel with a certain amount of reaction solvent. Colorless or light yellow crystals are gradually precipitated. After 5 hours, the crystallization is complete. The reaction solution is suction filtered and the filter cake is washed with methanol. Secondly, the excess stannous salt was washed off, and the filter cake was dried at room temperature to obtain 27g of 1,3-diphenyl-1,3-propanedione organotin PVC heat stabilizer.

[0021] Example 2

[0022] Pour nitrogen into an ultrasonic reaction vessel equipped with a stirring device, then add 300 mL of a dichloromethane solution containing 22.5 g (0.1 mol) of 1,3-diphenyl-1,3-propanedione, and add 100 mL of ammonia At the reaction temperature of 0°C, slowly drip 300 mL of methanol solution with 12g (0.05mol) of stannous chloride dihydrate dissolved in the ultrasonic reaction vessel at a reaction temperature of 0°C, and turn on the stirring device and the ultrasonic generator during the dropping process. Set the frequency to 100KHz. After the addition, the solution is clear at this time, stop stirring, keep the ultrasonic generator working, slowly decrease the temperature to 0℃, and the reaction solution is still. Open the exhaust hole on the ultrasonic reaction vessel and keep it open. The incoming nitrogen is discharged from the exhaust hole, and the nitrogen is discharged from the ultrasonic reaction vessel with a certain amount of reaction solvent. Colorless or light yellow crystals are gradually precipitated. After 5 hours, the crystallization is complete. The reaction solution is suction filtered, and the filter cake is washed with methanol several times. To wash off the excess stannous salt, the filter cake was dried at room temperature to obtain 22g of 1,3-diphenyl-1,3-propanedione organotin PVC heat stabilizer.

[0023] Example 3

[0024] Pour nitrogen into an ultrasonic reaction vessel equipped with a stirring device, then add 300 mL of a dichloromethane solution containing 22.5 g (0.1 mol) of 1,3-diphenyl-1,3-propanedione, and add 100 mL of ammonia At a reaction temperature of 50°C, slowly drop 300 mL of a methanol solution with 16g (0.066mol) of stannous chloride dihydrate dissolved in the ultrasonic reaction vessel, and turn on the stirring device and ultrasonic generator during the dropping process. Set the frequency to 80KHz. After the addition, the solution is clear at this time. Stop stirring, keep the ultrasonic generator working, slowly cool to 0°C, and the reaction solution is still. Open the exhaust hole on the ultrasonic reaction vessel and keep it open. The incoming nitrogen is discharged from the exhaust hole, and the nitrogen is discharged from the ultrasonic reaction vessel with a certain amount of reaction solvent. Colorless or light yellow crystals are gradually precipitated. After 5 hours, the crystallization is complete. The reaction solution is suction filtered, and the filter cake is washed with methanol several times. To wash off the excess stannous salt, the filter cake was dried at room temperature to obtain 28g of 1,3-diphenyl-1,3-propanedione organotin PVC heat stabilizer.