Beta-diketone organotin PVC heat stabilizer and preparation method thereof

A heat stabilizer and diketone technology, which is applied in the field of β-diketone organotin PVC heat stabilizer and its preparation, can solve the problems of inconvenience in transportation and storage, and achieve convenient storage, convenient use, and promotion of analysis. crystal effect

Inactive Publication Date: 2016-11-09
南通德发生物化工有限公司
2 Cites 6 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Organotin heat stabilizers have the advantages of good thermal stability, compatibility and transparenc...
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Abstract

The invention discloses a beta-diketone organotin PVC heat stabilizer and a preparation method thereof, and belongs to the technical field of a PVC heat stabilizer. According to main points of the technical scheme, the beta-diketone organotin PVC heat stabilizer has a structural formula as shown in the specification, wherein R is phenyl or heptadecyl. The invention also discloses a preparation method of the beta-diketone organo tin PVC heat stabilizer. Advantages of an organotin stabilizing agent and a beta-diketone compound auxiliary heat stabilizer are combined, thus achieving the effects of the two substances. Then, the product is more convenient to use. In the preparation method of the beta-diketone organotin PVC heat stabilizer, the use of ultrasonic wave can avoid ammonium chloride which is generated after a reaction and doped in the product from affecting quality of the product; and by the use of nitrogen during the whole reaction, a solvent is not easy to volatilize under the condition of 0 DEG C. through nitrogen for solvent volatilization, crystallization can be promoted, and the influence of oxygen on the combination of a beta-diketone compound and stannous ion can be avoided.

Application Domain

Tin organic compoundsGroup 4/14 organic compounds without C-metal linkages

Technology Topic

SolventChemistry +7

Examples

  • Experimental program(6)

Example Embodiment

[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.

Example Embodiment

[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.

Example Embodiment

[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.

PUM

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