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Ultrasonic preparation method of fine transparent nucleating agent

A transparent nucleating agent, ultrasonic technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. , to achieve the effect of improving optical transparency, improving nucleation efficiency, and low energy consumption

Active Publication Date: 2012-04-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the nucleating agent prepared by this process can improve the mechanical properties and transparency of polypropylene, it still has the following disadvantages: high melting point, cannot be melted and dispersed at the resin processing temperature, resulting in poor dispersion compatibility in the resin, affecting Nucleation effect, and the nucleating agent particles are large, the shape of the nucleating agent cannot be well grasped, and the particle size of the nucleating agent cannot be effectively controlled
The reaction operation must be carried out in multiple steps, with many equipments, large investment, complex operation process, cumbersome operation, intermediate materials must be transported many times, and the waste gas smell is strong, which is not conducive to environmental protection

Method used

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  • Ultrasonic preparation method of fine transparent nucleating agent
  • Ultrasonic preparation method of fine transparent nucleating agent
  • Ultrasonic preparation method of fine transparent nucleating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Weigh 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate raw material, add it to methanol, according to mass ratio, 2,2'-methylene-bis(4, Sodium 6-di-tert-butylphenoxy)phosphate:methanol=1:6. The above solution was placed in a water bath of an ultrasonic generator, the temperature of the water bath was 30° C., the ultrasonic frequency was 59 kHz, and the ultrasonic power density was 150 watts per liter of solution. Stir while ultrasonically oscillating to completely dissolve the above raw materials. Then add a mass concentration of 5% aluminum chloride aqueous solution, in molar ratio, 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate:aluminum chloride=2:1 ; Under the conditions of pH=4 and temperature 50° C., ultrasonic vibration reaction was carried out for 2 hours.

[0036] The obtained white precipitate was collected by suction filtration, and the filter cake was washed with water until the filtrate was neutral, and then dried at 80°C for 2 hour...

Embodiment 2

[0038] Weigh 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)phosphate raw material, add it to methanol, by mass ratio, 2,2'-methylene-bis(4, 6-di-tert-butylphenoxy)phosphate:methanol=1:6. The above solution was placed in a water bath of an ultrasonic generator, the temperature of the water bath was 30° C., the ultrasonic frequency was 59 kHz, and the ultrasonic power density was 150 watts per liter of solution. Stir while ultrasonically oscillating to completely dissolve the above raw materials. Then add the aluminum chloride aqueous solution that mass concentration is 5%, in molar ratio, 2,2'-methylene-bis(4,6-di-tert-butylphenoxy) phosphate: aluminum chloride=2:1 ; Under the conditions of pH = 6 and temperature 50°C, carry out ultrasonic oscillation reaction for 2 hours; then add lithium laurate, according to the mass ratio, 2,2'-methylene-bis(4,6-di-tert-butylphenoxy ) Phosphate: lithium laurate=2:1, and continue ultrasonic oscillation for 20 minutes.

[0039] The obtained w...

Embodiment 3

[0041] Weigh 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate raw material, add it to methanol, according to mass ratio, 2,2'-methylene-bis(4, Sodium 6-di-tert-butylphenoxy)phosphate:methanol=1:6. The above solution was placed in a water bath of an ultrasonic generator, the temperature of the water bath was 30° C., the ultrasonic frequency was 59 kHz, and the ultrasonic power density was 150 watts per liter of solution. Stir while ultrasonically oscillating to completely dissolve the above raw materials. Then add a mass concentration of 5% aluminum chloride aqueous solution, in molar ratio, 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate:aluminum chloride=2:1 ; Under the conditions of pH=4 and temperature 50°C, carry out ultrasonic oscillation reaction for 2 hours; then add sodium stearate and silicate, according to the mass ratio, 2,2'-methylene-bis(4,6-di-tert Butylphenoxy)sodium phosphate: sodium stearate: silicate = 4:2:1, continue ultrasonic osci...

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Abstract

The invention relates to an ultrasonic auxiliary coprecipitation method for preparing a fine polypropylene transparent nucleating agent. The method is characterized in that an ultrasonic auxiliary coprecipitation process is employed during synthetic process of organic phosphate to obtain the fine powder particles by one step, the composition and particle size of the transparent nucleating agent can be effectively controlled by changing a synthetic condition and an ultrasonic condition, the fine transparent nucleating agent with average particle size of 1-5 micrometers can be obtained. The ultrasonic preparation method of fine transparent nucleating agent is used for the field of auxiliary agent treatment by polypropylene. The transparent nucleating agent is capable of substantially raising the nucleation efficiency during polypropylene treatment, forming minimal polypropylene spherocrystals, and substantially raising a plurality of performances of the optical transparency, rigidity, intensity, thermal deformation temperature of resin.

Description

technical field [0001] The invention relates to a polypropylene nucleating agent, in particular to a preparation method of a polypropylene transparent nucleating agent. Background technique [0002] As a highly efficient polypropylene transparent nucleating agent, substituted aryl organic phosphates are widely used as nucleating modifiers for polypropylene resins, and are applied to the modification of polypropylene resins, wherein substituted diaryl organic phosphates such as bis( 4,6-di-tert-butylphenoxy)sodium phosphate, 2,2′-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate, etc., can significantly improve the processing of these resins performance. Literature "High Performance of Polypropylene-Nucleating Agent" ("Chemical Industry", 1999 (8), p11), "Influence of Nucleating Agent on the Properties of Polypropylene" ("Synthetic Resins and Plastics", 2001, 18( 4), 39-41) have been reported. [0003] At present, the synthesis of substituted aryl organic phosphates ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08L23/12C08K5/527
Inventor 褚海斌顾民吕静兰徐耀辉李伟
Owner CHINA PETROLEUM & CHEM CORP
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