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Method for preparing organic phosphate nucleating agent through ultrasonic sedimentation

An organophosphate and nucleating agent technology, which is applied in the field of preparation of organophosphate nucleating agents, can solve the problems of large time and energy consumption, complicated operation, and reduced nucleation performance, and achieve low energy consumption and high nucleation efficiency The effect of high and narrow particle size distribution

Active Publication Date: 2010-03-10
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 The nucleating 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
Because this method needs to grind the raw materials in two different equipment, and the grinding time is long, the energy consumption is high, the operation is complicated, and the output is not high
Another disadvantage of this method is that if the grinding or ball milling time is short, the particles will not be fine enough to obtain micronized products, and if the grinding or ball milling time is long, it will not only consume a lot of time and energy, but also destroy the original crystalline state of the nucleating agent, resulting in Reduced nucleation performance

Method used

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  • Method for preparing organic phosphate nucleating agent through ultrasonic sedimentation
  • Method for preparing organic phosphate nucleating agent through ultrasonic sedimentation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh the crude material of 2,2′-methylene-bis(4-methyl, 6-tert-butylphenoxy) potassium phosphate, add it to the mixed organic solvent of acetone and 1,4-dioxane, In organic solvents, according to the mass ratio,

[0031] Acetone:1,4-dioxane=3:1,

[0032] After stirring and dissolving completely, add water to prepare a raw material solution, according to the mass ratio,

[0033] Organic solvent: water: crude 2,2'-methylene-bis(4-methyl, 6-tert-butylphenoxy) phosphate potassium = 3:0.4:1;

[0034] Place the above-mentioned raw material solution in a water bath of the ultrasonic generator at a temperature of 25°C. Turn on the ultrasonic wave and perform ultrasonic oscillation for 45 minutes, the ultrasonic frequency is 59kHz, the ultrasonic power density is 150 watts per liter of solution, and white flocculent precipitate is produced. Then suction filtration, and the filter cake was dried at 80°C for 2 hours to obtain the corresponding 2,2'-methylene-bis(4-methyl, 6-tert-butylp...

Embodiment 2

[0035] Weigh the crude material of 2,2'-methylene-bis(4,6-di-tert-butylphenoxy) sodium phosphate, add it to the acetone solvent, stir to dissolve completely, then add water to obtain a raw material solution, press Mass ratio,

[0036] Acetone solvent: water: 2,2'-methylene-bis(4,6-di-tert-butylphenoxy) sodium phosphate crude product=3:0.4:1,

[0037] Place the above-mentioned raw material solution in the water bath of the ultrasonic generator, the temperature of the water bath is 25° C., turn on the ultrasonic wave and perform ultrasonic oscillation for 45 minutes, the ultrasonic frequency is 59 kHz, and the ultrasonic power density is 100 W / L of the solution. A white flocculent precipitate is produced, and then filtered with suction. The filter cake is dried at 80°C for 2 hours to obtain a free-flowing white powder, which is the corresponding 2,2'-methylene-bis(4,6-di-tert-butyl) Phenoxy) sodium phosphate nucleating agent product. The product is a free-flowing white powder with ...

Embodiment 3

[0039] Weigh bis[2,2'-methylene-bis(4,6-di-tert-butylphenoxy) phosphoric acid] hydroxyaluminum crude raw material, add it to the mixed organic solvent of ethanol and petroleum ether, press in the organic solvent Mass ratio,

[0040] Ethanol: Petroleum Ether = 1:1,

[0041] After stirring and dissolving completely, add water to prepare a raw material solution, according to the mass ratio,

[0042] Organic solvent: water: bis[2,2'-methylene-bis(4,6-di-tert-butylphenoxy) phosphoric acid] crude aluminum hydroxy = 4:0.5:1,

[0043] Place the above-mentioned raw material solution in the water bath of the ultrasonic generator, the temperature of the water bath is 25° C., turn on the ultrasonic wave and perform ultrasonic oscillation for 45 minutes, the ultrasonic frequency is 40 kHz, and the ultrasonic power density is 100 W / L of the solution. A white flocculent precipitate is produced, and then filtered with suction. The filter cake is dried at 80°C for 2 hours to obtain a free-flowing whi...

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Abstract

The invention relates to a method for preparing an ultra-fine organic phosphate nucleating agent through ultrasonic sedimentation. The method controls the separation grain size of the organic phosphate through the condition of a solvent and the ultrasonic sedimentation to finally obtain the ultra-fine organic phosphate nucleating agent. The organic phosphate nucleating agent has high nucleating efficiency during polypropylene processing, and can finally form tiny polypropylene spherulites, thereby significantly increasing various performances of rigidity, strength, distortion temperature and the like of resin.

Description

Technical field [0001] The invention relates to a polypropylene nucleating agent, in particular to a preparation method of an organic phosphate nucleating agent. Background technique [0002] Substituted aryl organic phosphates are widely used as nucleation modifiers for polypropylene resins, and are used in the modification of polypropylene resins. Among them, 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 properties of these resins. Literature "High-performance polypropylene-nucleating agent" ("Chemical Industry", 1999(8), p11), "The effect of nucleating agent on polypropylene properties" ("Synthetic Resins and Plastics", 2001, 18( 4), 39-41) are reported. [0003] At present, the synthesis of substituted aryl organic phosphates is to prepare diaryl organic phosphates by reacting substituted aryl phenols with phosphorylatio...

Claims

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Application Information

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IPC IPC(8): C08K5/527C08L23/12
Inventor 顾民张丽英李伟徐耀辉张浩吕静兰
Owner CHINA PETROLEUM & CHEM CORP
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