Preparation method of ultrafine organic phosphate nucleating agent

An organic phosphate and nucleating agent technology, applied in the petrochemical field, can solve the problem of inability to obtain ultra-fine organic phosphate nucleating agent, etc., and achieve the effects of improving rigidity, uniform particle size and stable quality

Active Publication Date: 2012-03-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a preparation method of an ultrafine organophosphate nucleating agent, which is used to solve the problem that the ultrafine organophosphate nucleating agent cannot be obtained in the prior art

Method used

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  • Preparation method of ultrafine organic phosphate nucleating agent
  • Preparation method of ultrafine organic phosphate nucleating agent
  • Preparation method of ultrafine organic phosphate nucleating agent

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preparation example Construction

[0029] A kind of ultrafine preparation method of organophosphate nucleating agent, comprises the following steps:

[0030] The first step is to dissolve the raw materials:

[0031] Be that the crude product of the substituted diaryl organic phosphate nucleating agent of formula (I) is a raw material with the general structure formula,

[0032]

[0033] (I) In the formula: R1 is the alkyl group of C1~C6, R2 is the alkyl group of C1~C6, R3 is the alkyl group of hydrogen atom or C1~C4, M is one of following metal atom or group: sodium, potassium , lithium, calcium, magnesium, aluminum, zinc, barium, copper, tin, zirconium, aluminum hydroxy, ammonium; n is 1 or 2;

[0034] Use at least one of the following as a solvent: acetone, ethanol, methanol, propanol, isopropanol, butanol, petroleum ether, tetrahydrofuran, ethyl acetate, toluene, ethylbenzene, N-N dimethylformamide and 1,4 - dioxane;

[0035] The raw material is added into the solvent and stirred to form a raw material...

Embodiment 1

[0051] Weigh 2,2'-methylene-bis(4-methyl, 6-tert-butylphenoxy)potassium phosphate crude raw material, add acetone and 1,4-dioxane mixed solvent, by molar ratio , acetone: 1,4-dioxane = 80: 20, after stirring and dissolving completely, a solution with a raw material content of 30% was obtained.

[0052] Use the feed pump to inject the above solution into the spray dryer, and the gas-liquid mass ratio is M G : M L =1.6:1, the air inlet temperature of the spray dryer is 140°C-160°C, and the outlet air temperature is 40°C-60°C. After drying by spraying, the solid dry powder was collected in a cyclone.

[0053] Add the solid dry powder into the mixed organic solvent of acetone and 1,4-dioxane, by mass ratio, acetone:1,4-dioxane=3:1, then add water to prepare the raw material solution, press Mass ratio, organic solvent: water: 2,2'-methylene-bis(4-methyl, 6-tert-butylphenoxy)potassium phosphate crude product=3:0.4:1;

[0054] The above raw material solution was placed in a const...

Embodiment 2

[0056] Weigh 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate crude raw material, add it into ethanol, stir and dissolve completely, and obtain a solution with a raw material content of 20%.

[0057] Use a feed pump to inject the above solution into the spray dryer. The air inlet temperature of the spray dryer is 140°C-160°C, the outlet air temperature is 40°C-60°C, and the gas-liquid mass ratio is M G : M L =1.45:1. After drying by spraying, the solid dry powder was collected in a cyclone.

[0058] Add the solid dry powder into acetone, and then add water according to the mass ratio to obtain a raw material solution, according to the mass ratio, organic solvent: water: 2,2'-methylene-bis(4,6-di-tert-butylbenzene Oxygen)sodium phosphate crude product=2:1.8:1.

[0059] The above raw material solution was placed in a constant temperature water bath with a temperature of 25 °C. Start stirring, carry out solvent dispersion and crushing, stir for 45 minutes, collect...

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Abstract

The invention discloses a preparation method of an ultrafine organic phosphate nucleating agent, and the method comprises the following steps: dissolving a substituted diaryl organic phosphate nucleating agent crude product which is used as a raw material to obtain a raw material solution; performing spray drying of the obtained raw material solution in a spraying manner; then adding the obtainedspray-drying product into a solvent, adding water, stirring and dispersing in the combined solvent for crushing; performing liquid-solid separation of the crushed material, drying to obtain the ultrafine organic phosphate nucleating agent. The ultrafine organic phosphate nucleating agent prepared by the method of the invention has stable quality, a uniform particle size, and high yield, and the crystal form of the nucleating agent is not destroyed. The nucleating agent product can increase nucleation effect, and reduce the using amount of the nucleating agent.

Description

technical field [0001] The invention relates to the technical field of petrochemical industry, in particular to a preparation method of an ultrafine organic phosphate nucleating agent. Background technique [0002] Substituted aryl organic phosphates are widely used as nucleating modifiers for polypropylene resins, and are used in the modification of polypropylene resins, where 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 (see "High Performance of Polypropylene - Synthesis Nucleating agent", "Chemical Industry", 1999(8), p11), and "The influence of nucleating agent on the properties of polypropylene", "Synthetic Resins and Plastics", 2001, 18(4), 39-41). [0003] At present, the synthesis of substituted aryl organic phosphates is to prepare diaryl organic phosphates by reacting substituted ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/12C08K9/00C08K5/527
Inventor 顾民张丽英徐耀辉吕静兰张浩李伟褚海斌
Owner CHINA PETROLEUM & CHEM CORP
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