Ultrafine organic ammonium phosphate nucleating agent and preparation method thereof

An organic ammonium salt and organic phosphate technology, applied in the field of material science, can solve the problems of high solvent use requirements, complex preparation process, wide particle size distribution, etc., and achieve short processing time, simple process and narrow particle size distribution. Effect

Active Publication Date: 2013-04-03
贵州省复合改性聚合物材料工程技术研究中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is: to provide a kind of ultra-micronization organophosphate ammonium salt nucleating agent and preparation method thereof, it solves the problem that existing organophosphate ammonium salt nucleating agent has larger particle size, wide particle size distribution and complex preparation process As well as the high requirements for the use of solvents, so as to improve the performance of the organophosphate ammonium salt nucleating agent, and become a new type of high-efficiency organophosphate nucleating agent

Method used

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  • Ultrafine organic ammonium phosphate nucleating agent and preparation method thereof
  • Ultrafine organic ammonium phosphate nucleating agent and preparation method thereof
  • Ultrafine organic ammonium phosphate nucleating agent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Example 1 of the present invention: Weigh 5g of unrefined 2,2'-methylene-bis(4,6-di-tert-butylphenyl) ammonium salt nucleating agent, and add it directly to the supercritical CO 2 Inside the reactor, the reactor temperature is set to 40℃, the pressure is 20MPa, the speed is 200 rpm, supercritical CO 2 React in the medium for 2h to obtain organic phosphate supercritical CO 2 Processing product; supercritical CO 2 The processed product is added to 25ml of water, and the material B is obtained after fully stirring and dispersing; the material B is subjected to rotary evaporation and drying to obtain an ultrafine organic phosphate nucleating agent.

[0025] After testing, in Example 1, the yield of the ultrafine organic phosphate nucleating agent was more than 95%, and its shape was figure 2 Shown.

[0026] according to figure 2 It can be seen that the product of Example 1 forms a woven and fluffy structure through fine needle-like bodies. The average long diameter of the needle...

Embodiment 2

[0027] Example 2 of the present invention: Weigh 5g of unrefined 2,2'-methylene-bis(4,6-di-tert-butylphenyl) ammonium salt nucleating agent, and directly add it to the reaction kettle, 40℃, 20MPa, 200 rpm, supercritical CO 2 React in the medium for 2h to obtain organic phosphate supercritical CO 2 Processing product; supercritical CO 2 The processed product was dissolved in 56.5ml (with a mass of 45g) of absolute ethanol, and then 5ml of water was added and dispersed in a combined solvent to obtain material B; material B was dried by rotary evaporation to obtain an ultrafine organic phosphate nucleating agent.

[0028] After testing, in Example 2, the yield of the ultrafine organic phosphate nucleating agent was more than 95%, the average particle size was 300 nm, and the shape was as image 3 Shown.

[0029] according to image 3 It can be seen that the product has a uniform spherical structure with an average particle size of less than 300 nm, which can be uniformly dispersed in t...

Embodiment 3

[0030] Example 3 of the present invention: Weigh 5g of unrefined 2,2'-methylene-bis(4,6-di-tert-butylphenyl) ammonium salt nucleating agent, and directly add it to the reactor, 40℃, 20MPa, 200 rpm, co-solvent 25ml absolute ethanol (mass 20g), supercritical CO 2 React in the medium for 2h to obtain organic phosphate supercritical CO 2 Processing product; supercritical CO 2 The processed product was dissolved in 50ml (40g in mass) of absolute ethanol and dispersed in a combined solvent to obtain material B; material B was dried by rotary evaporation to obtain an ultrafine organic phosphate nucleating agent.

[0031] After testing, in Example 2, the yield of the ultrafine organic phosphate nucleating agent was more than 95%, and the shape was as Figure 4 Shown.

[0032] according to Figure 4 It can be seen that the edge of the product is an aggregated structure of needle-like bodies. The average long diameter of the needle-like bodies is 300 nm, which fall off during processing and...

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Abstract

The invention discloses an ultrafine organic ammonium phosphate nucleating agent and a preparation method thereof. The structure formula of the nucleating agent is as described in the specification, wherein R1, R2, R3 and R4 are all hydrogen atoms or alkyls or branched chain alkyls of C1-C4; R1, R2, R3 and R4 are identical, partially identical or totally different; and the partially identical structure can be a left-and-right symmetrical structure, that is, R1 is identical with R4; R2 is identical with R3; but R1 is different from R4. The ultrafine organic ammonium phosphate nucleating agent is prepared by using supercritical CO2 via a solvent dispersion method; the product is ultrafine powder particles, is dispersed uniformly, and has narrow particle size distribution and high nucleating efficiency; and finally finer polypropylene sphaerocrystal can be obtained. The preparation method is simple in process, short in processing time and low in energy consumption; and the prepared nucleating agent has good crystal forms and fine particles.

Description

Technical field [0001] The invention relates to the field of materials science, in particular to an ultrafine organic ammonium phosphate nucleating agent and a preparation method thereof. Background technique [0002] The applicant’s previous research results show that organic ammonium phosphate is a new and effective nucleating agent for semi-crystalline resins, which can significantly improve the transparency and mechanical strength of the resin, among which 2,2'-methylene Di-bis(4,6-di-tert-butylphenyl) ammonium phosphate has the same nucleation effect as 2,2'-methylene-bis(4,6-di-tert-butylphenyl) sodium phosphate , And its melting point is significantly reduced. This nucleating agent is a columnar crystalline compound. In order to further improve its performance and make it a new type of high-efficiency nucleating agent instead of sodium salt nucleating agent, ultra-fine processing is required to reduce its particle size , To further improve its dispersion compatibility in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/527C08L23/12
CPCY02P20/54
Inventor 于杰龙丽娟秦舒浩何文涛张凯李娟向宇姝尹晓刚何敏
Owner 贵州省复合改性聚合物材料工程技术研究中心
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