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Preparation method of organic phosphate type polypropylene transparent nucleating agent

A technology of transparent nucleating agent and organic phosphate, which is applied in the fields of organic chemistry, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc. problem, to achieve the effect of improving transparency, high conversion rate and fine particle size

Active Publication Date: 2013-05-01
国家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

However, due to the high melting point of organic phosphate nucleating agents, generally above 300 ° C, which is higher than the melting temperature of polymers, resulting in poor dispersion and poor anti-reflection effect, the recommended dosage is about 0.3% of the base resin. , and the cost is higher

Method used

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  • Preparation method of organic phosphate type polypropylene transparent nucleating agent
  • Preparation method of organic phosphate type polypropylene transparent nucleating agent
  • Preparation method of organic phosphate type polypropylene transparent nucleating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1: the preparation of nucleating agent

[0045] (1) install thermometer and reflux condenser on the four-necked flask of 250ml;

[0046] (2) Take 12.72g of the raw material 2,2′-methylenebis(4,6-di-tert-butylphenyl)sodium phosphate and add it to a four-necked flask, and then add 100 ml of methanol to the flask;

[0047] (3) Warm up to 40°C under nitrogen protection and stirring, and stir for 15 minutes to completely dissolve 2,2'-methylenebis(4,6-di-tert-butylphenyl)sodium phosphate;

[0048] (4) At a constant temperature of 40°C, slowly add dropwise 15 ml of a concentrated methanol solution containing 1.669 g of aluminum trichloride hexahydrate;

[0049] (5) After the dropwise addition is completed, keep the reaction at 40°C for 4 hours;

[0050] (6) Add 16ml 40% silica sol and continue the reaction for 1h;

[0051] (7) After the reaction is completed, cool to room temperature, adjust the pH value to 6.0 with NaOH solution, filter after standing still, wa...

Embodiment 2

[0052]Example 2: Take 12g of the raw material 2,2'-methylenebis(4,6-di-tert-butylphenyl)sodium phosphate, add 100ml of ethanol, heat to 70°C under the protection of nitrogen atmosphere, and stir to 2,2 ′-Methylenebis(4,6-di-tert-butylphenyl)sodium phosphate is completely dissolved, and the temperature is kept at 70°C, and the ethanol solution containing 1.7g of aluminum trichloride hexahydrate is slowly added dropwise. After the drop is completed, the constant temperature reaction 1h, add 10ml of 5% silica sol, continue the constant temperature reaction for 1.5h, cool to room temperature, adjust the pH value to 6.0 with NaOH solution, filter after standing, wash the filter cake repeatedly with water and dry to obtain a white powder, which is the desired product.

Embodiment 3

[0053] Example 3: Take 13g of the raw material 2,2'-methylenebis(4,6-di-tert-butylphenyl)sodium phosphate, add 100ml of ethylene glycol, heat to 80°C under the protection of nitrogen atmosphere, and stir to 2 , 2′-methylenebis(4,6-di-tert-butylphenyl)sodium phosphate is completely dissolved, keep the temperature at 80°C, slowly add ethylene glycol solution containing 1.6g aluminum trichloride hexahydrate dropwise, and the dropwise addition is completed Afterwards, react at a constant temperature for 6 hours, add 50ml of 20% silica sol, continue to react at a constant temperature for 0.5h, cool to room temperature, adjust the pH value to 6.0 with NaOH solution, filter after standing, wash the filter cake repeatedly and dry to obtain a white powder, which is desired product.

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Abstract

The invention discloses a preparation method of an organic phosphate type polypropylene transparent nucleating agent, which comprises the steps of: adding 2,2'- methylenebis(4,6-di-tert-butylphenyl) sodium phosphate into liquid alcohol, mixing, heating and stirring under the atmosphere of nitrogen until 2,2'-methylenebis(4,6-di-tert-butylphenyl) sodium phosphate is completely dissolved; adding analcoholic solution of aluminium trichloride hexahydrate for reacting at constant temperature; adding silica sol to continue reaction at constant temperature; cooling to room temperature; regulating apH value to 6.0; and standing, filtering and drying to obtain the transparent nucleating agent. The transparent nucleating agent can be used as a homo-polypropylene or polypropylene random copolymer nucleating agent, and is soluble in polymer melts at the melting temperature of polymers, therefore, nucleated products induced by the nucleating agent have higher transparency. The preparation methodof the nucleating agent has a simple process, and the product of the nucleating agent have the advantages of high conversion rate, fine grain size, low melting point, better dispersity, high nucleating efficiency and no agglomeration phenomenon in the melt extrusion process, and is an excellent polypropylene nucleating agent.

Description

technical field [0001] The invention relates to the technical field of polypropylene nucleating agents, in particular to a preparation method of an organophosphate type polypropylene transparent nucleating agent. Background technique [0002] Polypropylene is a kind of semi-transparent crystalline material with excellent performance, low price and wide application. By adding nucleating agent, its crystallinity and transparency can be improved, and transparent polypropylene material with better performance can be obtained. [0003] There are many types of polypropylene nucleating agents, mainly inorganic and organic. Inorganic nucleating agents mainly include talcum powder, white carbon black and mica, etc. They are the earliest and cheap, and can increase the rigidity and heat distortion temperature of polymer products, but the disadvantage is that they affect the transparency and surface gloss of polypropylene. There are many kinds of organic nucleating agents, and they ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08L23/12C08L23/14C08K5/527
Inventor 于杰刘辉张敏敏秦舒浩何敏
Owner 国家复合改性聚合物材料工程技术研究中心