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Preparation method for nano-montmorillonite modified organophosphate nucleating agent

An organic phosphate and nano-montmorillonite technology, applied in the field of organic phosphate nucleating agents, can solve problems such as reducing the heat release rate of resin, improve thermal stability and various mechanical properties, reduce agglomeration, and enhance dispersibility. Effect

Active Publication Date: 2012-02-22
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

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Problems solved by technology

When the nano-montmorillonite is dispersed in the resin, the montmorillonite sheet will accumulate on the surface of the material along with the gasified resin, forming a denser carbon layer, which reduces the heat release rate of the resin.

Method used

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  • Preparation method for nano-montmorillonite modified organophosphate nucleating agent
  • Preparation method for nano-montmorillonite modified organophosphate nucleating agent
  • Preparation method for nano-montmorillonite modified organophosphate nucleating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Take 10 g of nano-montmorillonite and disperse it in 50% (weight) ethanol aqueous solution to make a solution with a concentration of 0.048 g / ml, then add 3.28 g of γ-aminopropyltriethoxysilane, and reflux at 70 ° C 24h, rotary steamed to 50ml to obtain amino-modified nano-montmorillonite, and then another 6.18g of 2,2'-methylene-bis(4,6-di-tert-butylphenol) phosphorus oxychloride was dissolved in 50ml of absolute ethanol Add amino-modified nano-montmorillonite, stir at 50°C for 3 hours, filter, wash, and vacuum-dry to obtain nano-montmorillonite-modified organophosphate nucleating agent. The obtained nucleating agent has good nucleating effect, and has the functions of flame retardancy and gas barrier.

[0016] The infrared spectra of nano-montmorillonite, amino-modified nano-montmorillonite, organophosphorus oxychloride and modified organophosphate are as follows: figure 1 As shown, the amino-modified nano-montmorillonite has a wave number of 1080cm -1 Si...

Embodiment 2

[0022] Embodiment 2: get nanometer montmorillonite 9.5g to be dispersed in the ethanol aqueous solution of 45% (weight) and make the solution that concentration is 0.045g / ml, then add 3.0g gamma-aminopropyltriethoxysilane, at 65 Reflux at ℃ for 24 hours, rotary evaporate to 50ml to obtain amino-modified nano-montmorillonite, and then take another 5.5g of 2,2'-methylene-bis(4,6-di-tert-butylphenol)phosphoryl chloride and dissolve it in 50ml without Add amino-modified nano-montmorillonite to water ethanol, stir at 50° C. for 3 hours, filter, wash, and vacuum-dry to obtain nano-montmorillonite-modified organophosphate nucleating agent. The obtained nucleating agent has good nucleating effect, and has the functions of flame retardancy and gas barrier.

Embodiment 3

[0023] Embodiment 3: get nanometer montmorillonite 11.0g to be dispersed in the ethanol aqueous solution of 55% (weight) and make the solution that concentration is 0.05g / ml, then add 4.5g gamma-aminopropyltriethoxysilane, at 70 Reflux at ℃ for 24 hours, rotary evaporate to 50ml to obtain amino-modified nano-montmorillonite, and then take another 6.8g of 2,2'-methylene-bis(4,6-di-tert-butylphenol)phosphoryl chloride and dissolve it in 50ml without Add amino-modified nano-montmorillonite to water ethanol, stir at 50° C. for 3 hours, filter, wash, and vacuum-dry to obtain nano-montmorillonite-modified organophosphate nucleating agent. The obtained nucleating agent has good nucleating effect, and has the functions of flame retardancy and gas barrier.

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Abstract

The present invention discloses a preparation method for a nano-montmorillonite modified organophosphate nucleating agent. The method comprises the following steps: dispersing nano-montmorillonite in an aqueous solution of ethanol; adding a silane coupling agent; carrying out refluxing under a heating condition to obtain amino-modified nano-montmorillonite; adding a 2,2'-methylene-bis(4,6-di-tert-butylphenol)phosphoryl chloride solution, and stirring; after completing the reaction, carrying out treatments of filtering, washing and vacuum drying to obtain the nano-montmorillonite modified organophosphate nucleating agent. According to the present invention, the organophosphate is linked on the surface of the nano-montmorillonite by chemical bonds so as to effectively reduce the agglomeration of the organophosphate in the resin matrix, and enhance the dispersity of the organophosphate in the matrix, such that the heterogeneous nucleation effect of the nucleating agent can be effectivelyprovided; with the introduction of the inorganic nano-montmorillonite, thermal stability and various mechanical properties of the material can be further improved.

Description

technical field [0001] The invention relates to the technical field of organophosphate nucleating agents, in particular to a preparation method of a nano-montmorillonite-modified organophosphate nucleating agent. Background technique [0002] Organophosphate nucleating agents are widely used in the processing of high crystallinity polypropylene, which can endow products with higher transparency, rigidity and heat distortion temperature. Organophosphate nucleating agents mainly include phosphate metal salts and Phosphate ester basic metal salts and their complexes, etc. These products can also be divided into three generations. The first generation of products came out in the early 1980s, represented by NA-10 of Japan Asahi Denka; the second generation of products was NA-11 launched by Asahi Denka in the mid-1980s, and its nucleation performance was better than that of NA- 10. When the compounding amount is less than 0.1%, the stiffening effect is even higher than that of so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/02C08K5/523
Inventor 于杰秦舒浩何敏何文涛吴丹华许琛罗筑张敏敏秦军鲁圣军薛斌李庆丰张纯郭建兵
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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