Preparation method of polypropylene beta crystalline nucleating agent

A technology of β crystal form and nucleating agent, which is applied in the field of preparation of polypropylene β crystal form nucleating agent, and can solve problems such as inability to carry out large-scale industrial production

Active Publication Date: 2011-05-04
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the defects in the prior art that the preparation of the polypropylene beta crystal form nucleating agent needs to be reacted under high pressure, which has strict requirements on the product

Method used

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  • Preparation method of polypropylene beta crystalline nucleating agent

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preparation example Construction

[0011] The preparation method of the polypropylene beta crystal form nucleating agent provided by the invention comprises that in the presence of a catalyst and a solvent, a dibasic carboxylic acid is contacted with an amine to carry out condensation reaction. In the present invention, the selection of the catalyst and the solvent takes into account the solubility of the solvent to the catalyst and the reaction raw materials such as dicarboxylic acid and amine and the reactivity of the reaction system of the dicarboxylic acid and amine, Therefore, in the method provided by the invention, the catalyst is selected from one or more of phosphorus pentoxide, polyphosphoric acid and triphenyl phosphite, and the polyphosphoric acid can be diphosphoric acid, tripolyphosphoric acid and tetrapolyphosphoric acid. At least one of phosphoric acid (also known as polyphosphoric acid), and pyridine is selected as the solvent, so as to ensure that the reaction system of the dicarboxylic acid an...

Embodiment 1

[0022] This example is used to illustrate the preparation method of the polypropylene β crystal form nucleating agent provided by the present invention.

[0023] Preparation of N, N'-dicyclopentyl terephthalamide

[0024] Add 0.022 mol of terephthalic acid and 100 ml of pyridine (1.24 mol) into a four-port reaction kettle equipped with a stirrer, an addition funnel, a thermometer and a condenser, and stir to dissolve. Then, add 0.054 moles of cyclopentylamine and 0.054 moles of triphenyl phosphite under stirring, and react at 100°C for 1.5 hours under normal pressure, then add a solution with a volume ratio of isopropanol / water of 1:1 300 ml, stirred for 30 minutes, then filtered, and the filtered precipitate was washed with tap water, and dried to obtain 6.3 g of white powder as nucleating agent A1. It was identified that the white powder was 0.021 mol of N,N'-dicyclopentyl terephthalamide, therefore, the yield was 95.45%.

Embodiment 2

[0029] This example is used to illustrate the preparation method of the polypropylene β crystal form nucleating agent provided by the present invention.

[0030] Preparation of N, N'-dihexyl-2,6-naphthalene dicarboxamide

[0031] Add 0.026 mol of 2,6-naphthalene dicarboxylic acid and 100 ml of pyridine (1.24 mol) into a four-port reaction kettle equipped with a stirrer, an addition funnel, a thermometer and a condenser, and stir to dissolve. Then, add 0.052 mole of hexylamine and 0.062 mole of polyphosphoric acid under stirring, react at 120°C for 1 hour under normal pressure, add isopropanol / water volume ratio and be 300 milliliters of the solution of 1:1, Stir for 30 minutes, then filter, wash the filtered precipitate with tap water, and dry to obtain 9.15 g of white powder as nucleating agent A2. It was identified that the white powder was 0.024 mol of N,N'-dihexyl-2,6-naphthalene dicarboxamide, therefore, the yield was 92.31%.

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Abstract

The invention relates to a preparation method of a polypropylene beta crystalline nucleating agent, comprising the following steps of: contacting dicarboxylic acid with amine to carry out condensation reaction in the presence of a catalyst and a solvent, wherein the amine is primary amine and/or secondary amine, the catalyst is one or more of phosphorus pentoxide, polyphosphoric acid and triphenyl phosphate, the solvent is pyridine, and the mole ratio of the using amounts of the catalyst to the pyridine is 1: (10-30). The preparation method can be used for sufficiently preparing the amides polypropylene beta crystalline nucleating agent from the primary amine and/or the secondary amine under normal pressure.

Description

technical field [0001] The invention relates to a preparation method of a polypropylene beta crystal form nucleating agent. Background technique [0002] Since Leugering discovered in 1967 that the addition of γ crystal dye quinacridone can transform α crystal polypropylene into β crystal, the research on β crystal nucleating agents in the world has been carried out for more than 40 years. [0003] In 1995, Wolfschwenger Johannes and others used a pimelate nucleating agent to obtain β-crystalline polypropylene during the granulation process of polypropylene, but the modification effect of the nucleating agent was not obvious, and the crystallization temperature did not increase significantly. On the contrary, the flexural modulus is reduced, and at the same time, due to the thermal decomposition of some dicarboxylates, precipitation is formed in the final product. On this basis, A.L Besson et al. used imidic acid to react with fatty acid salts containing II a metals in the ...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/65C07C233/06C08K5/20C08L23/12
Inventor 张敏宏张毅李卫红张新军钟健丁京殷喜平郑建坡伊红亮蒋绍洋赵立红孟凡立刘波安少军
Owner CHINA PETROLEUM & CHEM CORP
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