Preparation method of amide polypropylene beta crystal form nucleating agent by taking p-phenylenediamine as skeleton

A technology for p-phenylenediamine and amides, which is applied in the field of nucleating agent preparation, can solve the problems of expensive catalysts, the synthesis method is not specific enough, and is not economical enough, and achieves the effects of simple operation, convenient source of raw materials, and stable storage.

Active Publication Date: 2014-01-29
山西科通化工有限公司
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Problems solved by technology

The synthetic methods given in these documents are not specific enough, a

Method used

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  • Preparation method of amide polypropylene beta crystal form nucleating agent by taking p-phenylenediamine as skeleton

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example 1

[0024] In a 500 ml reaction flask equipped with stirring, thermometer, reflux condensation tail gas absorption device and constant pressure dropping funnel device, add 150 ml of solvent chloroform, 10.8 g of p-phenylenediamine, and 16 g of acid-binding agent pyridine, and drop them under ice bath conditions. Add 30g of cyclohexanoyl chloride, after the dropwise addition, heat up to reflux temperature and react for 3h. After the reaction is terminated, add an appropriate amount of water to evaporate the solvent, wash and dry with hot water ethanol to obtain 31.7g of the product, with a melting point of 333.8°C, and the purity according to HPLC analysis is greater than 98%.

example 2

[0026] In a 2000 ml reaction flask equipped with stirring, thermometer, reflux condensation tail gas absorption device and constant pressure dropping funnel device, add 1000 ml of solvent chloroform, 64.8 g of p-phenylenediamine, and 96 g of acid-binding agent pyridine, and drop them under ice bath conditions. Add 180g of cyclohexanoyl chloride, after the dropwise addition, heat up to reflux temperature and react for 3h. After the reaction is terminated, add an appropriate amount of water to evaporate the solvent, wash and dry with hot water ethanol to obtain 195.7g of the product, with a melting point of 333.6°C, and the purity according to HPLC analysis is greater than 98%.

[0027] The structure of the nucleating agent is determined by infrared spectrum, elemental analysis and high-performance liquid chromatography analysis, and good effect is obtained when it is tried for polypropylene.

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Abstract

The invention discloses a preparation method of an amide polypropylene beta crystal form nucleating agent by taking p-phenylenediamine as a skeleton. The preparation method disclosed by the invention comprises the following steps of putting p-phenylenediamine into a flask, adding a solvent and an acid-binding agent in sequence, carrying out the temperature in an ice-water bath, dropping cyclohexanecarboxylic acid chloride, controlling the dropping temperature, increasing the temperature to reflux temperature after dropping, keeping the temperature for three hours, evaporating out the solvent, and washing through hot water and alcohol to obtain N-N'-1,4 benzene dicyclohexyl formamide. The preparation method disclosed by the invention has the benefits that raw materials are easily obtained, the process operation is simple, and the prepared product is high in yield and purity, has a good nucleating effect and is easy for industrialization.

Description

technical field [0001] The invention relates to a preparation method of N-N'-1,4-phenylenedicyclohexylcarboxamide, an amide polypropylene beta crystal nucleating agent with p-phenylenediamine as a skeleton, and belongs to the field of nucleating agent preparation. Background technique [0002] The structural formula of N-N'-1,4-phenylenedicyclohexylcarboxamide, the nucleating agent of polypropylene beta crystal form, is: [0003] [0004] The literature reports on N-N'-1,4-benzenedicyclohexylcarboxamide mainly contain the following items: [0005] 1 The patent whose publication number is CN102634119 mentions the structure and application of N-N'-1,4-benzenedicyclohexylcarboxamide, but does not disclose its synthesis method. [0006] 2 The patent with the publication number CN 1098725 mentions (1) adding an activator such as phosphorus pentoxide or phosphite, and reacting p-phenylenediamine with cyclohexane carboxylic acid to obtain the corresponding N-N'-1,4 phenylenedi...

Claims

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Application Information

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IPC IPC(8): C07C233/62C07C231/02
Inventor 王克智李训刚刘凤玉张惠芳李向阳毛晨曦张建军王冉王改敬代燕琴王凯张鸿宇巩翼龙
Owner 山西科通化工有限公司
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