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Normal pressure synthesis method of oleamide

An oleic acid amide, atmospheric synthesis technology, applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds and other directions, can solve the problems of side reactions, high reaction temperature and pressure, difficult to control, etc. The effect of industrialized production, mild process conditions and low cost

Inactive Publication Date: 2014-12-10
NANTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are many synthetic routes of oleic acid amide in the industry, and there are generally disadvantages such as long reaction time, high reaction temperature and pressure, and difficult separation and purification.
Among them, the synthesis of oleic acid amide from fatty acid and ammonia needs to be carried out under high temperature and higher pressure; the reaction of oleoyl chloride and ammonia is too intense, difficult to control, and causes side reactions; the reaction speed of acid anhydride and ammonia is very slow; methyl oleate and ammonia Ammonia reaction also requires high pressure, and the process is more complicated

Method used

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  • Normal pressure synthesis method of oleamide
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  • Normal pressure synthesis method of oleamide

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Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: the preparation method of solid acid catalyst

[0021] (1) Preparation of immersion liquid

[0022] Add 6.2 g (0.1 mol) of boric acid, 29.4 g (0.3 mol) of phosphoric acid, and 9.382 g (0.005 mol) of ammonium phosphomolybdate to 250 mL of water, heat, stir to dissolve, and filter to obtain a milky white dipping solution.

[0023] (2) Preparation of catalyst

[0024] Grind the granular ZSM-5 molecular sieve, sieve it, take the 40-60 mesh molecular sieve and dry it at 150 ° C for 1.5 hours, after cooling, it is completely immersed in the immersion solution described in (1), immersed for 24 hours, filtered and placed in a crucible , dried at 60°C for 1h, dried at 80°C for 1h, dried at 100°C for 1h, dried at 120°C for 1h, dried at 150°C for 5h, then transferred to a muffle furnace and calcined at 200°C, 300°C, and 400°C respectively 1h, calcined at 500°C for 2h, cooled to room temperature, taken out with crucible tongs, sieved to obtain a solid acid catalyst,...

Embodiment 2

[0025] Embodiment 2: the synthesis technique of atmospheric catalysis synthesis oleic acid amide

[0026] In a 100mL three-necked flask, add 5.68g (0.02mol) oleic acid, 2.4g (0.04mol) urea, 0.17g solid acid catalyst, stir mechanically, heat up to 160°C, react for 2h, and cool to about 100°C , add 10% potassium hydroxide methanol solution and 10mL water, adjust the pH value of the solution to 8~9, filter while hot, remove the solid acid catalyst, transfer the filtrate to a 250mL three-necked flask, add 20mL absolute ethanol and 1g activated carbon, Heat to reflux for 40min, filter while hot, remove activated carbon, transfer the filtrate to a 250ml beaker, cool below 0°C, and filter to obtain the crude product. The crude product was recrystallized with acetone to obtain a white powdery solid, which was vacuum-dried at 50°C and weighed 5.1 g. The yield of the product was 90.6%, and the melting point was 73.4°C-75.6°C. The product purity of oleic acid amide was analyzed by HPLC ...

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Abstract

The invention discloses a normal pressure synthesis method of oleamide. The method comprises the following steps: (1) preparation of a solid acid catalyst, namely adding boric acid, phosphoric acid and phosphomolybdic acid to water, heating and stirring until the materials are dissolved, and filtering to obtain impregnation liquid; grinding a ZSM-5 molecular sieve, sieving, drying and cooling, impregnating in the impregnation liquid, filtering, drying and baking at high temperature to obtain the solid acid catalyst; and (2) catalytic synthesis of oleamide under normal pressure, namely conducting a synthesis reaction under normal pressure by taking oleic acid and urea as raw materials and the solid acid catalyst as a catalyst to obtain oleamide. According to the synthesis method disclosed by the invention, a novel solid acid catalyst is prepared, and the oleamide is prepared from oleic acid and urea through catalytic synthesis under normal pressure and not too high temperature; and the synthesis method is gentle in technological condition, safe, low in cost, favorable for industrial production and high in yield.

Description

technical field [0001] The present invention relates to a normal pressure synthesis method of oleic acid amide. Background technique [0002] Oleic acid amide is an important long-chain fatty amide, which can form a monomolecular film at the interface of substances and is a good non-ionic surfactant. It is widely used in slip agents and antistatic agents for engineering plastics, functional additives for chemicals, drug release agents, lubricants and gloss agents for paper coatings, anti-embroidery agents for metals, and auxiliary agents for photographic photosensitive materials, etc. At present, there are many synthetic routes of oleic acid amide in industry, and there are common disadvantages such as long reaction time, high reaction temperature and pressure, and difficulty in separation and purification. Among them, the synthesis of oleic acid amide from fatty acid and ammonia needs to be carried out under high temperature and high pressure; the reaction between oleoyl c...

Claims

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Application Information

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IPC IPC(8): C07C231/10C07C233/09B01J31/26
Inventor 姜国民江国庆顾学芳田澍詹文毅颜瑞郭小青
Owner NANTONG UNIVERSITY