Method for preparing nonane diacid by ozone-hydrogen peroxide mixed oxidant catalysizing

A technology of mixing oxidants and hydrogen peroxide, which is applied in the preparation of carboxylic acids by ozone oxidation, organic chemistry, etc., can solve the problems of increasing the solvent recovery process, increasing the corrosion of reaction equipment, and being unfavorable to environmental protection, etc., and achieves convenient operation and high reaction yield , the effect of mild reaction conditions

Inactive Publication Date: 2007-03-14
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of solvent dichloroethane in this method increases the corrosion of the system to the reaction equi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 125ml three-necked flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 20 grams of oleic acid (the actual oleic acid content is 73%), 0.6 grams of phosphotungstic acid, and 0.7 grams of cetyltrimethylammonium chloride . Stir and heat to 60°C, inject ozone with a concentration of 3%, and the flow rate is 200ml / min; add hydrogen peroxide with a concentration of 30% in batches, the total amount is 40ml; react at 70°C for 1 hour; then heat up To 100°C, react for 10 hours; add a small amount of evaporated water during the reaction. After the reaction, it was separated while it was hot, the lower layer was a white water phase, and the upper layer was an oil phase. The water phase was refrigerated and crystallized at 0-5°C, and white azelaic acid crystals were precipitated, followed by suction filtration and drying. After extracting the oil phase with 50ml of boiling water several times, the extract was refrigerated at 0-5°C for crys...

Embodiment 2

[0020] In a 125ml three-necked flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 20 grams of oleic acid (the actual oleic acid content is 73%), 0.6 grams of phosphotungstic acid, and 0.7 grams of cetyltrimethylammonium chloride . Stir and heat to 60°C, inject ozone with a concentration of 3%, and the flow rate is 200ml / min; add hydrogen peroxide with a concentration of 30% in batches, the total amount is 100ml; react at 70°C for 1 hour; then heat up To 105°C, react for 12 hours; add a small amount of evaporated water during the reaction. After the reaction, it was separated while it was hot, the lower layer was a white water phase, and the upper layer was an oil phase. The water phase was refrigerated and crystallized at 0-5°C, and white azelaic acid crystals were precipitated, followed by suction filtration and drying. After extracting the oil phase with 50ml of boiling water several times, the extract was refrigerated at 0-5°C for cry...

Embodiment 3

[0022] In this example, mixed fatty acids were used as raw materials to prepare azelaic acid.

[0023] First, add 100 grams of cottonseed oil and 50 ml of deionized water into a 500 ml three-neck flask, stir slowly and heat to 80°C, add 100ml of 40% NaOH aqueous solution dropwise within 30 minutes, stir slowly at 80°C for 3 hours; wait until the temperature drops to Below 40°C, add a 1:1 sulfuric acid aqueous solution dropwise while stirring until the reaction solution is completely separated; separate the upper layer oil, and wash with water until neutral to obtain 85 grams of mixed fatty acids.

[0024] In a 125ml three-necked flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 20 grams of the above-mentioned mixed fatty acids (62% of which contains oleic acid), 0.6 grams of phosphotungstic acid, and 0.7 grams of hexadecyl trimethyl chloride Ammonium. The subsequent operation steps are exactly the same as the process steps of the above-m...

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Abstract

The present invention relates to process of catalytically oxidizing oleic acid or mixed fatty acid obtained through hydrolyzing animal and vegetable grease with mixed oxidant of ozone and hydrogen peroxide to prepare azelaic acid, and belongs to the field of organic compound preparing technology. By using ozone and hydrogen peroxide as mixed oxidant, phosphotungstic acid as catalyst and quaternary ammonium salt as phase transfer reagent, and through the reaction at 60-70 deg.c and normal pressure and the further reaction at 95-105 deg.c for 8-12 hr, the material oleic acid or mixed fatty acid is oxidized and cracked to prepare azelaic acid.

Description

technical field [0001] The invention relates to a method for preparing azelaic acid by using a mixed oxidant of ozone and low-concentration hydrogen peroxide to catalyze the oxidation of oleic acid or mixed fatty acids (containing oleic acid) produced by hydrolysis of animal and vegetable oils. It belongs to the technical field of organic compound preparation. Background technique [0002] Azelaic acid is an important intermediate in organic synthesis. It has a wide range of industrial uses. It is mainly used to synthesize plasticizers in plastics and rubber industries; it is also important in the fields of synthetic fragrances, lubricants, oils and polyphenolamine resins. application. In addition, azelaic acid has important uses in the manufacture of electrolytic capacitors and the prevention and treatment of skin diseases. [0003] The preparation of azelaic acid from cheap oleic acid or mixed fatty acids (containing oleic acid) produced by the hydrolysis of animal and v...

Claims

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Application Information

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IPC IPC(8): C07C55/18C07C51/34
Inventor 陈烨璞史春薇陈欣
Owner SHANGHAI UNIV
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