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Method for synthesizing anchoic acid through combined oxidation of hydrogen peroxide and potassium permanganate

A technology of potassium permanganate and hydrogen peroxide, which is applied to chemical instruments and methods, separation/purification of carboxylic acid compounds, oxidation to prepare carboxylic acids, etc., can solve the problems of troublesome post-processing, short reaction time, and high price. To achieve the effect of saving time, speeding up response and saving energy

Active Publication Date: 2015-03-25
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent 200710042766.6 discloses a method for preparing azelaic acid with a solid acid catalyst, which is characterized by a short reaction time and no pollution to the oxidant; the disadvantage is that the concentration of the oxidant hydrogen peroxide is required to be higher than 50%, which is expensive and not easy to produce in China. have to
Although the yield of azelaic acid prepared by oxidation of oleic acid by potassium permanganate method is relatively high, due to the need for a large amount of potassium permanganate oxidizing agent, the amount of manganese dioxide solid produced as a by-product is also large, and post-processing is troublesome, so this method is rarely used
Chinese patent 200610029216.6 discloses a method for preparing azelaic acid by catalytic oxidation of an ozone-hydrogen peroxide mixed oxidant. The advantage of this method is that it does not use high-concentration hydrogen peroxide; the disadvantage is that two-step reactions are required, and ozone reacts at high temperature prone to explosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 500mL four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser, add 50 grams of oleic acid, 5 grams of phosphotungstic acid catalyst, and 3 grams of benzyltriethylammonium chloride, and the flow rate of oxygen is 15g. / L. Quickly stir and heat to 75°C, add 2 grams of potassium permanganate, add 200ml of hydrogen peroxide with a mass concentration of 15%, and react for 5 hours. After the reaction, put the mixed solution in a separatory funnel for separation. The lower part of the water layer and the upper part of the oil layer are easy to separate. Refrigerate and crystallize the separated water phase at 3°C; wash the manganese dioxide with 300ml of boiling water three times, heat and concentrate the obtained liquid at 100°C to 50mL, and refrigerate at 0-5°C for crystallization, white powder is precipitated, and the two parts The liquid is suction filtered and dried to obtain azelaic acid, and the calculated yield is about 90.01%....

Embodiment 2

[0014] In a 500mL four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 50 grams of oleic acid, 5 grams of phosphotungstic acid catalyst, and 3 grams of benzyltriethylammonium chloride. 20g / L. Quickly stir and heat to 95°C, add 2 grams of potassium permanganate, add 200ml of hydrogen peroxide with a mass concentration of 30% in batches, and react for 6 hours. Manganese is in the lower part of the water layer, and the oil layer is on the top, which is easy to separate. Refrigerate and crystallize the separated water phase at 0~5°C; wash manganese dioxide three times with 300ml of boiling water, heat and concentrate the obtained liquid at 100°C to 50mL, refrigerate and crystallize at 0~5°C, white powder precipitates, and The two parts of the liquid were suction filtered and dried to obtain azelaic acid, and the calculated yield was about 99.01%. The melting point is 105.5-107.0°C.

Embodiment 3

[0016] In a 500mL four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 50 grams of oleic acid, 5 grams of phosphotungstic acid catalyst, and 3 grams of benzyltriethylammonium chloride. 5g / L. Quickly stir and heat to 60°C, add 2 grams of potassium permanganate, add 200ml of hydrogen peroxide with a mass concentration of 5% in batches, and react for 1 hour. Manganese is in the lower part of the water layer, and the oil layer is on the top, which is easy to separate. Refrigerate and crystallize the separated water phase at 0~5°C; wash manganese dioxide three times with 300ml of boiling water, heat and concentrate the obtained liquid at 100°C to 50mL, refrigerate and crystallize at 0~5°C, white powder precipitates, and The two parts of the liquid were suction filtered and dried to obtain azelaic acid, and the calculated yield was about 69.01%. The melting point is 104.5-106.0°C.

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Abstract

The invention relates to a method for synthesizing anchoic acid through combined oxidation of hydrogen peroxide and potassium permanganate. The method comprises the following steps: mixing oleic acid, a phosphotungstic acid catalyst and benzyl triethyl ammonium chloride, and rapidly stirring and heating under the condition of introducing oxygen; adding potassium permanganate, adding a hydrogen peroxide solution, and separating the mixed liquid in a separating funnel after reaction is ended, wherein manganese dioxide is arranged at the lower part of a water layer; an oil layer is arranged on the water layer and is easy to separate; refrigerating and crystallizing the separated water phase, and separating out white powder; and carrying out suction filtration and drying, so as to obtain anchoic acid solid. According to the method disclosed by the invention, other chemical apparatuses do not need to be used in the overall reaction process, so that energy consumption is lowered; the reaction speed is increased; the time is saved; a lot of organic solvents are not required in the reaction; and the method is environment-friendly and relatively high in reaction yield; a one-step reaction process is simple; a reaction system is easy to separate; the production cost is effectively reduced; and the method is environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing azelaic acid through combined oxidation using oleic acid, hydrogen peroxide and potassium permanganate as oxidation. Background technique [0002] Azelaic acid can be used as a raw material for spices, lubricating oils, oils, polyamide resins and for alkyd resins, paints and chemical synthesis. Most of azelaic acid is used to produce dioctyl azelate (DOZ) plasticizers . [0003] The preparation of azelaic acid and pelargonic acid by oxidizing oleic acid with hydrogen peroxide is the main method of synthesizing azelaic acid and pelargonic acid at present. Chinese patent 200710042766.6 discloses a method for preparing azelaic acid with a solid acid catalyst, which is characterized by a short reaction time and no pollution to the oxidant; the disadvantage is that the concentration of the oxidant hydrogen peroxide is required to be h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/18C07C51/285
CPCC07C51/16C07C51/285C07C51/43C07C51/48C07C55/18
Inventor 史春薇周文丰赵杉林陈平仲崇民宋锦玉王亚新尚艳闫玉玲宋官龙洪滟
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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