Method for preparing hydroperoxidation p-menthane by catalytic air oxidation p-menthane

A technology of hydrogen peroxide and air oxidation, which is applied to the preparation of peroxygen compounds, chemical instruments and methods, and the preparation of organic compounds, etc. It can solve the problems of large raw material circulation, long reaction time, and many by-products

Inactive Publication Date: 2008-07-23
HUNAN UNIV
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  • Abstract
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AI Technical Summary

Problems solved by technology

More by-products due to long reaction time
Due to the low single-pass conversion rate of Menthane, resulting in a larg

Method used

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  • Method for preparing hydroperoxidation p-menthane by catalytic air oxidation p-menthane
  • Method for preparing hydroperoxidation p-menthane by catalytic air oxidation p-menthane

Examples

Experimental program
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Effect test

Embodiment 1

[0011] With 2mg metalloporphyrins with general formula (I) structure, R 2 =R 3 = H, R 1 =Cl, M=Mn, add 250ml of p-menthane, and pass through normal pressure air at a flow rate of 600ml / min. The reaction was stirred at 120° C. for 4 hours, and the yield of hydrogen peroxide to menthane was 15.8%. However, in the non-catalyzed oxidation process without adding metalloporphyrin under this condition, the yield of hydrogen peroxide to menthane is only 4.1%.

Embodiment 2

[0013] With 2mg metalloporphyrins with general formula (I) structure, R 2 =R 3 = H, R 1 =Cl, M=Fe, add 250ml of p-menthane, and pass air at normal pressure at a flow rate of 600ml / min. The reaction was stirred at 120° C. for 4 hours, and the yield of hydrogen peroxide to menthane was 13.6%. However, in the non-catalyzed oxidation process without adding metalloporphyrin under this condition, the yield of hydrogen peroxide to menthane is only 4.1%.

Embodiment 3

[0015] 5mg has the metalloporphyrin of general formula (II) structure, R 2 =R 3 = H, R 1 =Cl,M 1 = M 2 =Mn, 5 mg of manganese acetate was added to 250 ml of p-menthane, and air at normal pressure was fed in at a flow rate of 600 ml / min. The reaction was stirred at 120° C. for 5 hours, and the yield of hydrogen peroxide to menthane was 19.7%. However, in the non-catalyzed oxidation process without adding metalloporphyrin, the yield of menthane by hydrogen peroxide is only 5.8%.

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Abstract

The invention discloses a method that menthane is catalyzed and oxygenated selectively by air into hydrogen peroxide p-menthane, which is characterized in that: the oxidant is air or oxygen-enriched air or oxygen; the pressure controlling the reaction is atmospheric pressure (at an atmospheric pressure); reaction temperature is 80 to 140 DEG C; Mu-oxygen-metalloporphyrin and single metalloporphyrin or the supported object of general formula (I) or (II) are selected as main catalyst with the concentration of 1 to 90 ppm; transition metal salts or oxide are used as co-catalyst; molar ration between the main catalyst and co-catalyst is 1: (0.5 to 5); reaction period is 1 to 10 hours; the reaction can be made at single constant temperature and also can be firstly made at constant temperature for one period before temperature is immediately decreased to certain temperature point for continuous reaction. The method that menthane is catalyzed and oxygenated selectively by air into hydrogen peroxide p-menthane has the advantages of short reaction period, high single-pass conversion rate upon menthane, good selectivity of hydrogen peroxide p-menthane, high recovery rate, high purity and easy separation and purification, and thus can avoid producing over-oxidation products.

Description

Technical field: [0001] The invention relates to a method for selectively catalytically oxidizing p-menthane into hydrogen peroxide p-menthane by air or oxygen-enriched air. Background technique: [0002] P-menthane is an important fine chemical product, which is generally obtained from forestry products by hydrogenation of dipentene. P-menthane hydrogen peroxide (PMHP for short) is an excellent olefin polymerization initiator, and is currently mainly used as an initiator for low-temperature emulsion polymerization of styrene-butadiene rubber in China. Oxidation of p-menthane with air or oxygen-enriched air is an important method to obtain p-menthane hydrogen peroxide. At present, the industrial production of hydrogen peroxide from the oxidation of p-menthane adopts non-catalytic oxidation technology, which usually reacts at a temperature of about 110-140°C, uses air as the oxidant, and the reaction time is as long as more than 30 hours. The yield of hydrogen peroxide to m...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/08B01J31/22B01J31/26
Inventor 阳卫军郭灿城陶能烨
Owner HUNAN UNIV
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