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Method for preparing organic lactone

A technology of organic and lactones, which is applied in the field of catalysis for the preparation of organic lactones by oxidation of organic ketones, can solve the problems of low catalyst activity and selectivity, difficult recycling of catalysts, and low efficiency, and achieve cheap catalysts, good industrial application prospects, Prepare simple effects

Inactive Publication Date: 2014-09-03
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods generally do not use a catalyst, and the efficiency is very low; even if some use a catalyst, the activity and selectivity of the catalyst are very low, and the catalyst is difficult to recycle, etc.

Method used

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  • Method for preparing organic lactone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In the three-necked glass bottle, add successively 0.5 grams of the above-mentioned cubic cobalt tetraoxide catalyst synthesized, 10 grams of cyclopentanone, 10 grams of benzaldehyde and 200 milliliters of carbon tetrachloride, feed oxygen, and the flow rate of oxygen is 100 milliliters / minute, while stirring After reacting at 40° C. for 3 hours, gas chromatography-mass spectrometry analysis results showed that the product was the target product valerolactone, and gas chromatography analysis results showed that the selectivity and yield of valerolactone were 100% and 99%, respectively. After the catalyst was recycled 10 times, the selectivity and yield of valerolactone were still 100% and 99.2%, respectively.

Embodiment 2

[0035] Add 0.2 grams of the above-mentioned cubic cobalt tetroxide catalyst, 10 grams of cyclohexanone, 20 grams of butyraldehyde and 200 milliliters of 1,2-dichloroethane in the three-necked glass bottle successively, and feed oxygen at a flow rate of 200 milliliters / Minutes, after stirring for 1 hour at 80°C, the gas chromatography-mass spectrometry analysis results showed that the product was the target product caprolactone, and the gas chromatography analysis results showed that the selectivity and yield of caprolactone were 100% respectively and 99.5%.

Embodiment 3

[0037] Add 0.8 grams of the above-mentioned cubic cobalt tetroxide catalyst, 10 grams of 2-methylcyclohexanone, 40 grams of p-chlorobenzaldehyde and 200 milliliters of acetonitrile into the three-necked glass bottle successively, and feed oxygen at a flow rate of 400 milliliters / minute , after reacting at 30°C under stirring for 9 hours, the gas chromatography-mass spectrometry analysis results showed that the product was the target product 2-methylcaprolactone, and the gas chromatography analysis results showed that the selectivity of 2-methylcaprolactone and yields are both 100%.

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Abstract

The invention provides a method for preparing organic lactone. The method is characterized in that: cubic cobaltosic oxide is taken as a catalyst, and the catalyst is prepared with a hydrothermal method; and organic ketone is taken as a substrate, oxygen or air is taken as an oxygen source, an organic lactone substance is taken as a reducing agent, and an organic solvent is added into a reaction system. The method has the advantages that: the catalyst is easy to prepare; reaction conditions are mild, and the method is safe, reliable and environmentally-friendly; the selectivity and yield of an obtained target product are close to 100 percent; and the catalyst can be used for repeatedly. Due to the adoption of the method, the problems of poor safety, low yield and the like existing in the conventional lactone preparation process are solved, and the method has a good industrial application prospect.

Description

【Technical field】 [0001] The invention relates to the field of industrial catalysis in the petrochemical industry, in particular to a catalytic method for preparing organic lactones by oxidation of organic ketones. 【Background technique】 [0002] Organic lactone is an important organic synthesis intermediate, mainly used in the synthesis of polyester and copolymerization or blending modification with other esters, for example, polyε-caprolactone (PCL) is derived from ε-caprolactone (CL ) Linear aliphatic polyester obtained by ring-opening polymerization. Lactone can also be used as a strong solvent to dissolve many polymer resins, and has good solubility for some insoluble resins. For example, caprolactone can dissolve chlorinated polyolefin resins and "ESTANE" polyurethane resins. [0003] So far, the synthesis of organic lactones has problems in raw material quality, production safety and product stability, and the synthesis technology is difficult. Currently, only a few ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07B41/12C07D309/30C07D313/04B01J23/75
Inventor 尹双凤郭明奇李岳芳陈浪
Owner HUNAN UNIV
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