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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 efficiency, difficult catalyst recycling, low catalyst activity and selectivity, etc., and achieves simple preparation, good industrial application prospects, Catalyst cheap effect

Inactive Publication Date: 2014-12-10
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
  • Method for preparing organic lactone
  • Method for preparing organic lactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 0.5 g of the above-mentioned synthesized hexagonal prism-shaped Co-MFI catalyst, 10 g of cyclopentanone, 10 g of benzaldehyde, and 200 ml of carbon tetrachloride in sequence into a three-necked glass bottle, and feed oxygen at a flow rate of 100 ml / min, after reacting at 40 DEG C under stirring for 4 hours, the gas chromatography-mass spectrometry analysis result shows that the product is the target product valerolactone, and the gas chromatography analysis result shows that the selectivity and yield of valerolactone are respectively 100 % and 99%. After the catalyst was recycled 10 times, the selectivity and yield of valerolactone were still 100% and 99.2%, respectively.

Embodiment 2

[0038] Add 0.2 g of the Co-MFI catalyst with hexagonal prism shape synthesized above, 10 g of cyclohexanone, 20 g of butyraldehyde, and 200 ml of 1,2-dichloroethane into a three-necked glass bottle in sequence, and then inject oxygen, oxygen Flow velocity is 200 milliliters / minute, after reacting at 80 ℃ under stirring for 1 hour, gas chromatography-mass spectrometry analysis result shows that product is target product caprolactone, and gas chromatography analysis result shows the selectivity and recovery of caprolactone. The rates are 100% and 99.5%, respectively.

Embodiment 3

[0040] Add 0.8 g of the above-mentioned hexagonal prism-shaped Co-MFI catalyst, 10 g of 2-methylcyclohexanone, 40 g of p-chlorobenzaldehyde, and 200 ml of acetonitrile into a three-necked glass bottle in sequence, and then introduce oxygen at a flow rate of Be 400 milliliters / minute, after reacting at 30 ℃ under stirring for 9 hours, gas chromatography-mass spectrometry analysis result shows that product is target product 2-methyl caprolactone, and gas chromatography analysis result shows that 2-methyl caprolactone The selectivity and yield of lactone are both 100%.

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Abstract

The invention provides a method for preparing organic lactone. The method is characterized in that: a load type catalyst Co-MFI having a hexagonal prism morphology is used as a catalyst, and the catalyst is prepared by a method of hydrothermal crystallization synthesis; organic ketone is used as a substrate, oxygen or air is used as oxygen sources, organic aldehyde substances are used as reducing agents, and an organic solvent is added into a reaction system. The method has the advantages that: the catalyst is easy to prepare; the reaction conditions are mild, safe, reliable, green and environment-friendly; the selectivity and the yield of target products approach to 100 percent; and the catalyst can be repeatedly recycled. According to the method, the problems of low safety, low yield and the like in the conventional preparation process of the lactone 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): C07D309/30C07D313/04B01J29/76
CPCY02P20/584
Inventor 尹双凤郭明奇李岳芳陈浪周永波邱仁华
Owner HUNAN UNIV
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