CN102603447A - Method for preparing organic lactone - Google Patents
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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]
The present invention relates to the Industrial Catalysis field of petrochemical industry, relate in particular to a kind of catalysis process that organic oxidation of ketones prepares organic lactone that is used for.
[background technology]
Organic lactone is a kind of important organic synthesis intermediate, be mainly used in synthesizing polyester and with other copolymerization of ester class or blending and modifying, for example poly-epsilon-caprolactone (PCL) is the linear aliphatic adoption ester by 6-caprolactone (CL) ring-opening polymerization gained.Lactone can also dissolve many fluoropolymer resins as a kind of strong solvent, to the solvency power that the resin of some indissolubles is done well, can dissolve the urethane resin of chlorinated polyolefin resin and " ESTANE " like caprolactone.
Up to now, there is the difficult problem of aspects such as stability of security and the product of raw materials quality, production in organic lactone synthetic, and the synthetic technology difficulty is big, have only seldom several companies of states such as American and Britain, day producing at present, and China mainly relies on import.
In recent years, along with the continuous expansion of organic lactone (especially 6-caprolactone) Application Areas, the market requirement also constantly increases thereupon, and the exploitation of lactone synthetic technology is also more and more come into one's own.The compound method of organic lactone that present document has been reported comprises that mainly adopting peroxy acid oxidation style, lower concentration H2O2, O2/ air etc. is synthetic lactone of oxygenant oxidation pimelinketone and biological oxidation process.But these methods generally do not adopt catalyzer, and efficient is very low; Even some adopts catalyzer, activity of such catalysts and selectivity are all very low, and catalyzer is difficult to recycling etc.
To the deficiency of existing organic lactone synthesis technique, industry is just being put forth effort on and is being designed and developed high efficiency method and the catalyzer that the organic oxidation of ketones with strong development prospect prepares organic lactone.
[summary of the invention]
The purpose of this invention is to provide and a kind ofly prepare the method for organic lactone, to overcome above-mentioned defective of the prior art by organic ketone catalyzed oxidation.
For reaching goal of the invention, the present invention proposes following technical scheme:
The organic ketone of a kind of catalyzed oxidation prepares the method for organic lactone, comprises following step: get the catalyzer of reacting weight, organic ketone, organic aldehyde and organic solvent and place reactor drum to mix; Aerating oxygen under agitation after 0.5-10 hour, promptly gets the title product lactone in room temperature to 100 ℃ following reaction.
Among above-mentioned organic lactone preparation method, the catalyzer that is adopted is the cubic tricobalt tetroxide.
Among above-mentioned organic lactone preparation method, also comprise the step for preparing catalyzer cubic three powder blues in advance, comprising:
The inorganic base substance (like sodium hydrogencarbonate, saleratus, salt of wormwood, yellow soda ash, ammoniacal liquor, sodium hydroxide, Pottasium Hydroxide) and the P123 template of S1. getting reacting weight (are EO
20PO
70EO
20, wherein EO is an oxyethyl group, PO is a propoxy-) and be dissolved in wiring solution-forming in the deionized water;
S2. the cobalt salt (like Xiao Suangu, NSC 51149, Cobaltous diacetate etc.) of getting reacting weight is dissolved in and is made into the aqueous solution that contains cobalt ion in the deionized water;
S3. under vigorous stirring, the aqueous solution that will contain cobalt ion dropwise adds in the solution that contains template and mineral alkali and (drips off about the pH=7 of back), drips continued and stirs 0.5 hour;
S4. above-mentioned solution is poured in the reaction kettle, in 180 ℃ of crystallization 24 hours;
S5. precipitate 3 times with deionized water wash,, promptly got catalyzer in 2 hours 300 ℃ of roastings in 80 ℃ of oven dry down.
Among above-mentioned organic lactone preparation method, organic ketone finger ring pentanone, 2-methyl-cyclopentanone, 3-methyl-cyclopentanone, pimelinketone, 2-methylcyclohexanone, 3-methylcyclohexanone, 4-methylcyclohexanone etc.
Among above-mentioned organic lactone preparation method, organic aldehyde refers to acetaldehyde, butyraldehyde, phenyl aldehyde, o-chlorobenzaldehyde, 4-chloro-benzaldehyde etc.
Among above-mentioned organic lactone preparation method, organic solvent refers to acetonitrile, ETHYLE ACETATE, 1,2-ethylene dichloride, trichloromethane, tetrachloromethane etc.
Among above-mentioned organic lactone preparation method, the mass ratio of catalyzer and organic ketone is [0.01-0.2]: 1, and the mol ratio of organic aldehyde and organic ketone is [1-4]: 1, the mol ratio of oxygen and organic ketone is [1-50]: 1.
Preferably, among above-mentioned organic lactone preparation method, the temperature of control reaction system is at 30-80 ℃ and sustained reaction 2-5 hour.
Provided by the present inventionly prepare the method for lactone by the ketone catalyzed oxidation, the reaction process gentleness is easy to control.Obtaining higher productive rate with optionally simultaneously, safe, the environmental protection of this method, and also catalyst system therefor is cheap, preparation is simple, the stability height, can repeatedly reuse, and has favorable industrial application prospect.
[Brief Description Of Drawings]
The Electronic Speculum figure of the cubic tricobalt tetroxide that provides among the present invention of being shown in Figure 1.
[embodiment]
Below in conjunction with embodiments of the invention and comparative example the present invention is further specified:
One, the preparation of catalyzer
Catalyzer used among the following embodiment of the present invention is all got by following method preparation:
Getting 7.56 gram sodium hydrogencarbonates and 4 gram template P123 is dissolved in 600 ml deionized water and is configured to solution; Getting 26.2 gram Cobaltous nitrate hexahydrates is dissolved in 240 ml deionized water and is configured to cobalt nitrate solution.Under vigorous stirring, cobalt nitrate solution dropwise is added in the solution that contains P123 template and sodium hydrogencarbonate and (drips off about the pH=7 of back), drip continued and stirred 0.5 hour.Be poured into then in the reaction kettle, in 180 ℃ of crystallization 24 hours.At last, precipitate 3 times with deionized water wash, in 80 ℃ of oven dry down, promptly got the cubic tricobalt tetroxide in 2 hours 300 ℃ of roastings, its Electronic Speculum figure is shown in accompanying drawing 1.
In the above-mentioned steps, can adopt alternative sodium hydrogencarbonates such as other inorganic base such as saleratus, salt of wormwood, yellow soda ash, ammoniacal liquor, sodium hydroxide, Pottasium Hydroxide; Replacement such as also available other cobalt salt such as NSC 51149, Cobaltous diacetate Xiao Suangu can be prepared the cubic tricobalt tetroxide equally.
Two, test and analysis
Gas phase-mass spectrograph combined instrument the GC/MS (6890N/5973N) of the configuration HP-5MS capillary chromatographic column (30m * 0.45mm * 0.8 μ m) of Agilent company production is adopted in the structural analysis of reaction product in following embodiment of the present invention and the Comparative Examples.The analysis of target product selectivity and productive rate is then adopted by the configuration hydrogen flame detector of Agilent company production and the gas chromatograph Agilent GC 7820A of AB-FFAP capillary chromatographic column (30m * 0.25mm * 0.25 μ m).
Three, embodiment
Embodiment 1
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.5 gram, ketopentamethylene 10 grams, phenyl aldehyde 10 grams and tetracol phenixin in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 100 ml/min; Under agitation reaction is after 3 hours down in 40 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is the title product valerolactone, and the gas chromatographic analysis result shows that the selectivity of valerolactone and yield are respectively 100% and 99%.Catalyzer through 10 recycles after, the selectivity of valerolactone and yield still are respectively 100% and 99.2%.
Embodiment 2
In three mouthfuls of vials, add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.2 gram, pimelinketone 10 grams, butyraldehyde 20 grams and 1 successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 200 ml/min, under agitation after reacting 1 hour under 80 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is the title product caprolactone, and the gas chromatographic analysis result shows that the selectivity of caprolactone and yield are respectively 100% and 99.5%.
Embodiment 3
Add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.8 gram, 2-methylcyclohexanone 10 grams in three mouthfuls of vials successively, to 200 milliliters of chlorobenzene aldehyde 40 grams and acetonitriles; Aerating oxygen; Oxygen gas flow rate is 400 ml/min; Under agitation reaction is after 9 hours down in 30 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity and the yield of 2-methyl caprolactone are 100%.
Embodiment 4
Add 200 milliliters of above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.0 grams, 3-methylcyclohexanone 10 grams, 4-chloro-benzaldehyde 30 grams and acetonitriles in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 300 ml/min; Under agitation reaction is after 5 hours down in 60 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 3-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 3-methyl caprolactone and yield are respectively 100% and 99.6%.
Embodiment 5
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.5 grams, 4-methylcyclohexanone 10 grams, butyraldehyde 20 grams and trichloromethane alkane in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 150 ml/min; Under agitation reaction is after 10 hours down in 40 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 4-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 4-methyl caprolactone and yield are respectively 100% and 99.8%.
Embodiment 6
In three mouthfuls of vials, add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.2 grams, 2-methyl-cyclopentanone 10 grams, phenyl aldehyde 20 grams and 1 successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 50 ml/min, under agitation after reacting 2 hours under 80 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methylpent lactone, and the gas chromatographic analysis result shows that the selectivity of 2-methylpent lactone and yield are respectively 100% and 99.5%.
Embodiment 7
Add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.4 gram, 3-methyl-cyclopentanone 10 grams in three mouthfuls of vials successively, to 200 milliliters in phenyl aldehyde 30 grams and tetracol phenixin; Aerating oxygen; Oxygen gas flow rate is 140 ml/min; Under agitation reaction is after 3 hours down in 60 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 3-methylpent lactone, and the gas chromatographic analysis result shows that the selectivity of 3-methylpent lactone and yield are 100% and 100%.
Embodiment 8
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.3 gram, 4-methyl-cyclopentanone 10 grams, adjacent phenyl aldehyde 30 grams and ETHYLE ACETATE in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 250 ml/min; Under agitation reaction is after 2 hours down in 50 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 4-methylpent lactone, and the gas chromatographic analysis result shows that the selectivity of 4-methylpent lactone and yield are respectively 100% and 99.5%.Catalyzer through 10 recycles after, the selectivity and the yield of 4-methylpent lactone still are respectively 100% and 99.4%.
Embodiment 9
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.4 gram, 2-methyl-cyclopentanone 10 grams, butyraldehyde 20 grams and tetracol phenixin in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 150 ml/min; Under agitation reaction is after 3 hours down in 60 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methylpent lactone, and the gas chromatographic analysis result shows that the selectivity of 2-methylpent lactone and yield are respectively 100% and 99.4%.
Embodiment 10
Add 200 milliliters of above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.5 gram, 3-methyl-cyclopentanone 10 grams, 4-chloro-benzaldehyde 25 grams and acetonitriles in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 300 ml/min; Under agitation reaction is after 2 hours down in 80 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 3-methylpent lactone, and the gas chromatographic analysis result shows that the selectivity of 3-methylpent lactone and yield are respectively 100% and 99.4%.
Embodiment 11
Add 200 milliliters of above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.2 grams, ketopentamethylene 10 grams, phenyl aldehyde 15 grams and acetonitriles in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 120 ml/min; Under agitation reaction is after 2 hours down in 70 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is the title product valerolactone, and the gas chromatographic analysis result shows that the selectivity of valerolactone and yield are respectively 100% and 99.6%.
Embodiment 12
In three mouthfuls of vials, add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.9 gram, ketopentamethylene 10 grams, acetaldehyde 8 grams and 1 successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 80 ml/min, under agitation after reacting 4 hours under 50 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is the title product valerolactone, and the gas chromatographic analysis result shows that the selectivity of valerolactone and yield are 100%.
Embodiment 13
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.5 grams, ketopentamethylene 10 grams, 4-chloro-benzaldehyde 25 grams and tetracol phenixin in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 250 ml/min; Under agitation reaction is after 2 hours down in 60 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is the title product valerolactone, and the gas chromatographic analysis result shows that the selectivity of valerolactone and yield are respectively 100% and 99.8%.
Embodiment 14
In three mouthfuls of vials, add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.0 grams, pimelinketone 10 grams, phenyl aldehyde 250 grams and 1 successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 150 ml/min, under agitation after reacting 2 hours under 80 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is the title product caprolactone, and the gas chromatographic analysis result shows that the selectivity of caprolactone and yield are respectively 100% and 99.6%.
Embodiment 15
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.4 gram, 2-methyl-cyclopentanone 10 grams, phenyl aldehyde 15 grams and tetracol phenixin in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 100 ml/min; Under agitation reaction is after 4 hours down in 30 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methylpent lactone, and the gas chromatographic analysis result shows that the selectivity of 2-methylpent lactone and yield are respectively 100% and 99.5%.
Embodiment 16
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.2 grams, 4-ketopentamethylene 10 grams, 4-chloro-benzaldehyde 25 grams and ETHYLE ACETATE in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 200 ml/min; Under agitation reaction is after 2 hours down in 60 ℃, and the gas chromatographic analysis result shows that the gas chromatograph-mass spectrometer analytical results shows that product is a title product 4-valerolactone, and the selectivity of 4-valerolactone and yield are respectively 100% and 99.8%.
Embodiment 17
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.8 gram, pimelinketone 10 grams, phenyl aldehyde 30 grams and tetracol phenixin in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 120 ml/min; Under agitation reaction is after 3 hours down in 50 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is the title product caprolactone, and the gas chromatographic analysis result shows that the selectivity of caprolactone and yield are respectively 100% and 99.8%.
Embodiment 18
In three mouthfuls of vials, add above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 1.2 grams, 2-methylcyclohexanone 10 grams, 4-chloro-benzaldehyde 35 grams and 1 successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen; Oxygen gas flow rate is 120 ml/min; Under agitation reaction is after 1 hour down in 70 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 2-methyl caprolactone and yield are respectively 100% and 99.0%.
Embodiment 19
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.4 gram, 2-methylcyclohexanone 10 grams, acetaldehyde 20 grams and tetracol phenixin in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 100 ml/min; Under agitation promptly get title product 2-methyl caprolactone in reaction under 50 ℃ after 3 hours, the gas chromatographic analysis result shows that the selectivity of 2-methyl caprolactone and yield are respectively 100% and 99.4%.
Embodiment 20
Add 200 milliliters in above-mentioned institute synthetic cubic tricobalt tetroxide catalyzer 0.4 gram, 2-methylcyclohexanone 10 grams, phenyl aldehyde 25 grams and dichloro two ethane in three mouthfuls of vials successively; Aerating oxygen; Oxygen gas flow rate is 120 ml/min; Under agitation reaction is after 7 hours down in 45 ℃, and the gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 2-methyl caprolactone and yield are respectively 100% and 99.6%.
Three, comparative example
In order to further specify the meliority of catalyzer of the present invention, select following catalyzer example as a comparison for use.
Comparative example 1
In three mouthfuls of vials, add tricobalt tetroxide catalyzer 0.4 gram, 2-methylcyclohexanone 10 grams, acetaldehyde 20 grams and 1 that are purchased successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 100 ml/min, under agitation after reacting 3 hours under 50 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 2-methyl caprolactone and yield are respectively 95% and 65%.
Comparative example 2
In three mouthfuls of vials, add Antimony Trioxide: 99.5Min 0.4 gram, 2-methylcyclohexanone 10 grams, acetaldehyde 20 grams and 1 that are purchased successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 100 ml/min, under agitation after reacting 3 hours under 50 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 2-methyl caprolactone and yield are respectively 95% and 30.6%.
Comparative example 3
In three mouthfuls of vials, add chromium sesquioxide 0.4 gram, 2-methylcyclohexanone 10 grams, acetaldehyde 20 grams and 1 that are purchased successively; 200 milliliters of 2-ethylene dichloride; Aerating oxygen, oxygen gas flow rate are 100 ml/min, under agitation after reacting 3 hours under 50 ℃; The gas chromatograph-mass spectrometer analytical results shows that product is a title product 2-methyl caprolactone, and the gas chromatographic analysis result shows that the selectivity of 2-methyl caprolactone and yield are respectively 90% and 20.6%.
Can find out that by the foregoing description and comparative example do not adopt in the catalyzer Comparative Examples of the present invention, the selectivity of title product lactone and yield are all lower, and adopt catalyzer of the present invention, have reduced reaction conditions, make that the reaction process gentleness is easy to control.In addition, this catalyzer is cheap and easy to get, the preparation simple, stability is high, and can be repeatedly used and reduce cost.
The above embodiment has only expressed several kinds of embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with accompanying claims.
Claims (8)
1. one kind prepares the method for organic lactone by organic ketone catalyzed oxidation, comprises following step:
Get the catalyzer of reacting weight, organic ketone, organic aldehyde and organic solvent and place, mix in reaction vessel;
Aerating oxygen in reaction system under agitation reacted 0.5-10 hour down in 25-100 ℃, promptly got.
2. according to claim 1ly prepare the method for organic lactone, it is characterized in that described catalyzer is the cubic tricobalt tetroxide by organic ketone catalyzed oxidation.
3. according to claim 2ly prepare the method for organic lactone, it is characterized in that, also comprise the step for preparing catalyzer cubic three powder blues in advance, comprising by organic ketone catalyzed oxidation:
The inorganic base substance and the P123 template of S1. getting reacting weight are dissolved in wiring solution-forming in the deionized water;
S2. the cobalt salt of getting reacting weight is dissolved in and is made into the aqueous solution that contains cobalt ion in the deionized water;
S3. under vigorous stirring, the aqueous solution that will contain cobalt ion dropwise adds in the solution that contains template and mineral alkali;
S4. above-mentioned solution is poured in the reaction kettle into crystallization;
S5. with the deionized water wash deposition, dry, roasting promptly gets catalyzer.
4. according to any described method for preparing organic lactone by organic ketone catalyzed oxidation of claim 1-3; It is characterized in that said organic ketone is ketopentamethylene, 2-methyl-cyclopentanone, 3-methyl-cyclopentanone, pimelinketone, 2-methylcyclohexanone, 3-methylcyclohexanone or 4-methylcyclohexanone.
5. describedly prepare the method for organic lactone according to any one of claim 1-3, it is characterized in that said organic aldehyde is acetaldehyde, butyraldehyde, phenyl aldehyde, o-chlorobenzaldehyde or 4-chloro-benzaldehyde by organic ketone catalyzed oxidation.
6. describedly prepare the method for organic lactone according to any one of claim 1-3, it is characterized in that said organic solvent is acetonitrile, ETHYLE ACETATE, 1,2-ethylene dichloride, trichloromethane or tetrachloromethane by organic ketone catalyzed oxidation.
7. according to any described method for preparing organic lactone by organic ketone catalyzed oxidation of claim 1-3; It is characterized in that; The mass ratio of said catalyzer and organic ketone is [0.01-0.2]: 1; The mol ratio of organic aldehyde and organic ketone is [1-4]: 1, and the mol ratio of oxygen and organic ketone is [1-50]: 1.
8. describedly prepare the method for organic lactone according to any one of claim 1-3, it is characterized in that the temperature of preferably controlling reaction system is at 30-80 ℃ and sustained reaction 2-5 hour by organic ketone catalyzed oxidation.
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| CN105130947A (en) * | 2015-07-21 | 2015-12-09 | 刘小秦 | Industrial production method of [epsilon]-caprolactone |
| CN109833872A (en) * | 2019-02-28 | 2019-06-04 | 天津大学 | The cobalt oxide bulk phase catalyst and its preparation method and application of controllable product distribution |
| CN109833872B (en) * | 2019-02-28 | 2021-11-16 | 天津大学 | Cobalt oxide bulk phase catalyst capable of regulating and controlling product distribution and preparation method and application thereof |
| CN111018823A (en) * | 2019-12-12 | 2020-04-17 | 河南能源化工集团研究总院有限公司 | Process for preparing epsilon-caprolactone and co-producing methacrylic acid by cyclohexanone |
| CN113198472A (en) * | 2021-04-13 | 2021-08-03 | 南京工业大学 | Magnetic catalyst and preparation and application thereof |
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