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Silica gel loaded type catalyst and application of catalyst in Baeyer-Villiger reaction

A supported catalyst and catalyst technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve poor solubility, difficult catalyst recovery and reuse, loss of enzyme activity, etc. problems, to achieve the effect of simple recycling, improved cleaning and safety, and simple preparation

Inactive Publication Date: 2014-06-11
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the enzyme-catalyzed reaction parameters such as temperature and ionic strength must be precisely controlled. Once the range of change exceeds its allowable value, the activity of the enzyme will be lost.
Enzymes usually show the highest catalytic activity in aqueous solution, while most synthetic organic compounds tend to have poor solubility in aqueous solution. In addition, there are also disadvantages that catalysts are difficult to recycle and reuse.

Method used

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  • Silica gel loaded type catalyst and application of catalyst in Baeyer-Villiger reaction
  • Silica gel loaded type catalyst and application of catalyst in Baeyer-Villiger reaction
  • Silica gel loaded type catalyst and application of catalyst in Baeyer-Villiger reaction

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preparation example Construction

[0018] Step 1, preparation of silica gel supported catalyst:

[0019] 1. Add 1g of silica gel to a three-necked flask, pour 10ml of concentrated nitric acid to submerge the silica gel, and react at 80°C for 8 hours. After the reaction, filter and dry to obtain the product. This step is to remove impurities in the silica gel by acid treatment.

[0020] 2. Add the silica gel from the previous step into the three-necked flask, use ethanol as the solvent, add 1ml of phenyltrimethoxysilane coupling agent, add acetic acid to adjust the pH to about 4, and react at 70°C for 15h. After the reaction, pour the mixture into distilled water, filter while hot, and dry the product.

[0021] 3. Add the product from the previous step into a three-necked flask, add 5mL of 98wt% sulfuric acid for sulfonation, the reaction time is 20h, and the temperature is 30°C. After the reaction, pour into water to fully precipitate, filter, and dry to obtain a silica gel-loaded catalyst.

[0022] 4. A...

Embodiment 1

[0028] In a 50 mL three-neck flask, add 0.45 g of 2-heptylcyclopentanone, dropwise add hydrogen peroxide with a mass fraction of 30%, the molar ratio of hydrogen peroxide to 2-heptylcyclopentanone is 2.5 / 1, and then Add a silica gel-supported catalyst whose mass is 20% of the mass of 2-heptylcyclopentanone, stir with a magnetic force, and react at 40° C. for 24 hours. The mixture was filtered through a glass funnel to remove the catalyst. The filtrate was left standing to separate the organic phase. Take 2 mL of 5% sodium bicarbonate aqueous solution to wash the organic phase three times, then wash with distilled water until the organic phase is neutral, adjust the aqueous phase to weak alkalinity with 5% sodium bicarbonate aqueous solution and extract with ethyl acetate, The ethyl acetate extract was combined with the organic phase, vacuum rotary evaporated, vacuum rotary evaporated solvent, weighed and analyzed by gas chromatography. The conversion of 2-heptylcyclopent...

Embodiment 2

[0032] In a 50 mL three-necked flask, add 0.21 g of cyclopentanone, dropwise add hydrogen peroxide with a mass fraction of 30%, the molar ratio of hydrogen peroxide to cyclopentanone is 2.5 / 1, and then add a silica gel-supported catalyst, the mass fraction of which is 20% of the mass of cyclopentanone, stirred by magnetic force, and reacted at 10°C for 24 hours. The mixture was filtered through a glass funnel to remove the catalyst. The filtrate was left standing to separate the organic phase. Take 2 mL of 5% sodium bicarbonate aqueous solution to wash the organic phase three times, then wash with distilled water until the organic phase is neutral, adjust the aqueous phase to weak alkalinity with 5% sodium bicarbonate aqueous solution and extract with ethyl acetate, The ethyl acetate extract was combined with the organic phase, the solvent was evaporated in vacuo, weighed and analyzed by gas chromatography. The conversion of cyclopentanone was 70%. The yield of delta-va...

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Abstract

The invention discloses a silica gel loaded type catalyst and an application of the catalyst in a Baeyer-Villiger reaction. The silica gel loaded type catalyst is used for catalytically oxidizing cyclic ketone to synthesize a built-in compound. The specific steps are as follows: the cyclic ketone and an organic solvent are added into a container and a hydrogen peroxide solution is dropped; after the dropping, the silica gel loaded type catalyst and a solvent are added and are agitated to react; after the reaction, a target product is obtained by centrifuging, washing, extracting and distilling. The silica gel loaded type catalyst has the advantages that the preparation is simple, the conversion rates of 2-heptyl cyclopentanone, cyclopentanone, cyclohexanone and adamantane are improved, and the atom utilization rate of the reaction is improved; the silica gel loaded type catalyst can be repeatedly used; no waste acid treatment is carried out, and energy conservation and emission reduction are realized; the silica gel loaded type catalyst has the characteristics of good selectivity, high atom efficiency, moderate reaction conditions, clean environment and the like, and is suitable for industrial engineering application.

Description

technical field [0001] The invention relates to a silica gel-supported catalyst and its application in Baeyer-Villiger reaction, in particular to a method for the silica gel-supported catalyst to catalyze the oxidation of cyclic ketones to synthesize lactone compounds, which belongs to the field of organic chemical preparation. Background technique [0002] Supported catalysts, also known as supports, are one of the components of supported catalysts. Catalytically active components are carried on the surface of the carrier, and the carrier is mainly used to support the active component to make the catalyst have specific physical properties, while the carrier itself generally does not have catalytic activity. Most carriers are products in the catalyst industry, commonly used are alumina carriers, silica gel carriers, activated carbon carriers, and some natural products such as pumice, diatomaceous earth, etc. "Active component name-carrier name" is often used to indicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07D309/30C07D313/04C07D313/06
Inventor 彭新华邢婉贞马庆国
Owner NANJING UNIV OF SCI & TECH
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