Method for preparing 2,5-hexanedione under catalysis of solid acid

A solid acid catalysis, solid acid catalyst technology, applied in the preparation of heterocyclic compounds, organic chemistry, etc., can solve the problems of difficult separation of reaction products, environmental pollution, etc., to achieve the effect of suppressing side reactions, reducing the difficulty of separation, and mild reaction conditions

Active Publication Date: 2016-03-30
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
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Problems solved by technology

The hydrolysis of 2,5-dimethylfuran is an acid-catalyzed process, and the selection of an appropriate acid catalyst is the key to its effective hydrolysis. Among them, mineral acids such as hydrochloric acid, phosphoric acid or phosphoric acid are commonly prepared by hydrolysis, but these mineral acids are homogeneous The catalytic system, the reaction system and the reaction product are not easy to separate, which is easy to cause environmental pollution

Method used

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  • Method for preparing 2,5-hexanedione under catalysis of solid acid
  • Method for preparing 2,5-hexanedione under catalysis of solid acid
  • Method for preparing 2,5-hexanedione under catalysis of solid acid

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 1ml of 2,5-dimethylfuran into the container, then add 12ml of methyl isobutyl ketone, 0.2ml of deionized water and 0.8g of Hβ molecular sieve (silicon to aluminum ratio of 20), and mix well. The container was placed in a constant temperature reactor at 180° C., stirred continuously, and reacted for 5 hours. After the reaction, the container was put into an ice bath to quench the reaction, and the temperature of the system dropped rapidly to room temperature. The reaction product is taken out, the organic phase and the solid catalyst are separated by centrifugation, the organic phase is collected, and the catalyst is recovered. The organic phase obtained is distilled under reduced pressure, removes organic solvent, obtains product (see attached figure 2 with 3 ). The conversion rate of the raw material and the yield of the product were determined by gas chromatography external standard method, and the purity of the product was determined by liquid chromatography....

Embodiment 2

[0030] First add 1ml of raw material 2,5-dimethylfuran into the container, then add 10ml of methyl isobutyl ketone, 0.8g of USY molecular sieve (silicon-aluminum ratio of 5), and 0.1ml of deionized water. After mixing evenly, put it into a reactor, stir, and react at a constant temperature of 180° C. for 5 hours. After the reaction is completed, the reaction product is quenched in a low temperature, and the temperature is rapidly dropped to normal temperature. Then centrifuge, recover the catalyst, collect the organic phase, distill the obtained organic phase under reduced pressure, remove the organic solvent, and obtain the product. The conversion rate of the raw material and the yield of the product were determined by gas chromatography external standard method, and the purity of the product was determined by liquid chromatography. The results showed that the conversion rate of the raw material 2,5-dimethylfuran was 85%, the purity of the product was 90%, and the yield of 2...

Embodiment 3

[0032] Into the container, sequentially add: 1ml 2,5-dimethylfuran, 12ml methyl isobutyl ketone, 0.1ml deionized water, 1.2g ZSM-5 zeolite molecular sieve (silicon-alumina ratio is 20), and mix evenly. The container was placed in a constant temperature reactor and reacted at 200° C. for 5 hours. After the reaction, the system was rapidly dropped to normal temperature. The reaction solution is separated from the solid phase and the organic phase, the catalyst is recovered, and the organic phase is collected. The organic phase was distilled under reduced pressure to remove the organic solvent to obtain the product. The conversion rate of the raw material and the yield of the product were determined by gas chromatography external standard method, and the purity of the product was determined by liquid chromatography. The results showed that the conversion rate of the raw material 2,5-dimethylfuran was 82%, the purity of the product was 92%, and the yield of 2,5-hexanedione was 7...

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Abstract

The invention provides a method for preparing 2,5-hexanedione under the catalysis of solid acid. The method comprises the following steps: adding an organic solvent with weak polarity, a solid acid catalyst and distilled water into a raw material 2,5-dimethylfuran and carrying out a reaction at a temperature of 80 to 200 DEG C for 1 to 12 h; quenching a reaction system so as to allow the temperature of the system to rapidly drop to normal temperature, taking out a reaction solution, then subjecting the reaction solution to filtering or centrifugation, drying the solid catalyst and recovering the dried solid catalyst; and collecting an organic phase, subjecting the obtained organic phase to reduced-pressure distillation and removing the organic solvent so as to obtain 2,5-hexanedione. The method provided by the invention has the advantages of easiness in separation and no pollution.

Description

technical field [0001] The invention belongs to a method for preparing 2,5-hexanedione by using solid acid molecular sieve as a catalyst. Background technique [0002] In recent years, 2,5-hexanedione has received more and more attention as an important chemical intermediate. At present, it is mainly used as a high boiling point solvent for synthetic resins, nitro spray paints, colorants, printing inks, etc., leather tanning agents, rubber vulcanization accelerators, pesticides, and pharmaceutical raw materials, and can also be used in pesticides and food additives. , spices, electroplating spray paint, photographic chemicals and many other fields. [0003] There are many preparation methods of 2,5-hexanedione, usually hydrolysis of 2,5-dimethylfuran is the main method. The hydrolysis of 2,5-dimethylfuran is an acid-catalyzed process, and the selection of an appropriate acid catalyst is the key to its effective hydrolysis. Among them, mineral acids such as hydrochloric aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/59C07C49/12
CPCC07C45/59C07C49/12
Inventor 侯相林李岳秦邓天昇杨永兴
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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