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Method for preparing 2,5-acetonyl acetone

A technology of hexanedione and acidic aqueous solution is applied in the preparation of heterocyclic compounds, the preparation of carbonyl compounds by hydrolysis, organic chemistry, etc. Effect

Active Publication Date: 2019-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the highest yield they obtained was only 24.5%, and the production efficiency was low

Method used

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  • Method for preparing 2,5-acetonyl acetone
  • Method for preparing 2,5-acetonyl acetone
  • Method for preparing 2,5-acetonyl acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-21

[0024] Grind and dry willow, pine, mulberry, birch, newspaper, cotton, cotton thread, cotton cloth, etc., take 20g and add it to a 4L reaction kettle, add 2g of 5% Pd / C, add 0.4L of 36% hydrochloric acid aqueous solution and 1.2 L of chloroform, filled with 6MPa hydrogen, reacted at 100°C for 2 hours.

[0025] Table 1 Different raw materials for preparing 2,5-hexanedione

[0026]

[0027] Note: It can be seen from Example 12 that lignin cannot generate 2,5-hexanedione, and hemicellulose rich in five-carbon sugars will generate a large amount of furfural, and its further conversion products are also five-carbon Levulinic acid, thus theoretically impossible to convert the five-carbon sugar directly into 2,5-hexanedione containing six carbon atoms. Therefore, the yield of 2.5-hexanedione in the above table is calculated based on the mass of the six-carbon sugar in each raw material, and the following tables all calculate the yield of 2,5-hexanedione according to this method. ...

Embodiment 22-38

[0031] Put 20g of cellulose into a 4L reactor, add 2g of noble metal catalyst, add 0.4L of 36% hydrochloric acid aqueous solution and 1.2L of chloroform, fill with 6MPa hydrogen, and react at 100°C for 2 hours.

[0032] Table 2 Different catalysts prepare 2,5-hexanedione

[0033]

[0034] It can be seen from Table 2 that catalysts with different contents, different supports and different noble metal supports can effectively catalyze the reaction, among which Pd has the best activity among all noble metals; among all supports, activated carbon and alumina are the most active. Good; when the metal loading is greater than 1%, an ideal yield of 2,5-hexanedione can be obtained.

Embodiment 39-56

[0036] Put 20g of cellulose into a 4L reactor, add 2g of 1% Pd / C catalyst, add 0.4L of 36% aqueous hydrochloric acid and 1.2L of chloroform, fill in a certain pressure of hydrogen, and react at different reaction temperatures certain hours.

[0037] Table 3 Different reaction conditions prepare 2,5-hexanedione

[0038]

[0039] As can be seen from Table 3, the reaction can be effectively catalyzed under different reaction times, different hydrogen pressures and different reaction temperatures. Even at room temperature, a 23% yield of 2,5-hexanedione can be obtained, increasing the reaction temperature can increase the yield of 2,5-hexanedione, and the maximum yield is 65% at 80 degrees. Continue to increase the reaction temperature, the yield of 2,5-hexanedione decreases slightly, indicating that under high temperature conditions, 2,5-hexanedione will be further converted into other substances. When the reaction time is 0.1 hour, there is already a 45% yield of 2,5-hexane...

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Abstract

The invention relates to a method for preparing 2,5-acetonyl acetone from raw biomass, paper products, cotton products and lignocellulose platform chemical compounds. A reaction system is an acid water solution and organic solvent two-phase system; a catalyst is a supported noble metal catalyst; under the conditions of certain temperature and hydrogen gas pressure, the raw biomass, the paper products, the cotton products and the lignocellulose platform chemical compounds can be used for preparing 2,5-acetonyl acetone products with high yield in one step. The method has the characteristics of mild reaction temperature and high product selectivity; an effective path for preparing the 2,5-acetonyl acetone from biomass is provided.

Description

technical field [0001] The invention relates to a method for preparing 2,5-hexanedione. Specifically, raw biomass, paper products, cotton products, and lignocellulosic platform compounds are used as raw materials, A / B loaded noble metal catalysts, acidic aqueous solution, and organic solvent two-phase reaction system are used. A method for preparing 2,5-hexanedione in one step with high yield starting from biomass or its platform compounds. Background technique [0002] The increasing scarcity of fossil resources, the increase in oil prices, the massive emissions of greenhouse gases, and the demand for energy in society require people to look for new energy sources that can replace fossil resources. Biomass, as the only renewable organic carbon source, can be used to produce fuels, chemicals and carbon materials, and has become a hot research topic at present. [0003] 2,5-Hexanedione is an important organic chemical, widely used in synthetic resins, nitro spray paints, co...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C45/59C07C45/60C07C49/12
Inventor 李广亿李宁张涛王爱琴王晓东丛昱
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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