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a co 2 /h 2 o The method for preparing 3-acetylpropanol from furfural (or furfuryl alcohol) in the system

A technology for acetylpropanol and furfural, applied in the field of 3-acetylpropanol synthesis, can solve the problems of low reaction substrate concentration, difficult recovery of catalysts, expensive raw material alkynes, etc., to avoid subsequent treatment processes and waste generation, The effect of low cost and easy availability of raw materials

Active Publication Date: 2021-06-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, metal complexes such as gold, ruthenium, and platinum are used as catalysts to obtain 3-acetylpropanol through the hydration of alkynes (ACSCatal., 2016, 6, 7363-7376; Chemistry 2014, 20, 1918-1930; Eur.J . Inorg.Chem., 2004, 2004, 810-817; Organometallics 2013, 32, 2814-2826; Dalton Trans 2010, 39, 10601-10607.), but the catalyst is difficult to recover, the reaction substrate concentration is low, and the raw alkyne Disadvantages such as high price affect its wide-scale application in industry

Method used

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  • a co <sub>2</sub> /h <sub>2</sub> o The method for preparing 3-acetylpropanol from furfural (or furfuryl alcohol) in the system

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Experimental program
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Effect test

Embodiment 1

[0019] Furfuryl alcohol catalytic conversion reaction is carried out in a volume of 50mL autoclave, add 100mg furfuryl alcohol, 15mg (2wt%) Ru / CMK3 catalyst, pass into hydrogen replacement 3 times, then pass into carbon dioxide and hydrogen (pressure ratio is 3:1), Keep the total reaction pressure at 4MPa, heat the autoclave to 60°C in 15 minutes, stop the reaction after 20 hours of reaction, drop to room temperature, open the vent valve to reduce the pressure in the kettle to normal pressure, and the conversion rate of furfuryl alcohol is 100%, 3 - The yield of acetylpropanol is 62%.

Embodiment 2-9

[0021] The catalytic conversion reaction of furfural is carried out in an autoclave with a volume of 50 mL. Add 100 mg of furfural and 30 mg of activated catalyst, replace it with hydrogen for 3 times, and then feed a certain proportion of carbon dioxide and hydrogen to maintain the total reaction pressure at 4 MPa. The autoclave is heated to After a certain temperature and a certain time of reaction, stop the reaction, drop to room temperature, open the vent valve to reduce the pressure in the kettle to normal pressure. The test results are listed in Table 1.

[0022] Table 1:

[0023]

[0024] From the results in Table 1, it can be seen that the catalyst showed higher activity and 3-acetylpropanol selectivity to furfural, and mild reaction conditions were beneficial to the conversion of furfural, while CO 2 / H 2 The O medium promotes the ring opening of furan, which is beneficial to the conversion of furfural to 3-acetylpropanol. Therefore, this catalytic system has im...

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Abstract

The present invention relates to a CO 2 / H 2 The method for preparing 3-acetylpropanol from furfural (or furfuryl alcohol) in O system. with CO 2 / H 2 The in-situ acid system formed by O is used as a medium to convert furfural (or furfuryl alcohol) into 3-acetylpropanol in one step under the catalysis of a bifunctional catalytic system. The catalyst is a supported ruthenium-based catalyst, and the Ru content is 0.1-10wt% of the total mass of the catalyst. The present invention modulates CO 2 / H 2 Volume ratio, under optimal reaction conditions, the yield of 3-acetylpropanol can reach more than 84%. The invention has the obvious advantages of cheap and easy-to-obtain raw materials, simple operation, recyclable use, and easy recovery.

Description

technical field [0001] The invention relates to the field of 3-acetylpropanol synthesis, in particular to a 2 / H 2 A method for preparing 3-acetylpropanol from furfural (or furfuryl alcohol) in O system. Background technique [0002] Furfural (furfuryl alcohol) is one of the important biomass-based platform compounds, and it is also the only important industrial raw material that can be completely extracted from agricultural and forestry wastes. Due to its very active chemical properties, furfural can derive many high value-added chemicals through oxidation, hydrogenation, chlorination, esterification and condensation reactions. C5-keto compounds, as very important and common organic compounds, can be used as intermediates in drug synthesis. [0003] 3-acetylpropanol, an important class of pharmaceutical intermediates and organic synthesis intermediates, can be used in the synthesis of antimalarials and vitamin B. Currently, the synthesis of 3-acetylpropanol is mainly ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/00C07C45/59C07C49/17B01J23/46
Inventor 刘菲刘巧云乔波涛王爱琴张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI