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Method for directly preparing alkyl levulinate from furfural

A technology of levulinate and furfural, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of increasing costs, and achieve the effects of easy synthesis, mild reaction conditions, and low cost

Active Publication Date: 2018-10-19
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process can achieve high product yield without using hydrogen, but the participation of precious metals in the catalyst increases the cost of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Change Zr(NO 3 ) 4 • 5H 2 O was dissolved in deionized water, and then the carrier MCM-41 was added. After 124 hours of continuous stirring, it was distilled under reduced pressure at 50°C until the water completely evaporated; then dried at 80°C for 24 hours, and finally calcined at 550°C for 6 hours to prepare ZrO 2 / MCM supported molecular sieve, where Zr(NO 3 ) 4 • 5H 2 The mass ratio of O to carrier is 0.37:1;

[0018] (2) Take the loaded molecular sieve ZrO 2 / MCM and ion exchange resin Amberlyst 15 are added to the reaction kettle, and then the mixture of isopropanol and furfural is added, reacted at 130°C for 24h, cooled and filtered to obtain isopropyl levulinate, in which the supported molecular sieve and ion exchange resin The mass ratio is 2:1. The mixture of isopropanol and furfural is prepared by mixing isopropanol and furfural in a volume ratio of 25:1. Analyzed by gas chromatography, the conversion rate of furfural is 97.0%, and the yield of isopropyl lev...

Embodiment 2

[0020] (1) Change Zr(NO 3 ) 4 • 5H 2 O was dissolved in deionized water, and then the carrier MCM-41 was added. After continuous stirring for 18 hours, it was distilled under reduced pressure at 40°C until the water was completely evaporated; then dried at 90°C for 17 hours, and finally calcined at 600°C for 6 hours to prepare ZrO 2 / MCM supported molecular sieve, where Zr(NO 3 ) 4 • 5H 2 The mass ratio of O to carrier is 0.4:1;

[0021] (2) Take the loaded molecular sieve ZrO 2 / MCM and ion exchange resin Amberlyst 15 are added to the reactor, and then the mixture of isopropanol and furfural is added, reacted at 140°C for 18h, cooled and filtered to obtain isopropyl levulinate, in which the supported molecular sieve and ion exchange resin The mass ratio is 3:1. The mixture of isopropanol and furfural is prepared by mixing isopropanol and furfural in a ratio of 21:1 by volume. Analyzed by gas chromatography, the conversion rate of furfural is 94.4% and the yield of isopropyl levuli...

Embodiment 3

[0023] (1) Change Zr(NO 3 ) 4 • 5H 2 O was dissolved in deionized water, and then the carrier MCM-41 was added. After continuous stirring for 12 hours, it was distilled under reduced pressure at 60°C until the water was completely evaporated; then dried at 100°C for 12 hours, and finally calcined at 580°C for 6 hours to prepare ZrO 2 / MCM supported molecular sieve, where Zr(NO 3 ) 4 • 5H 2 The mass ratio of O to carrier is 0.55:1;

[0024] (2) Take the loaded molecular sieve ZrO 2 / MCM and ion exchange resin Amberlyst 15 are added to the reactor, and then the mixture of isopropanol and furfural is added, reacted at 150℃ for 12h, cooled and filtered to obtain isopropyl levulinate, in which the supported molecular sieve and ion exchange resin The mass ratio is 2.5:1. The mixture of isopropanol and furfural is prepared by mixing isopropanol and furfural in a volume ratio of 28:1. Analyzed by gas chromatography, the conversion rate of furfural is 90.8%, and the yield of isopropyl levul...

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Abstract

The invention discloses a method for directly preparing alkyl levulinate from furfural. The method is characterized in that the furfural is used as raw materials; low-grade alkanol is used as a reaction medium; a combination of a supported molecular sieve ZrO2 / MCM and ion exchange resin Amberlyst-15 is used as a catalyst; reaction is performed for 8 to 24h at 130 to 150 DEG C; an alkyl levulinateproduct with the yield reaching up to 85.3 percent can be obtained. In the process, the used catalyst system is cheap and can be easily obtained; the catalyst can be easily separated, recovered and repeatedly used; the one-step synthetic process is simple; the equipment is simplified; the reaction conditions are mild; the additional addition of hydrogen gas is not needed; the safe and environment-friendly effects are achieved; the conversion efficiency is high; the target product yield is high; good industrial application prospects are realized.

Description

Technical field [0001] The invention relates to a catalyst system and a preparation method for directly synthesizing levulinate by one-step conversion of biomass-based furfural, and belongs to the technical field of biomass energy chemical industry. Background technique [0002] Furfural (Furfural, CAS No: 98-01-1), also known as 2-furancarboxaldehyde, is a derivative in which the hydrogen atom at the 2-position of furan is replaced by an aldehyde group; it can be used from abandoned agricultural and forestry crops such as corn cob, bagasse and chaff Made by hydrolysis in acidic medium. Furfural can be used to synthesize various fine chemicals through oxidation reaction, oxidation esterification reaction and reduction hydrogenation reaction. At present, the world can produce 600,000 tons of furfural every year, so it is urgent to develop new technology to improve the utilization value of furfural. [0003] Alkyl Levulinate is an important chemical intermediate and new energy chem...

Claims

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Application Information

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IPC IPC(8): C07C67/00C07C69/716
CPCC07C67/00C07C69/716
Inventor 彭林才高雪影余鑫
Owner KUNMING UNIV OF SCI & TECH
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