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Catalyst for producing levulinate through furfural and preparation method and application of catalyst

A technology of levulinic acid ester and catalyst, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of increasing investment and safety risks, and achieves improved economy, safety, and high activity. , the effect of mild reaction conditions

Active Publication Date: 2016-07-06
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the process uses high-pressure hydrogen, increasing investment and safety risks

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] First, weigh 1.0gH 3 PW 12 o 40 , add 10mL water to make a solution, add 10gSiO 2 , impregnated at room temperature for 8h, and baked in a muffle furnace at 250°C for 4h. Then, add 200mL chloroplatinic acid aqueous solution to the above sample, then add 0.5g sodium borohydride, stir for 1h, centrifuge to separate the solid, and dry at 80°C for 20h to obtain Pt-H 3 PW 12 o 40 / SiO 2 Catalyst, wherein the mass content of Pt is 1%, H 3 PW 12 o 40 The mass content is 10%.

[0024] Put 2g furfural, 15g methanol and 0.5g Pt-H 3 PW 12 o 40 / SiO 2 Added to the autoclave. Heating the reaction system to 160°C and continuing to heat for 10h, cooling the reaction kettle, taking out the product, centrifuging and analyzing by gas chromatography, the conversion rate of furfural was 100%, and the total yield of levulinic acid ester reached 76.4%.

Embodiment 2

[0026] First, weigh 2.0gH 4 SiW 12 o 40 , add 20mL water to make a solution, add 10gZrO 2 , impregnated at room temperature for 10 h, and baked at 200 ° C for 5 h in a muffle furnace. Then, add 200mL chloroplatinic acid aqueous solution to the above sample, then add 1.0g sodium borohydride, stir for 0.5h, centrifuge to separate the solid, and dry at 100°C for 12h to obtain Pt-H 4 SiW 12 o 40 / ZrO 2 Catalyst, wherein the mass content of Pt is 1%, H 4 SiW 12 o 40 The mass content is 20%.

[0027] Put 2g furfural, 10g ethanol, 5g propanol and 0.5g Pt-H 4 SiW 12 o 40 / ZrO 2 Added to the autoclave. Heating the reaction system to 160° C. and continuing heating for 15 hours, cooling the reaction vessel, taking out the product, centrifuging and analyzing by gas chromatography, the conversion rate of furfural was 100%, and the total yield of levulinic acid ester reached 80.1%.

Embodiment 3

[0029] First, weigh 2.0gH 4 SiW 12 o 40 , add 20mL water to make a solution, add 10gZrO 2 , impregnated at room temperature for 15h, and baked in a muffle furnace at 350°C for 2h. Then, add 200 mL palladium chloride aqueous solution to the above sample, then add 1.0 g sodium borohydride, stir for 3 h, centrifuge to separate the solid, and dry at 110 °C for 10 h to obtain Pd-H 4 SiW 12 o 40 / ZrO 2 Catalyst, wherein the mass content of Pd is 2%, H 4 SiW 12 o 40 The mass content is 20%.

[0030] Put 3g furfural, 20g n-propanol and 0.4g Pd-H 4 SiW 12 o 40 / ZrO 2into the autoclave. Heat the reaction system to 200°C and continue heating for 24 hours, cool the reactor, take out the product, centrifuge and analyze by gas chromatography, the conversion rate of furfural is 100%, and the total yield of levulinic acid ester reaches 78.9%.

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PUM

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Abstract

The invention discloses a catalyst for producing levulinate through furfural. The catalyst comprises the following components in percentage by mass: 0.5-5% of metal components, 5-30%of acid components, and the balance of carriers. The catalyst disclosed by the invention has the advantages of simple process, mild reaction conditions, low energy consumption, zero pollution and high yield.

Description

technical field [0001] The invention belongs to a method for preparing levulinic acid ester, in particular to a catalyst for producing levulinic acid ester from furfural, a preparation method and application. Background technique [0002] Furfural is an important biomass platform chemical and basic chemical industry raw material, which can be produced by hydrolyzing waste agricultural and forestry crops such as corncobs, bagasse and chaff in acidic medium. Traditionally, furfural is mainly synthesized into fine chemicals such as furfuryl alcohol, 2-methylfuran and tetrahydrofuran through catalytic hydrogenation. Now, the world can produce 200,000 tons of furfural every year, so it is urgent to develop new technology to convert furfural. [0003] Levulinate is widely used as a solvent, food additive and liquid fuel additive, and can also be used to synthesize liquid fuel γ-valerolactone. At present, there are mainly two synthesis methods of levulinate: (1) alcoholysis of su...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J31/38B01J31/26B01J27/055B01J27/18B01J27/185B01J27/188B01J27/19C07C69/716C07C67/00
CPCB01J23/30B01J27/055B01J27/18B01J27/185B01J27/188B01J27/19C07C67/00C07D307/44C07C69/716
Inventor 樊卫斌朱善辉王建国秦张峰岑友良
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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