Method for preparing 2-butanol through catalytic hydrogenation of levulinic acid

Abstract

The invention discloses a method for preparing 2-butanol by catalytic hydrogenation of levulinic acid, which comprises the following steps: by taking levulinic acid as a raw material and isopropanol as a solvent, carrying out hydrodeoxygenation under the action of a reduced nano gamma-aluminum oxide loaded RuMn or NiMn catalyst to prepare 2-butanol with high selectivity at the reaction temperature of 190-250 DEG C for 1-5 hours, the hydrogen pressure in the reaction system is 1-5 MPa. The reaction process is simple, conditions are mild, and the whole reaction process is basically free of carbon deposition. The preparation process of the catalyst is short in time consumption and simple in process, and has a very good application prospect.

Description

Technical field:

[0001] The invention relates to a method for preparing 2-butanol by catalytic hydrogenation of levulinic acid. Background technique:

[0002] In the face of the depletion of fossil energy and the need for sustainable development of chemical production, the technology of producing fuels and chemicals from renewable resources has been vigorously developed in recent years. Among them, levulinic acid is an important platform compound for biomass conversion and utilization, and its source is mainly prepared from biomass raw materials, including lignocellulose, starch and sugar raw materials. At present, the method for preparing levulinic acid from biomass is mainly the acid-catalyzed conversion method. In addition, as one of the top 12 most promising platform compounds from biomass, levulinic acid can be used as a feedstock to prepare a series of high value-added chemicals, such as γ-valerolactone (GVL), Levulinate, 1,4-pentanediol (1,4-PD), 2-methyltetrahydrof...

Examples

Embodiment 1

[0033] Catalyst preparation:

[0034] (1) the ruthenium chloride of 0.4054g and the manganese nitrate aqueous solution of 4.8857g are added to the water to form a solution, stirred uniformly;

[0035] (2) 2.1g of γ-nano-alumina and 0.2765g of ethylene glycol are slowly added to the above-mentioned solution one by one, stirring while adding, until the solution just impregnates the carrier, and the loadings of ruthenium and manganese are respectively 5wt% and 25wt%;

[0036] (3) The above solution was sonicated at room temperature for 30 minutes and then stirred at room temperature for 12h;

[0037] (4) The solution after stirring for 12 hours was evaporated to dryness in an oil bath at 60°C with a rotary evaporator, and then placed in an oven at 100°C for 10 hours to completely remove water to obtain a solid;

[0038] (5) the obtained solid is ground with a mortar and sieved with a sieve and then roasted in a muffle furnace. The heating rate of the muffle furnace is 2°C / min, t...

Embodiment 2

[0041] Catalyst preparation: same as Example 1.

[0042] Reaction evaluation: the prepared 5%Ru-25%Mn / γ-Al 2 O 3The catalyst was heated in H at 400 °C (heating rate of 4 °C / min) using a reduction furnace. 2 with N 2 Reduction was carried out for 5h in an atmosphere with a volume ratio of 1:9. Then add in the autoclave, add levulinic acid and isopropanol, mix evenly, and seal the reactor; wherein, the quality of levulinic acid is 3% of the quality of isopropanol; the quality of catalyst is 33.3% of levulinic acid; then Use nitrogen to replace the air in the autoclave several times, and then replace the nitrogen in the autoclave with hydrogen several times, then fill with 5MPa hydrogen, react at 190 ° C for 4 hours, cool down to room temperature after the reaction, and use gas chromatography and GC-MS. The liquid and gas phase components were analyzed, and the conversion of levulinic acid was 100%, and the yield of 2-butanol was 63.25%. The reaction evaluation conditions an...

Embodiment 3

[0044] Catalyst preparation: (1) 0.4054g of ruthenium chloride and 3.9085g of manganese nitrate aqueous solution were added to water to form a solution, and stirred evenly; (2) 2.1g of γ-nano-alumina and 0.2765g of ethylene glycol were slowly added to the above In the solution, add and stir until the solution just soaks the carrier, and the loadings of ruthenium and manganese are 5wt% and 20wt% respectively; (3) The above solution is sonicated at room temperature for 30 minutes and then stirred at room temperature for 12h; (4) ) After stirring the solution for 12 hours, use a rotary evaporator to evaporate most of the water in an oil bath at 60°C, then place it in an oven at 100°C to dry for 10 hours to completely remove the water to obtain a solid; (5) Use a mortar for the obtained solid. After grinding and sieving with a sieve, it was calcined in a muffle furnace. The heating rate of the muffle furnace was 2 °C / min, the roasting temperature was 300 °C, and the roasting time w...

Technical field:

[0001] The invention relates to a method for preparing 2-butanol by catalytic hydrogenation of levulinic acid. Background technique:

[0002] In the face of the depletion of fossil energy and the need for sustainable development of chemical production, the technology of producing fuels and chemicals from renewable resources has been vigorously developed in recent years. Among them, levulinic acid is an important platform compound for biomass conversion and utilization, and its source is mainly prepared from biomass raw materials, including lignocellulose, starch and sugar raw materials. At present, the method for preparing levulinic acid from biomass is mainly the acid-catalyzed conversion method. In addition, as one of the top 12 most promising platform compounds from biomass, levulinic acid can be used as a feedstock to prepare a series of high value-added chemicals, such as γ-valerolactone (GVL), Levulinate, 1,4-pentanediol (1,4-PD), 2-methyltetrahydrof...

Examples

Embodiment 1

[0033] Catalyst preparation:

[0034] (1) the ruthenium chloride of 0.4054g and the manganese nitrate aqueous solution of 4.8857g are added to the water to form a solution, stirred uniformly;

[0035] (2) 2.1g of γ-nano-alumina and 0.2765g of ethylene glycol are slowly added to the above-mentioned solution one by one, stirring while adding, until the solution just impregnates the carrier, and the loadings of ruthenium and manganese are respectively 5wt% and 25wt%;

[0036] (3) The above solution was sonicated at room temperature for 30 minutes and then stirred at room temperature for 12h;

[0037] (4) The solution after stirring for 12 hours was evaporated to dryness in an oil bath at 60°C with a rotary evaporator, and then placed in an oven at 100°C for 10 hours to completely remove water to obtain a solid;

[0038] (5) the obtained solid is ground with a mortar and sieved with a sieve and then roasted in a muffle furnace. The heating rate of the muffle furnace is 2°C / min, t...

Embodiment 2

[0041] Catalyst preparation: same as Example 1.

[0042] Reaction evaluation: the prepared 5%Ru-25%Mn / γ-Al 2 O 3The catalyst was heated in H at 400 °C (heating rate of 4 °C / min) using a reduction furnace. 2 with N 2 Reduction was carried out for 5h in an atmosphere with a volume ratio of 1:9. Then add in the autoclave, add levulinic acid and isopropanol, mix evenly, and seal the reactor; wherein, the quality of levulinic acid is 3% of the quality of isopropanol; the quality of catalyst is 33.3% of levulinic acid; then Use nitrogen to replace the air in the autoclave several times, and then replace the nitrogen in the autoclave with hydrogen several times, then fill with 5MPa hydrogen, react at 190 ° C for 4 hours, cool down to room temperature after the reaction, and use gas chromatography and GC-MS. The liquid and gas phase components were analyzed, and the conversion of levulinic acid was 100%, and the yield of 2-butanol was 63.25%. The reaction evaluation conditions an...

Embodiment 3

[0044] Catalyst preparation: (1) 0.4054g of ruthenium chloride and 3.9085g of manganese nitrate aqueous solution were added to water to form a solution, and stirred evenly; (2) 2.1g of γ-nano-alumina and 0.2765g of ethylene glycol were slowly added to the above In the solution, add and stir until the solution just soaks the carrier, and the loadings of ruthenium and manganese are 5wt% and 20wt% respectively; (3) The above solution is sonicated at room temperature for 30 minutes and then stirred at room temperature for 12h; (4) ) After stirring the solution for 12 hours, use a rotary evaporator to evaporate most of the water in an oil bath at 60°C, then place it in an oven at 100°C to dry for 10 hours to completely remove the water to obtain a solid; (5) Use a mortar for the obtained solid. After grinding and sieving with a sieve, it was calcined in a muffle furnace. The heating rate of the muffle furnace was 2 °C / min, the roasting temperature was 300 °C, and the roasting time w...

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