Method for catalyzing levulinic acid or levulinic acid ester to gamma-valerolactone by in-situ reduction of basic copper carbonate/hydroxyl aluminium oxide

A technology for catalyzing levulinic acid and aluminum oxyhydroxide, which is applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., and can solve problems such as increased production costs and high reaction temperatures , to achieve good catalytic activity, simple reaction system, and strong operational safety

Active Publication Date: 2019-04-30
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method reaction temperature is higher (180 ℃-280 ℃), increased production cost

Method used

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  • Method for catalyzing levulinic acid or levulinic acid ester to gamma-valerolactone by in-situ reduction of basic copper carbonate/hydroxyl aluminium oxide
  • Method for catalyzing levulinic acid or levulinic acid ester to gamma-valerolactone by in-situ reduction of basic copper carbonate/hydroxyl aluminium oxide
  • Method for catalyzing levulinic acid or levulinic acid ester to gamma-valerolactone by in-situ reduction of basic copper carbonate/hydroxyl aluminium oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 0.67mmol methyl levulinate, 0.1g Cu 2 (OH) 2 CO 3 / AlOOH (Cu / Al=3 / 1) and 20ml of isopropanol were placed in a 35mL autoclave. After the autoclave was sealed, the reaction was stirred at 180°C for 5h. After the autoclave was cooled, it was tested.

[0046] where Cu 2 (OH) 2 CO 3 The preparation method of / AlOOH catalyst is: with 3.624g Cu (NO 3 ) 2 ·3H 2 O and 1.875gAl 2 (NO 3 ) 3 9H 2 O was dissolved in 40 mL of deionized water and stirred at room temperature for several minutes; subsequently, with 1mol / L Na 2 CO 3 Adjust the pH of the solution to 8-9, stir for ten minutes, and let it stand overnight; then filter it with suction, wash it four or five times with deionized water, and dry it in an oven at 80°C; then grind it and bake it in a muffle furnace at 200°C. Finally, Cu with a Cu / Al molar ratio of 3 / 1 is obtained 2 (OH) 2 CO 3 / AlOOH.

[0047] Such as figure 1 As indicated, the resulting solution was detected by gas chromatography-mass spectrometr...

Embodiment 2

[0050] 0.67mmol methyl levulinate, 0.1g Cu 2 (OH) 2 CO 3 / AlOOH (Cu / Al=3 / 1) and 20ml of isopropanol were placed in a 35mL autoclave. After the autoclave was sealed, the reaction was stirred at 180°C for 1h. After the autoclave was cooled, it was tested.

[0051] where Cu 2 (OH) 2 CO 3 The preparation method of / AlOOH catalyst is: with 3.624g Cu (NO 3 ) 2 ·3H 2 O and 1.875gAl 2 (NO 3 ) 3 9H 2 O was dissolved in 40 mL of deionized water and stirred at room temperature for several minutes; subsequently, with 1mol / L Na 2 CO 3 Adjust the pH of the solution to 8-9, stir for ten minutes, and let it stand overnight; then filter it with suction, wash it four or five times with deionized water, and dry it in an oven at 80°C; then grind it and bake it in a muffle furnace at 200°C. Finally, Cu with a Cu / Al molar ratio of 3 / 1 is obtained 2 (OH) 2 CO 3 / AlOOH.

[0052] The obtained solution was detected by gas chromatography-mass spectrometry (TRACE DSQ GC-MS). According t...

Embodiment 3

[0054] 0.67mmol methyl levulinate, 0.1g Cu 2 (OH) 2 CO 3 / AlOOH (Cu / Al=3 / 1) and 20ml of isopropanol were placed in a 35mL autoclave. After sealing the autoclave, the reaction was stirred and reacted at 180°C for 24h. After the autoclave was cooled, it was to be tested.

[0055] where Cu 2 (OH) 2 CO 3 The preparation method of / AlOOH catalyst is: with 3.624g Cu (NO 3 ) 2 ·3H 2 O and 1.875gAl 2 (NO 3 ) 3 9H 2 O was dissolved in 40 mL of deionized water and stirred at room temperature for several minutes; subsequently, with 1mol / L Na 2 CO 3 Adjust the pH of the solution to 8-9, stir for ten minutes, and let it stand overnight; then filter it with suction, wash it four or five times with deionized water, and dry it in an oven at 80°C; then grind it and bake it in a muffle furnace at 200°C. Finally, Cu with a Cu / Al molar ratio of 3 / 1 is obtained 2 (OH) 2 CO 3 / AlOOH.

[0056] The obtained solution was detected by gas chromatography-mass spectrometry (TRACE DSQ GC-M...

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Abstract

The invention discloses a method for catalyzing levulinic acid or levulinic acid ester to gamma-valerolactone by in-situ reduction of basic copper carbonate/hydroxyl aluminium oxide, and the reactionprocess is as follows: adding the levulinic acid or levulinic acid ester, a secondary alcohol and the basic copper carbonate/hydroxyl aluminum oxide (Cu2(OH) 2CO3/AlOOH) into a high-pressure reactionkettle, uniformly mixing, sealing, and reacting at 140-220 DEG C for 1-24 hours, and cooling to obtain a gamma-valerolactone solution. The reaction has a good yield in a short time of 5 hours, and theexperiment process is simple and convenient to operate, and the method is low in cost and relatively low in reaction temperature and has a good industrial production prospect.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for in-situ reduction of basic copper carbonate / aluminum oxyhydroxide to catalyze levulinic acid or levulinic acid ester to gamma-valerolactone. Background technique [0002] Due to the limited natural resources and the increasing demand for energy, the selective conversion of biomass into fuels and chemicals is of great significance in the rapidly developing human society. Among the different approaches to biomass conversion, catalytic routes are particularly important, and many biomasses can be produced through careful design of catalytic systems for the production of derived chemicals and fuels. γ-valerolactone is considered as one of the most promising platform compounds for the sustainable production of fuels and high value-added chemicals, which can be obtained by hydrogenolysis of levulinic acid or its esters from lignocellulose. [0003] There are two ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01J27/236B01J37/16B01J23/72B01J35/02
CPCC07D307/33B01J23/72B01J27/236B01J35/023B01J37/16
Inventor 田戈马明伟刘辉曹靖劼
Owner JILIN UNIV
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