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Method for preparing 2-methoxy-4-methylphenol from biomass-based vanillin

A technology based on methylphenol and vanillin, applied in the field of biomass-based vanillin to prepare 2-methoxy-4-methylphenol, can solve the problems of high cost and unfavorable industrial production, achieve low price and avoid catalytic activity Not high or deactivated, the effect of changing electronic properties

Pending Publication Date: 2022-06-24
SHAANXI UNIV OF SCI & TECH
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  • Description
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of method that biomass-based vanillin prepares 2-methoxy-4-methylphenol, to solve the problem that the active metal component of catalyst in the prior art is noble metal , the cost is high, which is not conducive to the problem of industrial production

Method used

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  • Method for preparing 2-methoxy-4-methylphenol from biomass-based vanillin
  • Method for preparing 2-methoxy-4-methylphenol from biomass-based vanillin
  • Method for preparing 2-methoxy-4-methylphenol from biomass-based vanillin

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preparation example Construction

[0029] 1. The preparation method of the catalyst:

[0030] 1.1 mL of methyl methacrylate, 21 mL of styrene, 0.92 mL of acrylic acid and 0.49 g of ammonium bicarbonate were added to 100 mL of deionized water, added to a round-bottomed flask, heated and stirred in an oil bath until the temperature rose to 0.53 g of ammonium persulfate was added at 70° C., and then heated to 80° C. and stirred for 12 h. After stirring, centrifugation and washing were completed, and the centrifuged samples were obtained into polystyrene nanospheres. Polystyrene nanospheres can not only be used as the hard template of the catalyst, but also easily decomposed at high temperature, so there is no need to specially remove the template, and the polystyrene nanospheres also have the characteristics of uniform particle size distribution.

[0031] The polystyrene nanospheres and 2-methylimidazole were added to a round-bottomed flask containing deionized water, and the mixing mass ratio of the polystyrene n...

Embodiment 1

[0035] Example 1 (Co@NHCS-600)

[0036] 0.3 g of polystyrene nanospheres, 5.5 g of 2-methylimidazole and 20 mL of deionized water were added to a round-bottomed flask, and after sonicating for 30 min, transferred to an oil bath and stirred; 1.55 mmol of cobalt nitrate hexahydrate was added. It was added to 3 mL of deionized water, and then transferred to the previous round-bottomed flask. During the transfer, it was added dropwise. After the addition was completed, the mixture was stirred at room temperature for 6 h. After stirring, the samples were centrifuged and washed with deionized water and methanol (water and methanol were washed twice each), and the washed samples were placed in an oven at 110° C. overnight. The samples were calcined in a tube furnace at a calcination temperature of 600 °C, kept for 4 h, and the heating rate was 5 °C / min.

Embodiment 2

[0037] Example 2 (Co@NHCS-900)

[0038] 0.3 g of polystyrene nanospheres, 5.5 g of 2-methylimidazole and 20 mL of deionized water were added to a round-bottomed flask, and after sonicating for 30 min, transferred to an oil bath and stirred; 1.55 mmol of cobalt nitrate hexahydrate was added. It was added to 3 mL of deionized water, and then transferred to the previous round-bottomed flask. During the transfer, it was added dropwise. After the addition was completed, the mixture was stirred at room temperature for 6 h. After stirring, the samples were centrifuged and washed with deionized water and methanol (water and methanol were washed twice each), and the washed samples were placed in an oven at 110° C. overnight. The samples were calcined in a tube furnace at a calcination temperature of 900 °C, kept for 4 h, and the heating rate was 5 °C / min.

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Abstract

The invention provides a method for preparing 2-methoxy-4-methylphenol from biomass-based vanillin and a preparation method of the 2-methoxy-4-methylphenol. According to the method, vanillin, a catalyst and a solvent are added into a reaction kettle, chemical reaction is carried out in the reaction kettle to obtain the required 2-methoxy-4-methylphenol, the catalyst is a nitrogen-doped hollow carbon sphere loaded non-noble metal Co catalyst, the main structure of the catalyst is a hollow carbon sphere, the hollow structure is used as a carrier, and the carrier is used as a solvent. Metal particles are loaded on the carrier, and the surface of the carrier has a mesoporous structure, so that a unique confinement effect can be provided for hydrodeoxygenation reaction of vanillin, the metal nanoparticles can be stabilized, the stability of the catalyst can be improved, meanwhile, strong metal-carrier interaction can be formed, and the electronic property of the metal surface can be effectively changed; furthermore, adsorption and activation of vanillin and an intermediate vanillyl alcohol on the surface of the catalyst can be enhanced, and the selectivity of preparing 2-methoxy-4-methylphenol by hydrodeoxygenation of vanillin is improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for preparing 2-methoxy-4-methylphenol from biomass-based vanillin. Background technique [0002] With the rapid development of modern society, the demand for energy is expected to increase further in the coming decades. At present, the supply of energy mainly depends on fossil energy, but the excessive exploitation and utilization of fossil energy will not only lead to resource depletion, but also bring about a series of environmental problems. Therefore, it is necessary to find solutions that can replace or reduce the use of fossil energy. It is a new type of green energy to solve the problem of energy demand in the development of modern society. As a natural renewable resource, biomass has received extensive attention in recent years because it can be efficiently converted into various chemicals and fuels, which can effectively solve current energy...

Claims

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Application Information

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IPC IPC(8): C07C41/18C07C41/26B01J27/24B01J35/08
CPCC07C41/18C07C41/26B01J27/24B01J35/51B01J35/40C07C43/23
Inventor 吴君靳明赵峻锋严鑫悦谢宇航刘立乾李宜晟
Owner SHAANXI UNIV OF SCI & TECH
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