Preparation method of 2-methoxy-4-methylphenol based on selective hydrodeoxygenation of vanillin

A technology of selective hydrogenation and methyl phenol, applied in the preparation of organic compounds, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of low energy efficiency, high temperature and high pressure, high hydrogen pressure, etc., and achieve simple reaction process, The effect of low cost and high yield

Pending Publication Date: 2022-06-03
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of preparation method based on vanillin selective hydrodeoxygenation 2-methoxy-4 methylphenol, to solve the prior art, the selective catalysis of vanillin Harsh reaction conditions, high temperature and high pressure, poor stability, high hydrogen pressure and low energy efficiency

Method used

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  • Preparation method of 2-methoxy-4-methylphenol based on selective hydrodeoxygenation of vanillin
  • Preparation method of 2-methoxy-4-methylphenol based on selective hydrodeoxygenation of vanillin
  • Preparation method of 2-methoxy-4-methylphenol based on selective hydrodeoxygenation of vanillin

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Experimental program
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Effect test

Embodiment 1～ Embodiment 9

[0036] Precipitation method: Dopamine hydrochloride and silica (2:1) were polymerized under a magnetic stirrer for 20 h, washed and dried, and calcined to 1000° C. under a nitrogen atmosphere. Remove the silica with NaOH solution, wash and dry by centrifugation, weigh 0.05g of the dried sample, add 20ml of deionized water, and adjust the pH of the solution to 9-10. The mass content of the catalyzed addition is 5%. After ultrasonic dispersion, sodium borohydride is added, and the molar ratio of sodium borohydride and the metal source is 30: 1. In the presence of sodium borohydride, it is fully reduced for 5h, washed and dried to obtain the obtained solution. described catalyst.

[0037] 0.01g, 0.005g, 0.008g or 0.015g of the above-mentioned deposition-precipitation method-Pt@CNS catalyst (wherein Pt: 5wt%, calcination temperature is 1000 ℃), 0.076g vanillin (vanillin and catalyst The mass ratios were 5:1, 7.6:1, 15.2:1, and 9.5:1) and 5 mL of isopropanol were added to a 50 mL ...

Embodiment 10

[0049] Dopamine hydrochloride and silica (mass ratio: 2:1 were polymerized under a magnetic stirrer for 20h, washed and dried, and calcined to a target temperature of 900°C under a nitrogen atmosphere). Use a certain concentration of NaOH solution to remove silica, wash and dry, weigh 0.05g of the dried sample, add 20ml of deionized water, and add chloroplatinic acid. The amount of nitric acid target added in the catalyst is the mass of the active component in the catalyst The content is 4.25%. After ultrasonic dispersion, sodium borohydride was added, the molar ratio of sodium borohydride and metal source was 30:1, fully reduced in the presence of sodium borohydride for 6 hours, washed and dried to obtain the catalyst.

[0050] 0.01 g impregnation method-Pt@CNS catalyst (wherein Pt: 4.25 wt%, calcination temperature is 900 °C), 0.076 g vanillin (the mass ratio of vanillin and catalyst is 7.6:1) and 5 mL isopropanol were added to 50 mL glass In the test tube, after the gas wa...

Embodiment 11

[0053] Dopamine hydrochloride and silica (mass ratio of 1:1 were polymerized under a magnetic stirrer for 24 hours, washed and dried, and calcined to a target temperature of 900°C under a nitrogen atmosphere). Use a certain concentration of NaOH solution to remove silica, wash and dry, weigh 0.05g of the dried sample, add 20ml of deionized water, and add chloroplatinic acid. The amount of chloroplatinic acid added in the catalyst is the active component in the catalyst. The mass content is 2.5%. After ultrasonic dispersion, sodium borohydride was added, the molar ratio of sodium borohydride and metal source was 30:1, fully reduced in the presence of sodium borohydride for 6 hours, washed and dried to obtain the catalyst.

[0054] 0.01 g of impregnation method-Pt@CNS catalyst (wherein Pt: 2.5 wt%, calcination temperature is 900 ° C), 0.076 g of vanillin and 5 mL of isopropanol were added to the lining of a 30 mL autoclave, and high-purity hydrogen was introduced to replace 5 A...

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Abstract

The invention discloses a 2-methoxy-4-methylphenol preparation method based on vanillin selective hydrodeoxygenation, which comprises the following steps: adding a reactant vanillin into a reaction kettle containing a certain amount of solvent, and carrying out hydrodeoxygenation reaction in the presence of a catalyst to obtain 2-methoxy-4-methylphenol, the catalyst is a porous carbon nanosphere loaded with a metal active component, the expression of the catalyst is M (at) CNS, M is any one of metal ruthenium, platinum, palladium, iridium, rhodium and gold, and CNS is a porous carbon nanosphere carrier. The porous carbon nanosphere not only has the characteristics of large specific surface area, abundant shell pore channels and easy regulation and control of pore diameter, but also has high dispersity and uniform size of loaded metal nanoparticles. The catalyst can realize high-efficiency and high-selectivity hydrodeoxygenation of vanillin under mild conditions to prepare 2-methoxy-4-methylphenol.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 2-methoxy-4-methylphenol based on vanillin selective hydrodeoxygenation. Background technique [0002] Biomass is a huge system composed of numerous polymers that can be converted into biomass platform molecules through a series of refining techniques, such as fermentation, cracking, catalysis, and chemical reactions, which can be further converted into targets molecular. The use of renewable biomass to replace limited fossil fuels has been recognized as a potential solution for the sustainable production of liquid fuels and valuable chemicals, but biomass has a high oxygen content and cannot be used directly, often requiring some It can be used by people only after special processing, including hydrodeoxygenation, zeolite cracking and water-phase reforming, etc. Hydrodeoxygenation method can significantly reduce the oxygen content of c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/18B01J23/42B01J23/44B01J23/46B01J23/52B01J37/03B01J37/16B01J37/02
CPCC07C41/18B01J23/42B01J23/44B01J23/52B01J23/462B01J23/464B01J23/468B01J37/035B01J37/16B01J37/0201C07C43/23Y02P30/20
Inventor 吴君陈鑫祥严鑫悦王成兵靳明谢宇航
Owner SHAANXI UNIV OF SCI & TECH
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