Non-supported mesoporous hydrodeoxygenation catalyst, preparation and application thereof

A deoxygenation catalyst, unsupported technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, hydrocarbon production from oxygen-containing organic compounds, etc. Complex process and other problems, to achieve the effects of excellent water resistance, high deoxidation rate, and simple preparation process

Pending Publication Date: 2021-11-19
SOUTHWEST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After careful study of the above preparation scheme, it is not difficult to find that the synthesis process is relatively complicated and not efficient enough, and the reaction conditions are not mild enough.

Method used

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  • Non-supported mesoporous hydrodeoxygenation catalyst, preparation and application thereof
  • Non-supported mesoporous hydrodeoxygenation catalyst, preparation and application thereof
  • Non-supported mesoporous hydrodeoxygenation catalyst, preparation and application thereof

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preparation example Construction

[0032] At the same time, the invention also discloses a method for preparing a non-supported mesoporous hydrodeoxygenation catalyst, the catalyst is prepared by mixing soluble nickel salt, soluble niobium salt and organic acid, ultrasonic oscillation, drying, roasting and reduction, Specifically include the following steps:

[0033] S1, dissolving soluble nickel salt and organic acid in ethanol solution, dissolving soluble niobium salt in water, mixing with each other, stirring evenly, adding nitric acid to adjust pH value to form a mixture;

[0034] S2. Heat the above mixture to 60-100°C, stir until viscous, and then oscillate ultrasonically for 10-30min;

[0035]S3. Put the viscous mixture in an oven and dry it in an environment of 80-120°C for 4-10 hours to obtain a dried mixture;

[0036] S4, heating the dried mixture in a muffle furnace at a rate of 2-10°C / min to 400-600°C for 3-6h;

[0037] S5. Place the calcined precursor in a tube furnace at 300-500°C under 10vol% H ...

Embodiment 1

[0041] Embodiment 1 mesoporous catalyst preparation

[0042] The bulk catalyst was prepared by sol-gel method. Take a certain amount of nickel nitrate, niobium oxalate, citric acid in proportion, mol ratio Nb:Ni=0.1:0.9, mol ratio (Nb+Ni): citric acid=1:1 (wherein, " (Nb+Ni) mol " means the sum of moles of niobium element and nickel element), nickel nitrate and citric acid are dissolved in ethanol solution, niobium oxalate is dissolved in water, the above solutions are mixed evenly and the pH value is adjusted to 1 with nitric acid, and the mixed solution is placed Heat in an oil bath at 90°C with magnetic stirring until viscous, oscillate ultrasonically for 15 minutes and then dry at 100°C for 10 hours to obtain a xerogel; put the xerogel in a muffle furnace for 500°C and bake it for 5 hours, then place it in a tube furnace at 400°C 10vol%H 2 / Ar atmosphere for 3 h to obtain the non-supported mesoporous hydrodeoxygenation catalyst. The XRD spectrum of the bulk type Ni-Nb c...

Embodiment 2

[0043] Embodiment 2 mesoporous catalyst preparation

[0044] The bulk catalyst was prepared by sol-gel method. Take a certain amount of nickel chloride, niobium oxalate, citric acid in proportion, mol ratio Nb:Ni=0.2:0.8, mol ratio (Nb+Ni): citric acid=1:2 (wherein, " (Nb+Ni) mol” means the sum of moles of niobium and nickel), nickel chloride and citric acid are dissolved in ethanol solution, niobium oxalate is dissolved in water, and the mixture is placed in an oil bath at 90°C and heated with magnetic stirring until Viscous, ultrasonically oscillated for 15 minutes and then dried at 90°C for 8 hours to obtain a xerogel; put the xerogel in a muffle furnace at 500°C for 4 hours, and then in a tube furnace at 450°C with 10vol%H 2 / Ar atmosphere reduction for 4h to obtain the non-supported mesoporous hydrodeoxygenation catalyst. The XRD spectrum of the bulk type Ni-Nb composite catalyst prepared by the present embodiment is as follows figure 1 Shown; The scanning electron mic...

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Abstract

The invention relates to a non-supported mesoporous hydrodeoxygenation catalyst, which comprises elemental nickel and diniobium pentaoxide, wherein a molar ratio of the elemental nickel to the diniobium pentaoxide is 7:2-18:1. The preparation method comprises the following steps: dissolving a nickel salt and citric acid in an ethanol solution, dissolving a niobium salt in water, mixing, adjusting the pH value to 1-4 by using nitric acid, placing in an oil bath at a temperature of 80-100 DEG C, heating and stirring until the mixture is viscous, ultrasonically oscillating for 15-30 minutes, drying at a temperature of 80-120 DEG C for 4-10 hours, roasting at a temperature of 400-600 DEG C for 3-6 hours, and reducing at a temperature of 300-500 DEG C for 3-5 hours in a 10vol% H2/Ar atmosphere, wherein BET determination results show that the catalyst is of a mesoporous structure; and putting the catalyst and bio-oil into a batch reactor, and carrying out hydrodeoxygenation reaction for 1-8 hours at a hydrogen pressure of 1-4 MPa and a temperature of 180-250 DEG C to obtain a bio-oil hydrodeoxygenation product. The method is simple and efficient in synthesis and mild in reaction condition.

Description

technical field [0001] The invention relates to the field of biomass catalysis, in particular to a non-loaded mesoporous hydrodeoxygenation catalyst and its preparation and application. Background technique [0002] Due to the dual pressure of energy shortage and environmental degradation, countries all over the world are scrambling to develop safe and environmentally friendly renewable new energy sources. Among many renewable energy sources, biomass energy is rich in content, wide in sources, cheap and easy to obtain, and meets the requirements of sustainable development. At present, a lot of research work is devoted to the conversion of biomass into fuels and high value-added products, especially the research on the preparation of fuels by hydrodeoxygenation of woody biomass has received extensive attention. [0003] The oxygen content in bio-oil can reach up to 40-50%, affecting its stability. At present, most of the common hydrodeoxygenation catalysts are transition me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/847B01J35/10B01J37/03B01J37/08B01J37/18C07C1/22C07C13/18C11C3/12
CPCB01J23/8474B01J35/1019B01J35/1061B01J37/036B01J37/082B01J37/18C07C1/22C11C3/123C11C3/126C07C2523/847C07C13/18
Inventor 徐娟侯英刘祥义张凯向凤红付晓娜
Owner SOUTHWEST FORESTRY UNIVERSITY
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