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Preparation method and application of carbon-nitrogen co-doped iron-cobalt-based catalyst

A co-doping, iron-cobalt-based technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. problem, to achieve the effect of improving catalytic activity and directional selectivity, increasing active sites, and increasing force

Inactive Publication Date: 2021-10-22
哈尔滨领昇生物医药科技有限公司
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Problems solved by technology

The biological depolymerization method is specifically divided into enzymatic hydrolysis and microbial fermentation. Compared with the chemical method, it is more environmentally friendly and has high selectivity, but the depolymerization rate is low, takes a long time, and the cost of raw materials is high, easy to deactivate, and harmful to the environment. Large-scale industrial applications with high requirements and no lignin

Method used

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  • Preparation method and application of carbon-nitrogen co-doped iron-cobalt-based catalyst

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preparation example Construction

[0025] The present invention provides the preparation method of the carbon-nitrogen co-doped iron-cobalt-based catalyst of an embodiment, comprising the following steps:

[0026] S1: Dissolve iron salt and cobalt salt in deionized water, stir magnetically at 50-80°C for 3-5 hours to obtain a mixed solution; the ratio of iron salt, cobalt salt and deionized water is 1mmol:(0.3-0.5)mmol : 5mL; Described iron salt is one or more in ferrous nitrate, ferrous sulfate, ferrous chloride; Described cobalt salt is one or more in cobalt nitrate, cobalt sulfate, cobalt chloride;

[0027] S2: Add an equal volume of 0.4-0.5mol / L sodium oxalate solution dropwise to the mixed solution, stir and react at 20-60°C for 6-12h, filter, and dry to obtain an iron-cobalt oxalate precursor;

[0028] S3: Place the iron-cobalt oxalate precursor in a tube furnace, heat-treat at 300-600°C for 1-3 hours, and then feed CH at a flow rate of 250-500 sccm 4 and NH 3 mixed gas, after vapor deposition for 2 to ...

Embodiment 1

[0032] A preparation method for a carbon-nitrogen co-doped iron-cobalt-based catalyst, comprising the following steps:

[0033] S1: Dissolve 10 mmol of ferrous nitrate and 3 mmol of cobalt nitrate in 50 mL of deionized water, and stir magnetically at 50° C. for 3 h to obtain a mixed solution;

[0034] S2: Add 50mL of 0.4mol / L sodium oxalate solution dropwise to the mixed solution, stir and react at 20°C for 6h, filter and dry to obtain the iron-cobalt oxalate precursor;

[0035] S3: Place the iron-cobalt oxalate precursor in a tube furnace, heat-treat at 300 °C for 1 h, and then feed CH at a flow rate of 250 sccm 4 and NH 3 the mixed gas, the CH 4 , NH 3 The volume ratio is 1:0.5, and after vapor deposition for 2 hours, it is ground to the micro-nano level to obtain the iron-cobalt material;

[0036] S4: Add 1mL carbon source sol solution to 0.5g iron-cobalt material, and described carbon source sol solution is formulated according to the ratio of 1g:1.5g:10mL by chitosan,...

Embodiment 2

[0038] A preparation method for a carbon-nitrogen co-doped iron-cobalt-based catalyst, comprising the following steps:

[0039] S1: Dissolve 10 mmol of ferrous sulfate and 4 mmol of cobalt sulfate in 50 mL of deionized water, and stir magnetically at 70° C. for 3 to 5 hours to obtain a mixed solution;

[0040] S2: Add 50mL of 0.45mol / L sodium oxalate solution dropwise to the mixed solution, stir and react at 50°C for 8h, filter and dry to obtain the iron-cobalt oxalate precursor;

[0041] S3: Place the iron-cobalt oxalate precursor in a tube furnace, heat-treat at 450°C for 1-3h, and then feed CH at a flow rate of 350sccm 4 and NH 3 the mixed gas, the CH 4 , NH 3 The volume ratio is 1:0.6, and after vapor deposition for 2 to 4 hours, it is ground to the micro-nano level to obtain iron-cobalt materials;

[0042] S4: Add 1mL carbon source sol solution to 0.6g iron-cobalt material, described carbon source sol solution is formulated according to the ratio of 1g:2g:10mL by chit...

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Abstract

The invention discloses a preparation method and application of a carbon-nitrogen co-doped iron-cobalt-based catalyst, and the preparation method comprises the following steps: S1, dissolving an iron salt and a cobalt salt in deionized water, and magnetically stirring at 50-80 DEG C for 3-5 hours to obtain a mixed solution; S2, dropwise adding an isometric 0.4-0.5 mol / L sodium oxalate solution into the mixed solution, stirring and reacting at 20-60 DEG C for 6-12 hours, filtering and drying; S3, placing the obtained cobalt iron oxalate precursor in a tubular furnace, carrying out heat treatment at 300-600 DEG C for 1-3 hours, introducing a mixed gas of CH4 and NH3 at a flow rate of 250-500 sccm, carrying out vapor deposition for 2-4 hours, and grinding to a micro-nano level; and S4, adding a carbon source sol solution into the obtained iron-cobalt material, carbonizing for 1-3 hours, introducing NH3 at the flow rate of 200-400 sccm under the condition of 500-600 DEG C, continuously treating for 0.5-1.5 hours, activating, carrying out secondary vapor deposition, cooling, crushing, washing and drying. The metal elements Fe and Co and oxides thereof form a defect energy state between a valence band and a conduction band by doping non-metal elements carbon and nitrogen, so that lattice distortion is caused, and the catalytic activity and directional selectivity of the catalyst are improved.

Description

technical field [0001] The invention belongs to the technical field of catalyst synthesis, and in particular relates to a preparation method and application of a carbon-nitrogen co-doped iron-cobalt-based catalyst. Background technique [0002] Lignin is a biopolymer with a three-dimensional network structure formed by the interconnection of three phenylpropane units through ether bonds and carbon-carbon bonds. It contains rich aromatic ring structures, aliphatic and aromatic hydroxyl groups, and quinone groups and other active groups. , is the second largest biomass resource after cellulose in the plant kingdom. Lignin accounts for 15% to 30% of the total biomass, and its main function is to support the water transport and structural integrity of plants, specifically composed of p-hydroxyphenyl (H), guaiacyl (G) and syringyl (S) The phenolic polymers formed are then linked together by various C-O and C-C bonds, such as α-o-4, α-α, β-o-4, β-β and 4-O-5 bonds. The natural r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08C07C41/01C07C43/23
CPCB01J27/24B01J37/086B01J37/084C07C41/01C07C43/23
Inventor 宋冬雪李伟
Owner 哈尔滨领昇生物医药科技有限公司
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