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Composite carbide catalyst and preparing method and application thereof

A composite carbide and catalyst technology, which can be used in carbon compound catalysts, hydrocarbon production from carbon oxides, physical/chemical process catalysts, etc., can solve problems such as wide product distribution, and achieve wide reaction temperature, narrow product distribution The effect of high activity and olefin selectivity

Inactive Publication Date: 2016-07-27
NINGXIA UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of composite carbide catalyst and its preparation method and application, aim at solving the problem that the product distribution is wide in the existing synthesis gas conversion olefin process; Improve C 2 -C 4 Olefin selectivity, inhibiting the formation of heavy hydrocarbons

Method used

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  • Composite carbide catalyst and preparing method and application thereof

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preparation example Construction

[0025] Such as figure 1 Shown, the preparation method of the composite carbide catalyst of the embodiment of the present invention comprises the following steps:

[0026] S101: Weigh a certain amount of iron nitrate Fe(NO 3 ) 3 9H 2 O and ammonium molybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O, respectively or mechanically mixed in the air atmosphere, the temperature is 400-600 ° C, and roasted for 2-8 hours to obtain Fe, Mo oxide precursors or Fe-Mo mixed oxide precursors;

[0027] S102: Grinding a certain amount of Fe, Mo oxide or mixed oxide precursor, respectively placing them in different carbonization atmospheres, and performing temperature-programmed carbonization. Fe oxide precursor at 300-450°C, CO / H 2 Under the atmosphere, reduction carbonization treatment 3-8h, N 2 Cooled to room temperature under atmosphere, O 2 / N 2 (1v%O 2 ) passivation for 1-5h to obtain powdered carbide A; Mo oxide precursors or Fe, Mo mixed oxide precursors with different ratios in C / H 2 U...

Embodiment 1

[0036] Weigh Fe(NO 3 ) 3 9H 2 O20.20g, (NH 4 ) 6 Mo 7 o 24 4H 2 O43.25g was calcined at 500°C in air for 5h to obtain Fe and Mo oxide precursors; a certain amount of iron oxide was 2 (molar ratio 1:1) atmosphere, reduction carbonization treatment 5h, N 2 Cooled to room temperature under atmosphere, O 2 / N 2 (1v%O 2 ) passivation for 5h to obtain powdered iron carbide; molybdenum oxide precursor was ground and placed in CH 4 / H 2 (Molar ratio 1:4) in a carbonization atmosphere, the temperature was programmed to carbonize at 700°C, and kept for 4h, N 2 Cooled to room temperature under atmosphere, O 2 / N 2 (1v%O 2 ) passivation for 5h, to obtain powdered molybdenum carbide. Weigh a certain amount of two kinds of carbides, grind and mix them evenly, weigh 2.0732g of potassium carbonate according to the Mo / K molar ratio of 2.3:1, and make it into a solution with a certain concentration, mix it with the above powder by dipping method, and dry it at 100°C. Catalyst p...

Embodiment 2

[0038] Weigh Fe(NO 3 ) 3 9H 2 O20.20g, (NH 4 ) 6 Mo 7 o 24 4H 2 O49.43g was mechanically mixed and calcined at 500°C for 5h in the air to obtain the Fe-Mo oxide precursor; the obtained Fe-Mo mixed oxide precursor was dissolved in CH 4 / H 2 (molar ratio 1:4) atmosphere, 700 ℃ reduction carbonization 4h, N 2 Cooled to room temperature under atmosphere, O 2 / N 2 (1v%O 2 ) passivation for 5 hours to obtain powdered Fe-Mo composite carbide; according to the Mo / K molar ratio of 4:1, weigh 1.3821 potassium carbonate, and configure it into a solution with a certain concentration, mix it with the above powder by impregnation method, and dry it at 100 °C. Catalyst powder is obtained; the obtained powder is ground, tableted and granulated to obtain a composite carbide catalyst. Catalyst reaction conditions: H 2 / CO=1, 2.0MPa, 350℃, space velocity 4000h -1 . CO conversion rate 80.2%, CH 4 The selectivity is 21.2%, C 2 = -C 4 = Accounting for 48.5% of the total hydrocar...

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Abstract

The invention discloses a composite carbide catalyst and a preparing method and application thereof.The preparing method includes the steps that a precursor of Fe oxide and a precursor of Mo oxide or a precursor of mixed oxide are ground to be put into different carbonization atmospheres, heated and carbonized; the precursor of the Fe oxide is reduced and carbonized at the temperature of 300 DEG C-450 DEG C in the CO / H2 atmosphere, and cooled to be at the room temperature in the N2 atmosphere, O2 / N2 passivating treatment is carried out, and powder carbide A is obtained; the precursor of the Mo oxide or the precursor of the Fe and Mo mixed oxide in different proportions is reduced and carbonized at the temperature of 650 DEG C-800 DEG C in the C / H2 carbonization atmosphere, and cooled to be at the room temperature in the N2 atmosphere, O2 / N2 passivating treatment is carried out, and powder carbide B or powder Fe-Mo compound carbide C is obtained, wherein the molar ratio of Fe to Mo to K of the catalyst is (50-60):(30-55):(3-15).The composite carbide catalyst is used for a syngas olefin preparing reaction, and has the advantages of being broad in reaction temperature, high in activity and olefin selectivity and narrow in product distribution range.

Description

technical field [0001] The invention belongs to the technical fields of energy and chemical industry, and in particular relates to a composite carbide catalyst and its preparation method and application. Background technique [0002] Low-carbon olefins (including ethylene, propylene and butene) are important basic organic chemical raw materials with a wide range of applications. At present, the production process of low-carbon olefins mainly adopts the petrochemical route of cracking naphtha and light diesel oil. Due to the increasing shortage of global oil resources, the production process and raw materials of low-carbon olefins must develop in a diversified manner. In recent years, the non-petroleum route methanol-to-olefins (MTO, MTP) process has developed rapidly. With the increasing demand for low-carbon olefins, the direct production of low-carbon olefins (C2=-C4=) by Fischer-Tropsch synthesis has attracted widespread attention. Obtaining olefins has simple process f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/22C07C1/04C07C11/04C07C11/06C07C11/08
CPCY02P20/52B01J27/22C07C1/044C07C2527/22C07C11/04C07C11/06C07C11/08
Inventor 张建利刘俊杰赵天生马清祥范素兵
Owner NINGXIA UNIVERSITY