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Oxide carrier-loaded cobalt catalyst and preparation method and application thereof

An oxide carrier, cobalt catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve high operating costs, catalyst loss of activity, catalyst loss It can improve the ability of sulfur resistance and achieve the effect of good activity.

Active Publication Date: 2011-04-13
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above catalysts can obtain good catalytic activity and long-chain hydrocarbon selectivity, and have very high requirements on the purity of the synthesis gas, especially sulfur and sulfur compound impurities, and generally require that the total sulfur content in the synthesis gas should not exceed 2ppm ( In terms of sulfur element), when the total sulfur content is too high, the metal active components in the catalyst will be generated metal sulfides, thereby causing the catalyst to lose activity (Zhang Bijiang, coal-based synthetic liquid fuel, first edition, Shanxi Science and Technology Publishing Society, 1993, 15), this phenomenon is easy to appear especially in industrial-scale Fischer-Tropsch synthesis
Raw synthesis gas produced by coal gasification contains H 2 S, CS 2 , COS and other sulfides, although the feed gas has undergone a desulfurization process before it enters the Fischer-Tropsch synthesis, it requires very high operating costs to keep it below 2ppm for a long time, and occasional accidents such as power outages during operation may also cause the sulfur content to exceed the standard, resulting in catalyst deactivation, therefore, it is very necessary to improve the sulfur resistance of the catalyst itself

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a kind of Al 2 o 3 Loaded cobalt catalyst, wherein the carrier contains 0.01wt% of boron element; 25wt% of cobalt element and 0.1wt% of ruthenium element are contained in the catalyst, and its preparation method is as follows: 6g boric acid and 9994gAl 2 o 3 The powders (purity 98.6%) were mixed, then added 5% concentrated nitric acid (65wt%) relative to the total mass of the two and deionized water of 30% of the total mass of the two, kneaded in a kneader for 30min, and extruded Bars, made into round bars with a diameter of 2.0mm and a length of 4-6mm, dried at 80°C for 2h, then heated to 120°C for 4h, and finally placed in a muffle furnace and roasted at 350°C for 4h to obtain boron-containing 0.01wt% Al 2 o 3 carrier.

[0025] Take the above carrier 65.9g, 61.7g Co(NO 3 ) 2 ·6H 2 O was made into a 53ml solution, impregnated onto the carrier by the method of impregnating the full pores, dried at 120°C for 4 hours after standing for 2 hours, and made into a cat...

Embodiment 2

[0028] a kind of Al 2 o 3 Loaded cobalt catalyst, wherein the carrier contains 0.01wt% boron element, 20wt% cobalt element, 0.1wt% ruthenium element, and 0.5wt% lanthanum element in the catalyst. Its preparation method is as follows:

[0029] Get the carrier 72.7g among the embodiment 1, add and use 1.56g lanthanum nitrate hexahydrate [La(NO 3 ) 3 ·6H 2 O] The 58ml solution prepared was left to stand for 2h, dried at 120°C for 4h, and then roasted at 400°C for 4h, and 49.3g of Co(NO 3 ) 2 ·6H 2 The 58ml solution prepared by O was left to dry and then dried at 120°C for 4 hours to make an intermediate, and then 49.3g Co(NO 3 ) 2 ·6H 2 O and 0.31g Ru(NO)(NO 3 ) 3 Make 50ml mixed solution and immerse the intermediate, dry it at 120°C for 4h and then bake it at 400°C for 4h to make 20%Co, 0.1%Ru, 0.5%La / 0.01B-Al 2 o 3 catalyst.

[0030] Get 5.0g of this catalyst in the fixed bed reactor with the H of 20L / h flow 2 Fischer-Tropsch synthesis reaction is carried out afte...

Embodiment 3

[0032] a kind of Al 2 o 3 Supported cobalt catalyst, wherein the carrier contains 0.01wt% boron element, 15wt% cobalt element, 0.1wt% platinum element and 20wt% zirconium element in the catalyst. Its preparation method is as follows:

[0033] Get the carrier 58g among the embodiment 1, with 74.8g zirconium nitrate [Zr(NO 3 ) 4 ·5H 2 O] Make 50ml solution and impregnate it on the carrier, let it stand to dry, dry it at 120℃ for 6h, then roast it at 400℃ for 4h, after cooling, add 74.0g cobalt nitrate [Co(NO 3 ) 2 ·6H 2 O] and 0.164g platinum nitrate [Pt(NO 3 ) 4 ] made 50ml mixed solution, let stand for 2h, dry at 120°C for 4h, then roast at 400°C for 4h to get 15%Co, 0.1%Pt, 20%Zr / 0.01B-Al 2 o 3 catalyst.

[0034] Get 5.0g of this catalyst in the fixed bed reactor with the H of 20L / h flow 2 Fischer-Tropsch synthesis reaction was carried out after reduction at 400°C and atmospheric pressure for 10 hours, at a volume ratio of H 2 :CO=2:1, total gas flow rate 10.0L / h,...

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Abstract

The invention discloses an oxide carrier-loaded cobalt catalyst and a preparation method and application thereof. In the catalyst, the Al2O3 or SiO2 which is modified by boric acid or borate is used as a carrier; the treated carrier contains 0.01 to 10 weight percent of boron; and the carrier loads 10 to 35 percent of cobalt by an impregnation method and introduces one or two of Mg, Ca, Ba, Ru, Zr, La, Ce and Pt to serve as an auxiliary agent by post-impregnation or coimpregnation, wherein the auxiliary agent accounts for 0.09 to 20.1 weight percent of the catalyst. The catalyst has obviously-improved sulfur resistance, has high activity when sulfur content reaches 200ppm, has high catalytic performance, and has CO conversion activity of more than 55 percent, methane selectivity of less than 10 percent and C5<+> selectivity of more than 80 percent when Fischer-Tropsch reaction is performed under the condition that the gas flow passing through every gram of catalyst is 2.0L every hour at the temperature of 210 DEG C under the pressure of 2.0MPa.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic catalysts, in particular to an oxide carrier-supported cobalt catalyst and its preparation method and application. The catalyst prepared by the invention has good sulfur resistance, good CO conversion activity and long-chain hydrocarbon selectivity , suitable for catalyzing the Fischer-Tropsch synthesis reaction. Background technique [0002] Fischer-Tropsch synthesis is a reaction in which a mixture of carbon monoxide and hydrogen (synthesis gas) is converted into hydrocarbon compounds under catalytic conditions. In Fischer-Tropsch synthesis catalysts, metals of Group VIII or their oxides are often used. Among these metals In addition to iron directly using its oxides to make catalysts, other metals are expensive. In order to make the most effective use of their catalytic performance and reduce the amount of raw materials, they are often loaded on an inert carrier by impregnation...

Claims

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Application Information

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IPC IPC(8): B01J23/75B01J23/89C10G2/00
Inventor 李金林张煜华刘家举胡春玲胡红军
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES