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Sulfurization method of sulfur-tolerant methanation catalyst

A technology for sulfur-resistant methanation and catalyst, which is used in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., to achieve the effects of improved catalytic activity and stability, high sulfur loading rate, and reduced sulfurization cost.

Inactive Publication Date: 2015-07-15
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The sulfidation method of the above-mentioned catalyst is not specifically for the sulfidation method of the sulfur-resistant methanation catalyst. In particular, in the above-mentioned existing sulfidation methods, the catalyst is subjected to constant temperature sulfidation at a specific temperature, so there are above The problem that the sulfur rate needs to be improved

Method used

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  • Sulfurization method of sulfur-tolerant methanation catalyst
  • Sulfurization method of sulfur-tolerant methanation catalyst
  • Sulfurization method of sulfur-tolerant methanation catalyst

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Experimental program
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Effect test

Embodiment 1

[0021] Such as figure 1 As shown, in the reaction system of four reactors connected in series, the sulfur-resistant methanation catalysts numbered NICE-1, NICE-2, NICE-3, NICE-4 and NiICE-5 were used to carry out the sulfuration experiment of the method of the present invention. The loading method and loading amount of each catalyst are as described in the above embodiment, and the total loading amount of the catalyst is 800ml.

[0022] After the reactor system is airtight, use H 2 S concentration is 3% by volume in H 2 S / H 2 The mixed gas raised the reactors to normal operating pressure, and then raised the temperature of each reactor to 250°C at a rate of 20°C / hour. After the temperature of each reactor is stabilized, feed the above-mentioned H into each reactor at the same time. 2 S / H 2 Mixed gas to carry out sulfidation operation on the catalyst until H 2 S / H 2 The mixed gas penetrates the entire catalyst bed.

[0023] in H 2 S / H 2 After the mixed gas penetrates ...

Embodiment 2

[0029] Such as figure 1 As shown, in the reaction system of four reactors connected in series, the sulfur-resistant methanation catalysts numbered NICE-1, NICE-2, NICE-3, NICE-4 and NiICE-5 were used to carry out the sulfuration experiment of the method of the present invention. Mix five catalysts numbered NICE-1, NICE-2, NICE-3, NICE-4 and NiICE-5 with 8.1 grams, 7.4 grams, 10.7 grams, 27.4 grams and 28.8 grams of sulfur powder according to the loading ratio .

[0030] The loading method and loading amount of each catalyst are as described in the above embodiment, and the total loading amount of the catalyst is 800 mL.

[0031] After the reaction system is airtight, the system is raised to normal operating pressure with hydrogen, and then the temperature of each reactor is raised to 200°C at a temperature increase rate of 20°C / h. After the temperature of each reactor is stabilized, start the compressor to establish a normal hydrogen circulation until the hydrogen sulfide ga...

Embodiment 3

[0052] Such as figure 1 As shown, in the reaction system of four reactors connected in series, the sulfur-resistant methanation catalysts numbered NICE-1, NICE-2, NICE-3, NICE-4 and NiICE-5 were used to carry out the sulfuration experiment of the method of the present invention. The loading method and loading amount of each catalyst are as described in the above embodiment, and the total loading amount of the catalyst is 800ml.

[0053] After the reactor system is airtight, use H 2 S concentration is 3% by volume in H 2 S / H 2 The mixed gas raised the reactor to normal operating pressure, and then raised the temperature of each reactor to 200°C at a rate of 20°C / hour. After the temperature of each reactor is stabilized, feed the above-mentioned H into each reactor at the same time. 2 S / H 2 Mixed gas to carry out sulfidation operation on the catalyst until H 2 S / H 2 The mixed gas penetrates the entire catalyst bed.

[0054] After the hydrogen sulfide gas penetrates throu...

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Abstract

The invention discloses a sulfurization method of a sulfur-tolerant methanation catalyst. The method comprises a step of performing constant-temperature sulfurization on the catalyst with a sulfurizing agent and / or sulfur-containing reductive gas at two different temperatures. The preferred implementation method comprises the steps of performing constant-temperature sulfurization on the catalyst with a sulfurizing agent and / or sulfur-containing reductive gas at two different temperatures of 400-500 DEG C and 400-600 DEG C. The sulfur-tolerant methanation catalyst takes Co and / or Ni as an auxiliary agent, Mo and W and / or V oxide or sulfide as a catalytic active component, one or several oxides of Mg, Ce, Zr, Y, La and Ti as a carrier modifying agent and Al2O3 or ZrO2 as a carrier. The sulfur feeding amount, catalytic activity and stability of the sulfur-tolerant methanation catalyst prepared with the sulfurization method are remarkably improved.

Description

technical field [0001] The invention relates to a sulfuration method of a sulfur-resistant methanation catalyst. Background technique [0002] Sulfur-resistant methanation catalysts with oxides or sulfides of Mo, W and / or V as catalytically active components must undergo sulfidation treatment to activate them before use. There are various catalyst sulfide activation methods in the prior art, Including in-line vulcanization and off-line vulcanization. [0003] US5017535 discloses a method for preparing a sulfided or presulfided catalyst, which proposes to contact the sulfide with the hydrogenation catalyst outside the reactor for off-line sulfidation. In this method, the fresh catalyst is soaked in the organic sulfide solution or sprayed on the catalyst with the organic sulfide solution, then the catalyst is dried to remove the solvent, and then the catalyst containing sulfide is loaded into the reactor for vulcanization. The disadvantage of this sulfidation method is that...

Claims

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Application Information

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IPC IPC(8): B01J37/20
Inventor 龙俊英秦绍东汪国高田大勇孙守理孙琦
Owner CHNA ENERGY INVESTMENT CORP LTD