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Preparation method of catalyst for alternative natural gas preparation through synthesis gas methanation

A technology that replaces natural gas and catalysts. It is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc. It can solve the problems of waste catalyst pollution, achieve high reactivity, reduce concentration difference, and improve selectivity. Effect

Active Publication Date: 2017-07-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only utilizes the Mo, Co and alumina supports in the spent hydrotreating catalyst, but also makes full use of the Ni and V deposited on the spent hydrotreating catalyst, which solves the pollution problem of spent catalysts, saves resources and improves benefits , is technically easy to implement, and the resulting synthesis gas methanation catalyst has the characteristics of low cost, high utilization rate of metal components and good selectivity

Method used

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  • Preparation method of catalyst for alternative natural gas preparation through synthesis gas methanation
  • Preparation method of catalyst for alternative natural gas preparation through synthesis gas methanation

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Experimental program
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Effect test

Embodiment 1

[0033] The spent hydrotreating catalyst (MoCo / Al 2 o 3 ), the oil on the surface of the catalyst was removed by petroleum ether extraction, dried at 110°C for 8 h, and the obtained catalyst was calcined at 450°C for 4 h to obtain a spent catalyst after treatment (containing Mo: 12.8 wt%, Co: 2.3 wt%, V: 2.5wt%, Ni: 1.9wt%, Al 2 o 3 : 71.2 wt%), grind the catalyst to 200 mesh (referring to passing through a 200 mesh sieve), weigh 100g of the powder, add 260mL of 98 wt% concentrated sulfuric acid, stir at 50°C to dissolve the solid, collect the filtrate by filtration, and pour it into Add 38.15g of nickel nitrate to the filtrate, stir and dissolve, then add 27.31g of citric acid (the molar ratio of citric acid to Mo in the waste agent is 1), and then add 750.79g of ethyl orthosilicate to control the pH value of the system to 4.0. Stir at 70°C until a gel is formed, age the gel at room temperature for 8 hours, then dry at 110°C for 8 hours, and calcinate the resulting solid at...

Embodiment 2

[0035] The spent hydrotreating catalyst (MoCo / Al 2 o 3 ), the oil on the surface of the catalyst was removed by petroleum ether extraction, dried at 110°C for 8 h, and the obtained catalyst was calcined at 450°C for 4 h to obtain a spent catalyst after treatment (containing Mo: 12.8 wt%, Co: 2.3 wt%, V: 2.5wt%, Ni: 1.9wt%, Al 2 o 3 : 71.2 wt%), grind the catalyst to 200 mesh (referring to passing through a 200 mesh sieve), weigh 100g of the powder, add 300mL of a mixed solution of 98 wt% concentrated sulfuric acid and 65 wt% concentrated nitric acid, the volume ratio is 2:1, Stir at constant temperature at 50°C to dissolve the solid, collect the filtrate by filtration, add 11.73g of nickel nitrate to the filtrate, stir and dissolve, add 40.98g of citric acid (the molar ratio of citric acid to Mo in the waste agent is 1.5), and then add 1155.93g tetraethyl orthosilicate, control the pH value of the system to 4.0, stir at 70°C until a gel is formed, age the gel at room temper...

Embodiment 3

[0037] The spent hydrotreating catalyst (MoCo / Al 2 o 3 ), the oil on the surface of the catalyst was removed by petroleum ether extraction, dried at 110°C for 8 h, and the obtained catalyst was calcined at 450°C for 4 h to obtain a spent catalyst after treatment (containing Mo: 12.8 wt%, Co: 2.3 wt%, V: 2.5wt%, Ni: 1.9wt%, Al 2 o 3 : 71.2 wt%), grind the catalyst to 200 mesh (referring to passing through a 200 mesh sieve), weigh 100g of the powder, add 450mL of a mixed solution of 35 wt% concentrated hydrochloric acid and 65 wt% concentrated nitric acid, the volume ratio is 1:1, Stir at constant temperature at 50°C to dissolve the solid, collect the filtrate by filtration, add 54.01g of nickel nitrate to the filtrate, stir and dissolve, add 13.66g of citric acid (the molar ratio of citric acid to Mo in the waste agent is 0.5), and then add 507.7g tetraethyl orthosilicate, control the pH value of the system to 4.0, stir at 70°C until a gel is formed, age the gel at room temp...

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Abstract

The invention relates to a preparation method of a catalyst for alternative natural gas preparation through synthesis gas methanation. The catalyst comprises an active component, an auxiliary agent, and a carrier. The preparation method comprises: preparing a catalyst precursor A, and reducing the catalyst precursor A; dissolving an auxiliary agent precursor in water, and uniformly mixing with a furfural aqueous solution; adding the obtained mixture and the catalyst precursor A to a high pressure reaction kettle, adding a solution C, and carrying out a reaction; and treating and separating the obtained solid-liquid mixture, filtering the obtained solid sample, drying, and calcining to obtain the catalyst. According to the present invention, the waste residue oil hydrotreating catalyst is completely utilized so as to save the cost; and the catalyst has characteristics of high reaction activity, metal consumption reducing, and methane selectivity improving.

Description

technical field [0001] The invention relates to a preparation method of a synthetic gas methanation to substitute natural gas catalyst, in particular to a preparation method of a supported molybdenum-based catalyst for synthetic gas methanation to substitute natural gas. Background technique [0002] Methanation refers to CO / CO 2 with H 2 Under certain temperature, pressure and catalyst action, generate CH 4 At present, this reaction is widely used in the removal of trace carbon in the synthesis of ammonia or hydrogen production, methanation of coke oven gas, and coal-to-natural gas. Methanation is an important catalytic technology, especially in fuel applications, where it can be used to increase the calorific value of gas, allowing the conversion of coke oven gas, coal or biomass to natural gas. In recent years, with the rapid development of my country's coal-based natural gas industry, methanation, one of the core technologies, has received more and more attention. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/887
CPCB01J23/8877B01J37/18
Inventor 孙晓丹张舒冬刘继华
Owner CHINA PETROLEUM & CHEM CORP
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