CN111545054B - Application of spinel catalytic material - Google Patents

Application of spinel catalytic material Download PDF

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CN111545054B
CN111545054B CN202010558449.5A CN202010558449A CN111545054B CN 111545054 B CN111545054 B CN 111545054B CN 202010558449 A CN202010558449 A CN 202010558449A CN 111545054 B CN111545054 B CN 111545054B
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spinel
hydrogen sulfide
hydrogen
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catalytic material
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CN111545054A (en
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张鑫
蒋国霞
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University of Chinese Academy of Sciences
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B01D53/8612—Hydrogen sulfide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/02—Preparation of sulfur; Purification
    • C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
    • C01B17/0495—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by dissociation of hydrogen sulfide into the elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/102—Removal of contaminants of acid contaminants
    • C10L3/103—Sulfur containing contaminants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/40—Mixed oxides
    • B01D2255/405—Spinels
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

The invention discloses an application of a spinel catalytic material. The spinel catalytic material is applied to the thermal catalytic decomposition of hydrogen sulfide or the preparation of hydrogen and elemental sulfur from hydrogen sulfide in acid gas. The invention relates to a method for preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide, which comprises the following steps: and catalyzing the hydrogen sulfide or the hydrogen sulfide in the acid gas by using the spinel catalytic material to perform decomposition reaction, thereby obtaining hydrogen and elemental sulfur. The spinel material has a stable structure during a thermal catalytic reaction, and has good thermal stability, sulfur resistance, temperature fluctuation resistance, high-temperature sintering resistance and thermal shock resistance; acid gas H of spinel material in chemical industry2The S shows excellent catalytic activity in catalytic decomposition reaction, and 50 percent of H can be obtained2Yield (800 ℃ C.).

Description

Application of spinel catalytic material
Technical Field
The invention relates to application of a spinel catalytic material, in particular to application of the spinel catalytic material in preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide, and belongs to the field of acid gas treatment and resource recovery.
Background
A large amount of hydrogen sulfide acid gas is generated in the production process of coal chemical industry and natural gas chemical industry. Hydrogen sulfide is a colorless gas with strong toxicity and malodor, and is also a nerve agent. The main organs with toxic action are central nervous system and respiratory system, and can also damage organs such as heart and the like; the most sensitive tissues to toxic effects are the brain and mucosa in contact with the tissue. According to estimation, the chemical industry in China can generate over 1200 million tons of acid gas every year. At present, the method aims at the chemical industry H2And (2) treating the acid gas by adopting a traditional Claus process method to treat hydrogen sulfide, and oxidizing the hydrogen sulfide into elemental sulfur and water:
H2S+3/2O2→SO2+H2O
2H2S+SO2→3/xSx+2H2O
although the claus process can realize the harmless treatment of hydrogen sulfide, hydrogen with higher added value is converted into water, thereby wasting precious resources. The hydrogen energy is the fuel which is hopeful to replace fossil energy in the future, and the industrial hydrogen is produced by reforming or electrolyzing water from light hydrocarbon, coal, natural gas, methanol and the like at present, so the cost is high, the price is high, and the industrial hydrogen is difficult to be widely used as the fuel. Therefore, if hydrogen sulfide can be decomposed, hydrogen sulfide can be rendered harmless, and hydrogen gas and elemental sulfur having high added values can be obtained. Besides, the recycling of hydrogen energy in the petroleum processing process is realized, and simultaneously, the emission of a large amount of carbon dioxide brought by the traditional hydrocarbon reforming hydrogen production can be reduced, so that the method has great practical significance.
However, the thermal decomposition reaction of hydrogen sulfide is a strongly endothermic reaction and is limited by the thermodynamic equilibrium, with only a very low equilibrium conversion at low temperatures (only 20% for hydrogen sulfide at 1000 ℃ and 38% for 1200 ℃). The catalytic decomposition of hydrogen sulfide can not only effectively improve the yield of hydrogen and sulfur, but also reduce the reaction temperature, and is a mode which is simple and stable in operation and can be widely applied. At present, hydrogen sulfide decomposition catalysts are mainly focused on metal sulfides (e.g., FeS, CuS and NiS), metal disulfides (e.g., MoS)2，WS2，FeS2，CoS2And NiS2) And the like. However, at present, the activity of all the catalysts is generally not high (the hydrogen yield is 20 percent at 770 ℃). Therefore, the development of a catalyst and a catalysis method which have simple preparation and operation and can efficiently decompose hydrogen sulfide to prepare hydrogen and sulfur at higher temperature has important significance.
Spinel is a compositionally controlled, wide variety of crystalline materials that may contain one or more metal elements, with nearly all main group metals and transition metals entering the spinel structure. Due to various compositions, electronic configurations and valence states, the spinel has excellent catalytic performance; and the spinel material has simple synthesis method and easy operation. The spinel material has a melting point of 2135 ℃, a refractoriness of about 1900 ℃, good thermal shock resistance, strong stability and wide application range.
Disclosure of Invention
The invention aims to provide application of a spinel catalytic material, in particular to application of the spinel catalytic material in preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide.
The spinel catalytic material provided by the invention is applied to preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide.
In the application, the general formula of the spinel catalytic material is AB2O4Wherein A is at least one of Li, Ba, Ca, Mn, Mg, Fe, Cu, Zn, Ni and Co, B is at least one of Cr, Ni, Fe, Co, Al and Mn, and AB2O4Not being ZnFe2O4。
In the above application, the reaction conditions of the spinel catalytic material in the thermal catalytic decomposition of hydrogen sulfide are as follows:
the temperature may be 300 to 1100 ℃, specifically 500, 550, 600, 700, 750, 800 ℃, 500 to 800 ℃ or 400 to 1000 ℃, and the reaction pressure may be normal pressure.
The invention also provides the application of the spinel catalytic material in preparing hydrogen and elemental sulfur by the thermal catalytic decomposition of hydrogen sulfide in acid gas;
the hydrogen sulfide in the acid gas is derived from the acid gas generated in at least one of the fields of petrochemical industry, coal chemical industry and natural gas chemical industry.
In the application, the general formula of the spinel catalytic material is AB2O4Wherein A is at least one of Li, Ba, Ca, Mn, Mg, Fe, Cu, Zn, Ni and Co, B is at least one of Cr, Ni, Fe, Co, Al and Mn, and AB2O4Not being ZnFe2O4。
In the above application, the reaction conditions of the spinel catalytic material in the thermal catalytic decomposition of hydrogen sulfide in acidic gas are as follows:
the temperature may be 300 to 1100 ℃, specifically 500, 550, 600, 700, 750, 800 ℃, 500 to 800 ℃ or 400 to 1000 ℃, and the reaction pressure may be normal pressure.
The invention further provides a method for preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide, which comprises the following steps: and catalyzing the hydrogen sulfide or the hydrogen sulfide in the acid gas by using the spinel catalytic material to perform decomposition reaction, thereby obtaining hydrogen and elemental sulfur.
In the method, the volume percentage concentration of the hydrogen sulfide in the acid gas can be 0.1-100%; the volume percentage concentration of ammonia can be 0-50%; the volume percentage concentration of the carbon dioxide can be 0-50%; the volume percentage concentration of the hydrocarbons can be 0-10%; the water volume percentage concentration can be 0-30%.
In the present invention, the acid gas may be an acid gas commonly used in the art.
In the above method, the conditions of the decomposition reaction are as follows:
the temperature can be 300-1100 ℃, specifically 500, 550, 600, 700, 750, 800 ℃, 500-800 ℃ or 400-1000 ℃, and the reaction pressure is normal pressure.
In the above method, when the spinel catalyst material catalyzes the hydrogen sulfide in the acid gas to be carried out on the catalytic reaction bed, the space velocity of the acid gas can be 1000h-1～50000h-1Specifically 24000h-1、1000h-1～24000h-1、24000h-1～50000h-1Or 15000h-1～40000h-1。
In the present invention, the normal pressure is a common knowledge in the art, and refers to an atmospheric pressure, i.e. a gas pressure generated by the atmosphere in our ordinary life, and a standard atmospheric pressure is 101325 Pa.
The invention has the following advantages:
(1) the spinel material has stable structure during catalytic reaction, and has good thermal stability, sulfur resistance, temperature fluctuation resistance, high-temperature sintering resistance and thermal shock resistance.
(2) Acid gas H of spinel material in chemical industry2The S shows excellent catalytic activity in catalytic decomposition reaction, and 50 percent of H can be obtained2Yield (800 ℃ C.).
Drawings
FIG. 1 shows FeAl2O4XRD pattern of catalytic material.
FIG. 2 is a graph showing the effect of different temperatures on the yield of hydrogen from hercynite catalyzed decomposition of hydrogen sulfide in example 1 of the present invention.
FIG. 3 is a graph showing the effect of different temperatures on the yield of hydrogen from magnesium aluminate spinel catalyzed hydrogen sulfide decomposition in example 2 of the present invention.
FIG. 4 is a graph showing the results of the comparative example method.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Examples 1,
FeAl2O4The spinel synthesis method comprises the following steps:
(1) mixing Fe (NO)3)3，Al(NO3)3Preparing aqueous solution according to the molar ratio of 1:2, mixing, and adding a small amount of nitric acid to prevent ion hydrolysis;
(2) under the condition of rapid stirring, adding ammonia water, and keeping the pH value of the solution at 8-9;
(3) filtering the generated precipitate, washing, and drying at 90 ℃ overnight;
(4) calcining the dried product in a muffle furnace at 900 ℃ for 5 hours to obtain FeAl2O4Spinel.
The prepared FeAl is filled in a quartz reaction tube2O4Spinel is used as a catalyst to form a catalyst bed layer, and then mixed gas containing hydrogen sulfide is introduced into the catalyst bed layer to carry out gas-solid phase catalytic reaction, so that the decomposition of the hydrogen sulfide is realized. And a temperature thermocouple is inserted into the center of the catalyst bed layer, and quartz wool is filled at the two ends of the catalyst bed layer for fixing.
FeAl2O4The mass of the spinel catalyst is 0.5g, and the particle size is 20-40 meshes; the temperature of the catalyst bed layer is 500-800 ℃; controlling the flow of the reactant gas using a mass flow meter, wherein H2The concentration of S is 1000ppm, and the reaction space velocity is 24000h-1The reaction pressure is normal pressure.
And (3) observing the influence of the synthesized hercynite on the reaction of preparing hydrogen and sulfur by decomposing hydrogen sulfide. Gas used for gas component and concentration after reactionAnd detecting by using a phase chromatograph. In this reaction the catalyst activity is determined by H2Conversion of S (in H)2Meter) to represent:
H2conversion of S (H)2Yield) H in off-gas2Concentration of gas/H in gas inlet2Concentration of S gas × 100%.
As shown in FIG. 2, it can be seen from FIG. 2 that the yield of hydrogen produced by decomposing hydrogen sulfide with hercynite according to the present invention is H with increasing temperature2The conversion rate of S is increased and can reach 50% at 800 ℃.
Examples 2,
MgAl2O4The spinel synthesis method comprises the following steps:
(1) mixing Mg (NO)3)2，Al(NO3)3Preparing aqueous solution according to the molar ratio of 1:2, mixing, and adding a small amount of nitric acid to prevent ion hydrolysis;
(2) under the condition of rapid stirring, adding ammonia water, and keeping the pH value of the solution at 8-9;
(3) filtering the generated precipitate, washing, and drying at 90 ℃ overnight;
(4) calcining the dried product in a muffle furnace at 900 ℃ for 5 hours to obtain MgAl2O4Spinel.
The prepared MgAl is filled in a quartz reaction tube2O4Spinel is used as a catalyst to form a catalyst bed layer, and then mixed gas containing hydrogen sulfide is introduced into the catalyst bed layer to carry out gas-solid phase catalytic reaction, so that the decomposition of the hydrogen sulfide is realized. And a temperature thermocouple is inserted into the center of the catalyst bed layer, and quartz wool is filled at the two ends of the catalyst bed layer for fixing.
MgAl2O4The mass of the spinel catalyst is 0.5g, and the particle size is 20-40 meshes; the temperature of the catalyst bed layer is 500-800 ℃; controlling the flow of the reactant gas using a mass flow meter, wherein H2The concentration of S is 1000ppm, and the reaction space velocity is 24000h-1The reaction pressure is normal pressure.
And (3) observing the influence of the synthesized hercynite on the reaction of preparing hydrogen and sulfur by decomposing hydrogen sulfide. Gas used for gas component and concentration after reactionAnd detecting by using a phase chromatograph. In this reaction the catalyst activity is determined by H2Conversion of S (in H)2Meter) to represent:
H2conversion of S (H)2Yield) H in off-gas2Concentration of gas/H in gas inlet2Concentration of S gas × 100%.
As shown in FIG. 3, it can be seen from FIG. 3 that the yield of hydrogen produced by the decomposition of hydrogen sulfide by the magnesium aluminate spinel according to the present invention is H with an increase in temperature2The conversion rate of S is increased and can reach 40% at 800 ℃.
Comparative example (c),
The catalyst was prepared according to the following literature: tz.kraia, n.kaklidis, m.konsolakis, g.e.marnellos, Hydrogen production by H2S decomposition over ceria supported transition metal(Co,Ni,Feand Cu)catalysts.International Journal of Hydrogen Energy,44(2019)9753-9762。
A series of CeO was prepared by tz2The catalyst loaded with Co, Ni, Cu and Fe is evaluated for the activity in the range of 550-850 ℃, and the evaluation conditions are as follows: h2The S concentration is 10000ppm, and the space velocity (Conversion) is 13500h-1As can be seen from FIG. 4, it has H temperatures of 700 ℃ and 850 DEG C2S conversion was 15% and 30% (H), respectively2The yield is less than or equal to 15% and less than or equal to 30% definitely).
Catalyst pair H of the present invention and comparative example2Compared with S conversion experiments, the yield of the invention is obviously improved.

Claims (4)

1. The spinel catalytic material is applied to preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide;
the general formula of the spinel catalytic material is AB2O4Wherein A is at least one of Li, Ba, Ca, Mn, Mg, Fe, Cu, Zn, Ni and Co, B is at least one of Cr, Ni, Fe, Co, Al and Mn, and AB2O4Not being ZnFe2O4；
The reaction conditions of the spinel catalytic material in the thermal catalytic decomposition of hydrogen sulfide are as follows:
the temperature is 500-1100 ℃, and the reaction pressure is normal pressure.
2. The spinel catalytic material is applied to preparing hydrogen and elemental sulfur by the thermal catalytic decomposition of hydrogen sulfide in acid gas;
hydrogen sulfide in the acid gas is derived from the acid gas generated in at least one field of petrochemical industry, coal chemical industry and natural gas chemical industry;
the general formula of the spinel catalytic material is AB2O4Wherein A is at least one of Li, Ba, Ca, Mn, Mg, Fe, Cu, Zn, Ni and Co, B is at least one of Cr, Ni, Fe, Co, Al and Mn, and AB2O4Not being ZnFe2O4；
The reaction conditions of the spinel catalytic material in the thermal catalytic decomposition of hydrogen sulfide in acid gas are as follows:
the temperature is 500-1100 ℃, and the reaction pressure is normal pressure.
3. A method for preparing hydrogen and elemental sulfur by thermally catalyzing and decomposing hydrogen sulfide is characterized by comprising the following steps: catalyzing hydrogen sulfide or hydrogen sulfide in acid gas by using a spinel catalytic material to perform decomposition reaction to obtain hydrogen and elemental sulfur;
the general formula of the spinel catalytic material is AB2O4Wherein A is at least one of Li, Ba, Ca, Mn, Mg, Fe, Cu, Zn, Ni and Co, B is at least one of Cr, Ni, Fe, Co, Al and Mn, and AB2O4Not being ZnFe2O4；
The conditions of the decomposition reaction were as follows:
the temperature is 500-1100 ℃, and the reaction pressure is normal pressure.
4. The method of claim 3, wherein: when the spinel catalytic material catalyzes the hydrogen sulfide in the acid gas to be carried out on the catalytic reaction bed, the space velocity of the acid gas is 1000h-1~50000 h-1。
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