CN116216742A - Improved method for preparing synthetic ammonia from coke oven gas - Google Patents

Improved method for preparing synthetic ammonia from coke oven gas Download PDF

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Publication number
CN116216742A
CN116216742A CN202310057218.XA CN202310057218A CN116216742A CN 116216742 A CN116216742 A CN 116216742A CN 202310057218 A CN202310057218 A CN 202310057218A CN 116216742 A CN116216742 A CN 116216742A
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gas
raw material
adsorption
stage
methane
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宋尉源
杨皓
杨鹏
秦小燕
陈程
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Sichuan Tianren Energy Technology Co ltd
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Sichuan Tianren Energy Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/04—Preparation of ammonia by synthesis in the gas phase
    • 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
    • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
    • C01B2203/0211—Processes for making hydrogen or synthesis gas containing a reforming step containing a non-catalytic reforming step
    • C01B2203/0216—Processes for making hydrogen or synthesis gas containing a reforming step containing a non-catalytic reforming step containing a non-catalytic steam reforming step

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

The invention discloses an improved method for preparing synthetic ammonia from coke oven gas, which is characterized in that compressed coke oven gas is sent to first-stage adsorption, methane-rich gas is obtained from the first-stage adsorption phase, part of methane-rich gas is sent out to be used as fuel gas to be called as a product 1, and the rest of methane-rich gas is sent to a non-catalytic reforming reformer to be called as a reforming raw material 1; the first-stage non-adsorption phase deoxidizes and then is sent to a second-stage adsorption separation, and the non-adsorption phase obtains an ammonia synthesis raw material 1; the adsorption phase obtains reforming raw material 2; mixing and compressing a reforming raw material 1, a reforming raw material 2 and a reforming raw material 3 obtained by the subsequent third-stage adsorption, sending the mixture and compressed air into a non-catalytic reforming reformer to prepare nitrogen-rich raw material gas, carrying out combined conversion with steam to obtain nitrogen-rich conversion gas, carrying out deoxidation and third-stage adsorption separation, obtaining an ammonia synthesis raw material 2 by a non-adsorption phase, and compressing the ammonia synthesis raw materials 1 and 2 into an ammonia synthesis system to obtain a product 2; the partial desorption of the adsorption phase to obtain a carbon dioxide-lean gas is called reforming raw material 3; the adsorption phase continues to deeply desorb to obtain a product 3, thereby realizing the recycling of the whole components of the coke oven gas.

Description

Improved method for preparing synthetic ammonia from coke oven gas
Technical Field
The invention relates to the field of chemical industry and energy conservation, in particular to an improved method for preparing synthetic ammonia from coke oven gas.
Background
H in coke oven gas 2 ~58%、CH 4 ~25%、CO~5%、N 2 ~5%、C 2 ~3%、CO 2 ~1.5%、O 2 0.5% to 2% of impurities, which contain a large amount of high-value H 2 、CO、CH 4 The components can be used for raw foodThe methane production product and the synthetic ammonia product realize high-value recycling.
CN202111272968 discloses a process for preparing liquefied natural gas and co-producing liquid ammonia or hydrogen from coke oven gas with transformation decarburization, which comprises the following steps: the coke oven gas is subjected to compression purification, hydrodesulfurization, transformation, decarburization, methanation, cryogenic separation and other process units, the liquid after cryogenic separation is an LNG product, and the gas after reheating can be used as a hydrogen-nitrogen raw material of a downstream ammonia synthesis device to produce a liquid ammonia product or used as a raw material of a PSA hydrogen extraction device to produce pure hydrogen. The method comprises the steps of using most of CO and H in coke oven gas 2 Methane production by methanation with only a small residual part of unreacted H 2 The purified LNG is sent to ammonia synthesis, and the cryogenic separation device for producing LNG has large equipment investment and high operation cost.
CN202010600507.6 discloses an improved process for preparing ammonia and CNG from coke oven gas, wherein the coke oven gas is compressed to 0.4-1.8 MPa, carbon monoxide is converted into hydrogen and carbon dioxide through conversion to be called as conversion gas, the carbon monoxide concentration of the conversion gas is less than or equal to 0.5%, and hydrogen sulfide, organic sulfur, carbon dioxide and C are removed through pressure swing adsorption n H m Part of methane is called decarbonizing gas, the sum of carbon monoxide and carbon dioxide in the decarbonizing gas is less than or equal to 1.0 percent, and the decarbonizing gas is sent to fine desulfurization and purification to reach that the total sulfur is less than or equal to 0.1ppm and is called fine degassing; meanwhile, the regenerated gas with the calorific value within +/-5% of that of the coke oven gas is obtained, and the regenerated gas flows back into the fuel gas of the coke oven; the refined degassing is sent to a methanation purification device to remove carbon monoxide and carbon dioxide until the total sum of the carbon monoxide and the carbon dioxide is less than or equal to 10ppm, and the refined degassing is called methanation gas; delivering the methanated gas to a pressure swing adsorption purification device to prepare CNG with the methane concentration of more than 95%, wherein the concentration and the calorific value of the toxic gas of the CNG accord with the standard of fuel gas, and meanwhile, obtaining coarse degassing with the methane concentration of less than or equal to 8%; the crude degassing enters a pressure swing adsorption fine-removing device to separate methane until the concentration is less than or equal to 0.5 percent, which is called a fine degassing ammonia-sending synthesis system, and the desorption gas is compressed and sent into the crude-removing device to be circularly separated. The method is characterized in that most CO in the coke oven gas is converted to produce hydrogen, raw material gas is purified in a methanation mode, methane and hydrogen and nitrogen are further separated and are respectively used for preparing CNG and synthesizing ammonia, and the greatest problem of the method is that N in the coke oven gas 2 The content is usually only 5%, and the coke oven is transformedH in the air 2 The content is up to more than 60%, the hydrogen-nitrogen ratio of the raw material gas in the ammonia synthesis section after methane separation does not meet the process requirement of 3:1, but nitrogen is required to be prepared by additionally adding devices such as air separation and the like, so that the ammonia production cost of the process is increased.
CN201811324441 discloses a process for preparing ammonia synthesis gas by combining blast furnace gas and coke oven gas, wherein the blast furnace gas is sent to a first pressure swing adsorption process for removing CO 2 The second pressure swing adsorption process further removes CO 2 Purifying CO by a copper molecular sieve, wherein the purified gas is used as a first synthesis ammonia feed gas; after desulfurization, compression, transformation and variable-removal, the concentrated CO gas separated from the coke oven gas mixed blast furnace gas is sent to a third pressure swing adsorption process to remove CO therein 2 Then sending the mixture to a fourth pressure swing adsorption process for separating CH 4 Obtaining CH 4 Rich CH with a mixed concentration of CnHm higher than 75% 4 Gas is used as chemical raw material, and lean CH is obtained at the same time 4 The gas is continuously sent to the fifth pressure swing adsorption purification CH 4 Purifying CO by 5A molecular sieve to obtain CO-removed gas, and removing CO in the CO-removed gas 2 The concentration is less than or equal to 10ppm, the concentration of CO is less than or equal to 10ppm, and the concentration of CH4 is necessarily lower than 0.1 percent, so that the ammonia is used as ammonia synthesis gas II; mixing two ammonia synthesis gases to form total raw material gas for ammonia synthesis, and regulating the gas quantity of the first pressure swing adsorption blast furnace to enable the molar ratio of synthesis hydrogen to nitrogen to reach 3:1. the method comprises the steps of converting blast furnace gas into hydrogen and nitrogen with high nitrogen concentration, proportioning the hydrogen and nitrogen with high hydrogen concentration after methane removal and the like of coke oven gas, and then achieving the requirement that the hydrogen-nitrogen ratio of ammonia synthesis gas is 3:1, and simultaneously producing methane-rich gas as a byproduct. The process requires the addition of a blast furnace gas as a nitrogen source to supplement, and cannot meet the conditions of the synthesis ammonia production in the case of only a coke oven gas source.
Therefore, the existing ammonia production process using coke oven gas has the main problem of needing an additional Gao Danqi source (such as blast furnace gas) for proportioning; however, if coke oven gas is used alone, expensive air separation nitrogen production equipment and high compression energy consumption are required, or methane is produced by sacrificing the yield of synthesis ammonia produced from the coke oven gas.
Disclosure of Invention
Improved method for preparing synthetic ammonia from coke oven gasThe method is characterized in that coke oven gas is compressed to 0.1-2.5MPa and sent to a first stage of adsorption, and the adsorption phase of the first stage of adsorption obtains carbon dioxide and C n H m Methane is used as methane-rich gas, 60-90% of the methane-rich gas is externally sent to be used as fuel gas to be called as a product 1, 10-40% of the methane-rich gas is sent to a non-catalytic reforming converter to be called as a reforming raw material 1, and the non-adsorption phase gas of the first-stage adsorption takes methane as a control index, and the volume concentration of the methane is less than 1%; deoxidizing the first-stage non-adsorption phase gas, then delivering the deoxidized gas to a second-stage adsorption separation, and obtaining the CO+CO-containing gas from the second-stage non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with O < 10ppm is referred to as ammonia synthesis feedstock 1; the mixed gas containing carbon monoxide, methane, a small amount of carbon dioxide and a small amount of hydrogen obtained by the second-stage adsorption phase is called a reforming raw material 2; mixing and compressing the reforming raw material 1, the reforming raw material 2 and the reforming raw material 3 obtained by the subsequent third-stage adsorption, sending the mixture and compressed air which is 1-10 times of the compressed air to a non-catalytic reforming reformer to prepare nitrogen-rich raw material gas, carrying out combined conversion on the nitrogen-rich raw material gas and by-product steam of the non-catalytic reforming reformer to obtain nitrogen-rich conversion gas, carrying out deoxidation and third-stage adsorption separation on the nitrogen-rich conversion gas, and obtaining the CO+CO-containing product from a non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with the concentration of O less than 10ppm are taken as an ammonia synthesis raw material 2, and the ammonia synthesis raw materials 1 and 2 are compressed and sent to an ammonia synthesis system to obtain synthetic ammonia, namely a product 2; the third stage adsorption phase is partially desorbed to obtain lean carbon dioxide gas which is called reforming raw material 3 and sent to the non-catalytic reforming reformer; the third stage of adsorption is used for continuous deep desorption to obtain concentrated carbon dioxide, and can be used for liquefying or sending out as carbonized raw material called product 3, thereby realizing the full-component recycling application of coke oven gas.
The invention has the advantages that:
1. compared with the existing process for preparing synthetic ammonia from coke oven gas, the non-catalytic reforming conversion process is used for replacing the traditional air separation nitrogen preparation process, is used for supplementing nitrogen required by synthetic ammonia, and solves the problems of huge construction investment and high energy consumption cost of air separation equipment;
2. the non-catalytic reforming conversion process can produce steam as a byproduct, and the steam can be just used as the raw material gas of the subsequent CO conversion process, so that the heat waste of the single non-catalytic reforming conversion is avoided, the problem of raw material steam source of the subsequent CO conversion process is solved, and the energy utilization efficiency is effectively improved by combining the steam and the raw material gas;
3. the reforming conversion process simultaneously converts partial cheaper methane-rich gas separated from the coke oven gas into high-value H 2 CO and further converts CO into H through a conversion process 2 The high-value recycling of raw materials is realized, and the yield of synthetic ammonia is improved;
4. lean CO effluent in third stage adsorption for the present application 2 Partial decomposition of the inspiration gas, by means of feeding into a non-catalytic reforming reformer, achieves a CO-lean state 2 Recycling of the gas, avoiding high value H therein 2 Waste of components such as CO and the like, thereby realizing the full component utilization of the coke oven gas;
5. the byproduct methane-rich gas product and the high-concentration CO2 product gas further improve the recycling efficiency of the coke oven gas, increase the additional production value of the whole process and realize the high-value utilization of resources.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict.
Example 1: compressing coke oven gas to 0.8MPa, delivering to first stage adsorption, and obtaining carbon dioxide and C from the adsorption phase of the first stage adsorption n H m Methane is used as methane-rich gas, 66% of the methane-rich gas is externally sent to be used as fuel gas to be called as a product 1, 34% of the methane-rich gas is sent to a non-catalytic reforming reformer to be called as a reforming raw material 1, and the non-adsorption phase gas of the first-stage adsorption takes methane as a control index, and the volume concentration of methane is less than 1%; deoxidizing the first-stage non-adsorption phase gas, then delivering the deoxidized gas to a second-stage adsorption separation, and obtaining the CO+CO-containing gas from the non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with O < 10ppm is referred to as ammonia synthesis feedstock 1; second oneThe mixed gas obtained by the stage adsorption phase and containing carbon monoxide, methane, a small amount of carbon dioxide and a small amount of hydrogen is called as reforming raw material 2; mixing and compressing reforming raw material 1, reforming raw material 2 and reforming raw material 3 obtained by the subsequent third-stage adsorption, sending the mixture and compressed air which is 2.6 times of the compressed air to a non-catalytic reforming reformer to prepare nitrogen-rich raw material gas, carrying out combined conversion on the nitrogen-rich raw material gas and by-product steam of the non-catalytic reforming reformer to obtain nitrogen-rich conversion gas, carrying out deoxidation and third-stage adsorption separation on the nitrogen-rich conversion gas, and obtaining CO+CO-containing gas from a non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with the concentration of O less than 10ppm are taken as an ammonia synthesis raw material 2, and the ammonia synthesis raw materials 1 and 2 are compressed and sent to an ammonia synthesis system to obtain synthetic ammonia, namely a product 2; the third stage adsorption phase is partially desorbed to obtain lean carbon dioxide gas which is called reforming raw material 3 and sent to the non-catalytic reforming reformer; the third stage of adsorption is used for continuous deep desorption to obtain concentrated carbon dioxide, and can be used for liquefying or sending out as carbonized raw material called product 3, thereby realizing the full-component recycling application of coke oven gas.
Example 2: compressing coke oven gas to 1.2MPa, delivering to first stage adsorption, and obtaining carbon dioxide and C from the adsorption phase of the first stage adsorption n H m Methane is used as methane-rich gas, 74% of the methane-rich gas is externally sent to be used as fuel gas to be called as a product 1, 26% of the methane-rich gas is sent to a non-catalytic reforming reformer to be called as a reforming raw material 1, and the non-adsorption phase gas of the first-stage adsorption takes methane as a control index, and the volume concentration of methane is less than 1%; deoxidizing the first-stage non-adsorption phase gas, then delivering the deoxidized gas to a second-stage adsorption separation, and obtaining the CO+CO-containing gas from the non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with O < 10ppm is referred to as ammonia synthesis feedstock 1; the mixed gas containing carbon monoxide, methane, a small amount of carbon dioxide and a small amount of hydrogen obtained by the second-stage adsorption phase is called a reforming raw material 2; mixing and compressing reforming raw material 1, reforming raw material 2 and reforming raw material 3 obtained by the subsequent third-stage adsorption, sending the mixture and 3.3 times of compressed air to a non-catalytic reforming reformer to prepare nitrogen-rich raw material gas, carrying out combined conversion on the nitrogen-rich raw material gas and by-product steam of the non-catalytic reforming reformer to obtain nitrogen-rich conversion gas, carrying out deoxidation and third-stage adsorption separation on the nitrogen-rich conversion gas, and obtaining CO+CO-containing gas from a non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with O less than 10ppm are taken as ammonia synthesis raw material 2, and ammonia synthesis raw materials 1 and 2 are compressed to form ammonia synthesis systemObtaining synthetic ammonia referred to as product 2; the third stage adsorption phase is partially desorbed to obtain lean carbon dioxide gas which is called reforming raw material 3 and sent to the non-catalytic reforming reformer; the third stage of adsorption is used for continuous deep desorption to obtain concentrated carbon dioxide, and can be used for liquefying or sending out as carbonized raw material called product 3, thereby realizing the full-component recycling application of coke oven gas.
Example 3: compressing coke oven gas to 1.8MPa, delivering to first stage adsorption, and obtaining carbon dioxide and C from the adsorption phase of the first stage adsorption n H m The methane is used as methane-rich gas, 83% of the methane-rich gas is externally sent to be used as fuel gas to be called as a product 1, 27% of the methane-rich gas is sent to a non-catalytic reforming reformer to be called as a reforming raw material 1, and the non-adsorption phase gas of the first-stage adsorption takes the methane as a control index, and the volume concentration of the methane is less than 1%; deoxidizing the first-stage non-adsorption phase gas, then delivering the deoxidized gas to a second-stage adsorption separation, and obtaining the CO+CO-containing gas from the non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with O < 10ppm is referred to as ammonia synthesis feedstock 1; the mixed gas containing carbon monoxide, methane, a small amount of carbon dioxide and a small amount of hydrogen obtained by the second-stage adsorption phase is called a reforming raw material 2; mixing and compressing reforming raw material 1, reforming raw material 2 and reforming raw material 3 obtained by the subsequent third-stage adsorption, sending the mixture and compressed air which is 5.1 times of the compressed air to a non-catalytic reforming reformer to prepare nitrogen-rich raw material gas, carrying out combined conversion on the nitrogen-rich raw material gas and by-product steam of the non-catalytic reforming reformer to obtain nitrogen-rich conversion gas, carrying out deoxidation and third-stage adsorption separation on the nitrogen-rich conversion gas, and obtaining CO+CO-containing gas from a non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with the concentration of O less than 10ppm are taken as an ammonia synthesis raw material 2, and the ammonia synthesis raw materials 1 and 2 are compressed and sent to an ammonia synthesis system to obtain synthetic ammonia, namely a product 2; the third stage adsorption phase is partially desorbed to obtain lean carbon dioxide gas which is called reforming raw material 3 and sent to the non-catalytic reforming reformer; the third stage of adsorption is used for continuous deep desorption to obtain concentrated carbon dioxide, and can be used for liquefying or sending out as carbonized raw material called product 3, thereby realizing the full-component recycling application of coke oven gas.

Claims (1)

1. An improved method for preparing synthetic ammonia from coke-oven gas is characterized in that the coke-oven gas is compressed to 0.1-2.5MPa and sent to first-stage adsorption, and the adsorption phase of the first-stage adsorption obtains carbon dioxide and C n H m Methane is used as methane-rich gas, 60-90% of the methane-rich gas is externally sent to be used as fuel gas to be called as a product 1, 10-40% of the methane-rich gas is sent to a non-catalytic reforming converter to be called as a reforming raw material 1, and the non-adsorption phase gas of the first-stage adsorption takes methane as a control index, and the volume concentration of the methane is less than 1%; deoxidizing the first-stage non-adsorption phase gas, then delivering the deoxidized gas to a second-stage adsorption separation, and obtaining the CO+CO-containing gas from the second-stage non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with O < 10ppm is referred to as ammonia synthesis feedstock 1; the mixed gas containing carbon monoxide, methane, a small amount of carbon dioxide and a small amount of hydrogen obtained by the second-stage adsorption phase is called a reforming raw material 2; mixing and compressing the reforming raw material 1, the reforming raw material 2 and the reforming raw material 3 obtained by the subsequent third-stage adsorption, sending the mixture and compressed air which is 1-10 times of the compressed air to a non-catalytic reforming reformer to prepare nitrogen-rich raw material gas, carrying out combined conversion on the nitrogen-rich raw material gas and by-product steam of the non-catalytic reforming reformer to obtain nitrogen-rich conversion gas, carrying out deoxidation and third-stage adsorption separation on the nitrogen-rich conversion gas, and obtaining the CO+CO-containing product from a non-adsorption phase 2 +O 2 +H 2 Hydrogen and nitrogen with the concentration of O less than 10ppm are taken as an ammonia synthesis raw material 2, and the ammonia synthesis raw materials 1 and 2 are compressed and sent to an ammonia synthesis system to obtain synthetic ammonia, namely a product 2; the third stage adsorption phase is partially desorbed to obtain lean carbon dioxide gas which is called reforming raw material 3 and sent to the non-catalytic reforming reformer; the third stage of adsorption is used for continuous deep desorption to obtain concentrated carbon dioxide, and can be used for liquefying or sending out as carbonized raw material called product 3, thereby realizing the full-component recycling application of coke oven gas.
CN202310057218.XA 2023-01-17 2023-01-17 Improved method for preparing synthetic ammonia from coke oven gas Pending CN116216742A (en)

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