CN114751386A - General nitrogen deoxidization purification method and device based on methanol cracking reaction - Google Patents

General nitrogen deoxidization purification method and device based on methanol cracking reaction Download PDF

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CN114751386A
CN114751386A CN202210579890.0A CN202210579890A CN114751386A CN 114751386 A CN114751386 A CN 114751386A CN 202210579890 A CN202210579890 A CN 202210579890A CN 114751386 A CN114751386 A CN 114751386A
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methanol
mixed gas
nitrogen
gas
cracking reaction
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李晓刚
李玉柱
马力
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Jiangsu Zhongke Juyuan Hydrogen Energy Technology Co ltd
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/04Purification or separation of nitrogen
    • C01B21/0405Purification or separation processes
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    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/22Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
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    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
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Abstract

The invention provides a general nitrogen deoxidization purification method based on a methanol cracking reaction, which comprises the following steps: s1, heating and pressurizing the methanol to obtain methanol gas with the temperature of 220-270 ℃ and the pressure of 0.6-2.0 Mpa; s2, introducing the heated and pressurized methanol gas into a cracker containing a solid catalyst, and carrying out cracking reaction of methanol under the action of the solid catalyst to obtain CO2CO and H2The first mixed gas of (1); s3, introducing the first mixed gas and the common nitrogen into a deaerator, and removing oxygen in the common nitrogen to obtain a second mixed gas, wherein the temperature in the deaerator is 650-700 ℃; and S4, carrying out gas separation on the second mixed gas to obtain nitrogen with the oxygen content of less than or equal to 0.0005%. Compared with the method for purifying common nitrogen by deoxidizing based on the methanol cracking reaction, the method for purifying common nitrogen by deoxidizing based on the methanol cracking reaction provided by the invention independently adopts H2With respect to reaction with oxygen in the general nitrogen, supply of hydrogen can be avoidedInconvenience and greatly improved safety of production.

Description

General nitrogen deoxidization purification method and device based on methanol cracking reaction
Technical Field
The application belongs to the technical field of nitrogen production, and particularly relates to a common nitrogen deoxidization purification method and device based on a methanol cracking reaction.
Background
The nitrogen gas produced by the conventional nitrogen producing system has a purity of about 99.5%, which is called "common nitrogen", and contains about 0.5% of oxygen, but in the electronic industry sector, especially in the manufacturing process of semiconductor devices and integrated circuits, a large amount of high-purity nitrogen gas (having a purity of about 99.999%) is required as a shielding gas, a diluent gas, a carrier gas, etc., and the nitrogen gas is used as a base material for manufacturing large-scale integrated circuits, and the purity thereof directly affects the yield and reliability of electronic products, so that the common nitrogen needs to be purified to high-purity nitrogen.
The existing general nitrogen purification methods generally include two methods, the first method is a hydrogen preparation method, such as hydrogen production by water electrolysis, hydrogen production by natural gas and the like, hydrogen is used as a deoxidizer to remove impurity oxygen in nitrogen, and the second method is a catalyst method, namely, under the action of a carbon-supported catalyst, the impurity oxygen in nitrogen reacts with carbon provided by the catalyst, so that the impurity oxygen contained in nitrogen is removed. However, although these two methods can remove oxygen in nitrogen, the first hydrogen preparation method requires a hydrogen source and has a certain safety problem, and the second catalyst method requires consumption of the carbon-supported catalyst itself, and therefore, the catalyst must be replaced periodically, which is inconvenient to use.
Disclosure of Invention
The present invention is directed to solving or improving at least one of the above technical problems.
The technical scheme of the first aspect of the invention provides a method for purifying common nitrogen by removing oxygen based on a methanol cracking reaction.
The technical scheme of the second aspect of the invention provides a common nitrogen oxygen removal purification device based on a methanol cracking reaction.
The technical scheme of the first aspect of the invention provides a methanol cracking reaction-based method for purifying common nitrogen by removing oxygen, which comprises the following steps:
step S1, heating and pressurizing the methanol to obtain methanol gas with the temperature of 220-270 ℃ and the pressure of 0.6-2.0 MPa;
step S2, the heated and pressurized methanol gas is introduced into a cracker containing solid catalyst to be cracked in the solidCracking reaction of methanol under the action of catalyst to obtain CO2CO and H2The first mixed gas of (1);
step S3, introducing the first mixed gas and common nitrogen into a deaerator, and removing oxygen in the common nitrogen to obtain a second mixed gas, wherein the temperature in the deaerator is 650-700 ℃;
and step S4, performing gas separation on the second mixed gas to obtain nitrogen with the oxygen content less than or equal to 0.0005%.
The invention provides a method for preparing methanol by using a solid catalyst, which comprises the steps of heating and pressurizing methanol to obtain heated and pressurized methanol gas, and then introducing the heated and pressurized methanol gas into a cracker containing the solid catalyst, so that the methanol can be subjected to cracking reaction under the action of the solid catalyst to obtain CO 2CO and H2The first mixed gas of (1); introducing the first mixed gas and the common nitrogen into a deaerator together, so that CO and H in the first mixed gas2Can react with O2Reacting to remove oxygen in the common nitrogen to obtain a second mixed gas, wherein the second mixed gas comprises CO generated by the reaction2、H2O and nitrogen, and unreacted CO and H2. Of course, a nickel-based or noble metal catalyst can be arranged in the deaerator, so that the oxygen in the common nitrogen can be removed quickly under the action of the catalyst, wherein the common nitrogen refers to nitrogen with the purity of below 99.5%. It is worth noting that CO is present in the process2The second mixture, CO and H, is output from the deaerator without participating in the reaction2Capable of reacting with oxygen to form CO2And H2And O. Further, the second mixed gas is subjected to gas separation, and nitrogen with the oxygen content of less than or equal to 0.0005% can be obtained. The invention provides a methanol cracking reaction-based common nitrogen oxygen removal purification method, which takes methanol as a raw material and generates CO and H through the cracking reaction of the methanol2To remove oxygen from the primary nitrogen, thus ensuring the removal rate of oxygen, i.e. by CO and H2The oxygen in the common nitrogen is removed together, and compared with the prior art, H is singly adopted 2Or the carbon-supported catalyst is used for removing the oxygen in the common nitrogen, the production flow is simple and convenient, and the safety is high.Further, because the methanol cracking mode is adopted for hydrogen production, compared with the prior art that the oxygen in the common nitrogen is absorbed by adopting the water electrolysis hydrogen production, the methanol saves the cost, and compared with the natural gas hydrogen production, the methanol hydrogen production is not limited by the supply of the natural gas, and the deoxidation efficiency is improved.
In the technical scheme, before the heated and pressurized methanol gas is introduced into a cracker containing a solid catalyst, protective gas is introduced into the cracker for 3-10 min to discharge the air in the cracker.
In the technical scheme, before the heated and pressurized methanol gas is introduced into a cracker containing a solid catalyst, protective gas is introduced into the cracker for 3-10 min to exhaust air in the cracker, so that oxygen in the cracker can be exhausted, the oxygen content in the cracker is low, a large amount of CO can be generated in the cracking reaction of the methanol, and the later-stage deoxygenation efficiency is improved. In the method, after the cracking reaction, the content of CO in the obtained first mixed gas is 28-32 percent2Is 1% -2%, H 2The content of (A) is 65% -75%; further, the protective gas is high-purity nitrogen, which ensures that the oxygen in the cracker is completely discharged.
In the above technical solution, the solid catalyst comprises: copper oxide, zinc oxide, chromium oxide.
In this embodiment, the solid catalyst comprises: copper oxide, zinc oxide, chromium oxide; wherein, the copper oxide is a main catalyst component, can accelerate the reaction speed of methanol cracking, and can generate dehydrogenation reaction under the action of the catalyst to generate CO and H2The zinc oxide exists as a cocatalyst, so that the catalytic action can be further promoted, and the chromium oxide has better heat resistance and can maintain the stability of the catalytic action.
In the above technical solution, the step of performing gas separation on the second mixed gas to obtain nitrogen gas with an oxygen content of 0.0005% or less specifically includes: introducing the second mixed gas into a reactor containing copper oxide to remove CO and H in the second mixed gas2Obtaining a third mixed gas; to the third mixed gas in sequenceAnd (3) carrying out alkali washing and drying on the body to obtain nitrogen with the oxygen content of less than or equal to 0.0005%.
In the technical scheme, the second mixed gas is firstly introduced into a reactor containing copper oxide, and the reactor is heated, so that CO and H in the second mixed gas can be removed 2Obtaining a third mixed gas, wherein the third mixed gas comprises CO generated by the reaction2And H2O and nitrogen, then introducing the third mixed gas into an alkali tube to remove CO2Finally, the third mixed gas is dried by a drier to remove H2O; according to the scheme, the second mixed gas is introduced into the reactor containing the copper oxide, the alkali tube and the dryer in sequence, so that CO and H mixed with the nitrogen can be completely absorbed after the step of removing oxygen2、H2O and CO2To ensure the output of pure high-purity nitrogen.
The invention provides a general nitrogen deoxidization purification device based on methanol cracking reaction, which comprises: the heating pressurizer is used for heating and pressurizing the methanol to obtain methanol gas with the temperature of 220-270 ℃ and the pressure of 0.6-2.0 Mpa; the cracker is connected with the heating pressurizer, and after the heated and pressurized methanol gas is introduced into the cracker, the cracker is used for carrying out cracking reaction of methanol under the action of a solid catalyst to obtain the product containing CO2CO and H2The first mixed gas of (1); the deaerator is connected with the cracker, the first mixed gas and the common nitrogen can be deaerated after being introduced into the deaerator, so that a second mixed gas can be obtained, and the temperature in the deaerator is 650-700 ℃; and the gas separator is connected with the deaerator and is used for carrying out gas separation on the second mixed gas to obtain nitrogen with the oxygen content of less than or equal to 0.0005%.
The invention provides a general nitrogen deoxidization purification device based on a methanol cracking reaction, which comprises: the device comprises a heating pressurizer, a cracker, a deaerator and a gas separator, wherein the heating pressurizer is used for heating and pressurizing the methanol; the cracker is connected with the heating pressurizer and used for cracking the heated and pressurized methanol gas to generate CO2CO and H2The first mixed gas of (1); a deaerator connected with the cracker, a first mixed gas andafter the common nitrogen is introduced into the deaerator, CO and H in the first mixed gas2Oxygen in the common nitrogen can be removed, and a second mixed gas is obtained in the deaerator; the gas separator is connected with the deaerator, and can perform gas separation on the second mixed gas to obtain nitrogen with the oxygen content less than or equal to 0.0005%. The invention provides a methanol cracking reaction-based general nitrogen deoxidization and purification device, which takes methanol as a raw material and generates CO and H through the cracking reaction of the methanol2To remove oxygen from the primary nitrogen, thus ensuring the removal rate of oxygen, i.e. by CO and H2Together to absorb oxygen from the common nitrogen, in contrast to CO or H taken alone2Or the carbon-supported catalyst is used for absorbing the oxygen in the common nitrogen, the production flow is simple and convenient, and the safety is high. Further, the device can produce hydrogen by adopting a methanol cracking mode, so that the methanol is more cost-saving compared with the prior art that hydrogen is produced by electrolyzing water to absorb oxygen in common nitrogen, and compared with the hydrogen production by natural gas, the device is not limited by the supply of natural gas, and the deoxidation efficiency is improved.
In the above technical solution, the gas separator includes: a reactor connected with the deaerator and including a heating device and copper oxide capable of removing CO and H in the second mixed gas in a heated state2To obtain a third mixed gas; an alkali tube connected with the reactor for removing CO in the third mixed gas2(ii) a A drier connected with the alkali tube for removing H in the third mixed gas2O, obtaining nitrogen with the oxygen content of less than or equal to 0.0005 percent.
In this solution, the gas separator comprises: the reactor is connected with the deaerator and comprises a heating device and copper oxide, and the copper oxide can remove CO and H in the second mixed gas in a heating state2Obtaining a third mixed gas, wherein the third mixed gas comprises CO2And H2O and nitrogen; the alkali tube is connected with the reactor and is used for removing CO in the third mixed gas2(ii) a The drier is connected with the alkali tube and used for removing H in the third mixed gas2O, obtaining nitrogen with the oxygen content of less than or equal to 0.0005 percent. The device sequentially leads the second mixed gas into a reactor containing copper oxide and alkaliA tube and a dryer, so that CO and CO can be completely absorbed after the step of removing oxygen 2、H2And H2O, ensuring that pure high-purity nitrogen is output.
Additional aspects and advantages in accordance with the present invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of embodiments according to the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows a schematic flow diagram of a method for purifying common nitrogen by oxygen removal based on a methanol cracking reaction according to an embodiment of the present invention;
fig. 2 shows a schematic block diagram of a purification device for removing oxygen from common nitrogen based on methanol cracking reaction provided by the embodiment of the invention.
The corresponding relationship between the part names and the reference numbers in fig. 2 is as follows:
the method comprises the following steps of 1 heating pressurizer, 2 cracker, 21 solid catalyst, 3 deaerator, 4 gas separator, 41 reactor, 411 copper oxide, 42 alkali tube, 43 drier and 5 common nitrogen storage tank.
Detailed Description
In order to make the above-mentioned aspects, features and advantages of the embodiments according to the present invention more clearly understandable, the embodiments according to the present invention are described in further detail below with reference to the accompanying drawings and detailed description, and it is to be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of embodiments according to the invention, however, embodiments according to the invention may be practiced in other ways than those described herein, and therefore the scope of protection of embodiments according to the invention is not limited by the specific embodiments disclosed below.
Example one
As shown in fig. 1, this embodiment provides a method for purifying common nitrogen by oxygen removal based on methanol cracking reaction, which includes the following steps:
s1: heating and pressurizing the methanol to obtain methanol gas with the temperature of 220-270 ℃ and the pressure of 0.6-2.0 MPa;
s2: introducing the heated and pressurized methanol gas into a cracker containing a solid catalyst, and performing cracking reaction of methanol under the action of the solid catalyst to obtain CO2CO and H2The first mixed gas of (1);
s3: introducing the first mixed gas and common nitrogen into a deaerator, and removing oxygen in the common nitrogen to obtain a second mixed gas, wherein the temperature in the deaerator is 650-700 ℃;
s4: and carrying out gas separation on the second mixed gas to obtain nitrogen with the oxygen content of less than or equal to 0.0005%.
The general nitrogen deoxygenation purification method based on methanol cracking reaction provided by this embodiment includes heating and pressurizing methanol to obtain heated and pressurized methanol gas, and then introducing the heated and pressurized methanol gas into a cracker containing a solid catalyst, so that methanol can undergo a cracking reaction under the action of the solid catalyst to obtain CO 2CO and H2The first mixed gas of (1); specifically, the cracking process of methanol includes the following chemical reaction equation:
main reaction: CH (CH)3OH→CO+2H2-90.7kJ/mol
Auxiliary reaction: CO + H2O→CO2+H2+41.2kJ/mol
Auxiliary reaction: 2CO + O2→2CO2-283kJ/mol
After the cracking reaction of the methanol, the first mixed gas and the common nitrogen are jointly introduced into a deaerator, so that CO and H in the first mixed gas2Oxygen in the common nitrogen can be removed to obtain a second mixed gas. In particular, CO and H2The chemical reaction equation with oxygen is as follows:
2CO+O2→2CO2
O2+2H2→2H2O;
and (3) total reaction: CO + H2+O2→CO2+H2O;
In the process CO2The second mixture, CO and H, is output from the deaerator without participating in the reaction2Can absorb oxygen in nitrogen to generate CO2And H2And O. Further, the second mixed gas is subjected to gas separation, and nitrogen with the oxygen content of less than or equal to 0.0005% can be obtained. The invention provides a methanol cracking reaction-based common nitrogen oxygen removal purification method, which takes methanol as a raw material and generates CO and H through the cracking reaction of the methanol2To remove oxygen from the primary nitrogen, thus ensuring the removal rate of oxygen, i.e. by CO and H2Together to absorb oxygen from the common nitrogen, in contrast to CO or H taken alone2The production process is simple and convenient for absorbing the oxygen in the general nitrogen, and the safety is high. Further, the methanol cracking mode is adopted for hydrogen production, compared with the prior art that hydrogen is produced by water electrolysis to absorb oxygen in common nitrogen, the methanol saves more cost, and compared with the natural gas hydrogen production, the method is not limited by the supply of natural gas, and improves the deoxidation efficiency.
In the embodiment, before the heated and pressurized methanol gas is introduced into the cracker containing the solid catalyst, the protective gas is introduced into the cracker for 3min to 10min to exhaust the air in the cracker, so that the oxygen in the cracker can be exhausted, the oxygen content in the cracker is low, and the oxidation of CO into CO can be inhibited2The method ensures that a large amount of CO is generated in the cracking reaction of the methanol, and improves the later-stage deoxygenation efficiency. In the method, after the cracking reaction, the content of CO in the obtained mixed gas is 26-30 percent2Is 1% -3%, H2The content of (A) is 66% -73%; further, the protective gas is high purity nitrogen, which ensures that the oxygen in the cracker is completely removed.
In the above embodiment, the solid catalyst includes: copper oxide, zinc oxide, chromium oxide; wherein, the copper oxide is a main catalyst component, can accelerate the reaction speed of methanol cracking, and can perform the following dehydrogenation reaction under the action of the catalystThe CO and H produced2The zinc oxide exists as a cocatalyst, so that the catalytic action can be further promoted, and the chromium oxide has better heat resistance and can maintain the stability of the catalytic action.
In the above embodiment, the step of separating the second mixed gas is specifically to introduce the second mixed gas into a reactor containing copper oxide, and heat the reactor, so as to remove CO and H in the second mixed gas2To obtain a third mixed gas, wherein the third mixed gas comprises CO2And H2O and nitrogen.
Introducing the third mixed gas into an alkali tube to remove CO2For example, the alkali tube is sodium hydroxide solution, and the chemical reaction equation is:
CO2+2NaOH→Na2CO3+H2O;
finally, the third mixed gas is dried by a drier to remove H2O; according to the scheme, the second mixed gas is introduced into the reactor containing the copper oxide, the alkali tube and the dryer in sequence, so that CO and H mixed with nitrogen can be absorbed after the step of removing oxygen2、H2O and CO2Etc. to ensure the output of pure high purity nitrogen.
As shown in fig. 2, an embodiment of the second aspect of the present invention provides a device for purifying nitrogen based on methanol cracking reaction, including: a heating pressurizer 1 for heating and pressurizing methanol; a cracker 2 connected with the heating pressurizer 1 and used for cracking the heated and pressurized methanol gas to generate CO2CO and H2The first mixed gas of (1); the deaerator 3 is connected with the cracker 2, and after the first mixed gas and the common nitrogen are introduced into the deaerator 3, CO and H in the first mixed gas 2Oxygen in the common nitrogen can be removed to obtain a second mixed gas; the gas separator 4 is connected with the deaerator 3, and can perform gas separation on the second mixed gas to obtain nitrogen with the oxygen content less than or equal to 0.0005%.
The invention provides a methanol cracking reaction-based general nitrogen deoxidization and purification device, which comprises: a heating pressurizer 1, a cracker 2, a deaerator 3 and a gas separator 4, heating and pressurizingThe device 1 is used for heating and pressurizing the methanol; the cracker 2 is connected with the heating pressurizer 1 and is used for cracking the heated and pressurized methanol gas to generate CO2CO and H2The first mixed gas of (1); specifically, a solid catalyst 21 is provided in the cracker 2, and the heated and pressurized methanol gas can undergo dehydrogenation reaction under the action of the solid catalyst 21 to generate CO and H2And a small amount of CO2(ii) a The solid catalyst 21 includes copper oxide, zinc oxide, chromium oxide, and the like; one end of a deaerator 3 is connected with the cracker 2, the other end is connected with a common nitrogen storage tank 5, and after the first mixed gas and the common nitrogen are introduced into the deaerator 3, CO and H in the first mixed gas2Oxygen in the common nitrogen can be removed to obtain a second mixed gas; the gas separator 4 is connected with the deaerator 3, and can perform gas separation on the second mixed gas to obtain nitrogen with the oxygen content less than or equal to 0.0005%. The invention provides a methanol cracking reaction-based general nitrogen deoxidization and purification device, which takes methanol as a raw material and generates CO and H through the cracking reaction of the methanol 2To remove oxygen from the primary nitrogen, thus ensuring the removal rate of oxygen, i.e. by CO and H2Together to absorb oxygen from the nitrogen as compared to CO or H alone2The production process is simple and convenient for absorbing the oxygen in the general nitrogen, and the safety is high. Further, the device can produce hydrogen by adopting a methanol cracking mode, so that the methanol is more cost-saving compared with the prior art that hydrogen is produced by electrolyzing water to absorb oxygen in common nitrogen, and compared with the hydrogen production by natural gas, the device is not limited by the supply of natural gas, and the deoxidation efficiency is improved.
As shown in fig. 2, in this embodiment, the gas separator 4 includes: a reactor 41, an alkali tube 42 and a dryer 43, wherein the reactor 41 is connected with the deaerator 3 for removing CO and H in the second mixed gas2Obtaining a third mixed gas, wherein the third mixed gas comprises CO2And H2O and nitrogen; an alkali tube 42 is connected to the reactor 41 for removing CO from the third mixed gas2(ii) a A drier 43 is connected to the alkali pipe 42 for removing H from the third mixed gas2O, obtaining nitrogen with the oxygen content of less than or equal to 0.0005 percent. The device sequentially feeds the second mixed gas into the reactor 41 and alkaliA pipe 42 and a drier 43, so that CO and H can be completely absorbed after the oxygen removal step 2And H2O, ensuring that pure high-purity nitrogen is output.
In embodiments according to the present invention, the terms "first", "second", "third" are used only for descriptive purposes and are not to be construed as indicating or implying relative importance; the term "plurality" means two or more unless explicitly defined otherwise. The terms "mounted," "connected," "fixed," and the like are to be construed broadly, and for example, "connected" may be a fixed connection, a removable connection, or an integral connection; "connected" may be directly connected or indirectly connected through an intermediate. Specific meanings of the above terms in the embodiments according to the present invention can be understood by those of ordinary skill in the art according to specific situations.
Further, while operations are depicted in a particular order, this should be understood as requiring that such operations be performed in the particular order shown or in sequential order, or that all illustrated operations be performed, to achieve desirable results. Under certain circumstances, multitasking and parallel processing may be advantageous. Likewise, while several specific implementation details are included in the above discussion, these should not be construed as limitations on the scope of the invention. Certain features that are described in the context of separate embodiments can also be implemented in combination in a single implementation. Conversely, various features that are described in the context of a single implementation can also be implemented in multiple implementations separately or in any suitable subcombination.
Although the subject matter has been described in language specific to structural features and/or methodological acts, it is to be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or acts described above. Rather, the specific features and acts described above are disclosed as example forms of implementing the claims.
The above is only a preferred embodiment according to the present invention, and is not intended to limit the embodiment according to the present invention, and various modifications and variations may be made to the embodiment according to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the embodiment according to the present invention should be included in the protection scope of the embodiment according to the present invention.

Claims (6)

1. A general nitrogen deoxidization purification method based on a methanol cracking reaction is characterized by comprising the following steps:
step S1, heating and pressurizing the methanol to obtain methanol gas with the temperature of 220-270 ℃ and the pressure of 0.6-2.0 MPa;
step S2, introducing the heated and pressurized methanol gas into a cracker containing a solid catalyst, and carrying out cracking reaction of methanol under the action of the solid catalyst to obtain CO 2CO and H2The first mixed gas of (1);
step S3, introducing the first mixed gas and common nitrogen into a deaerator, and removing oxygen in the common nitrogen to obtain a second mixed gas, wherein the temperature in the deaerator is 650-700 ℃;
and step S4, performing gas separation on the second mixed gas to obtain nitrogen with the oxygen content less than or equal to 0.0005%.
2. The method for purifying general nitrogen based on methanol cracking reaction as claimed in claim 1, further comprising, before the step S2:
and introducing protective gas into the cracker for 3-10 min to discharge the air in the cracker.
3. The method for purifying general nitrogen based on methanol cracking reaction as claimed in claim 1, wherein in the step S2, the solid catalyst comprises:
copper oxide, zinc oxide and chromium oxide.
4. The method for purifying dinitrogen based on methanol cracking reaction of general nitrogen removal according to claim 1, wherein the step S4 includes:
introducing the second mixed gas into a reactor containing copper oxide, heating the copper oxide, and removing carbon monoxide and hydrogen in the second mixed gas to obtain a third mixed gas;
And sequentially carrying out alkali washing and drying on the third mixed gas to obtain nitrogen with the oxygen content of less than or equal to 0.0005%.
5. The utility model provides a general nitrogen purification device that deoxidises based on methanol cracking reaction which characterized in that includes:
the heating pressurizer is used for heating and pressurizing the methanol to obtain methanol gas with the temperature of 220-270 ℃ and the pressure of 0.6-2.0 MPa;
the cracker is connected with the heating pressurizer, after the heated and pressurized methanol gas is introduced into the cracker, the cracker is used for carrying out cracking reaction of methanol under the action of a solid catalyst to obtain CO2CO and H2The first mixed gas of (1);
the deaerator is connected with the cracker, the first mixed gas and the common nitrogen can be deaerated after being introduced into the deaerator, so that oxygen in the common nitrogen can be removed, a second mixed gas is obtained, and the temperature in the deaerator is 650-700 ℃;
and the gas separator is connected with the deaerator and is used for performing gas separation on the second mixed gas to obtain nitrogen with the oxygen content of less than or equal to 0.0005%.
6. The device for purifying and removing oxygen from common nitrogen based on methanol cracking reaction as claimed in claim 5, wherein the gas separator comprises:
A reactor connected with the deaerator, the reactor including a heating device and copper oxide capable of removing CO and H in the second mixed gas in a heated state2Obtaining a third mixed gas, wherein the third mixed gas comprises CO2、H2O and nitrogen;
alkali tube, and itsThe reactor is connected for removing CO in the third mixed gas2
A drier connected to the alkali tube for removing H in the third mixed gas2O, obtaining nitrogen with the oxygen content of less than or equal to 0.0005 percent.
CN202210579890.0A 2022-05-26 2022-05-26 General nitrogen deoxidization purification method and device based on methanol cracking reaction Pending CN114751386A (en)

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