CN114455554B - Nitrogen purification deoxidation material and nitrogen purification device - Google Patents

Nitrogen purification deoxidation material and nitrogen purification device Download PDF

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CN114455554B
CN114455554B CN202210181311.7A CN202210181311A CN114455554B CN 114455554 B CN114455554 B CN 114455554B CN 202210181311 A CN202210181311 A CN 202210181311A CN 114455554 B CN114455554 B CN 114455554B
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nitrogen
nitrogen purification
palladium catalyst
oxygen
water vapor
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CN114455554A (en
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邹德承
李铁
易海
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Hubei Jiuen Intelligent Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/04—Purification or separation of nitrogen
    • C01B21/0405—Purification or separation processes
    • C01B21/0494—Combined chemical and physical processing
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0001—Separation or purification processing
    • C01B2210/0003—Chemical processing
    • C01B2210/0004—Chemical processing by oxidation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0001—Separation or purification processing
    • C01B2210/0003—Chemical processing
    • C01B2210/0006—Chemical processing by reduction
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0001—Separation or purification processing
    • C01B2210/0009—Physical processing
    • C01B2210/0014—Physical processing by adsorption in solids
    • C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0045—Oxygen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/005—Carbon monoxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0051—Carbon dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0053—Hydrogen

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Abstract

The invention relates to a nitrogen purification deoxidation material and a nitrogen purification device, wherein the nitrogen purification deoxidation material comprises a palladium catalyst pretreated by mixed gas; the mixed gas comprises nitrogen and water vapor, and the volume concentration of the water vapor is at least 3%; the pretreatment is to fumigate the palladium catalyst by using mixed gas at the temperature of 260-550 ℃. According to the nitrogen purification deoxidizing material and the nitrogen purification device, the palladium catalyst is pretreated by the mixed gas, the mixed gas contains water vapor, the palladium catalyst is fumigated at a certain temperature, the obtained palladium catalyst can react with hydrogen at a lower reaction temperature, oxygen in nitrogen is removed, and low-energy-consumption nitrogen purification is realized.

Description

Nitrogen purification deoxidation material and nitrogen purification device
Technical Field
The invention relates to the technical field of electronic-grade purified gas manufacturing, in particular to a nitrogen purification and deoxidation material and a nitrogen purification device.
Background
In the electronic production industry, special gases such as high-purity oxygen, nitrogen, carbon dioxide, argon, propane, etc. are required, and the purity of the special gases is far higher than that of the common industrial gases. The purity of common industrial gases is within 99.99% (generally called 4, 9 grades), which can meet the use requirement, while the purity requirement of special gases, especially in advanced process integrated circuits, is more than 6 and 9. In fact, in the most advanced chip processes at present, the gas purity requirements are even as high as 10 to 9. China is limited by foreign countries in chip manufacturing, the purity requirement of the special gas cannot reach the standard, and 88% of market share is occupied by foreign electronic special gas manufacturers in the chip manufacturing industry of China at present.
High purity nitrogen in specialty gases is used as a shielding gas and carrier gas in the manufacture of integrated circuits, semiconductors, and electro-vacuum devices. For example, in the semiconductor industry, in order to provide the required energy to the reaction system, a solid film is deposited on the surface of a silicon wafer through gas mixing, the process is called Chemical Vapor Deposition (CVD), and high-purity nitrogen is used as a carrier gas in CVD. Further, high-purity nitrogen also serves as a gas for substitution, drying, storage, and transportation in the steps of epitaxy, photolithography, cleaning, evaporation, and the like.
High purity nitrogen is of such great importance and it is desirable to obtain nitrogen in large quantities and at higher purity by devising methods to feed air. However, the composition of air is complex, and solid impurities are not said to be the key to the high purification of nitrogen, as far as possible to reduce the content of gaseous impurities, such as oxygen, carbon dioxide, carbon monoxide, sulfur dioxide and noble gases. The process flow for obtaining high purity nitrogen gas to reach the PPB level is long, and one key process is to remove oxygen in air or industrial pure nitrogen. In the prior art, a technology for deoxidizing oxygen contained in nitrogen already exists, however, the treatment process needs to be carried out at high temperature, the energy consumption is high, and the treatment efficiency is not high.
Disclosure of Invention
In view of the above, it is desirable to provide a nitrogen purification apparatus for purifying deoxygenated material and nitrogen, which addresses at least one of the above-mentioned problems.
In a first aspect, the present application provides a nitrogen-purified deoxygenated material comprising a palladium catalyst pretreated with a mixed gas; the mixed gas comprises nitrogen and water vapor, and the volume concentration of the water vapor is at least 3%; the pretreatment is to fumigate the palladium catalyst by using mixed gas at the temperature of 260-550 ℃.
In certain implementations of the first aspect, the water vapor is at a concentration of 5% by volume.
With reference to the first aspect and the foregoing implementation manners, in certain implementation manners of the first aspect, the temperature of the mixed gas is 320 ℃.
With reference to the first aspect and the foregoing implementations, in certain implementations of the first aspect, the duration of the fumigating the palladium catalyst is from 5 to 12 hours.
In a second aspect, the present application further provides a nitrogen purification apparatus, including a carbon monoxide adsorption component, a carbon dioxide adsorption component, and an oxygen adsorption component, where the oxygen adsorption component includes a hydrogen delivery part and a heating reaction part, and the heating reaction part is filled with the nitrogen purification and deoxidation material as described in any one of the first aspect of the present application.
In certain implementations of the second aspect, the oxygen adsorption assembly further includes an oxygen sensor for detecting an oxygen content of the gas at the inlet end of the oxygen adsorption assembly, and an electrically controlled valve disposed at the outlet end of the hydrogen conveying portion for controlling a hydrogen flow rate of the hydrogen conveying portion.
With reference to the second aspect and the foregoing implementation manners, in certain implementation manners of the second aspect, the heating temperature of the heating reaction part is 200 to 320 ℃.
With reference to the second aspect and the implementations described above, in certain implementations of the second aspect, the heating temperature is 300 ℃.
With reference to the second aspect and the foregoing implementation manners, in certain implementation manners of the second aspect, the carbon monoxide adsorption assembly is filled with a manganin catalyst, and the carbon dioxide adsorption assembly is filled with a molecular sieve.
With reference to the second aspect and the foregoing implementation manners, in some implementation manners of the second aspect, the water vapor adsorption device further includes a water vapor adsorption component, and the water vapor adsorption component is filled with activated alumina.
The technical scheme provided by the embodiment of the invention has the following beneficial technical effects:
according to the nitrogen purification deoxidizing material and the nitrogen purification device, the palladium catalyst is pretreated by the mixed gas, the mixed gas contains water vapor, the palladium catalyst is fumigated at a certain temperature, the obtained palladium catalyst can react with hydrogen at a lower reaction temperature, oxygen in nitrogen is removed, and low-energy-consumption nitrogen purification is realized.
Additional aspects and advantages of the present invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic structural framework diagram of a nitrogen purification apparatus according to an embodiment of the present invention;
fig. 2 is a schematic structural frame diagram of a nitrogen purification apparatus according to another embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Possible embodiments of the invention are given in the figures. The invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein by the accompanying drawings. The embodiments described by way of reference to the drawings are illustrative for the purpose of providing a more thorough understanding of the present disclosure and are not to be construed as limiting the present invention. Furthermore, if a detailed description of known technologies is not necessary for illustrating the features of the present invention, such technical details may be omitted.
It will be understood by those skilled in the relevant art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It is to be understood that the term "and/or" as used herein is intended to include all or any and all combinations of one or more of the associated listed items.
The technical solution of the present invention and how to solve the above technical problems will be described in detail with specific examples.
Embodiments of a first aspect of the present application provide a nitrogen-purified deoxygenated material including a mixed gas pretreated palladium catalyst; the mixed gas comprises nitrogen and water vapor, and the volume concentration of the water vapor is at least 3%; the pretreatment is to fumigate the palladium catalyst by using mixed gas at the temperature of 260-550 ℃.
The palladium catalyst is a common deoxidation catalyst in the field of nitrogen purification, and oxygen can quickly and fully react with hydrogen with proper component proportion at 400-600 ℃ by the palladium catalyst to obtain moisture and remove oxygen included in nitrogen. However, in the removing process, the hydrogen or oxygen needs to be heated to about 500 ℃ to ensure the catalytic efficiency of the palladium catalyst, and further ensure that the oxygen is sufficiently and rapidly separated from the nitrogen, which is obviously an industrial production condition with high energy consumption.
Through test tests, the palladium catalyst purchased from the market and used for nitrogen deoxidation is pretreated, and the catalytic reaction temperature of the pretreated palladium catalyst is greatly reduced compared with that of the palladium catalyst without pretreatment. The palladium catalyst is fumigated by adopting water vapor with higher temperature, so that the crystal grain structure of the palladium catalyst can be changed, and the catalytic active sites in the palladium catalyst are increased, thereby greatly reducing the catalytic reaction temperature of the palladium catalyst.
The application provides a nitrogen purification deoxidation material is through adopting the palladium catalyst through the mist pretreatment, and wherein the mist contains vapor, heats the mist to the uniform temperature under, fumigates the palladium catalyst, and the palladium catalyst that obtains can promote oxygen and hydrogen reaction under lower reaction temperature, generates vapor to get rid of the oxygen in the nitrogen gas, reduce the deoxidation energy consumption by a wide margin.
Optionally, in some implementations of embodiments of the first aspect of the present application, the water vapor has a concentration of 5% by volume. The mixed gas can be 95% of nitrogen and 5% of water vapor. Experiments prove that when the volume concentration of the water vapor is not less than 3%, the pretreatment effect on the palladium catalyst is gradually obvious.
Optionally, with reference to the first aspect and the above implementations, in certain implementations of the first aspect, the temperature of the mixed gas is 320 ℃. The temperature of the mixed gas needs to be heated to 260-550 ℃, and the increasing effect on the catalytic active sites of the palladium catalyst is not obvious any more when the temperature is above 550 ℃.
Optionally, in certain embodiments of the first embodiment, the duration of fumigating the palladium catalyst is from 5 to 12 hours. And (3) putting the palladium catalyst into a tank, introducing high-temperature mixed gas into the tank bottom, blowing the palladium catalyst, repeatedly rolling in the tank for 5-12 hours, and obtaining the pretreated palladium catalyst.
Based on the same inventive concept, the second aspect of the present application further provides a nitrogen purification apparatus 10, as shown in fig. 1, including a carbon monoxide adsorption module 11, a carbon dioxide adsorption module 12, and an oxygen adsorption module 13, where the oxygen adsorption module 13 includes a hydrogen gas delivery part and a heating reaction part, and the heating reaction part is filled with a nitrogen purification and deoxidation material as in any one of the first aspect of the present application. The nitrogen purification device consists of a plurality of adsorption components, and can absorb and remove carbon monoxide and carbon dioxide, then remove oxygen, then remove gases containing other components, and finally obtain nitrogen with higher purity. Air can be directly used as a nitrogen gas source for nitrogen production, and a nitrogen gas source formed by rough machining can also be used. The invention adopts nitrogen with lower catalytic reaction temperature to purify the deoxidation material, and can achieve the same deoxidation effect with lower energy consumption.
Optionally, in some implementations of the embodiment of the second aspect, the oxygen adsorption assembly 13 further includes an oxygen sensor and an electrically controlled valve, the oxygen sensor is used for detecting the oxygen content of the gas at the inlet end of the oxygen adsorption assembly, and the electrically controlled valve is disposed at the outlet end of the hydrogen conveying portion and is used for controlling the hydrogen flow rate of the hydrogen conveying portion. The oxygen content of the gas of input through the inlet end department that detects oxygen adsorption component, with data input to the controller, through the automatically controlled valve that the controller allotment is located the end of giving vent to anger of hydrogen conveying part, the hydrogen content of control input in oxygen adsorption component 13 makes hydrogen and oxygen mix according to the proportion of abundant reaction, and abundant reaction in the palladium catalyst to fully deoxidize the oxygen in the nitrogen gas, and avoid appearing the secondary pollution to nitrogen gas.
From a hardware perspective, the controller may be a CPU (Central Processing Unit), a general-purpose Processor, a DSP (Digital Signal Processor), an ASIC (Application Specific Integrated Circuit), an FPGA (Field-Programmable Gate Array), or other Programmable logic device, a transistor logic device, a hardware component, or any combination thereof. Which may implement or perform the various illustrative logical blocks, modules, and circuits described in connection with the disclosure. The controller may also be a combination of computing functions, e.g., comprising one or more microprocessors, DSPs, and microprocessors, among others.
Optionally, with reference to the second aspect and the foregoing implementation manners, in some implementation manners of the second aspect, the heating temperature of the heating reaction portion is 200 to 320 ℃. The heating mode can be electric heating, and the heating temperature is accurately controlled by a controller. Alternatively, in one embodiment, the heating temperature is 300 ℃ and the error range may be ± 5 ℃.
Optionally, in combination with the second aspect and the above implementations, in some implementations of the second aspect, the carbon monoxide adsorption module 11 is filled with a manganin catalyst, and the carbon dioxide adsorption module 12 is filled with a molecular sieve. These materials are common carbon monoxide or carbon dioxide adsorbents and are available directly from the market.
Optionally, with reference to the embodiment of the second aspect and the foregoing implementation manners, in some implementation manners of the second aspect, as shown in fig. 2, the nitrogen purification apparatus 10 further includes a water vapor adsorption component 14, and the water vapor adsorption component 14 is filled with activated alumina. The water vapor adsorption module 14 may be disposed behind the oxygen adsorption module 13 to absorb water vapor that would otherwise be present in the nitrogen source, as well as water vapor generated by the oxygen adsorption module 13. In addition to activated alumina, anhydrous nickel chloride, which has good moisture absorption, can be used, but the loading of the anhydrous nickel chloride needs to be taken into account.
According to the nitrogen purification deoxidizing material and the nitrogen purification device, the palladium catalyst is pretreated by the mixed gas, the mixed gas contains water vapor, the palladium catalyst is fumigated at a certain temperature, the obtained palladium catalyst can react with hydrogen at a lower reaction temperature, oxygen in nitrogen is removed, and low-energy-consumption nitrogen purification is realized.
The following are specific examples:
example 1:
the palladium catalyst pretreated by the high-temperature mixed gas containing water vapor is applied to deoxidation operation in the nitrogen purification process, so that the reaction temperature is greatly reduced, the production energy consumption is reduced, and high-purity nitrogen is obtained.
The palladium catalyst is purchased from a deoxidizing catalyst which is already applied in the market, the mixed gas contains 3 percent of water vapor, and the rest is nitrogen. Heating the mixed gas to 260 ℃, loading a palladium catalyst to be treated in a fumigation device, and fumigating the palladium catalyst for 5 hours.
And loading the pretreated palladium catalyst into an oxygen adsorption component of a nitrogen purification device. The nitrogen purification device is started, air is used as a nitrogen source, so that the air sequentially passes through the carbon monoxide adsorption component, the titanium dioxide adsorption component and the oxygen adsorption component, wherein the working temperature of the oxygen adsorption component is 200 ℃. And detecting to obtain a gas sample with the minimum value of 0.81PPM of oxygen content.
Example 2:
the mixed gas contains 3% water vapor and nitrogen in balance, and the mixed gas is heated to 300 deg.c to fumigate the palladium catalyst for 5 hr. The pretreated palladium catalyst is adopted for deoxidation operation, hydrogen with a corresponding proportion is input according to the detected oxygen content in the nitrogen source, the pretreated palladium catalyst can fully convert the oxygen in the nitrogen source into water vapor at the temperature of 200 ℃, and the minimum value of the oxygen content in a gas sample obtained after treatment is detected to be 0.78PPM.
Example 3:
the mixed gas contains 5% water vapor and nitrogen in balance, and the mixed gas is heated to 260 ℃ to fumigate the palladium catalyst for 5 hours. The pretreated palladium catalyst is adopted for deoxidation operation, hydrogen with a corresponding proportion is input according to the detected oxygen content in the nitrogen source, the pretreated palladium catalyst can fully convert the oxygen in the nitrogen source into water vapor at the temperature of 200 ℃, and the minimum value of the oxygen content in a gas sample obtained after treatment is detected to be 0.77PPM.
Example 3:
the mixed gas contains 5% water vapor and nitrogen in balance, and the mixed gas is heated to 260 ℃ to fumigate the palladium catalyst for 12 hours. The pretreated palladium catalyst is adopted for deoxidation operation, hydrogen with a corresponding proportion is input according to the detected oxygen content in the nitrogen source, the pretreated palladium catalyst can fully convert the oxygen in the nitrogen source into water vapor at the temperature of 200 ℃, and the minimum value of the oxygen content in a gas sample obtained after treatment is detected to be 0.78PPM.
Example 4:
the mixed gas contains 5% water vapor and nitrogen in balance, and the mixed gas is heated to 260 ℃ to fumigate the palladium catalyst for 8 hours. The pretreated palladium catalyst is adopted for deoxidation operation, hydrogen with a corresponding proportion is input according to the detected oxygen content in the nitrogen source, the pretreated palladium catalyst can fully convert the oxygen in the nitrogen source into water vapor at 320 ℃, and the minimum value of the oxygen content in a gas sample obtained after treatment is detected to be 0.69PPM.
Example 5:
the mixed gas contains 5% water vapor and nitrogen in balance, and the mixed gas is heated to 320 ℃ to fumigate the palladium catalyst for 8 hours. The pretreated palladium catalyst is adopted for deoxidation operation, hydrogen with a corresponding proportion is input according to the detected oxygen content in the nitrogen source, the pretreated palladium catalyst can fully convert the oxygen in the nitrogen source into water vapor at 300 ℃, and the minimum value of the oxygen content in a gas sample obtained after treatment is detected to be 0.54PPM.
Example 6:
the mixed gas contains 10% water vapor and nitrogen in balance, and the mixed gas is heated to 550 ℃ to fumigate the palladium catalyst for 12 hours. The pretreated palladium catalyst is adopted for deoxidation operation, hydrogen with a corresponding proportion is input according to the detected oxygen content in the nitrogen source, the pretreated palladium catalyst can fully convert the oxygen in the nitrogen source into water vapor at 320 ℃, and the minimum value of the oxygen content in a gas sample obtained after treatment is detected to be 0.60PPM.
Comparative example:
performing deoxidation operation by using a palladium catalyst, inputting hydrogen in a corresponding proportion according to the detected oxygen content in the nitrogen source, fully converting the oxygen in the nitrogen source into water vapor by using the palladium catalyst at 500 ℃, and detecting and processing to obtain a gas sample with the minimum value of about 1PPM of the oxygen content.
According to a large amount of test data, the examples and the comparative examples, the palladium catalyst treated by water vapor can be well applied in the operation process of deoxidizing nitrogen, the temperature of oxyhydrogen reaction is greatly reduced, the absorption degree of oxygen is improved, and the purity of nitrogen is improved.
Those of skill in the art will understand that various operations, methods, steps in the flow, measures, schemes discussed in this application can be alternated, modified, combined, or deleted. Further, various operations, methods, steps, measures, schemes in the various processes, methods, procedures that have been discussed in this application may be alternated, modified, rearranged, decomposed, combined, or eliminated. Further, the steps, measures, and schemes in the various operations, methods, and flows disclosed in the present application in the prior art can also be alternated, modified, rearranged, decomposed, combined, or deleted.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless otherwise specified.
In the description herein, particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples.
It should be understood that, although the steps in the flowcharts of the figures are shown in order as indicated by the arrows, the steps are not necessarily performed in order as indicated by the arrows. The steps are not performed in the exact order shown and may be performed in other orders unless explicitly stated herein. Moreover, at least a portion of the steps in the flow chart of the figure may include multiple sub-steps or multiple stages, which are not necessarily performed at the same time, but may be performed at different times, which are not necessarily performed in sequence, but may be performed alternately or alternately with other steps or at least a portion of the sub-steps or stages of other steps.
The foregoing is only a few embodiments of the present application and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present application, and that these improvements and modifications should also be considered as the protection scope of the present application.

Claims (9)

1. The nitrogen purification and deoxidation material is characterized by comprising a palladium catalyst pretreated by mixed gas; the mixed gas comprises nitrogen and water vapor, and the volume concentration of the water vapor is at least 3%; the pretreatment is to fumigate the palladium catalyst by using mixed gas at the temperature of 260-550 ℃, and the duration of fumigating the palladium catalyst is 5-12 hours.
2. The nitrogen purification deoxygenated material of claim 1, wherein the water vapor is present at a concentration of 5% by volume.
3. The nitrogen purification deoxygenated material of claim 1, wherein the temperature of the mixed gas is 320 ℃.
4. A nitrogen purification device, which is characterized by comprising a carbon monoxide adsorption component, a carbon dioxide adsorption component and an oxygen adsorption component, wherein the oxygen adsorption component comprises a hydrogen conveying part and a heating reaction part, and the heating reaction part is filled with the nitrogen purification and deoxidation material as claimed in any one of claims 1 to 3.
5. The nitrogen purification device according to claim 4, wherein the oxygen adsorption assembly further comprises an oxygen sensor for detecting the oxygen content of the gas at the inlet end of the oxygen adsorption assembly, and an electrically controlled valve disposed at the outlet end of the hydrogen conveying portion for controlling the hydrogen flow rate of the hydrogen conveying portion.
6. The nitrogen purification apparatus according to claim 4, wherein the heating temperature of the heating reaction section is 200 to 320 ℃.
7. A nitrogen purification apparatus according to claim 6, wherein the heating temperature is 300 ℃.
8. A nitrogen purification apparatus as claimed in claim 4, wherein the carbon monoxide adsorption module is packed with manganese copper catalyst and the carbon dioxide adsorption module is packed with molecular sieve.
9. The nitrogen purification device of claim 4, further comprising a water vapor adsorption module filled with activated alumina.
CN202210181311.7A 2022-02-25 2022-02-25 Nitrogen purification deoxidation material and nitrogen purification device Active CN114455554B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1210708A (en) * 1957-07-12 1960-03-10 Engelhard Ind Process for purifying gases, in particular nitrogen, with a view to the catalytic synthesis of ammonia
CN104511315A (en) * 2013-09-28 2015-04-15 中国石油化工股份有限公司 Regeneration method of palladium catalyst for hydrogenation reaction

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1210708A (en) * 1957-07-12 1960-03-10 Engelhard Ind Process for purifying gases, in particular nitrogen, with a view to the catalytic synthesis of ammonia
CN104511315A (en) * 2013-09-28 2015-04-15 中国石油化工股份有限公司 Regeneration method of palladium catalyst for hydrogenation reaction

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Denomination of invention: Nitrogen purification and deoxygenation materials and nitrogen purification equipment

Granted publication date: 20221108

Pledgee: Huangshi Jinshan New Area Branch of Hubei Bank Co.,Ltd.

Pledgor: Hubei jiuen Intelligent Technology Co.,Ltd.

Registration number: Y2024980004128