CN113856462A - Nitrogen purification device and method - Google Patents
Nitrogen purification device and method Download PDFInfo
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- CN113856462A CN113856462A CN202111308595.3A CN202111308595A CN113856462A CN 113856462 A CN113856462 A CN 113856462A CN 202111308595 A CN202111308595 A CN 202111308595A CN 113856462 A CN113856462 A CN 113856462A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
- B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas
Abstract
The invention relates to a nitrogen purification device and method, and belongs to the technical field of nitrogen purification. The device comprises a catalytic oxidation unit, a deoxidation adsorption unit and a regeneration unit which are connected in sequence, wherein a waste gas discharge branch is arranged between the catalytic oxidation unit and the deoxidation adsorption unit; the raw material gas is purified by a catalytic oxidation unit and a deoxidation adsorption unit to obtain a product gas with greatly improved purity; after the deoxidation adsorption unit is saturated, the purification is stopped, and the regeneration gas enters the deoxidation adsorption unit through the regeneration unitRegenerating the cells; when the purification device is used for the first time or is not used for a long time and then is started, the catalytic oxidation unit is heated to the working temperature to discharge the waste gas CO2Introducing raw gas to sweep the catalytic oxidation unit and the deoxidation adsorption unit, and introducing the waste gas CO2Discharging the purified plant through an exhaust gas discharge branch; the purification device and the method solve the problem of CO in the catalytic oxidizer2Release and inconvenient use of regeneration gas.
Description
Technical Field
The invention relates to a nitrogen purification device and method, and belongs to the technical field of nitrogen purification.
Background
Currently, nitrogen purification usually adopts front-end catalytic oxidation and back-end deoxidation and adsorption. H in nitrogen feed gas2CO and CH4Reducing component impurities are removed by catalytic oxidant at high temperature to generate H2O and CO2(ii) a In the deoxidation adsorber used for the back-end deoxidation adsorption, O2、H2O and CO2Is deeply removed to realize the purification of nitrogen. The deoxidized adsorbent works at normal temperature and is activated and regenerated at high temperature, and the regeneration gases are respectively hydrogen and nitrogen.
The nitrogen purification method has the following problems:
(1) catalytic oxidizer releases CO at high temperature2In particular, release a large amount of CO when used for the first time or not used for a long time2，CO2The oxygen is adsorbed by the deoxidation adsorber at the rear end, so that the deoxidation adsorber is easily saturated.
(2) When the deoxygenation adsorbent is regenerated, regenerated hydrogen and regenerated nitrogen need to be respectively introduced, so that the operation difficulty is high. Moreover, hydrogen is flammable and explosive gas, so that the safety risk is high, and the nitrogen purification device and the plant in which the nitrogen purification device is arranged are required to be in accordance with II CT4 level electrical explosion-proof according to the regulations. The nitrogen is a non-combustible gas, the nitrogen is generally a non-explosion-proof area when in use, the explosion-proof area and the non-explosion-proof area are isolated by an explosion-proof wall, and a gas pipeline cannot penetrate through the explosion-proof wall.
The defects cause inconvenience in the nitrogen purification process and cannot meet the requirement of industrial ring production of large-scale integrated circuits.
Disclosure of Invention
In view of the above, the present invention provides a nitrogen purification apparatus and method, which solves the problem of CO in catalytic oxidizer2Release and inconvenient use of regeneration gas.
In order to achieve the purpose of the invention, the following technical scheme is provided.
A nitrogen purification device comprises a catalytic oxidation unit, a deoxidation adsorption unit and a regeneration unit which are sequentially connected, wherein a waste gas discharge branch is arranged between the catalytic oxidation unit and the deoxidation adsorption unit; the catalytic oxidation unit is provided with a catalytic oxidant, and the deoxidation adsorption unit is provided with a deoxidation adsorbent.
The raw material gas is purified by a catalytic oxidation unit and a deoxidation adsorption unit to obtain a product gas.
And after the deoxidation adsorption unit is saturated in adsorption, stopping purification, and allowing the regeneration gas to enter the deoxidation adsorption unit through the regeneration unit for regeneration.
When the purification device is used for the first time or is not used for a long time and then is started, the catalytic oxidation unit is heated to the working temperature to discharge the waste gas CO2Introducing raw gas to sweep the catalytic oxidation unit and the deoxidation adsorption unit, and introducing the waste gas CO2And discharging the purified gas from the purification device through an exhaust gas discharge branch.
The raw material gas is nitrogen to be purified, and the product gas is purified nitrogen; preferably, the raw material gas is nitrogen with the purity of 99.999 percent, and the product gas is nitrogen with the purity of more than or equal to 99.9999 percent.
The regeneration gas is hydrogen and nitrogen; preferably, the flow ratio of the hydrogen to the nitrogen when the hydrogen and the nitrogen are introduced is 1:19 to 1: 24.
More preferably, the hydrogen and the nitrogen are mixed to prepare a regenerated hydrogen-nitrogen mixed gas as the regenerated gas, the volume fraction of the hydrogen in the regenerated hydrogen-nitrogen mixed gas is 4-5%, and the hydrogen is mixed according to the classification 3 part of the mixed gas: combustible gas classification (GB/T34710.3-2018), and the hydrogen-nitrogen mixture is not combustible when the volume fraction is less than or equal to 5.5 percent, so the purification device and the placing area are not explosion-proof electrically.
More preferably, the regenerated hydrogen-nitrogen mixed gas is placed in the cylinder group, so that the replacement and inspection interval of the gas cylinder during regeneration is reduced.
Preferably, in the purification device, the catalytic oxidation unit comprises a raw material gas inlet valve, a first pressure gauge branch pipe, a first pressure gauge root valve, a first pressure gauge, a first flowmeter, a catalytic heat exchanger and a catalytic oxidizer, and a catalytic oxidant is placed in the catalytic oxidizer.
The deoxidation adsorption unit comprises a first cooler, a first air inlet valve of the deoxidation adsorber, a second air inlet valve of the deoxidation adsorber and the deoxidation adsorber.
The exhaust gas discharge branch includes a second cooler and an exhaust gas discharge valve.
The regeneration unit comprises a regeneration first valve, a second pressure gauge branch pipe, a second pressure gauge root valve, a second pressure gauge, a second flowmeter, a one-way valve and a regeneration second valve.
The catalytic heat exchanger is characterized in that a raw material gas is connected with a tube pass inlet of the catalytic heat exchanger through a pipeline, a tube pass outlet of the catalytic heat exchanger is connected with an inlet of the catalytic oxidation device through a pipeline, an outlet of the catalytic oxidation device is connected with a shell pass inlet of the catalytic heat exchanger through a pipeline, and an outlet of the shell pass of the catalytic heat exchanger is connected with an inlet of the deoxidation absorber through a pipeline.
On the pipeline that the feed gas and catalytic heat exchanger tube side entry linkage, feed gas entry rear is equipped with feed gas admission valve, first manometer branch pipe and first flowmeter in proper order, first manometer branch pipe lower extreme with the tube coupling, the upper end is connected with first manometer, is equipped with first manometer root valve on the first manometer branch pipe of first manometer below.
On the pipeline connecting the shell pass outlet of the catalytic heat exchanger with the inlet of the deoxidation absorber, a first cooler, a first air inlet valve of the deoxidation absorber, an exhaust gas discharge branch and a second air inlet valve of the deoxidation absorber are sequentially arranged behind the shell pass outlet of the catalytic heat exchanger.
The exhaust emission branch is provided with a second cooler, and an exhaust emission valve is arranged behind the second cooler.
The back end of the pipeline connected with the outlet of the deoxidation absorber is divided into two branches, one branch is a regenerated gas pipeline connected with the regeneration unit, the other branch is a product gas pipeline used for releasing product gas, and a product valve is arranged on the product gas pipeline.
The regeneration gas is connected with the outlet of the deoxidation adsorber through a regeneration gas pipeline, a regeneration first valve is arranged behind a regeneration hydrogen-nitrogen mixed gas inlet on the regeneration gas pipeline, and a second pressure gauge branch pipe, a second flow meter, a one-way valve and a regeneration second valve are sequentially arranged behind the regeneration gas pipeline. The lower end of the second pressure gauge branch pipe is connected with a regenerated gas pipeline, the upper end of the second pressure gauge branch pipe is connected with a second pressure gauge, and a second pressure gauge root valve is arranged on the second pressure gauge branch pipe below the second pressure gauge.
The invention discloses a nitrogen purification method, which is carried out by adopting a nitrogen purification device and comprises the following steps:
closing the exhaust gas discharge valve and the regeneration second valve; opening a raw material gas inlet valve, a first pressure gauge root valve, a first gas inlet valve of a deoxidation absorber, a second gas inlet valve of the deoxidation absorber and a product valve;
and introducing the raw gas into the purification device, and purifying the raw gas by a first flowmeter, a catalytic heat exchanger tube pass, a catalytic oxidizer, a catalytic heat exchanger shell pass, a first cooler, a first gas inlet valve of a deoxidation adsorber, a second gas inlet valve of the deoxidation adsorber, the deoxidation adsorber and a product valve through a pipeline sequentially to obtain a product gas.
In the purification by catalytic heat exchanger, H2CO and CH4The reducing components are removed under the action of catalytic oxidant to generate H2O、CO2(ii) a At room temperature, O2、H2O and CO2Is deeply removed by deoxidation and adsorption in a deoxidation adsorber, O2And H2The minimum O can be reduced to below 1 ppb.
The operating temperature for purification in the catalytic heat exchanger is preferably 330 ℃.
After the deoxidation absorber is detected to be saturated in adsorption, the deoxidation absorber needs to be regenerated, and the steps are as follows:
raising the temperature of the deoxidation adsorber to a regeneration temperature, and closing a product valve and a first air inlet valve of the deoxidation adsorber; opening a regeneration first valve, a second pressure gauge root valve, a regeneration second valve and an exhaust gas discharge valve; and the regeneration gas is purged and discharged sequentially through a regeneration first valve, a second pressure gauge branch, a second flowmeter, a one-way valve, a regeneration second valve, a deoxidation absorber second air inlet valve, a second cooler and a waste gas discharge valve. And after the regeneration is finished, stopping heating the deoxidation absorber, closing the first regeneration valve, opening the first air inlet valve of the deoxidation absorber, replacing the regeneration gas with the feed gas, introducing the feed gas for purging, and purging the deoxidation absorber to the normal temperature.
Preferably, the regeneration temperature of the deoxidation adsorber is 350 ℃, the regeneration gas pressure is 0.4MPa, and the flow rate is 3Nm3H, after 24 hours of regeneration, the regeneration gas is changed into the raw material gas and is introduced at the flow rate of 6Nm and 0.4MPa3Blow cooling for 3h to normal temperature.
When the purification device is used for the first time or is not used for a long time and then is started, the catalytic oxidizer can release a large amount of CO at the high temperature of 330-500 DEG C2If the deoxygenation adsorber is introduced, CO2Will be fully adsorbed, causing saturation of the deoxygenating adsorber and hence the need to release CO from the catalytic oxidizer2Discharging the purification device; the method comprises the following specific steps:
closing a second air inlet valve of the deoxidation absorber, opening a raw material gas inlet valve, a first pressure gauge root valve, a first air inlet valve of the deoxidation absorber and an exhaust gas discharge valve; the temperature of the catalytic oxidizer is raised to 330-500 ℃; the raw gas is purged through a raw gas inlet valve, a first pressure gauge branch, a first flowmeter, a catalytic heat exchanger tube pass, a catalytic oxidizer, a catalytic heat exchanger shell pass, a first cooler, a first inlet valve of a deoxidation absorber, a second cooler and a waste gas discharge valve in sequence, and CO in the discharged waste gas is discharged2(ii) a After purging for 8h, sampling and detecting through an exhaust emission valve if CO is detected2Stopping purging when the concentration is less than or equal to 3 ppm.
Advantageous effects
1. The invention provides a nitrogen purification device and a nitrogen purification method, wherein the device comprises a catalytic oxidation unit, a deoxidation adsorption unit and a regeneration unit which are sequentially connected, and a waste gas discharge branch is arranged between the catalytic oxidation unit and the deoxidation adsorption unit; the raw gas is purified by a catalytic oxidation unit and a deoxidation adsorption unit to obtain product gas with greatly improved purity, and the purity of the raw gas nitrogen with the purity of 99.999 percent is improved to 99.9999 percent after catalytic oxidation and deoxidation adsorption; after the deoxidation adsorption unit is saturated in adsorption, stopping purification, and allowing the regeneration gas to enter the deoxidation adsorption unit through a regeneration unit for regeneration; when the purification device is used for the first time or is not used for a long timeWhen the catalytic oxidation unit is started, the catalytic oxidation unit is heated to the working temperature to discharge the waste gas CO2Introducing raw gas to sweep the catalytic oxidation unit and the deoxidation adsorption unit, and introducing the waste gas CO2Discharging the purified plant through an exhaust gas discharge branch; the device solves the problem of CO in the catalytic oxidizer2Release and inconvenient use of regeneration gas.
2. The invention provides a nitrogen purification device and a nitrogen purification method, wherein a non-combustible regenerated hydrogen-nitrogen mixed gas is prepared by mixing regenerated gas hydrogen and nitrogen, and the nitrogen purification device and electrical equipment in a placement area are changed from explosion-proof to non-explosion-proof, so that the equipment manufacturing and pipeline construction cost is saved, and the convenience of regeneration operation is improved.
Drawings
FIG. 1 is a schematic view of a nitrogen purification apparatus according to the present invention.
The method comprises the following steps of 1, a raw material gas inlet valve, 2, a first pressure gauge root valve, 3, a first pressure gauge, 4, a first flowmeter, 5, a catalytic heat exchanger, 6, a catalytic oxidizer, 7, a first cooler, 8, a first deoxidation adsorber inlet valve, 9, a second deoxidation adsorber inlet valve, 10, a second cooler, 11, an exhaust gas discharge valve, 12, a deoxidation adsorber, 13, a regeneration first valve, 14, a second pressure gauge root valve, 15, a second pressure gauge, 16, a second flowmeter, 17, a one-way valve, 18, a regeneration second valve and 19, wherein the raw material gas inlet valve, the first pressure gauge root valve, the first pressure gauge, the second flowmeter, the one-way valve and the product valve are arranged in sequence.
Detailed Description
The invention is described in detail below with reference to the drawings and specific examples, but the invention is not limited thereto.
Example 1
As shown in fig. 1, a purification apparatus for nitrogen gas, the purification apparatus comprising: the device comprises a catalytic oxidation unit, a deoxidation adsorption unit and a regeneration unit; and a waste gas discharge branch is arranged between the catalytic oxidation unit and the deoxidation adsorption unit, and waste gas of the catalytic oxidation unit can be discharged through the waste gas discharge branch.
The catalytic oxidation unit comprises a raw gas inlet valve 1, a first pressure gauge branch pipe, a first pressure gauge root valve 2, a first pressure gauge 3, a first flowmeter 4, a catalytic heat exchanger 5 and a catalytic oxidizer 6, wherein a catalytic oxidant is placed in the catalytic oxidizer 6.
The deoxygenation adsorption unit includes a first cooler 7, a deoxygenation adsorber first intake valve 8, a deoxygenation adsorber second intake valve 9, and a deoxygenation adsorber 12.
The exhaust gas discharge branch includes a second cooler 10 and an exhaust gas discharge valve 11.
The regeneration unit comprises a regeneration first valve 13, a second pressure gauge branch pipe, a second pressure gauge root valve 14, a second pressure gauge 15, a second flowmeter 16, a one-way valve 17 and a regeneration second valve 18.
The raw material gas is connected with a tube side inlet of a catalytic heat exchanger 5 through a pipeline, a tube side outlet of the catalytic heat exchanger 5 is connected with an inlet of a catalytic oxidation device 6 through a pipeline, an outlet of the catalytic oxidation device 6 is connected with a shell side inlet of the catalytic heat exchanger 5 through a pipeline, and a shell side outlet of the catalytic heat exchanger 5 is connected with an inlet of a deoxidation absorber 12 through a pipeline.
On the pipeline of feed gas and 5 tube side entry connections of catalytic heat exchanger, feed gas entry rear is equipped with feed gas admission valve 1, first manometer branch pipe and first flowmeter 4 in proper order, first manometer branch pipe lower extreme with the tube coupling, the upper end is connected with first manometer 3, is equipped with first manometer root valve 2 on the first manometer branch pipe of first manometer 3 below.
On a pipeline connecting the shell side outlet of the catalytic heat exchanger 5 with the inlet of the deoxidation absorber 12, a first cooler 7, a first air inlet valve 8 of the deoxidation absorber, an exhaust gas discharge branch and a second air inlet valve 9 of the deoxidation absorber are sequentially arranged behind the shell side outlet of the catalytic heat exchanger 5.
The exhaust gas discharge branch is provided with a second cooler 10, and an exhaust gas discharge valve 11 is arranged behind the second cooler 10.
The rear end of the pipeline connected with the outlet of the deoxidation absorber 12 is divided into two branches, one branch is a regeneration gas pipeline and is connected with the regeneration unit, and the other branch is a product gas pipeline and is used for releasing product gas.
The regenerated hydrogen-nitrogen mixed gas is connected with the outlet of the deoxidation adsorber 12 through a regenerated gas pipeline, a regenerated first valve 13 is arranged on the regenerated gas pipeline behind the regenerated hydrogen-nitrogen mixed gas inlet, and a second pressure gauge branch pipe, a second flowmeter 16, a one-way valve 17 and a regenerated second valve 18 are sequentially arranged behind the regenerated hydrogen-nitrogen mixed gas pipeline. The lower end of the second pressure gauge branch pipe is connected with a regenerated gas pipeline, the upper end of the second pressure gauge branch pipe is connected with a second pressure gauge 15, and a second pressure gauge root valve 14 is arranged on the second pressure gauge branch pipe below the second pressure gauge 15.
And a product valve 19 is arranged on a product gas pipeline, the product gas is purified nitrogen, and the purity is more than or equal to 99.9999%.
Example 2
A method for purifying nitrogen gas, which is performed by using the nitrogen gas purification apparatus described in example 1, and comprises the following steps:
closing the exhaust gas discharge valve 11 and the regeneration second valve 18; opening a raw material gas inlet valve 1, a first pressure gauge root valve 2, a first gas inlet valve 8 of a deoxidation adsorber, a second gas inlet valve 9 of the deoxidation adsorber and a product valve 19;
nitrogen with the purity of 99.999 percent is used as raw material gas and is introduced into the purification device, and the nitrogen is purified by a first flowmeter 4, a catalytic heat exchanger 5 tube pass, a catalytic oxidizer 6, a catalytic heat exchanger 5 shell pass, a first cooler 7, a deoxidation adsorber first air inlet valve 8, a deoxidation adsorber second air inlet valve 9, a deoxidation adsorber 12 and a product valve 9 through a pipeline in sequence, so that the nitrogen with the purity of more than or equal to 99.9999 percent is obtained.
The catalytic heat exchanger 5 is heated to 330 ℃ for purification, H2CO and CH4The reducing components are removed under the action of catalytic oxidant to generate H2O、CO2(ii) a At room temperature, O2、H2O and CO2Is deeply removed in the deoxidation adsorber 12, O2And H2The minimum O can be reduced to below 1 ppb.
After the deoxidation absorber 12 is found to be saturated in adsorption through detection, the deoxidation absorber 12 needs to be regenerated, and the steps are as follows:
the hydrogen and the nitrogen are mixed to prepare regenerated hydrogen-nitrogen mixed gas serving as regenerated gas to be placed in the bottle group, the volume fraction of the hydrogen in the regenerated hydrogen-nitrogen mixed gas is 4%, and the purification device and the electrical equipment in the placement area do not need to be explosion-proof.
During regeneration, the temperature of the deoxidation adsorber 12 is increased to 350 ℃, and the product valve 19 and the first air inlet valve 8 of the deoxidation adsorber are closed; opening the regenerative first valve 13, the second pressure gauge foot valve 14, the regenerative second valve 18 and the exhaust gas discharge valve 11; the pressure of the regeneration gas is 0.4MPa, and the flow rate is 3Nm3And/h, purging and then discharging the gas sequentially through a regeneration first valve 13, a second pressure gauge branch, a second flowmeter 16, a one-way valve 17, a regeneration second valve 18, a deoxidation adsorber 12, a deoxidation adsorber second air inlet valve 9, a second cooler 10 and an exhaust gas discharge valve 11, wherein after the regeneration is finished for 24h, the consumption of the regeneration gas is 72m3One bottle group (96 m)3) Thereby meeting the requirement of regeneration. Stopping heating the deoxidation adsorber 12, closing the regeneration first valve 13, opening the deoxidation adsorber first air inlet valve 8, replacing the regeneration gas with feed gas, introducing and purging at 0.4MPa and 6Nm flow3Blowing for 3h, and blowing the deoxidation absorber 12 to the normal temperature.
When the purification device is used for the first time or is not used for a long time and then is started, the catalytic oxidizer 6 can release a large amount of CO at the high temperature of 330-500 DEG C2If passed to the deoxygenation adsorber 12, CO2Will be fully adsorbed, causing saturation of the deoxygenation adsorber 12 and therefore the CO released by the catalytic oxidizer 6 will need to be removed2Is discharged through the exhaust gas discharge valve 11.
The specific implementation steps of the exhaust emission in the catalytic oxidation unit are as follows:
(1) closing a second air inlet valve 9 of the deoxidation adsorber, opening a raw material gas inlet valve 1, a first pressure gauge root valve 2, a first air inlet valve 8 of the deoxidation adsorber and an exhaust gas discharge valve 11; the temperature of the catalytic oxidizer 6 is raised to 330-500 ℃; the raw gas is purged through a raw gas inlet valve 1, a first pressure gauge branch, a first flowmeter 4, a catalytic heat exchanger 5 tube pass, a catalytic oxidizer 6, a catalytic heat exchanger 5 shell pass, a first cooler 7, a deoxidation absorber first inlet valve 8, a second cooler 10 and a waste gas discharge valve 11 in sequence, and waste gas CO is discharged2(ii) a After purging for 8h, sampling and detecting through an exhaust emission valve 11 if CO is detected2Stopping purging when the concentration is less than or equal to 3 ppm.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A nitrogen purification device is characterized in that: the purification device comprises a catalytic oxidation unit, a deoxidation adsorption unit and a regeneration unit which are connected in sequence, and a waste gas discharge branch is arranged between the catalytic oxidation unit and the deoxidation adsorption unit; a catalytic oxidation agent is placed in the catalytic oxidation unit, and a deoxygenation adsorbent is placed in the deoxygenation adsorption unit;
purifying the feed gas by a catalytic oxidation unit and a deoxidation adsorption unit to obtain a product gas;
after the deoxidation adsorption unit is saturated in adsorption, stopping purification, and allowing the regeneration gas to enter the deoxidation adsorption unit through a regeneration unit for regeneration;
when the purification device is used for the first time or is not used for a long time and then is started, the catalytic oxidation unit is heated to the working temperature to discharge the waste gas CO2Introducing raw gas to sweep the catalytic oxidation unit and the deoxidation adsorption unit, and introducing the waste gas CO2Discharging the purified plant through an exhaust gas discharge branch;
the raw material gas is nitrogen to be purified, and the product gas is purified nitrogen;
the regeneration gas is hydrogen and nitrogen.
2. A nitrogen purification apparatus as claimed in claim 1, wherein: the raw material gas is nitrogen with the purity of 99.999 percent, and the product gas is nitrogen with the purity of more than or equal to 99.9999 percent;
the flow ratio of the regeneration gas hydrogen to the nitrogen is 1: 19-1: 24.
3. A nitrogen purification apparatus as claimed in claim 1, wherein: mixing hydrogen and nitrogen to prepare regenerated hydrogen-nitrogen mixed gas as regenerated gas, and placing the regenerated hydrogen-nitrogen mixed gas in a bottle group, wherein the volume fraction of the hydrogen in the regenerated hydrogen-nitrogen mixed gas is 4-5%.
4. A nitrogen purification apparatus as claimed in claim 1, wherein: the raw material gas is nitrogen with the purity of 99.999 percent, and the product gas is nitrogen with the purity of more than or equal to 99.9999 percent;
mixing hydrogen and nitrogen to prepare regenerated hydrogen-nitrogen mixed gas as regenerated gas, and placing the regenerated hydrogen-nitrogen mixed gas in a bottle group, wherein the volume fraction of the hydrogen in the regenerated hydrogen-nitrogen mixed gas is 4-5%.
5. A purification apparatus for nitrogen according to any one of claims 1 to 4, wherein: the catalytic oxidation unit comprises a raw material gas inlet valve (1), a first pressure gauge branch pipe, a first pressure gauge root valve (2), a first pressure gauge (3), a first flowmeter (4), a catalytic heat exchanger (5) and a catalytic oxidation device (6), wherein a catalytic oxidation agent is placed in the catalytic oxidation device (6);
the deoxidation adsorption unit comprises a first cooler (7), a first deoxidation adsorber air inlet valve (8), a second deoxidation adsorber air inlet valve (9) and a deoxidation adsorber (12);
the exhaust gas discharge branch comprises a second cooler (10) and an exhaust gas discharge valve (11);
the regeneration unit comprises a regeneration first valve (13), a second pressure gauge branch pipe, a second pressure gauge root valve (14), a second pressure gauge (15), a second flowmeter (16), a one-way valve (17) and a regeneration second valve (18);
the raw material gas is connected with a tube side inlet of a catalytic heat exchanger (5) through a pipeline, a tube side outlet of the catalytic heat exchanger (5) is connected with an inlet of a catalytic oxidation device (6) through a pipeline, an outlet of the catalytic oxidation device (6) is connected with a shell side inlet of the catalytic heat exchanger (5) through a pipeline, and a shell side outlet of the catalytic heat exchanger (5) is connected with an inlet of a deoxidation absorber (12) through a pipeline;
a raw material gas inlet valve (1), a first pressure gauge branch pipe and a first flowmeter (4) are sequentially arranged behind a raw material gas inlet on a pipeline for connecting the raw material gas with a tube pass inlet of a catalytic heat exchanger (5), the lower end of the first pressure gauge branch pipe is connected with the pipeline, the upper end of the first pressure gauge branch pipe is connected with a first pressure gauge (3), and a first pressure gauge root valve (2) is arranged on the first pressure gauge branch pipe below the first pressure gauge (3);
on a pipeline connecting the shell pass outlet of the catalytic heat exchanger (5) with the inlet of the deoxidation absorber (12), a first cooler (7), a first air inlet valve (8) of the deoxidation absorber, an exhaust gas discharge branch and a second air inlet valve (9) of the deoxidation absorber are sequentially arranged behind the shell pass outlet of the catalytic heat exchanger (5);
a second cooler (10) is arranged on the exhaust gas discharge branch, and an exhaust gas discharge valve (11) is arranged behind the second cooler (10);
the rear end of a pipeline connected with the outlet of the deoxidation absorber (12) is divided into two branches, one branch is a regeneration gas pipeline and is connected with a regeneration unit, the other branch is a product gas pipeline and is used for releasing product gas, and a product valve (19) is arranged on the other branch;
the regeneration gas is connected with the outlet of the deoxidation adsorber (12) through a regeneration gas pipeline, a regeneration first valve (13) is arranged behind the inlet of the regeneration hydrogen-nitrogen mixed gas on the regeneration gas pipeline, and a second pressure gauge branch pipe, a second flowmeter (16), a one-way valve (17) and a regeneration second valve (18) are sequentially arranged behind the regeneration gas pipeline; the lower end of the second pressure gauge branch pipe is connected with a regenerated gas pipeline, the upper end of the second pressure gauge branch pipe is connected with a second pressure gauge (15), and a second pressure gauge root valve (14) is arranged on the second pressure gauge branch pipe below the second pressure gauge (15).
6. A method for purifying nitrogen is characterized in that: the method is carried out by using a nitrogen purification device according to claim 5, and comprises the following steps:
closing the exhaust gas discharge valve (11) and the regeneration second valve (18); opening a raw material gas inlet valve (1), a first pressure gauge root valve (2), a first gas inlet valve (8) of a deoxidation adsorber, a second gas inlet valve (9) of the deoxidation adsorber and a product valve (19);
the raw gas is introduced into the purification device, and the raw gas passes through a raw gas inlet valve (1) and a first pressure gauge branch through a pipeline in sequence, and is purified by a first flowmeter (4), a catalytic heat exchanger (5) tube pass, a catalytic oxidizer (6), a catalytic heat exchanger (5) shell pass, a first cooler (7), a first deoxidation adsorber inlet valve (8), a second deoxidation adsorber inlet valve (9), a deoxidation adsorber (12) and a product valve (19) to obtain product gas.
7. A method for purifying nitrogen as claimed in claim 6, wherein: the working temperature of the catalytic heat exchanger (5) during purification is 330 ℃.
8. A method for purifying nitrogen as claimed in claim 6, wherein: after the deoxidation absorber (12) is detected to be saturated in adsorption, the deoxidation absorber (12) needs to be regenerated, and the steps are as follows:
raising the temperature of the deoxygenation adsorber (12) to a regeneration temperature, closing the product valve (19) and the deoxygenation adsorber first inlet valve (8); opening a regeneration first valve (13), a second pressure gauge root valve (14), a regeneration second valve (18) and an exhaust gas discharge valve (11); the regeneration gas is purged and then discharged through a regeneration first valve (13), a second pressure gauge branch, a second flowmeter (16), a one-way valve (17), a regeneration second valve (18), a deoxidation adsorber (12), a deoxidation adsorber second air inlet valve (9), a second cooler (10) and a waste gas discharge valve (11) in sequence; and after the regeneration is finished, stopping heating the deoxidation absorber (12), closing the first regeneration valve (13), opening the first air inlet valve (8) of the deoxidation absorber, replacing the regeneration gas with the feed gas, introducing the feed gas for purging, and purging the deoxidation absorber (12) to the normal temperature.
9. A method for purifying nitrogen as claimed in claim 8, wherein: the regeneration temperature of the deoxidation absorber (12) is 350 ℃, the regeneration gas pressure is 0.4MPa, and the flow rate is 3Nm3H, after 24h of regeneration, the regeneration gas is changed into the raw material gas and is introduced at the flow rate of 6Nm and 0.4MPa3Blow cooling for 3h to normal temperature.
10. A method for purifying nitrogen as claimed in claim 6, wherein: when the purification device is used for the first time or is not used for a long time and then is started, the waste gas CO released by the catalytic oxidizer (6) needs to be treated2Discharging, comprising the following steps:
closing a second air inlet valve (9) of the deoxidation adsorber, opening a raw material gas inlet valve (1), a first pressure gauge root valve (2), a first air inlet valve (8) of the deoxidation adsorber and an exhaust gas discharge valve (11); the temperature of the catalytic oxidizer (6) is raised to 330 DEG C-500 ℃; the method comprises the steps of sequentially purging a raw gas by a raw gas inlet valve (1), a first pressure gauge branch, a first flowmeter (4), a catalytic heat exchanger (5) tube pass, a catalytic oxidizer (6), a catalytic heat exchanger (5) shell pass, a first cooler (7), a deoxidation adsorber first inlet valve (8), a second cooler (10) and a waste gas discharge valve (11), and discharging waste gas CO2(ii) a After purging for 8h, sampling and detecting through an exhaust gas discharge valve (11) if CO is detected2Stopping purging when the concentration is less than or equal to 3 ppm.
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| CN1130361A (en) * | 1994-07-08 | 1996-09-04 | 乔治·克劳德方法的研究开发空气股份有限公司 | Method and apparatus for producing nitrogen by combined gas permeation and adsorption |
| CN1508064A (en) * | 2002-12-13 | 2004-06-30 | 中国石油化工股份有限公司巴陵分公司 | Method for preparing high-purity nitrogen gas |
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| CN206985709U (en) * | 2017-07-25 | 2018-02-09 | 大连中鼎化学有限公司 | A kind of ultra-pure oxygen, nitrogen purifying system |
| CN110282608A (en) * | 2019-07-18 | 2019-09-27 | 大连中鼎化学有限公司 | A kind of purification devices and its technique for nitrogen, oxygen, argon gas and helium |
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| CN1130361A (en) * | 1994-07-08 | 1996-09-04 | 乔治·克劳德方法的研究开发空气股份有限公司 | Method and apparatus for producing nitrogen by combined gas permeation and adsorption |
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