CN113562708A - Low-energy-consumption preparation method for argon and nitrogen gas - Google Patents
Low-energy-consumption preparation method for argon and nitrogen gas Download PDFInfo
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- CN113562708A CN113562708A CN202110929110.6A CN202110929110A CN113562708A CN 113562708 A CN113562708 A CN 113562708A CN 202110929110 A CN202110929110 A CN 202110929110A CN 113562708 A CN113562708 A CN 113562708A
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 title claims abstract description 134
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052786 argon Inorganic materials 0.000 title claims abstract description 67
- 229910001873 dinitrogen Inorganic materials 0.000 title claims abstract description 25
- 238000005265 energy consumption Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 131
- 239000007788 liquid Substances 0.000 claims abstract description 82
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 41
- 239000012528 membrane Substances 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 26
- 238000012360 testing method Methods 0.000 claims abstract description 25
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 238000003860 storage Methods 0.000 claims abstract description 16
- 238000009834 vaporization Methods 0.000 claims abstract description 8
- 230000008016 vaporization Effects 0.000 claims abstract description 8
- 239000006200 vaporizer Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims description 37
- 238000000746 purification Methods 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- 229960000892 attapulgite Drugs 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 239000005543 nano-size silicon particle Substances 0.000 claims description 10
- 239000002121 nanofiber Substances 0.000 claims description 10
- 229910052625 palygorskite Inorganic materials 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 229920013716 polyethylene resin Polymers 0.000 claims description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 7
- 239000011344 liquid material Substances 0.000 claims description 6
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920005548 perfluoropolymer Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
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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
- C01B23/00—Noble gases; Compounds thereof
- C01B23/001—Purification or separation processes of noble gases
- C01B23/0036—Physical processing only
- C01B23/0042—Physical processing only by making use of membranes
- C01B23/0047—Physical processing only by making use of membranes characterised by the membrane
-
- 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
- B01D53/22—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 diffusion
- B01D53/228—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 diffusion characterised by specific membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/26—Polyalkenes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
-
- 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
- C01B21/0433—Physical processing only
- C01B21/0438—Physical processing only by making use of membranes
- C01B21/0444—Physical processing only by making use of membranes characterised by the membrane
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C5/00—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/10—Nitrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/18—Noble gases
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2221/00—Handled fluid, in particular type of fluid
- F17C2221/01—Pure fluids
- F17C2221/014—Nitrogen
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2221/00—Handled fluid, in particular type of fluid
- F17C2221/01—Pure fluids
- F17C2221/016—Noble gases (Ar, Kr, Xe)
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
- F17C2223/01—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the phase
- F17C2223/0107—Single phase
- F17C2223/0123—Single phase gaseous, e.g. CNG, GNC
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- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
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Abstract
The invention discloses a low-energy-consumption preparation method for argon and nitrogen gas, which comprises the following steps: 1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen; 2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is loaded into a vacuum gas cylinder, and a composite membrane is arranged in a shell of the impurity remover; 3) carrying out qualification test on the gas filled in the vacuum gas cylinder, and sending the qualified gas to a warehouse for storage; the method for producing argon and nitrogen gas can meet the requirements of the market on argon and nitrogen gas, ensure the yield and realize the requirements on the purity of the argon and nitrogen gas, and ensure that the purity of the argon and nitrogen gas reaches more than 99.9996 percent.
Description
Technical Field
The invention relates to the technical field of argon and nitrogen gas processing, in particular to a low-energy-consumption preparation method for preparing argon and nitrogen gas.
Background
Because the air contains more argon and nitrogen, the gas is often used as protective gas, carrier gas, diluent gas, standard gas and the like to be widely applied to various industries of national economy. The following discussion is representative of argon, and the process techniques are applicable to other inert gases as well.
At present, the industrial purity is often more than or equal to 99.9-99.99% in the preparation process, the requirement of high purity cannot be met, the purity of high-purity gas is more than or equal to 99.999-99.9999%, and the preparation method of high purity is complex, high in cost and poor in stability.
Disclosure of Invention
The invention provides a low-energy-consumption preparation method for preparing argon and nitrogen gas.
The scheme of the invention is as follows:
a low-energy-consumption preparation method for preparing argon and nitrogen gases comprises the following steps:
1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen;
2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is put into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 6-12 parts of polyethylene glycol, 50-70 parts of polyethylene resin, 3-7 parts of a dispersing agent, 4-6 parts of nano silicon carbide, 3-8 parts of nano fibers, 3-6 parts of attapulgite and 2-4 parts of a coupling agent;
3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
The air inlet of the impurity remover is communicated with the air outlet of the purifier, one side of the impurity remover is provided with the air inlet, the other side of the impurity remover is provided with the air outlet, and the composite membrane can be arranged in the impurity remover between the air outlet and the air inlet.
Preferably, the liquid substance is liquid argon, and the purifier is an argon purification device.
Preferably, the liquid substance is liquid nitrogen, and the purifier is a nitrogen purification device.
As a preferable technical scheme, the purity detection in the step 2) is performed after the gas passing through the impurity remover is kept stand for 8 hours, and the detected purity is more than or equal to 99.9996%.
Preferably, the diaphragm compressor pressurizes 0-15 mpa within 6 hours.
Preferably, the step 2) is carried out after being put into a vacuum cylinder and standing for more than 8 hours until the step 3).
As a preferable technical scheme, the liquid substance is liquid argon, and an argon purity analyzer is used for testing the gas filled in the vacuum gas cylinder in the step 3); the liquid material is liquid nitrogen, and a nitrogen purity detector is used for testing the gas filled in the vacuum gas cylinder in the step 3).
As a preferable technical scheme, the gas filled in the vacuum gas cylinder is tested in the step 3) to reach the standard of 99.999%.
Because the preparation method for preparing argon and nitrogen gas with low energy consumption is adopted, 1) liquid with the purity of 99.99 percent in the low-temperature liquid storage tank is sent into the vaporizer for vaporization, and the vaporized gas is purified in the purifier; the liquid is one of liquid argon or liquid nitrogen; 2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is put into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 6-12 parts of polyethylene glycol, 50-70 parts of polyethylene resin, 3-7 parts of a dispersing agent, 4-6 parts of nano silicon carbide, 3-8 parts of nano fibers, 3-6 parts of attapulgite and 2-4 parts of a coupling agent; 3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
The invention has the advantages that:
the method for producing argon and nitrogen gas can meet the requirements of the market on argon and nitrogen gas, ensure the yield and realize the requirements on the purity of the argon and nitrogen gas, and ensure that the purity of the argon and nitrogen gas reaches more than 99.9996 percent. The invention fully considers various factors to realize the preparation of high-purity argon and nitrogen gas, and realizes the operation with simple, stable, high-efficiency and low energy consumption.
Drawings
FIG. 1 is a flow chart of an embodiment of the present invention.
Detailed Description
In order to make up for the above deficiencies, the invention provides a preparation method for preparing argon and nitrogen gas with low energy consumption so as to solve the problems in the background art.
A low-energy-consumption preparation method for preparing argon and nitrogen gases comprises the following steps:
1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen;
2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is put into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 6-12 parts of polyethylene glycol, 50-70 parts of polyethylene resin, 3-7 parts of a dispersing agent, 4-6 parts of nano silicon carbide, 3-8 parts of nano fibers, 3-6 parts of attapulgite and 2-4 parts of a coupling agent;
3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
The liquid matter is liquid argon, and the purifier is an argon purification device.
The liquid state matter is liquid nitrogen, and the purifier is a nitrogen purification device.
And the purity detection in the step 2) is carried out after the gas passing through the impurity remover is kept stand for 8 hours, and the detected purity is more than or equal to 99.9996%.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
The liquid substance is liquid argon, and an argon purity analyzer is used for testing the gas filled in the vacuum gas cylinder in the step 3); the liquid material is liquid nitrogen, and a nitrogen purity detector is used for testing the gas filled in the vacuum gas cylinder in the step 3).
And 3) testing the gas filled in the vacuum gas cylinder in the step 3) until the standard reaches 99.999%.
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1:
1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen;
2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is loaded into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 12 parts of polyethylene glycol, 70 parts of polyethylene resin, 7 parts of a dispersing agent, 6 parts of nano silicon carbide, 8 parts of nano fibers, 6 parts of attapulgite and 4 parts of a coupling agent;
3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
The preparation method of the base film comprises the following steps: respectively grinding 70 parts by weight of polyethylene resin into powder with a preset particle size, adding 6 parts by weight of nano silicon carbide, 8 parts by weight of nano fibers and 6 parts by weight of attapulgite, stirring at the speed of 40-70 r/min for 1h to obtain a mixed material, and then adding 12 parts by weight of polyethylene glycol, 7 parts by weight of a dispersing agent and 4 parts by weight of an even chain; stirring the mixture for 30 minutes at the speed of 50-80 r/min, feeding the mixture into a film making machine to obtain a raw material, and passing the raw material through a stretching machine to obtain a base film;
preparing a separation layer solution: dissolving particles of the perfluoropolymer in a perfluorosolvent to prepare a separation layer solution with the concentration of 0.5-3 wt%, and then standing and defoaming for 1-4 h;
preparing a composite membrane: coating a separation layer on the obtained base film easily, and drying in the shade at room temperature for 20-240 min; heating at 40-120 ℃ for 5-240 min to obtain a preliminary composite film;
and step two, soaking the preliminary composite film in deionized water at the temperature of 50-90 ℃ for 1-24 h, and airing to obtain the composite film.
The liquid matter is liquid argon, the purifier is an argon purification device, and the argon purification device is an RZ-YA-35C type argon purification device of Swiss gas purification Hubei Limited.
The liquid substance is liquid nitrogen, the purifier is a nitrogen purification device, and the nitrogen purification device is an RZ-DYC-20 type nitrogen purification device of Rezee gas purification Hubei Limited company.
And the purity detection in the step 2) is carried out after the gas passing through the impurity remover is kept stand for 8 hours, and the detected purity is more than or equal to 99.9996%.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
The liquid substance is liquid argon, and an argon purity analyzer is used for testing the gas filled in the vacuum gas cylinder in the step 3); the liquid material is liquid nitrogen, and a nitrogen purity detector is used for testing the gas filled in the vacuum gas cylinder in the step 3).
And 3) testing the gas filled in the vacuum gas cylinder in the step 3) until the standard reaches 99.999%.
Example 2:
1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen;
2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is loaded into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 6 parts of polyethylene glycol, 50 parts of polyethylene resin, 3 parts of a dispersing agent, 4 parts of nano silicon carbide, 3 parts of nano fibers, 3 parts of attapulgite and 2 parts of a coupling agent;
3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
The preparation method of the base film comprises the following steps: respectively grinding 50 parts by weight of polyethylene resin into powder with a preset particle size, adding 4 parts by weight of nano silicon carbide, 3 parts by weight of nano fibers and 3 parts by weight of attapulgite, stirring at the speed of 40-70 r/min for 1h to obtain a mixed material, and then adding 6 parts by weight of polyethylene glycol, 3 parts by weight of a dispersing agent and 2 parts by weight of an even chain; stirring the mixture for 30 minutes at the speed of 50-80 r/min, feeding the mixture into a film making machine to obtain a raw material, and passing the raw material through a stretching machine to obtain a base film;
preparing a separation layer solution: dissolving particles of the perfluoropolymer in a perfluorosolvent to prepare a separation layer solution with the concentration of 0.5-3 wt%, and then standing and defoaming for 1-4 h;
preparing a composite membrane: coating a separation layer on the obtained base film easily, and drying in the shade at room temperature for 20-240 min; heating at 40-120 ℃ for 5-240 min to obtain a preliminary composite film;
and step two, soaking the preliminary composite film in deionized water at the temperature of 50-90 ℃ for 1-24 h, and airing to obtain the composite film.
The liquid matter is liquid argon, the purifier is an argon purification device, and the argon purification device is an RZ-YA-35C type argon purification device of Swiss gas purification Hubei Limited.
The liquid substance is liquid nitrogen, the purifier is a nitrogen purification device, and the nitrogen purification device is an RZ-DYC-20 type nitrogen purification device of Rezee gas purification Hubei Limited company.
And the purity detection in the step 2) is carried out after the gas passing through the impurity remover is kept stand for 8 hours, and the detected purity is more than or equal to 99.9996%.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
The liquid substance is liquid argon, and an argon purity analyzer is used for testing the gas filled in the vacuum gas cylinder in the step 3); the liquid material is liquid nitrogen, and a nitrogen purity detector is used for testing the gas filled in the vacuum gas cylinder in the step 3).
And 3) testing the gas filled in the vacuum gas cylinder in the step 3) until the standard reaches 99.999%.
Example 3:
1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen;
2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is loaded into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 10 parts of polyethylene glycol, 60 parts of polyethylene resin, 5 parts of a dispersing agent, 5 parts of nano silicon carbide, 4 parts of nano fibers, 4 parts of attapulgite and 2 parts of a coupling agent;
3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
The preparation method of the base film comprises the following steps: respectively grinding 60 parts by weight of polyethylene resin into powder with a preset particle size, adding 5 parts by weight of nano silicon carbide, 4 parts by weight of nano fibers and 4 parts by weight of attapulgite, stirring at the speed of 40-70 r/min for 1h to obtain a mixed material, and then adding 10 parts by weight of polyethylene glycol, 5 parts by weight of a dispersing agent and 2 parts by weight of an even chain; stirring the mixture for 30 minutes at the speed of 50-80 r/min, feeding the mixture into a film making machine to obtain a raw material, and passing the raw material through a stretching machine to obtain a base film;
preparing a separation layer solution: dissolving particles of the perfluoropolymer in a perfluorosolvent to prepare a separation layer solution with the concentration of 0.5-3 wt%, and then standing and defoaming for 1-4 h;
preparing a composite membrane: coating a separation layer on the obtained base film easily, and drying in the shade at room temperature for 20-240 min; heating at 40-120 ℃ for 5-240 min to obtain a preliminary composite film;
and step two, soaking the preliminary composite film in deionized water at the temperature of 50-90 ℃ for 1-24 h, and airing to obtain the composite film.
The liquid matter is liquid argon, the purifier is an argon purification device, and the argon purification device is an RZ-YA-35C type argon purification device of Swiss gas purification Hubei Limited.
The liquid substance is liquid nitrogen, the purifier is a nitrogen purification device, and the nitrogen purification device is an RZ-DYC-20 type nitrogen purification device of Rezee gas purification Hubei Limited company.
And the purity detection in the step 2) is carried out after the gas passing through the impurity remover is kept stand for 8 hours, and the detected purity is more than or equal to 99.9996%.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
The liquid substance is liquid argon, and an argon purity analyzer is used for testing the gas filled in the vacuum gas cylinder in the step 3); the liquid material is liquid nitrogen, and a nitrogen purity detector is used for testing the gas filled in the vacuum gas cylinder in the step 3).
And 3) testing the gas filled in the vacuum gas cylinder in the step 3) until the standard reaches 99.999%.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation method for preparing argon and nitrogen gas with low energy consumption is characterized by comprising the following steps:
1) sending the liquid with the purity of 99.99 percent in the low-temperature liquid storage tank into a vaporizer for vaporization, and purifying the vaporized gas in a purifier; the liquid is one of liquid argon or liquid nitrogen;
2) the gas treated by the purifier passes through an impurity remover and then is subjected to purity detection, the gas is sent to a diaphragm compressor after the purity detection is qualified, the gas is pressurized at 0-15 mpa and is put into a vacuum gas cylinder, a composite membrane is arranged in a shell of the impurity remover, the separation membrane comprises a base membrane and an effective separation layer, the effective separation layer is a copolymer of tetrafluoroethylene and a perfluorinated solvent, the thickness of the effective separation layer is 0.1-0.5 mu m, and the base membrane comprises 6-12 parts of polyethylene glycol, 50-70 parts of polyethylene resin, 3-7 parts of a dispersing agent, 4-6 parts of nano silicon carbide, 3-8 parts of nano fibers, 3-6 parts of attapulgite and 2-4 parts of a coupling agent;
3) and (5) carrying out qualified test on the gas filled in the vacuum gas cylinder, and sending the gas to a warehouse for storage after the gas is qualified.
2. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: the liquid matter is liquid argon, and the purifier is an argon purification device.
3. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: the liquid state matter is liquid nitrogen, and the purifier is a nitrogen purification device.
4. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: and the purity detection in the step 2) is carried out after the gas passing through the impurity remover is kept stand for 8 hours, and the detected purity is more than or equal to 99.9996%.
5. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: the diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
6. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
7. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: the liquid substance is liquid argon, and an argon purity analyzer is used for testing the gas filled in the vacuum gas cylinder in the step 3); the liquid material is liquid nitrogen, and a nitrogen purity detector is used for testing the gas filled in the vacuum gas cylinder in the step 3).
8. The method for preparing argon and nitrogen gas with low energy consumption as claimed in claim 1, wherein: and 3) testing the gas filled in the vacuum gas cylinder in the step 3) until the standard reaches 99.999%.
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