CN104108685B - The recycling reutilization technology of electrical network sulfur hexafluoride - Google Patents
The recycling reutilization technology of electrical network sulfur hexafluoride Download PDFInfo
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- CN104108685B CN104108685B CN201410355225.9A CN201410355225A CN104108685B CN 104108685 B CN104108685 B CN 104108685B CN 201410355225 A CN201410355225 A CN 201410355225A CN 104108685 B CN104108685 B CN 104108685B
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- 229910018503 SF6 Inorganic materials 0.000 title claims abstract description 239
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title claims abstract description 239
- 229960000909 sulfur hexafluoride Drugs 0.000 title claims abstract description 239
- 238000005516 engineering process Methods 0.000 title description 3
- 238000004064 recycling Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 162
- 238000001179 sorption measurement Methods 0.000 claims abstract description 141
- 239000012535 impurity Substances 0.000 claims abstract description 129
- 239000013067 intermediate product Substances 0.000 claims abstract description 122
- 238000007233 catalytic pyrolysis Methods 0.000 claims abstract description 68
- 238000000746 purification Methods 0.000 claims abstract description 43
- 238000007781 pre-processing Methods 0.000 claims abstract description 31
- 238000002203 pretreatment Methods 0.000 claims abstract description 10
- 239000003463 adsorbent Substances 0.000 claims description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 72
- 238000010521 absorption reaction Methods 0.000 claims description 62
- 238000005406 washing Methods 0.000 claims description 36
- 238000004140 cleaning Methods 0.000 claims description 32
- 239000003513 alkali Substances 0.000 claims description 29
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 20
- 230000002378 acidificating effect Effects 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 claims description 8
- WZJQNLGQTOCWDS-UHFFFAOYSA-K cobalt(iii) fluoride Chemical compound F[Co](F)F WZJQNLGQTOCWDS-UHFFFAOYSA-K 0.000 claims description 8
- 150000003464 sulfur compounds Chemical class 0.000 claims description 8
- 238000011084 recovery Methods 0.000 abstract description 26
- 230000009102 absorption Effects 0.000 description 57
- 239000002594 sorbent Substances 0.000 description 57
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 53
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 52
- 229910052731 fluorine Inorganic materials 0.000 description 52
- 239000011737 fluorine Substances 0.000 description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 35
- 239000000741 silica gel Substances 0.000 description 35
- 229910002027 silica gel Inorganic materials 0.000 description 35
- 239000000047 product Substances 0.000 description 34
- 239000002808 molecular sieve Substances 0.000 description 27
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 27
- 239000007788 liquid Substances 0.000 description 25
- 239000000463 material Substances 0.000 description 18
- 238000004821 distillation Methods 0.000 description 17
- 239000003518 caustics Substances 0.000 description 16
- 238000009833 condensation Methods 0.000 description 15
- 230000005494 condensation Effects 0.000 description 15
- 230000003213 activating effect Effects 0.000 description 13
- 230000020335 dealkylation Effects 0.000 description 13
- 238000006900 dealkylation reaction Methods 0.000 description 13
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 12
- 230000001105 regulatory effect Effects 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000003795 desorption Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 239000003507 refrigerant Substances 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- SIHSYLXYARNLCD-UHFFFAOYSA-N [O].[F].[S] Chemical compound [O].[F].[S] SIHSYLXYARNLCD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 208000011117 substance-related disease Diseases 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a kind of method reclaiming sulfur hexafluoride, comprise the following steps: the sulfur hexafluoride containing impurity is carried out pre-treatment, obtain the first intermediate product; Described first intermediate product is carried out catalytic pyrolysis, obtains the second intermediate product; Described second intermediate product is carried out purifying treatment, obtains the 3rd intermediate product; Described 3rd intermediate product is carried out pressure-variable adsorption process, obtains the 4th intermediate product; Described 4th intermediate product is carried out rectification process, obtains sulfur hexafluoride.The invention provides a kind of device reclaiming sulfur hexafluoride, comprising: pre-processing device; The catalytic pyrolysis equipment be connected with described pre-processing device; The purification apparatus be connected with described catalytic pyrolysis equipment; The variable-pressure adsorption equipment be connected with described purification apparatus; The rectifying device be connected with described variable-pressure adsorption equipment.The method and apparatus of recovery sulfur hexafluoride provided by the invention can reclaim and obtain the good sulfur hexafluoride of quality.
Description
Technical field
The present invention relates to recycling technical field, particularly relate to a kind of method and apparatus reclaiming sulfur hexafluoride.
Background technology
Sulfur hexafluoride is that France two chemist Moissan and Lebeau are in the artificial rare gas element of synthesis in 1900.Sulfur hexafluoride is a kind of strong electronegativity gas, and the tendency catching unbound electron is very strong.Pure sulfur hexafluoride is unreactiveness, by thermally-stabilised under normal temperature; At the temperature of 20 DEG C, 10 times that the high insulation resistance of sulfur hexafluoride is 3 times of air, high arc extinguishing ability is air, high heat conductance is air 2 times.Current, sulfur hexafluoride is mainly used in power industry, as the insulation of electric installation and/or arc extinguishing; For the preparation of sulfur hexafluoride breaker and gas-insulated switchgear (GISGasInsulatedSwitchgear); For the preparation of sulfur hexafluoride loading switch equipment; For the preparation of six-component force balance transmission of electricity pipeline; For the preparation of sulfur hexafluoride transformer and six-component force balance substation.Especially, sulfur hexafluoride has a wide range of applications in high pressure field of electrical equipment.
Run on containing plurality of impurities in the sulfur hexafluoride in electric installation, these impurity portion are from the impurity be mixed in sulfur hexafluoride synthesis preparation process; Part is run and sulfur hexafluoride degradation production at high temperature in failure process from equipment, and the by product that sulfur hexafluoride contact reacts material produces.Mainly contain air, water, oil in sulfur hexafluoride after using, fluoridize sulfurous acid, hydrofluoric acid, CF
4, C
2f
6, C
3f
8, CO
2, CO, CH
4, SO
2f
2, SOF
2, S
2oF
10and SO
2deng impurity.The existence of moisture, can reduce the medium recovery strength of sulfur hexafluoride, thus reduces the insulation characterisitic of equipment; Fluoridize sulfurous acid and hydrofluoric acid has severe toxicity, and can corrosion target and insulating material; Fluorocarbon can produce simple substance carbon at equipment surface carbon distribution, reduces the insulating property of equipment; Fluoridize the harm that to cause after sulfonyl enters air human body and environment; Impurity in sulfur hexafluoride harm for the operation of equipment and the security presence of environment; Sulfur hexafluoride Greenhouse effect are very big, do not process directly discharge serious harm living environment.Therefore cycle detection is carried out to the sulfur hexafluoride run, underproof sulfur hexafluoride is carried out recycle very necessary.
Application number is that the Chinese patent of 03153158.X discloses a kind of method and apparatus reclaiming sulfur hexafluoride from power distribution unit, said method comprising the steps of: 1), use adsorption unit that the sulfur hexafluoride in power distribution unit and the mixed gas that comprises its resolvent are carried out adsorption treatment, the resolvent of the sulfur hexafluoride in mixed gas is adsorbed, the mixed gas reduced with the concentration forming pure sulfur hexafluoride or sulfur hexafluoride decomposer; 2), to step 1) described in gas mixture carry out liquefaction processing, to obtain liquid sulfur hexafluoride; 3), step 2 is made) the liquid sulfur hexafluoride evaporation that obtains, obtain pure sulfur hexafluoride.The recovery method of this sulfur hexafluoride that prior art provides, the quality reclaiming the sulfur hexafluoride obtained can only reach the standard of GB/T12022-2006 " industrial sulfur hexafluoride ".
Summary of the invention
In view of this, the object of the present invention is to provide a kind of method and apparatus reclaiming sulfur hexafluoride, method provided by the invention can reclaim and obtain the good sulfur hexafluoride of quality.
The invention provides a kind of method reclaiming sulfur hexafluoride, comprise the following steps:
1), by the sulfur hexafluoride containing impurity carry out pre-treatment, remove containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product;
2), by described first intermediate product carry out catalytic pyrolysis, obtain the second intermediate product; The catalyzer of described catalytic pyrolysis is cobaltic fluoride;
3), by described second intermediate product carry out purifying treatment, remove the sulfur compound impurities in described second intermediate product, obtain the 3rd intermediate product;
4), by described 3rd intermediate product carry out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product;
5), by described 4th intermediate product carry out rectification process, remove the air in described 4th intermediate product and fluorocarbons impurities, obtain sulfur hexafluoride.
Preferably, described step 2) in the temperature of catalytic pyrolysis be 300 DEG C ~ 400 DEG C.
Preferably, described step 3) in purifying treatment comprise washing process and alkali cleaning process.
Preferably, described step 4) in pressure-variable adsorption process comprise low pressure adsorbent and High Pressure Absorption; The pressure of described low pressure adsorbent is 0.1MPa ~ 0.5MPa, removes the water in described 3rd intermediate product;
The pressure of described High Pressure Absorption is 2MPa ~ 5MPa; Remove the fluorochemical in described 3rd intermediate product and oil.
Preferably, described step 5) in rectification process comprise the first rectification process and the second rectification process, the pressure of described first rectification process is 1MPa ~ 5MPa, removes the air in described 4th intermediate product;
The pressure of described second rectification process is 0.5MPa ~ 1.6MPa, removes the fluorocarbon in described 4th intermediate product.
The invention provides a kind of device reclaiming sulfur hexafluoride, comprising:
Pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity;
The catalytic pyrolysis equipment be connected with described pre-processing device;
The purification apparatus be connected with described catalytic pyrolysis equipment, described purification apparatus is for removing containing the sulfocompound in the sulfur hexafluoride of impurity;
The variable-pressure adsorption equipment be connected with described purification apparatus, described variable-pressure adsorption equipment is for removing containing the water in the sulfur hexafluoride of impurity, fluorochemical and oil;
The rectifying device be connected with described variable-pressure adsorption equipment, described rectifying device is for removing containing the air in the sulfur hexafluoride of impurity and fluorocarbon.
Preferably, described pre-processing device comprises:
Acid adsorption tower,
The oil strainer be connected with described sour adsorption tower,
The drying adsorption tower be connected with described oil strainer, described drying adsorption tower is connected with described catalytic pyrolysis equipment.
Preferably, described purification apparatus comprises:
The washing equipment be connected with described catalytic pyrolysis equipment;
The alkali cleaning equipment that one end is connected with described washing equipment, the other end of described alkali cleaning equipment is connected with described variable-pressure adsorption equipment.
Preferably, described variable-pressure adsorption equipment comprises:
The low pressure adsorbent equipment be connected with described purification apparatus, described low pressure adsorbent equipment is for removing containing the water in the sulfur hexafluoride of impurity;
The High Pressure Absorption equipment of one end and described low pressure adsorbent equipment connection, described High Pressure Absorption equipment is for removing containing the fluorochemical in the sulfur hexafluoride of impurity and oil, and the other end of described High Pressure Absorption equipment is connected with described rectifying device.
Preferably, described rectifying device comprises:
The light point tower be connected with described variable-pressure adsorption equipment, described light point of tower is for removing containing the air in the sulfur hexafluoride of impurity;
The Chong Fenta be connected with described light point of tower, described heavy point of tower is for removing containing the fluorocarbon in the sulfur hexafluoride of impurity.
The invention provides a kind of method reclaiming sulfur hexafluoride, comprise the following steps: 1), by the sulfur hexafluoride containing impurity carry out pre-treatment, remove containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product; 2), by described first intermediate product carry out catalytic pyrolysis, obtain the second intermediate product; The catalyzer of described catalytic pyrolysis is cobaltic fluoride; 3), by described second intermediate product carry out purifying treatment, remove the sulfur compound impurities in described second intermediate product, obtain the 3rd intermediate product; 4), by described 3rd intermediate product carry out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product; 5), by described 4th intermediate product carry out rectification process, remove the air in described 4th intermediate product and fluorocarbons impurities, obtain sulfur hexafluoride.The method of this recovery sulfur hexafluoride provided by the invention, adopts the technique of first catalytic pyrolysis, again purifying treatment, can reclaim and obtain the good sulfur hexafluoride of quality.
The invention provides a kind of device reclaiming sulfur hexafluoride, comprising: pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity; The catalytic pyrolysis equipment be connected with described pre-processing device; The purification apparatus be connected with described catalytic pyrolysis equipment, described purification apparatus is for removing containing the sulfocompound in the sulfur hexafluoride of impurity; The variable-pressure adsorption equipment be connected with described purification apparatus, described variable-pressure adsorption equipment is for removing containing the water in the sulfur hexafluoride of impurity, fluorochemical and oil; The rectifying device be connected with described variable-pressure adsorption equipment, described rectifying device is for removing containing the air in the sulfur hexafluoride of impurity and fluorocarbon.The device of recovery sulfur hexafluoride provided by the invention, makes the sulfur hexafluoride containing impurity be introduced into catalytic pyrolysis equipment, then enters purification apparatus, adopts device provided by the invention to reclaim and obtains the good sulfur hexafluoride of quality.
Experimental result shows, adopts method and apparatus provided by the invention to reclaim the sulfur hexafluoride after using, and reclaims the standard of quality higher than GB/T12022-2006 " industrial sulfur hexafluoride " of the sulfur hexafluoride obtained.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only embodiments of the invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to the accompanying drawing provided.
The schema of the recovery sulfur hexafluoride method that Fig. 1 provides for the embodiment of the present invention;
The structural representation of the recovery sulfur hexafluoride device that Fig. 2 provides for the embodiment of the present invention;
The structural representation of the pre-processing device that Fig. 3 provides for the embodiment of the present invention;
The structural representation of the catalytic pyrolysis equipment that Fig. 4 provides for the embodiment of the present invention and purification apparatus;
The structural representation of the variable-pressure adsorption equipment that Fig. 5 provides for the embodiment of the present invention and rectifying device.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of method reclaiming sulfur hexafluoride, comprise the following steps:
1), by the sulfur hexafluoride containing impurity carry out pre-treatment, remove containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product;
2), by described first intermediate product carry out catalytic pyrolysis, obtain the second intermediate product; The catalyzer of described catalytic pyrolysis is cobaltic fluoride;
3), by described second intermediate product carry out purifying treatment, remove the sulfur compound impurities in described second intermediate product, obtain the 3rd intermediate product;
4), by described 3rd intermediate product carry out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product;
5), by described 4th intermediate product carry out rectification process, remove the air in described 4th intermediate product and fluorocarbons impurities, obtain sulfur hexafluoride.
The method of this recovery sulfur hexafluoride provided by the invention, adopts the technique of first catalytic pyrolysis, again purifying treatment, can reclaim and obtain the good sulfur hexafluoride of quality.
The schema of the recovery sulfur hexafluoride method that Fig. 1 provides for the embodiment of the present invention, reclaims sulfur hexafluoride according to the schema shown in Fig. 1, comprises the following steps:
Sulfur hexafluoride containing impurity is carried out pre-treatment, removes containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product.In the present invention, the described sulfur hexafluoride containing impurity is the sulfur hexafluoride after using.In the present invention, the impurity in the described sulfur hexafluoride containing impurity preferably includes air, water, oil, HF, S
2f
10, SF
4, SF
2, S
2f
2, H
2s, CF
4, C
2f
6, C
3f
8, CO
2, CO, CH
4, SO
2f
2, SOF
2, S
2oF
10and SO
2in one or more.In the present invention, described air is preferably 300ppm ~ 400ppm described containing the mass content in the sulfur hexafluoride of impurity, is more preferably 320ppm ~ 380ppm, most preferably is 340ppm ~ 360ppm.In the present invention, described CF
4be preferably 5ppm ~ 15ppm described containing the mass content in the sulfur hexafluoride of impurity, be more preferably 8ppm ~ 12pmm, most preferably be 10ppm.In the present invention, described C
2f
6be preferably 450ppm ~ 550ppm described containing the mass content in the sulfur hexafluoride of impurity, be more preferably 470ppm ~ 530ppm, most preferably be 480ppm ~ 500ppm.In the present invention, described C
2f
6described containing the preferred 200ppm ~ 300ppm of mass content in the sulfur hexafluoride of impurity, be more preferably 220ppm ~ 280ppm, most preferably be 240ppm ~ 260ppm.
In the present invention, described CO
2described containing the preferred 20ppm ~ 60ppm of mass content in the sulfur hexafluoride of impurity, be more preferably 30ppm ~ 50ppm, most preferably be 35ppm ~ 45ppm.In the present invention, described CO containing the preferred 4ppm ~ 10ppm of mass content in the sulfur hexafluoride of impurity described, be more preferably 5ppm ~ 8ppm, most preferably be 6ppm ~ 7ppm.In the present invention, described CH
4be preferably 0.1ppm ~ 0.5ppm described containing the mass content in the sulfur hexafluoride of impurity, be more preferably 0.2ppm ~ 0.4ppm, most preferably be 0.1ppm.In the present invention, described SO
2f
2and SOF
2the mass content of total mass in the described sulfur hexafluoride containing impurity be preferably 20ppm ~ 50ppm, be more preferably 30ppm ~ 40ppm, most preferably be 35ppm ~ 45ppm.In the present invention, described S
2oF
10be preferably 150ppm ~ 250ppm described containing the mass content in the sulfur hexafluoride of impurity, be more preferably 160ppm ~ 220ppm, most preferably be 170ppm ~ 200ppm.In the present invention, described SO
2be preferably 0.5ppm ~ 3ppm described containing the mass content in the sulfur hexafluoride of impurity, be more preferably 1ppm ~ 2.5ppm, most preferably be 1.5ppm ~ 2ppm.
The source of the present invention to the described sulfur hexafluoride containing impurity does not have special restriction, and those skilled in the art obtain, as collected the sulfur hexafluoride run in gas-insulated switchgear by collecting the sulfur hexafluoride after using.
Sulfur hexafluoride containing impurity is preferably carried out acid absorption by the present invention successively, oil filters and water absorption, obtains the first intermediate product.The present invention, by carrying out acid absorption, can remove the partially acidic material in described impure sulfur hexafluoride, as HF and SO
2.The present invention does not have special restriction to the kind of the sorbent material of described acid absorption and source, adopts the sorbent material that can be used for adsorber acid well known to those skilled in the art, can be bought obtain by market.In the present invention, the sorbent material of described acid absorption is preferably activated alumina.In an embodiment of the present invention, the sorbent material of described acid absorption can be the spherical adsorbent of BASFEngeihardF-200 model.In the present invention, the pressure of described acid absorption is preferably-0.04MPa ~-0.08MPa, is more preferably-0.05MPa ~-0.07MPa, most preferably is-0.06MPa.
The present invention filters by carrying out oil, can remove the part oil in described impure sulfur hexafluoride.In the present invention, the effect that described oil filters preferably makes the mass content of oil in the impure sulfur hexafluoride after filtration be 0.002ppm ~ 0.005ppm, is more preferably 0.003ppm ~ 0.004ppm.The present invention preferably adopts active carbon filter core to filter oil.In the present invention, the structure optimization of described active carbon filter core comprises one or more in boron silicate layer of fibers, glass layer, activated carbon fiber layers, non-woven cloth layer and stainless steel layer, more preferably comprises boron silicate layer of fibers, glass layer, activated carbon fiber layers, non-woven cloth layer and stainless steel layer.In the present invention, the structure optimization of described active carbon filter core comprises multilayer non-woven cloth layer.The source of the present invention to described active carbon filter core does not have special restriction, can be bought obtain by market.In the present invention, the pressure of described filter oil is preferably-0.04MPa ~-0.08MPa, is more preferably-0.05MPa ~-0.07MPa, most preferably is-0.06MPa.
The present invention, by carrying out water absorption, can remove the part water in described impure sulfur hexafluoride.The present invention does not have special restriction to the kind of the sorbent material that described water adsorbs and source, adopts siccative well known to those skilled in the art, can be bought obtain by market.In the present invention, the sorbent material of described water absorption is preferably silica gel, aluminium sesquioxide and 13X molecular sieve, is more preferably silica gel.In the present invention, the pressure of described water absorption is preferably-0.04MPa ~-0.08MPa, is more preferably-0.05MPa ~-0.07MPa, most preferably is-0.06MPa.
After obtaining the first intermediate product, described first intermediate product is carried out catalytic pyrolysis by the present invention, obtains the second intermediate product, and the catalyzer of described catalytic pyrolysis is cobaltic fluoride.In the present invention, the high price sulfocompound in described first intermediate product, as S
2f
10, SF
4, SF
2, S
2f
2, S
2oF
10and H
2s carries out catalytic pyrolysis under the effect of cobaltrichloride, changes sulfur hexafluoride and low price sulfocompound into.In the present invention, the temperature of described catalytic pyrolysis is preferably 300 DEG C ~ 400 DEG C, is more preferably 320 DEG C ~ 380 DEG C, most preferably is 340 DEG C ~ 360 DEG C, is the most preferably 350 DEG C.In the present invention, the pressure of described catalytic pyrolysis is preferably 100KPa ~ 101KPa.
After obtaining the second intermediate product, described second intermediate product is carried out purifying treatment by the present invention, removes the sulfur compound impurities in described second intermediate product, obtains the 3rd intermediate product.In the present invention, the low price sulfocompound of described sulfur compound impurities for obtaining after catalytic pyrolysis described in technique scheme, as SF
2, SF
4, S
2f
2and SOF
4.In the present invention, described purifying treatment preferably includes washing process and alkali cleaning process.Described second intermediate product is preferably first carried out washing process by the present invention, then carries out alkali cleaning process, obtains the 3rd intermediate product.In the present invention, described low price sulfocompound is hydrolyzed to fluorine sulphur oxygen species, as SOF by washing process
2and SO
2f
2, fluorine sulphur oxygen species obtains acid, as SO through being hydrolyzed further
2, HF, H
2sO
3; The acid obtained is removed by alkali cleaning.
The method of the present invention to described washing does not have special restriction, adopts water-washing technique scheme well known to those skilled in the art, described second intermediate product and water is mixed.In the present invention, the number of times of described washing is preferably 3 times ~ 8 times, is more preferably 4 times ~ 6 times, most preferably is 5 times.The method of the present invention to described alkali cleaning does not have special restriction, adopts alkali cleaning technical scheme well known to those skilled in the art, described second intermediate product and alkaline aqueous solution is mixed.In the present invention, the number of times of described alkali cleaning is preferably 3 times ~ 8 times, is more preferably 4 times ~ 7 times, most preferably is 6 times.The present invention does not have special restriction to the kind of alkali in described alkaline aqueous solution, adopts basic cpd well known to those skilled in the art.In the present invention, described basic cpd does not produce the material of insolubles after preferably making described second intermediate product alkali cleaning.In the present invention, described basic cpd is preferably potassium hydroxide.The mass concentration of the present invention to described alkaline aqueous solution does not have special restriction, meets actually operating condition.
After obtaining the 3rd intermediate product, described 3rd intermediate product is carried out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product.In the present invention, described pressure-variable adsorption process preferably includes low pressure adsorbent and High Pressure Absorption, and the pressure of described low pressure adsorbent is 0.1MPa ~ 0.3MPa, removes the water impurity in described 3rd intermediate product; The pressure of described High Pressure Absorption is 2.5MPa ~ 3.5MPa, removes the oil in described 3rd intermediate product and fluorochemical.In the present invention, the pressure of described low pressure adsorbent is more preferably 0.15MPa ~ 0.25MPa, most preferably is 0.2MPa.In the present invention, the temperature of described low pressure adsorbent is preferably 20 DEG C ~ 30 DEG C, is more preferably 22 DEG C ~ 28 DEG C, most preferably is 24 DEG C ~ 26 DEG C.In the present invention, the sorbent material of described low pressure adsorbent is preferably one or more in silica gel, activated alumina and fluorine sorbent material, is more preferably silica gel, activated alumina and fluorine sorbent material.The source of the present invention to described silica gel, activated alumina and fluorine sorbent material does not have special restriction, can be bought obtain by market.In an embodiment of the present invention, described fluorine sorbent material can be the fluorine sorbent material of F-03 model, also can be the fluorine sorbent material of KDHF-03 model.
The present invention preferably uses silica gel to carry out low pressure adsorbent to described 3rd intermediate product; Activated alumina is used to carry out low pressure adsorbent the product obtained after silica gel adsorption; The product obtained after being adsorbed by activated alumina uses fluorine sorbent material to carry out low pressure adsorbent, to remove the water impurity in described 3rd intermediate product.In the present invention, the number of times of described silica gel low pressure adsorbent is preferably 2 times ~ 4 times, is more preferably 3 times.In the present invention, the preferred < 800ppm of mass content of the water in products obtained after described silica gel adsorption.In the present invention, the number of times of described activated alumina low pressure adsorbent is preferably 1 time ~ 3 times, most preferably is 2 times.In the present invention, the preferred < 200ppm of mass content of the water in products obtained after described activated alumina absorption.In the present invention, the number of times of described fluorine sorbent material low pressure adsorbent is preferably 1 time.In the present invention, the preferred < 30ppm of mass content of water in described 4th intermediate product.
In the present invention, described silica gel low pressure adsorbent, activated alumina low pressure adsorbent are consistent with the temperature and pressure of low pressure adsorbent described in technique scheme with the pressure and temperature of fluorine sorbent material low pressure adsorbent, do not repeat them here.In the present invention, the pressure and temperature of described silica gel low pressure adsorbent, the temperature and pressure of activated alumina low pressure adsorbent can be identical with the temperature and pressure of fluorine sorbent material low pressure adsorbent, also can be different.In the present invention, the kind of the kind of described silica gel, activated alumina and fluorine sorbent material and source and silica gel, activated alumina and fluorine sorbent material described in technique scheme and originate consistent, does not repeat them here.
After described low pressure adsorbent completes, the present invention removes the water impurity in described 3rd intermediate product further preferably by activated alumina High Pressure Absorption, and the pressure of described activated alumina High Pressure Absorption is 2.5MPa ~ 3.5MPa.In the present invention, the pressure of described activated alumina High Pressure Absorption is more preferably 2.8MPa ~ 3.2MPa, most preferably is 3MPa.In the present invention, described activated alumina is consistent with activated alumina described in technique scheme, does not repeat them here.In the present invention, the number of times of described activated alumina High Pressure Absorption is preferably 1 time ~ 3 times, is more preferably 2 times.
In the present invention, the pressure of described High Pressure Absorption is more preferably 2.8MPa ~ 3.2MPa, most preferably is 3MPa.In the present invention, the sorbent material of described High Pressure Absorption is preferably fluorine sorbent material.In the present invention, the kind of the kind of described fluorine sorbent material and source and fluorine sorbent material described in technique scheme with originate consistent, do not repeat them here.In the present invention, the number of times of described fluorine sorbent material High Pressure Absorption is preferably 1 time ~ 3 times, is more preferably 2 times.The present invention preferably first removes the water impurity in described 3rd intermediate product, then the impurity fluorochemical removed in described 3rd intermediate product and oil.
After removing fluorochemical in described 3rd intermediate product and oil, the 3rd intermediate product removing fluorochemical and oil is preferably carried out High Pressure Absorption by the present invention, removes the carbide in described 3rd intermediate product and sulfide; The pressure of described High Pressure Absorption is consistent with the pressure of High Pressure Absorption described in technique scheme, does not repeat them here.In the present invention, the sorbent material removing described carbide and sulfide High Pressure Absorption is preferably 13X molecular sieve.The source of the present invention to described 13X molecular sieve does not have special restriction, can be bought obtain by market.In an embodiment of the present invention, described 13X molecular sieve can be the molecular sieve of 13X-HP model, also can be the molecular sieve of 13X-PG model.In the present invention, the number of times of described 13X molecular sieve High Pressure Absorption is preferably 1 time ~ 3 times, is more preferably 2 times.
The present invention, preferably while described pressure-variable adsorption process, carries out desorption and regeneration to the sorbent material that described pressure-variable adsorption adopts.In the present invention, the desorption pressures of described sorbent material is preferably-0.1MPa ~-0.5MPa, is more preferably-0.2MPa ~-0.3MPa.In the present invention, the desorption temperature of described sorbent material is preferably 25 DEG C ~ 100 DEG C, is more preferably 40 DEG C ~ 80 DEG C, most preferably is 50 DEG C ~ 70 DEG C.Described sorbent material preferably regenerates by the present invention under the condition of vacuum.In the present invention, the regeneration temperature of described silica gel is preferably 100 DEG C ~ 150 DEG C, is more preferably 120 DEG C ~ 130 DEG C.In the present invention, the regeneration temperature of described activated alumina is preferably 300 DEG C ~ 350 DEG C, is more preferably 320 DEG C ~ 330 DEG C.In the present invention, the regeneration temperature of described fluorine sorbent material is preferably 300 DEG C ~ 350 DEG C, is more preferably 320 DEG C ~ 330 DEG C.In the present invention, the regeneration temperature of described 13X molecular sieve is preferably 300 DEG C ~ 350 DEG C, is more preferably 320 DEG C ~ 330 DEG C.
After obtaining the 4th intermediate product, described 4th intermediate product is carried out rectification process by the present invention, removes the air in described 4th intermediate product and fluorocarbons impurities, obtains sulfur hexafluoride.In the present invention, described rectification process preferably includes the first rectification process and the second rectification process, and the pressure of described first rectification process is 1MPa ~ 5MPa, removes the water in described 4th intermediate product; The pressure of described second rectification process is 0.5MPa ~ 1.6MPa, removes the fluorocarbon in described 4th intermediate product.In the present invention, the pressure of described first rectification process is more preferably 2MPa ~ 3MPa.In the present invention, the cooling temperature of described first rectification process is preferably-50 DEG C ~-35 DEG C, is more preferably-45 DEG C ~-40 DEG C.In the present invention, the Heating temperature of described first rectification process is preferably 15 DEG C ~ 30 DEG C, is more preferably 20 DEG C ~ 25 DEG C.
In the present invention, the pressure of described second rectification process is more preferably 0.7MPa ~ 1.4MPa, most preferably is 0.8MPa ~ 1.2MPa.In the present invention, the cooling temperature of described second rectification process is preferably-25 DEG C ~-10 DEG C, is more preferably-20 DEG C ~-15 DEG C.In the present invention, the Heating temperature of described second rectification process is preferably-15 DEG C ~-5 DEG C, is more preferably-12 DEG C ~-8 DEG C.
The present invention preferably first removes the impurity air in described 4th intermediate product, then removes the impurity fluorocarbon in described 4th intermediate product.The present invention, by carrying out the first rectification process to described 4th intermediate product, obtains the first gaseous fraction and first liquid component; The preferred < 25% of the mass content of sulfur hexafluoride in described first gaseous fraction, the preferred > 75% of mass content of air; The preferred > 99.9% of the mass content of sulfur hexafluoride in described first liquid component, the preferred < 10ppm of mass content of air, fluorocarbon, as C
2f
6the preferred < 500ppm of mass content.In the present invention, the mass content of sulfur hexafluoride more preferably < 20% in described first gaseous fraction, the mass content more preferably > 80% of air.
The first gaseous fraction obtained preferably is carried out adsorption treatment by the present invention, reclaims the sulfur hexafluoride in described first gaseous fraction.The sorbent material of the present invention to adsorption treatment first gaseous fraction does not have special restriction, adopts the sorbent material that can be used for adsorb sulfur hexafluoride well known to those skilled in the art.In the present invention, described in adsorption treatment, the pressure of the first gaseous fraction is preferably 0.1MPa ~ 1.5MPa, is more preferably 0.5MPa ~ 1MPa.In the present invention, the temperature of the first gaseous fraction described in adsorption treatment is preferably 20 DEG C ~ 30 DEG C, is more preferably 24 DEG C ~ 28 DEG C.
After sulfur hexafluoride in described first gaseous fraction reclaims, component remaining in the first gaseous fraction is preferably carried out emptying process by the present invention.In the present invention, after described first gaseous fraction reclaims sulfur hexafluoride, the preferred < 5% of the mass content of sulfur hexafluoride in remaining ingredient.In the present invention, when described first gaseous fraction reclaims after sulfur hexafluoride, in remaining ingredient during the mass content > 5% of sulfur hexafluoride, the present invention preferably carries out desorb process to described remaining ingredient.In the present invention, the pressure of described desorb process is preferably 0.1MPa ~ 1.5MPa, is more preferably 0.5MPa ~ 1MPa.In the present invention, the temperature of described desorb process is preferably 50 DEG C ~ 100 DEG C, is more preferably 60 DEG C ~ 90 DEG C, most preferably is 70 DEG C ~ 80 DEG C.
Described first liquid component is preferably carried out the second rectification process by the present invention, removes the fluorocarbon in described first liquid component.In the present invention, it is consistent that described first liquid component carries out the pressure of the pressure of the second rectification process, cooling temperature and Heating temperature and the second rectification process described in technique scheme, cooling temperature and Heating temperature, do not repeat them here.
Described first liquid component, after the second rectification process, obtains the second gaseous fraction and second liquid component; The preferred > 99.95% of the mass content of sulfur hexafluoride in described second gaseous fraction, the preferred < 500ppm of mass content of fluorocarbon; The preferred < 60% of the mass content of sulfur hexafluoride in described second liquid component.
Described second gaseous fraction is preferably carried out rectification process by the present invention, removes the fluorocarbon in described second gaseous fraction further.In the present invention, described in rectification process, the pressure of the second gaseous fraction is preferably 0.5MPa ~ 1MPa, is more preferably 0.6MPa ~ 0.8MPa.In the present invention, the cooling temperature of the second gaseous fraction described in rectification process is preferably-30 DEG C ~-15 DEG C, is more preferably-25 DEG C ~-20 DEG C.In the present invention, the Heating temperature of the second gaseous fraction described in rectification process is preferably-12 DEG C ~-5 DEG C, is more preferably-10 DEG C ~-8 DEG C.Described second gaseous fraction is after rectification process, obtain the 3rd gas composition and the 3rd liquid ingredient, the preferred > 99.998% of mass content of sulfur hexafluoride in described 3rd gaseous fraction, the preferred < 50ppm of mass content of fluorocarbon; The preferred > 99.999% of mass content of sulfur hexafluoride, the preferred < 10ppm of foreign matter content in described 3rd liquid ingredient.
Described second liquid component is preferably carried out distillation process by the present invention, obtains the 4th gaseous fraction and the 4th liquid ingredient; The preferred > 95% of mass content of sulfur hexafluoride in described 4th gaseous fraction.In the present invention, the pressure of described distillation process is preferably 1.5MPa ~ 2MPa, is more preferably 1.6MPa ~ 1.8MPa.In the present invention, the cooling temperature of described distillation process is preferably-45 DEG C ~-30 DEG C, is more preferably-40 DEG C ~-35 DEG C.In the present invention, the Heating temperature of described distillation process is preferably-12 DEG C ~-5 DEG C, is more preferably-10 DEG C ~-8 DEG C.Described 4th liquid ingredient is preferably carried out emission treatment by the present invention.
Before carrying out rectification process to described 4th intermediate product, the present invention preferably carries out condensation process to described 4th intermediate product.In the present invention, the pressure of described condensation process is preferably 2MPa ~ 3MPa, is more preferably 2.2MPa ~ 2.8MPa, most preferably is 2.4MPa ~ 2.6MPa.In the present invention, the temperature of described condensation process is preferably-40 DEG C ~-20 DEG C, is more preferably-35 DEG C ~-25 DEG C, most preferably is-30 DEG C.In the present invention, the cold carrier of described condensation process is preferably dibasic alcohol.In an embodiment of the present invention, the cold carrier of described condensation process can be the glacial epoch refrigerant of LM series, as the glacial epoch refrigerant of LM-1 model.In the present invention, the glacial epoch refrigerant of described LM series has excellent antiseptic and rustproof property, Cooling Heat Transfer, Safety and Environmental Protection, and viscosity is little, and specific heat is large, the advantages such as thermal conductivity is high, and ability of cold carrier is strong.
The invention provides a kind of device reclaiming sulfur hexafluoride, comprising:
Pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity;
The catalytic pyrolysis equipment be connected with described pre-processing device;
The purification apparatus be connected with described catalytic pyrolysis equipment, described purification apparatus is for removing containing the sulfocompound in the sulfur hexafluoride of impurity;
The variable-pressure adsorption equipment be connected with described purification apparatus, described variable-pressure adsorption equipment is for removing containing the water in the sulfur hexafluoride of impurity, fluorochemical and oil;
The rectifying device be connected with described variable-pressure adsorption equipment, described rectifying device is for removing containing the air in the sulfur hexafluoride of impurity and fluorocarbon.
The device of recovery sulfur hexafluoride provided by the invention, makes the sulfur hexafluoride containing impurity be introduced into catalytic pyrolysis equipment, then enters purification apparatus, adopts device provided by the invention to reclaim and obtains the good sulfur hexafluoride of quality.
The structural representation of the recovery sulfur hexafluoride device that Fig. 2 provides for the embodiment of the present invention, the device of the recovery sulfur hexafluoride that the embodiment of the present invention provides comprises:
Pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity.In the present invention, the described sulfur hexafluoride containing impurity is consistent with the sulfur hexafluoride containing impurity described in technique scheme, does not repeat them here.
The structural representation of the pre-processing device that Fig. 3 provides for the embodiment of the present invention, as shown in Figure 3, in the present invention, described pre-processing device preferably includes sour adsorption tower 3, the oil strainer 4 be connected with described sour adsorption tower 3, the drying adsorption tower 5 be connected with described oil strainer 4.In the present invention, described sour adsorption tower 3 is for removing containing the partially acidic material in the sulfur hexafluoride of impurity.In the present invention, the sorbent material in described sour adsorption tower 3 is consistent with the sorbent material that acid described in technique scheme is adsorbed, and does not repeat them here.
In the present invention, described oil strainer 4 is for removing containing the part oil in the sulfur hexafluoride of impurity.In the present invention, the filter core in described oil strainer 4 is preferably the active carbon filter core described in technique scheme.In the present invention, described drying adsorption tower 5 is for removing containing the part water in the sulfur hexafluoride of impurity.In the present invention, the sorbent material in described drying adsorption tower 5 is consistent with the sorbent material that water described in technique scheme adsorbs, and does not repeat them here.
In the present invention, described pre-processing device preferably also comprises flow rate control device.In the present invention, described flow rate control device is for after controlling the sulfur hexafluoride pre-treatment containing impurity, and the material obtained enters the flow of catalytic pyrolysis equipment.In the present invention, described containing after the sulfur hexafluoride pre-treatment of impurity, the flow that the material obtained enters catalytic pyrolysis equipment is preferably 50Kg/h ~ 150Kg/h, is more preferably 80Kg/h ~ 120Kg/h, most preferably is 100Kg/h.
In the present invention, described flow rate control device comprises pressure adjustment basin 6, the vacuum pressure gauge 7 regulating basin 6 to be connected with described pressure, the variable valve 8 regulating basin to be connected with described pressure, the under meter 9 be connected with described variable valve 8.In the present invention, described pressure regulating tank 6 is for storing the material after drying adsorption tower 5 process, and the pressure of described pressure regulating tank 6 inside is preferably 0.2MPa ~ 0.4MPa, is more preferably 0.25MPa ~ 0.35MPa, most preferably is 0.3MPa.In the present invention, described vacuum pressure gauge 7 is for the pressure of measuring stress regulating tank 6 inside.In the present invention, described variable valve 8 enters the flow of catalytic pyrolysis equipment for the material of control pressure regulating tank 6 inside.In the present invention, the flow set of described variable valve 8 is preferably 50Kg/h ~ 150Kg/h, is more preferably 80Kg/h ~ 120Kg/h, most preferably is 100Kg/h.In the present invention, described under meter 9 is for testing the flow of the material of variable valve 8 release.In the present invention, there is between described variable valve 8 and under meter 9 information transmission association, by the aperture of the Flow-rate adjustment variable valve 8 of the display of under meter 9, ensure that the flow of variable valve 8 control is within the scope of 50Kg/h ~ 150Kg/h.
In the present invention, described pre-processing device preferably also comprises the e Foerderanlage of the sulfur hexafluoride containing impurity.In the present invention, the e Foerderanlage of the described sulfur hexafluoride containing impurity preferably includes and reclaims gas-reservoir tank 1, and the relief valve 2 be connected with described recovery gas-reservoir tank 1, described relief valve 2 is connected with described sour adsorption tower 3.In the present invention, described recovery gas-reservoir tank 1 is for depositing the described sulfur hexafluoride containing impurity.In the present invention, described relief valve 2 reclaims the flow that enter pressure regulating tank 6 of the sulfur hexafluoride containing impurity in gas-reservoir tank 1 by sour adsorption tower 3, oil strainer 4 and drying adsorption tower 5 for controlling.In the present invention, described relief valve 2 with between vacuum pressure gauge 7, there is information transmission and associate, when described vacuum pressure gauge 7 shows pressure < 0.4MPa, relief valve 2 is opened; As the pressure > 0.4MPa that described vacuum pressure gauge 7 shows, relief valve 2 cuts out.
The equipment of recovery sulfur hexafluoride provided by the invention comprises the catalytic pyrolysis equipment be connected with described pre-processing device, and described catalytic pyrolysis equipment is used under the effect of catalyzer, changing low price sulphide by containing the high sulphide in the sulfur hexafluoride of impurity into.In the present invention, described high sulphide is consistent with high sulphide described in technique scheme and low price sulphide with low price sulphide, does not repeat them here.In the present invention, the method for described catalytic pyrolysis is consistent with the method for catalytic pyrolysis described in technique scheme, does not repeat them here.
The structural representation of the catalytic pyrolysis equipment that Fig. 4 provides for the embodiment of the present invention and purification apparatus, as shown in Figure 4, in an embodiment of the present invention, described catalytic pyrolysis equipment can be pyrolyzer, and described pyrolyzer is connected with purification apparatus.The present invention preferably arranges two pyrolyzer and carries out catalytic pyrolysis simultaneously.In an embodiment of the present invention, described catalytic pyrolysis equipment comprises the first pyrolyzer and the second pyrolyzer, and one end of described first pyrolyzer is connected with described under meter 9, and the other end of described first pyrolyzer is connected with purification apparatus; One end of described second pyrolyzer is connected with described under meter 9, and the other end of described second pyrolyzer is connected with purification apparatus.
The device of recovery sulfur hexafluoride provided by the invention comprises the purification apparatus be connected with described catalytic pyrolysis equipment, the sulfide impurities that described purification apparatus produces for removing described catalytic pyrolysis equipment.In the present invention, described sulfide impurities is consistent with sulfide impurities described in technique scheme, does not repeat them here.In the present invention, described purification apparatus preferably includes washing equipment and alkali cleaning equipment, and described washing equipment is connected with described catalytic pyrolysis equipment; One end of described alkali cleaning equipment is connected with described washing equipment, and the other end of described alkali cleaning equipment is connected with variable-pressure adsorption equipment.In the present invention, the method for described washing and alkali cleaning wash with described in technique scheme and method consistent, do not repeat them here.The present invention preferably arranges 3 ~ 8 washing equipments, is more preferably 4 ~ 6, most preferably is 5.The present invention preferably arranges 3 ~ 8 alkali cleaning equipment, is more preferably 4 ~ 7, most preferably is 6.
In an embodiment of the present invention, described purification apparatus comprises the first water washing tank, described first water washing tank is connected with the first pyrolyzer and the second pyrolyzer, tank connected second water washing tank is washed with described first, tank connected 3rd water washing tank is washed with described second, with the 4th water washing tank of described 3rd water washing tank cracking, tank connected 5th water washing tank is washed with the described 4th, tank connected first caustic treater is washed with the described 5th, second caustic treater tank connected with described first alkali cleaning, three caustic treater tank connected with described second alkali cleaning, four caustic treater tank connected with described 3rd alkali cleaning, five caustic treater tank connected with described 4th alkali cleaning, one end and the tank connected hexabasic cleaning of evaporator of described 5th alkali cleaning, the other end of described hexabasic cleaning of evaporator is connected with variable-pressure adsorption equipment.
In the present invention, described purification apparatus preferably also comprises the first e Foerderanlage, described first e Foerderanlage be used for will the substance use that obtain after alkali cleaning device processes in variable-pressure adsorption equipment.In the present invention, one end of described first e Foerderanlage and alkali cleaning equipment connection, the other end of described first e Foerderanlage is connected with variable-pressure adsorption equipment.In an embodiment of the present invention, described first e Foerderanlage can be water-ring pump, and one section of described water-ring pump is connected with the 5th caustic treater, and the other end of described water-ring pump is connected with variable-pressure adsorption equipment.
The device of recovery sulfur hexafluoride provided by the invention comprises the variable-pressure adsorption equipment be connected with described purification apparatus, and described variable-pressure adsorption equipment is described containing water, fluorochemical and the oil in the sulfur hexafluoride of impurity for removing.In the present invention, described variable-pressure adsorption equipment preferably includes the low pressure adsorbent equipment be connected with described purifying treatment, and described low pressure adsorbent equipment is described containing the water in the sulfur hexafluoride of impurity for removing; The High Pressure Absorption equipment of one end and described low pressure adsorbent equipment connection, the other end of described High Pressure Absorption equipment is connected with rectifying device, and described High Pressure Absorption equipment is described containing the fluorochemical in the sulfur hexafluoride of impurity and oil for removing.
In the present invention, described low pressure adsorbent equipment preferably includes one or more in low pressure silica gel adsorption tower, low pressure activated alumina adsorption tower and low pressure fluorine adsorbent tower, more preferably comprises low pressure silica gel adsorption tower, low pressure activated alumina adsorption tower and low pressure fluorine adsorbent tower.In the present invention, described low pressure silica gel adsorption tower is connected with purification apparatus, described low pressure activated alumina adsorption tower is connected with described low pressure silica gel adsorption tower, one end of described low pressure fluorine adsorbent tower is connected with described low pressure activated alumina adsorption tower, and the other end of described low pressure fluorine adsorbent tower is connected with rectifying device.In the present invention, described low pressure adsorbent, silica gel low pressure adsorbent, activated alumina low pressure adsorbent are consistent with the method for low pressure adsorbent, silica gel low pressure adsorbent, activated alumina low pressure adsorbent and fluorine sorbent material low pressure adsorbent described in technique scheme with the method for fluorine sorbent material low pressure adsorbent, do not repeat them here.
The present invention preferably arranges 1 ~ 5 low pressure silica gel adsorption towers, is more preferably 2 ~ 4, most preferably is 3.The present invention preferably arranges 1 ~ 3 low pressure activated alumina adsorption towers, is more preferably 2.The present invention preferably arranges 1 low pressure fluorine adsorbent tower.
The structural representation of the variable-pressure adsorption equipment that Fig. 5 provides for the embodiment of the present invention and rectifying device, as shown in Figure 5, in an embodiment of the present invention, described low pressure adsorbent equipment comprises the first low pressure silica gel adsorption tower be connected with water-ring pump, the the second low pressure silica gel adsorption tower be connected with described first low pressure silica gel adsorption tower, the 3rd low pressure silica gel adsorption tower be connected with described second low pressure silica gel adsorption tower, the the first low pressure activated alumina adsorption tower be connected with described 3rd low pressure silica gel adsorption tower, the the second low pressure activated alumina adsorption tower be connected with described first low pressure activated alumina adsorption tower, the low pressure fluorine adsorbent tower be connected with described second low pressure activated alumina adsorption tower.
In the present invention, described High Pressure Absorption equipment preferably includes high pressure fluorine adsorbent tower, and one end of described high pressure fluorine adsorbent tower is connected with described low-voltage equipment, and the other end of described high pressure fluorine adsorbent tower is connected with rectifying device.In the present invention, described High Pressure Absorption is consistent with the method for the High Pressure Absorption described in technique scheme and fluorine sorbent material High Pressure Absorption with the method for fluorine sorbent material High Pressure Absorption, does not repeat them here.The present invention preferably arranges 1 ~ 3 high pressure fluorine adsorbent towers, is more preferably 2.
In the present invention, described High Pressure Absorption equipment preferably also comprises high pressure activating alumina adsorption tower, one end of described high pressure activating alumina adsorption tower and described low pressure adsorbent equipment connection, the other end of described high pressure activating alumina adsorption tower is connected with described high pressure fluorine adsorbent tower, and described high pressure activating alumina adsorption tower is used for removing the water in the described sulfur hexafluoride containing impurity further.The present invention preferably arranges 1 ~ 3 high pressure activating alumina adsorption towers, is more preferably 2.
In the present invention, described High Pressure Absorption equipment preferably also comprises high pressure 13X adsorbing tower with molecular sieve, one end of described high pressure 13X molecular sieve is connected with described high pressure activating alumina adsorption tower, the other end of described high pressure 13X adsorbing tower with molecular sieve is connected with rectifying device, and described high pressure 13X adsorbing tower with molecular sieve is described containing the carbide in the sulfur hexafluoride of impurity and sulfide for removing.In the present invention, the method for described 13X molecular sieve High Pressure Absorption is consistent with the method for 13X molecular sieve High Pressure Absorption described in technique scheme, does not repeat them here.The present invention preferably arranges 1 ~ 3 high pressure 13X adsorbing tower with molecular sieve, is more preferably 2.
In an embodiment of the present invention, described High Pressure Absorption equipment comprises: the first high pressure activating alumina adsorption tower be connected with described low pressure fluorine adsorbent tower, the the second high pressure activating alumina adsorption tower be connected with described first high pressure activating alumina adsorption tower, the the first high pressure fluorine adsorbent tower be connected with described second high pressure activating alumina adsorption tower, the the second high pressure fluorine adsorbent tower be connected with described first high pressure fluorine adsorbent tower, the the first high pressure 13X adsorbing tower with molecular sieve be connected with described second high pressure fluorine adsorbent tower, the second high pressure 13X adsorbing tower with molecular sieve that one end is connected with described first high pressure 13X adsorbing tower with molecular sieve, the other end of described second high pressure 13X adsorbing tower with molecular sieve is connected with rectifying device.
In the present invention, described variable-pressure adsorption equipment preferably also comprises the first supercharging equipment, and described first supercharging equipment is used for the product obtained after purification apparatus process to carry out pressure treatment, makes the product after pressure treatment enter low pressure adsorbent equipment.In the present invention, one end of described first supercharging equipment is connected with purification apparatus, the other end of described first supercharging equipment and low pressure adsorbent equipment connection.In an embodiment of the present invention, described first supercharging equipment is topping-up pump, and one end of described topping-up pump is connected with water-ring pump, and the other end of described topping-up pump is connected with the first low pressure silica gel adsorption tower.
In the present invention, described variable-pressure adsorption equipment preferably also comprises the second supercharging equipment, and described second supercharging equipment is used for the product obtained after low pressure adsorbent device processes to carry out pressure treatment, makes the product after pressure treatment enter High Pressure Absorption equipment.In the present invention, one end of described second supercharging equipment and low pressure adsorbent equipment connection, the other end of described second supercharging equipment and High Pressure Absorption equipment connection.In an embodiment of the present invention, described second supercharging equipment is molding machine, and one end of described molding machine is connected with low pressure fluorine adsorbent tower, and the other end of described molding machine is connected with the first high pressure activating alumina adsorption tower.
The device of recovery sulfur hexafluoride provided by the invention comprises the rectifying device be connected with described variable-pressure adsorption equipment, and described rectifying device is described containing the air in the sulfur hexafluoride of impurity and fluorocarbon for removing.As shown in Figure 5, in the present invention, described rectifying device preferably includes the light point tower be connected with described variable-pressure adsorption equipment, and described light point of tower is described containing the air in the sulfur hexafluoride of impurity for removing; The Chong Fenta be connected with described light point of tower, described heavy point of tower is described containing the fluorocarbon in the sulfur hexafluoride of impurity for removing.In the present invention, the tower pressure of described light point of tower is preferably 1MPa ~ 5MPa, is more preferably 2MPa ~ 3MPa.In the present invention, the tower top temperature of described light point of tower is preferably-50 DEG C ~-35 DEG C, is more preferably-45 DEG C ~-40 DEG C.In the present invention, the bottom temperature of described light point of tower is preferably 15 DEG C ~ 30 DEG C, is more preferably 20 DEG C ~ 25 DEG C.
In the present invention, the product liquid obtained after point tower process that kicks the beam enters Chong Fenta.In the present invention, the tower pressure of described heavy point of tower is preferably 0.5MPa ~ 1.6MPa, is more preferably 0.7MPa ~ 1.4MPa, most preferably is 0.8MPa ~ 1.2MPa.In the present invention, the tower top temperature of described heavy point of tower is preferably-25 DEG C ~-10 DEG C, is more preferably-20 DEG C ~-15 DEG C.In the present invention, the bottom temperature of described heavy point of tower is preferably-15 DEG C ~-5 DEG C, is more preferably-12 DEG C ~-8 DEG C.
In the present invention, described rectifying device preferably also comprises sulfur hexafluoride adsorption tower, and described sulfur hexafluoride adsorption tower is used for the sulfur hexafluoride in the gaseous product obtained after gently dividing tower process to reclaim.In the present invention, sulfur hexafluoride sorbent material used in described sulfur hexafluoride adsorption tower is consistent with sulfur hexafluoride sorbent material described in technique scheme, does not repeat them here.In the present invention, the tower pressure of described sulfur hexafluoride adsorption tower is preferably 0.1MPa ~ 1.5MPa, is more preferably 0.5MPa ~ 1MPa.In the present invention, the temperature of described sulfur hexafluoride adsorption tower is preferably 20 DEG C ~ 30 DEG C, is more preferably 24 DEG C ~ 28 DEG C.The gaseous product emptying that the present invention preferably will obtain after the process of sulfur hexafluoride adsorption tower.In the present invention, described sulfur hexafluoride adsorption tower is connected with described light point of tower.
In the present invention, described rectifying device preferably also comprises desorption tower, and described desorption tower is used for sulfur hexafluoride sorbent material desorb used for sulfur hexafluoride adsorption tower to reclaim rear re-using.In the present invention, the tower pressure of described desorption tower is preferably 0.1MPa ~ 1.5MPa, is more preferably 0.5MPa ~ 1MPa.In the present invention, the temperature of described desorption tower is preferably 50 DEG C ~ 100 DEG C, is more preferably 60 DEG C ~ 80 DEG C.In the present invention, described desorption tower is connected with described sulfur hexafluoride adsorption tower.
In the present invention, described rectifying device preferably also comprises dealkylation tower, and described dealkylation tower is used for the fluorocarbon in the gaseous product obtained after further removal heavily divides tower process.In the present invention, described dealkylation tower is connected with described heavy point of tower.In the present invention, the tower pressure of described dealkylation tower is preferably 0.5MPa ~ 1MPa, is more preferably 0.6MPa ~ 0.8MPa.In the present invention, the tower top temperature of described dealkylation tower is preferably-30 DEG C ~-15 DEG C, is more preferably-25 DEG C ~-20 DEG C.In the present invention, the bottom temperature of described dealkylation tower is preferably-12 DEG C ~-5 DEG C, is more preferably-10 DEG C ~-8 DEG C.The gaseous product obtained after dealkylation tower process and product liquid are preferably collected by the present invention, and described gaseous product is the good sulfur hexafluoride of quality, the preferred > 99.999% of the mass concentration of sulfur hexafluoride in described product liquid.
In the present invention, described rectifying device preferably also comprises distillation tower, described distillation tower for improve heavily divide tower process after the purity of sulfur hexafluoride in the product liquid that obtains.In the present invention, described distillation tower is connected with heavily dividing tower.In the present invention, the tower pressure of described distillation tower is preferably 1.5MPa ~ 2MPa, is more preferably 1.6MPa ~ 1.8MPa.In the present invention, the tower top temperature of described distillation tower is preferably-45 DEG C ~-30 DEG C, is more preferably-40 DEG C ~-35 DEG C.In the present invention, the bottom temperature of described distillation is preferably-12 DEG C ~-5 DEG C, is more preferably-10 DEG C ~-8 DEG C.The gaseous product obtained after distillation tower process is preferably collected by the present invention, and the product liquid obtained carries out emission treatment.
In the present invention, described rectifying device preferably also comprises the first condenser, and described first condenser is used for the product obtained after variable-pressure adsorption equipment process to carry out condensation, makes condensed product enter light point tower.In the present invention, one end of described first condenser is connected with variable-pressure adsorption equipment, and the other end of described first condenser is connected with a light point tower.In the present invention, the method for described condensation is consistent with the condensation method described in technique scheme, does not repeat them here.
In the present invention, described rectifying device preferably also comprises the second condenser, and described second cool condenser is used for the gaseous product obtained after heavily dividing tower process to carry out condensation, makes condensed product enter dealkylation tower.In the present invention, one end of described second condenser is connected with heavily dividing tower, and the other end of described second condenser is connected with dealkylation tower.In the present invention, the method for described condensation is consistent with the condensation method described in technique scheme, does not repeat them here.
As shown in Figure 5, the rectifying device that the embodiment of the present invention provides comprises: the first condenser be connected with the second high pressure 13X adsorbing tower with molecular sieve, the light point tower be connected with described first condenser, the sulfur hexafluoride adsorption tower be connected with described light point of column overhead, the Chong Fenta be connected with described light point of tower tower reactor, the second condenser be connected with described heavy point of column overhead, the dealkylation tower be connected with described second condenser, the distillation tower be connected with at the bottom of described heavy point of tower tower.
The equipment of recovery sulfur hexafluoride provided by the invention preferably also comprises filling apparatus, and described filling apparatus is for collecting the sulfur hexafluoride after recovery.In the present invention, described filling apparatus is connected with rectifying device.
Method and apparatus provided by the invention is reclaimed the sulfur hexafluoride obtained and carry out quality examination according to the standard of GB/T12022-2006 " industrial sulfur hexafluoride ", detected result shows, method and apparatus provided by the invention reclaims the standard-required of quality higher than GB/T12022-2006 " industrial sulfur hexafluoride " of the sulfur hexafluoride obtained.
The invention provides a kind of method reclaiming sulfur hexafluoride, comprise the following steps: 1), by the sulfur hexafluoride containing impurity carry out pre-treatment, remove containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product; 2), by described first intermediate product carry out catalytic pyrolysis, obtain the second intermediate product; The catalyzer of described catalytic pyrolysis is cobaltic fluoride; 3), by described second intermediate product carry out purifying treatment, remove the sulfur compound impurities in described second intermediate product, obtain the 3rd intermediate product; 4), by described 3rd intermediate product carry out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product; 5), by described 4th intermediate product carry out rectification process, remove the air in described 4th intermediate product and fluorocarbons impurities, obtain sulfur hexafluoride.The method of this recovery sulfur hexafluoride provided by the invention, adopts the technique of first catalytic pyrolysis purifying treatment again, can reclaim and obtain the good sulfur hexafluoride of quality.
The invention provides a kind of device reclaiming sulfur hexafluoride, comprising: pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity; The catalytic pyrolysis equipment be connected with described pre-processing device; The purification apparatus be connected with described catalytic pyrolysis equipment, described purification apparatus is for removing containing the sulfocompound in the sulfur hexafluoride of impurity; The variable-pressure adsorption equipment be connected with described purification apparatus, described variable-pressure adsorption equipment is for removing containing the water in the sulfur hexafluoride of impurity, fluorochemical and oil; The rectifying device be connected with described variable-pressure adsorption equipment, described rectifying device is for removing containing the air in the sulfur hexafluoride of impurity and fluorocarbon.The device of recovery sulfur hexafluoride provided by the invention, makes the sulfur hexafluoride containing impurity be introduced into catalytic pyrolysis equipment, then enters purification apparatus, adopts device provided by the invention to reclaim and obtains the good sulfur hexafluoride of quality.
Embodiment 1
According to the flow process shown in Fig. 1, the device of structure shown in Fig. 2 ~ Fig. 5 is adopted to reclaim the sulfur hexafluoride containing impurity, the schema of the recovery sulfur hexafluoride method that Fig. 1 provides for the embodiment of the present invention, the structural representation of the recovery sulfur hexafluoride device that Fig. 2 provides for the embodiment of the present invention, the structural representation of the pre-processing device that Fig. 3 provides for the embodiment of the present invention, the structural representation of the catalytic pyrolysis equipment that Fig. 4 provides for the embodiment of the present invention and purification apparatus, the structural representation of the variable-pressure adsorption equipment that Fig. 5 provides for the embodiment of the present invention and rectifying device; Sulfur hexafluoride containing impurity is the sulfur hexafluoride of the operation of collecting from gas-insulated switchgear, and it is 354ppm air that the described sulfur hexafluoride containing impurity comprises mass concentration, water, oil, the CF of 10ppm
4, the C of 482ppm
2f
6, the C of 260ppm
3f
8, the CO of 40ppm
2, the CH of the CO of 6.6ppm, 0.2ppm
4, the SO of 36ppm
2f
2and SOF
2, the S of 170ppm
2oF
10, the SO of 1ppm
2; Detailed process is:
The sulfur hexafluoride reclaimed containing impurity in gas-reservoir tank 1 is delivered in sour adsorption tower 3 by relief valve 2, in sour adsorption tower 3, adopts the activated alumina of F-200 model to carry out acid absorption to the sulfur hexafluoride containing impurity; The product obtained after being processed by sour adsorption tower 3 sends into oil strainer 4, the product obtained after adopting active carbon filter core filter acid adsorption tower 3 to process; The product obtained after being processed by oil strainer 4 sends into drying adsorption tower 5, and the product obtained after adopting silica gel to filter 4 process to oil carries out drying; The product storage obtained after being processed by drying adsorption tower 5 regulates in basin 6 at pressure, the switch of the pressure-controlling relief valve 2 shown by vacuum pressure gauge 7, as the little < 0.4MPa of pressure that vacuum pressure gauge 7 shows, relief valve 2 often leaves, as the pressure > 0.4MPa that vacuum pressure gauge 7 shows, closing pressure-regulating valve 2; Regulated by pressure in substance use to the first pyrolyzer in basin 6 and the second pyrolyzer, by under meter 9 regulating and controlling valve 8, the flow that under meter 9 is shown is in the scope of 80Kg/h ~ 100Kg/h.
In the first pyrolyzer and the second pyrolyzer, the material of conveying from pressure hold tank 6 is carried out catalytic pyrolysis, the catalyzer of described catalytic pyrolysis is cobaltic fluoride, and the temperature of described catalytic pyrolysis is 350 DEG C, and the pressure of described catalytic pyrolysis is normal pressure.
Make the product obtained after catalytic pyrolysis in the first pyrolyzer and the second pyrolyzer enter the first water washing tank, the second water washing tank, the 3rd water washing tank, the 4th water washing tank and the 5th water washing tank successively and carry out 5 washings, what load in described first water washing tank, the second water washing tank, the 3rd water washing tank, the 4th water washing tank and the 5th water washing tank is water; The product obtained after making washing enters the first caustic treater, the second caustic treater, the 3rd caustic treater, the 4th caustic treater, the 5th caustic treater and hexabasic cleaning of evaporator successively and carries out 6 alkali cleanings, load in described first caustic treater, the second caustic treater, the 3rd caustic treater, the 4th caustic treater, the 5th caustic treater and hexabasic cleaning of evaporator to be mass concentration be 30% potassium hydroxide aqueous solution.
The material obtained after alkali cleaning is sent into increase in pump by water-ring pump and pressurizes, the pressure of the material obtained after making alkali cleaning reaches 1.5MPa, make that the material after pressurization enters the first low pressure silica gel adsorption tower successively, the second low pressure silica gel adsorption tower, the 3rd low pressure silica gel adsorption tower carry out 3 silica gel low pressure adsorbent, the pressure of described silica gel low pressure adsorbent is 1.5MPa, and temperature is 25 DEG C; The product obtained after making silica gel low pressure adsorbent enters the first low pressure activated alumina adsorption tower successively and the second low pressure activated alumina adsorption tower carries out 2 activated alumina low pressure adsorbent, and the pressure of described activated alumina low pressure adsorbent is 1.5MPa, and temperature is 25 DEG C; The material obtained after making activated alumina low pressure adsorbent enters low pressure fluorine adsorbent tower and carries out fluorine sorbent material low pressure adsorbent, and described fluorine sorbent material is the fluorine sorbent material of F-03 model, and the pressure of described fluorine sorbent material low pressure adsorbent is 0.15MPa, and temperature is 25 DEG C.
The material obtained after making fluorine sorbent material low pressure adsorbent enters molding machine and pressurizes, by the pressurize substance that obtains after fluorine sorbent material low pressure adsorbent to 3MPa, make the material after pressurization enter the first high pressure activating alumina adsorption tower successively and the second high pressure activating alumina adsorption tower carries out 2 activated alumina High Pressure Absorptions, the pressure of described activated alumina High Pressure Absorption is 3MPa; The material obtained after making activated alumina High Pressure Absorption enters the first high pressure fluorine adsorbent tower successively and the second high pressure fluorine adsorbent tower carries out 2 fluorine sorbent material High Pressure Absorptions, the sorbent material of described fluorine sorbent material High Pressure Absorption is the fluorine sorbent material of KDHF-03 model, and the pressure of described fluorine sorbent material High Pressure Absorption is 3MPa; The product obtained after making fluorine sorbent material High Pressure Absorption enters the first high pressure 13X adsorbing tower with molecular sieve successively and the second high pressure 13X adsorbing tower with molecular sieve carries out 2 13X molecular sieve High Pressure Absorptions, the molecular sieve that the sorbent material that described 13X molecular sieve High Pressure Absorption uses is 13X-HP model, the pressure of described 13X molecular sieve High Pressure Absorption is 3MPa.
The product obtained after making 13X molecular sieve High Pressure Absorption enters the first condenser and carries out condensation, and the temperature of described condensation is-30 DEG C, and the pressure of described condensation is 2.5MPa, and the secondary refrigerant of described condensation is the glacial epoch refrigerant of LM-1 model.
The material obtained after making the first condenser process enters light point tower, and the tower pressure of described light point of tower is 2.5MPa, and tower top temperature is-43 DEG C, and bottom temperature is 23 DEG C.The gaseous matter obtained after making gently to divide tower process enters sulfur hexafluoride adsorption tower, and the sorbent material that described sulfur hexafluoride adsorption tower uses is gac, and the tower pressure of described sulfur hexafluoride adsorption tower is 1MPa, and temperature is 25 DEG C.
The liquid substance obtained after making gently to divide tower process enters Chong Fenta, and the tower pressure of described heavy point of tower is 1MPa, and tower top temperature is-15 DEG C, and bottom temperature is-10 DEG C.The gaseous matter obtained after making heavily to divide tower process enters dealkylation tower, and the tower pressure of described dealkylation tower is 0.8MPa, and tower top temperature is-23 DEG C, and bottom temperature is-8 DEG C.The gaseous matter obtained after dealkylation tower process and liquid substance are collected, described gaseous matter and liquid substance are reclaim the sulfur hexafluoride obtained.
The product liquid obtained after making heavily to divide tower process enters distillation tower, and the tower pressure of described distillation tower is 1.8MPa, and tower top temperature is-30 DEG C, and bottom temperature is-8 DEG C.Collected by the gaseous matter obtained after distillation tower process, the gaseous matter obtained after described distillation tower process is reclaim the sulfur hexafluoride obtained; The liquid substance obtained after distillation tower process is carried out emission treatment.
The embodiment of the present invention 1 is reclaimed the sulfur hexafluoride obtained and carry out quality examination according to the standard of GB/T12022-2006 " industrial sulfur hexafluoride ", detected result is as shown in table 1, and table 1 is the quality measurements that the embodiment of the present invention 1 reclaims the sulfur hexafluoride obtained.
Table 1 embodiment of the present invention 1 reclaims the quality measurements of the sulfur hexafluoride obtained
As shown in Table 1, the embodiment of the present invention 1 reclaims the standard-required of quality higher than GB/T12022-2006 " industrial sulfur hexafluoride " of the sulfur hexafluoride obtained.
As seen from the above embodiment, the invention provides a kind of method reclaiming sulfur hexafluoride, comprise the following steps: 1), by the sulfur hexafluoride containing impurity carry out pre-treatment, remove containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product; 2), by described first intermediate product carry out catalytic pyrolysis, obtain the second intermediate product; The catalyzer of described catalytic pyrolysis is cobaltic fluoride; 3), by described second intermediate product carry out purifying treatment, remove the sulfur compound impurities in described second intermediate product, obtain the 3rd intermediate product; 4), by described 3rd intermediate product carry out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product; 5), by described 4th intermediate product carry out rectification process, remove the air in described 4th intermediate product and fluorocarbons impurities, obtain sulfur hexafluoride.The method of this recovery sulfur hexafluoride provided by the invention, adopts the technique of first catalytic pyrolysis purifying treatment again, can reclaim and obtain the good sulfur hexafluoride of quality.
The invention provides a kind of device reclaiming sulfur hexafluoride, comprising: pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity; The catalytic pyrolysis equipment be connected with described pre-processing device; The purification apparatus be connected with described catalytic pyrolysis equipment, described purification apparatus is for removing containing the sulfocompound in the sulfur hexafluoride of impurity; The variable-pressure adsorption equipment be connected with described purification apparatus, described variable-pressure adsorption equipment is for removing containing the water in the sulfur hexafluoride of impurity, fluorochemical and oil; The rectifying device be connected with described variable-pressure adsorption equipment, described rectifying device is for removing containing the air in the sulfur hexafluoride of impurity and fluorocarbon.The device of recovery sulfur hexafluoride provided by the invention, makes the sulfur hexafluoride containing impurity be introduced into catalytic pyrolysis equipment, then enters purification apparatus, adopts device provided by the invention to reclaim and obtains the good sulfur hexafluoride of quality.
Claims (9)
1. reclaim a method for sulfur hexafluoride, comprise the following steps:
1), by the sulfur hexafluoride containing impurity carry out pre-treatment, remove containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity, obtain the first intermediate product;
2), by described first intermediate product carry out catalytic pyrolysis, obtain the second intermediate product; The catalyzer of described catalytic pyrolysis is cobaltic fluoride; The temperature of described catalytic pyrolysis is 300 DEG C ~ 400 DEG C;
3), by described second intermediate product carry out purifying treatment, remove the sulfur compound impurities in described second intermediate product, obtain the 3rd intermediate product;
4), by described 3rd intermediate product carry out pressure-variable adsorption process, remove water, fluorochemical and oily impurity in described 3rd intermediate product, obtain the 4th intermediate product;
5), by described 4th intermediate product carry out rectification process, remove the air in described 4th intermediate product and fluorocarbons impurities, obtain sulfur hexafluoride.
2. method according to claim 1, is characterized in that, described step 3) in purifying treatment comprise washing process and alkali cleaning process.
3. method according to claim 1, is characterized in that, described step 4) in pressure-variable adsorption process comprise low pressure adsorbent and High Pressure Absorption; The pressure of described low pressure adsorbent is 0.1MPa ~ 0.5MPa, removes the water in described 3rd intermediate product;
The pressure of described High Pressure Absorption is 2MPa ~ 5MPa; Remove the fluorochemical in described 3rd intermediate product and oil.
4. method according to claim 1, is characterized in that, described step 5) in rectification process comprise the first rectification process and the second rectification process, the pressure of described first rectification process is 1MPa ~ 5MPa, removes the air in described 4th intermediate product;
The pressure of described second rectification process is 0.5MPa ~ 1.6MPa, removes the fluorocarbon in described 4th intermediate product.
5. reclaim a device for sulfur hexafluoride, comprising:
Pre-processing device, described pre-processing device is for removing containing part oil, water and the acidic substance in the sulfur hexafluoride of impurity;
The catalytic pyrolysis equipment be connected with described pre-processing device;
The purification apparatus be connected with described catalytic pyrolysis equipment, described purification apparatus is for removing containing the sulfocompound in the sulfur hexafluoride of impurity;
The variable-pressure adsorption equipment be connected with described purification apparatus, described variable-pressure adsorption equipment is for removing containing the water in the sulfur hexafluoride of impurity, fluorochemical and oil;
The rectifying device be connected with described variable-pressure adsorption equipment, described rectifying device is for removing containing the air in the sulfur hexafluoride of impurity and fluorocarbon.
6. device according to claim 5, is characterized in that, described pre-processing device comprises:
Acid adsorption tower,
The oil strainer be connected with described sour adsorption tower,
The drying adsorption tower be connected with described oil strainer, described drying adsorption tower is connected with described catalytic pyrolysis equipment.
7. device according to claim 5, is characterized in that, described purification apparatus comprises:
The washing equipment be connected with described catalytic pyrolysis equipment;
The alkali cleaning equipment that one end is connected with described washing equipment, the other end of described alkali cleaning equipment is connected with described variable-pressure adsorption equipment.
8. device according to claim 5, is characterized in that, described variable-pressure adsorption equipment comprises:
The low pressure adsorbent equipment be connected with described purification apparatus, described low pressure adsorbent equipment is for removing containing the water in the sulfur hexafluoride of impurity;
The High Pressure Absorption equipment of one end and described low pressure adsorbent equipment connection, described High Pressure Absorption equipment is for removing containing the fluorochemical in the sulfur hexafluoride of impurity and oil, and the other end of described High Pressure Absorption equipment is connected with described rectifying device.
9. device according to claim 5, is characterized in that, described rectifying device comprises:
The light point tower be connected with described variable-pressure adsorption equipment, described light point of tower is for removing containing the air in the sulfur hexafluoride of impurity;
The Chong Fenta be connected with described light point of tower, described heavy point of tower is for removing containing the fluorocarbon in the sulfur hexafluoride of impurity.
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