CN117479995A - Regeneration method for acid gas adsorption device and method for manufacturing acid gas adsorption device - Google Patents
Regeneration method for acid gas adsorption device and method for manufacturing acid gas adsorption device Download PDFInfo
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- CN117479995A CN117479995A CN202380012205.9A CN202380012205A CN117479995A CN 117479995 A CN117479995 A CN 117479995A CN 202380012205 A CN202380012205 A CN 202380012205A CN 117479995 A CN117479995 A CN 117479995A
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- acid gas
- gas adsorption
- carbon dioxide
- substrate
- adsorption layer
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- 239000002253 acid Substances 0.000 title claims abstract description 249
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 212
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims description 57
- 238000011069 regeneration method Methods 0.000 title abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 99
- 239000000463 material Substances 0.000 claims abstract description 96
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 518
- 239000001569 carbon dioxide Substances 0.000 claims description 259
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 259
- 239000011230 binding agent Substances 0.000 claims description 82
- 238000005192 partition Methods 0.000 claims description 55
- 239000002798 polar solvent Substances 0.000 claims description 52
- 239000002245 particle Substances 0.000 claims description 39
- 230000001172 regenerating effect Effects 0.000 claims description 33
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- 239000002131 composite material Substances 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 claims description 15
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003586 protic polar solvent Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000012670 alkaline solution Substances 0.000 claims description 11
- 239000012621 metal-organic framework Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 229910052878 cordierite Inorganic materials 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 6
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 6
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052863 mullite Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 13
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- 238000000926 separation method Methods 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
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- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 239000013118 MOF-74-type framework Substances 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 239000004813 Perfluoroalkoxy alkane Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000013233 Zn4O(BBC)2 Substances 0.000 description 2
- 239000013231 Zn4O(BTE)(BPDC) Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
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- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
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- 238000002459 porosimetry Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- PEVRKKOYEFPFMN-UHFFFAOYSA-N 1,1,2,3,3,3-hexafluoroprop-1-ene;1,1,2,2-tetrafluoroethene Chemical compound FC(F)=C(F)F.FC(F)=C(F)C(F)(F)F PEVRKKOYEFPFMN-UHFFFAOYSA-N 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- FKJVYOFPTRGCSP-UHFFFAOYSA-N 2-[3-aminopropyl(2-hydroxyethyl)amino]ethanol Chemical compound NCCCN(CCO)CCO FKJVYOFPTRGCSP-UHFFFAOYSA-N 0.000 description 1
- WFCSWCVEJLETKA-UHFFFAOYSA-N 2-piperazin-1-ylethanol Chemical compound OCCN1CCNCC1 WFCSWCVEJLETKA-UHFFFAOYSA-N 0.000 description 1
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- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical group C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
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- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
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- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- GNVRJGIVDSQCOP-UHFFFAOYSA-N n-ethyl-n-methylethanamine Chemical compound CCN(C)CC GNVRJGIVDSQCOP-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 150000004885 piperazines Chemical class 0.000 description 1
- 239000003880 polar aprotic solvent Substances 0.000 description 1
- 229920000962 poly(amidoamine) Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The present invention provides a regeneration method of an acid gas adsorption device, which can smoothly recover acid gas recovery performance and reduce operation cost, and a manufacturing method of an acid gas adsorption device, which can manufacture an acid gas adsorption device with excellent acid gas recovery performance. The regeneration method of the acid gas adsorption device according to the embodiment of the present invention includes the following steps: a step of supplying a gas containing an acid gas to the acid gas adsorption device so as to contact the acid gas adsorption layer, and allowing the acid gas adsorption material to adsorb the acid gas; a step of separating the acid gas from the acid gas adsorbing material; a step of removing an acid gas adsorption layer of an acid gas adsorption apparatus, which is subjected to the step of adsorbing and the step of removing the acid gas, from the surface of the substrate; and forming an acid gas adsorption layer containing a porous support and an acid gas adsorption material on the surface of the substrate from which the acid gas adsorption layer has been removed.
Description
Technical Field
The present invention relates to a method for regenerating an acid gas adsorption apparatus and a method for manufacturing an acid gas adsorption apparatus.
Background
In recent years, in order to reduce environmental load, studies have been made to separate and recover acid gases contained in the atmosphere. Examples of such acid gases include carbon dioxide (hereinafter, sometimes referred to as CO) which mainly contributes to global warming 2 ). As a representative example of such studies, a carbon dioxide recovery, utilization and storage (Carbon dioxide Capture, utilization and Storage: CCUS) cycle is known. As a carbon dioxide adsorption apparatus for separating and recovering such carbon dioxide, CO has been proposed 2 An absorbent structure for trapping comprising a honeycomb substrate having a plurality of partition walls and a plurality of flow channels formed thereby, and functional structural unit groups disposed in and on the partition walls (for example, ginsengAs in patent document 1). In such CO 2 In the absorbent structure for capturing, CO can be captured from the gas fluid flowing in the absorbent structure 2 Can make captured CO 2 Disengaging under prescribed conditions. However, if CO described in patent document 1 is used 2 The absorbent structure for capturing repeatedly CO contained in the atmosphere 2 In (2), CO may be generated by repeating the heat treatment and the impurity contained in the atmosphere 2 The recovery rate gradually decreases. In this case, CO replacement is required 2 The overall absorbent structure for acquisition has a problem of an increase in running cost.
Prior art literature
Patent literature
Patent document 1: international publication No. 2013/119929
Disclosure of Invention
Technical problem to be solved by the invention
The main object of the present invention is to provide a method for regenerating an acid gas adsorption apparatus, which can smoothly recover acid gas recovery performance and reduce operation costs, and a method for producing an acid gas adsorption apparatus, which can produce an acid gas adsorption apparatus having excellent acid gas recovery performance.
Technical scheme for solving technical problems
[1] The method for regenerating an acid gas adsorption apparatus according to an embodiment of the present invention includes: a step of supplying a gas containing an acid gas to an acid gas adsorption apparatus comprising a substrate and an acid gas adsorption layer, the acid gas adsorption layer being disposed on the surface of the substrate and comprising a porous support and the acid gas adsorption material, so as to be in contact with the acid gas adsorption layer, and adsorbing the acid gas to the acid gas adsorption material; a step of separating the acid gas from the acid gas adsorbing material; a step of removing an acid gas adsorption layer of an acid gas adsorption apparatus, which has been subjected to the step of adsorbing the acid gas and the step of removing the acid gas, from the surface of the substrate; and forming an acid gas adsorption layer containing a porous support and an acid gas adsorption material on the surface of the substrate from which the acid gas adsorption layer has been removed.
[2] One embodiment is the method for regenerating an acid gas adsorption apparatus according to item [1] above, wherein the acid gas is carbon dioxide.
[3] An embodiment is the method for regenerating an acid gas adsorption apparatus according to item [1] or [2], wherein the substrate is a honeycomb substrate having partition walls defining a plurality of cells, and the acid gas adsorption layer is formed on the surfaces of the partition walls.
[4] An embodiment is the method for regenerating an acid gas adsorption apparatus according to any one of items [1] to [3], wherein the material constituting the base material contains at least 1 selected from the group consisting of cordierite, alumina, mullite, silicon carbide, a silicon-silicon carbide composite material and silicon nitride, the porous support contains a metal-organic framework and/or activated carbon, and the acid gas adsorption apparatus is heated to burn off the acid gas adsorption layer in the step of removing the acid gas adsorption layer from the surface of the base material.
[5] One embodiment is the method for regenerating an acid gas adsorption apparatus according to item [4] above, wherein in the step of removing the acid gas adsorption layer from the surface of the substrate, the acid gas adsorption apparatus is heated to 400 ℃ or higher.
[6] An embodiment is the method for regenerating an acid gas adsorption apparatus according to any one of items [1] to [3], wherein the material constituting the base material contains at least 1 selected from the group consisting of alumina, silicon carbide, and a silicon-silicon carbide composite material, the porous support contains mesoporous silica and/or zeolite, and in the step of removing the acid gas adsorption layer from the surface of the base material, the acid solution is brought into contact with the acid gas adsorption layer to dissolve the acid gas adsorption layer.
[7] An embodiment is the method for regenerating an acid gas adsorption apparatus according to item [6] above, wherein the acid solution contains at least 1 selected from hydrofluoric acid, sulfuric acid, nitric acid, hydrochloric acid, and phosphoric acid.
[8] An embodiment is the method for regenerating an acid gas adsorption apparatus according to any one of items [1] to [3], wherein the material constituting the substrate comprises silicon carbide and/or a silicon-silicon carbide composite material, the porous support comprises mesoporous alumina, and in the step of removing the acid gas adsorption layer from the surface of the substrate, an alkaline solution is brought into contact with the acid gas adsorption layer to dissolve the acid gas adsorption layer.
[9] An embodiment is the method for regenerating an acid gas adsorption apparatus according to item [8], wherein the alkaline solution contains at least 1 selected from sodium hydroxide and potassium hydroxide.
[10] An embodiment is the method for regenerating an acid gas adsorption apparatus according to any one of items [1] to [3], wherein the acid gas adsorption layer comprises particles comprising the porous support and the acid gas adsorption material and an organic binder capable of binding the particles, the organic binder is soluble in an aprotic polar solvent and substantially insoluble in a protic polar solvent, and the aprotic polar solvent is brought into contact with the acid gas adsorption layer to dissolve the organic binder in the step of removing the acid gas adsorption layer from the surface of the substrate.
[11] An embodiment is the method for regenerating an acid gas adsorption apparatus according to any one of items [1] to [10], wherein in the step of adsorbing the acid gas by the acid gas adsorbent, the gas containing the acid gas supplied to the acid gas adsorption apparatus is air.
[12] Another aspect of the present invention relates to a method for producing an acid gas adsorption apparatus, comprising: a step of supplying a gas containing an acid gas to an acid gas adsorption apparatus comprising a substrate and an acid gas adsorption layer, the acid gas adsorption apparatus being in contact with the acid gas adsorption layer, the acid gas adsorption layer being disposed on the surface of the substrate and comprising a porous support and an acid gas adsorption material, and adsorbing the acid gas by the acid gas adsorption material; a step of separating the acid gas from the acid gas adsorbing material; a step of removing an acid gas adsorption layer of an acid gas adsorption apparatus, which has been subjected to the step of adsorbing the acid gas and the step of removing the acid gas, from the surface of the substrate; and forming an acid gas adsorption layer containing a porous support and an acid gas adsorption material on the surface of the substrate from which the acid gas adsorption layer has been removed.
[13] An embodiment is the method for producing an acid gas adsorption apparatus according to item [12] above, wherein the acid gas is carbon dioxide.
Effects of the invention
According to the embodiment of the present invention, a method for regenerating an acid gas adsorption apparatus, which can smoothly recover acid gas recovery performance and can reduce operation costs, and a method for producing an acid gas adsorption apparatus, which can produce an acid gas adsorption apparatus having excellent acid gas recovery performance, can be realized.
Drawings
Fig. 1 is a schematic perspective view of a carbon dioxide adsorbing device according to an embodiment of the present invention.
Fig. 2 is a schematic cross-sectional view of the carbon dioxide adsorbing device shown in fig. 1.
Fig. 3 is a schematic perspective view of the carbon dioxide adsorbing layer removed from the carbon dioxide adsorbing device shown in fig. 1.
Detailed Description
Embodiments of the present invention will be described below with reference to the drawings, but the present invention is not limited to these embodiments.
A. Outline of regeneration method of acid gas adsorption device
Fig. 1 is a schematic perspective view of a carbon dioxide adsorbing device according to an embodiment of the present invention; FIG. 2 is a schematic cross-sectional view of the carbon dioxide adsorbing device of FIG. 1; fig. 3 is a schematic perspective view of the carbon dioxide adsorbing layer removed from the carbon dioxide adsorbing device shown in fig. 1.
The method for regenerating an acid gas adsorption apparatus according to one embodiment of the present invention includes: a step (adsorption step) of supplying a gas containing an acid gas to an acid gas adsorption apparatus 100 provided with a substrate 1 and an acid gas adsorption layer 15, the acid gas adsorption apparatus being configured to contact the acid gas adsorption layer 15, wherein the acid gas adsorption layer 15 is disposed on the surface of the substrate 1 and contains a porous support and an acid gas adsorbent, and the acid gas adsorbent adsorbs the acid gas; a step (separation step) of separating the acid gas from the acid gas adsorbing material; a step (removal step) of removing the acid gas adsorption layer 15 of the acid gas adsorption apparatus 100, which has been subjected to the adsorption step and the separation step, from the surface of the substrate; and a step (reforming step) of forming an acid gas adsorption layer 15 containing a porous support and an acid gas adsorbent on the surface of the substrate 1 from which the acid gas adsorption layer 15 has been removed.
The present inventors have found that the lifetime of a base material is longer than that of an acid gas adsorbing material, and completed the present invention. More specifically, the acid gas adsorption layer of the acid gas adsorption apparatus having been subjected to the adsorption step and the desorption step is removed from the surface of the substrate, and then a new acid gas adsorption layer is formed on the surface of the substrate. Thereby regenerating the acid gas adsorption device. Therefore, the substrate can be reused, and the excellent acid gas recovery performance can be smoothly recovered. As a result, the running cost can be reduced.
Examples of the acid gas include carbon dioxide (CO) 2 ) Hydrogen sulfide, sulfur dioxide, nitrogen dioxide, and hydrogen chloride.
In one embodiment, the acid gas is carbon dioxide (CO 2 ). In the present embodiment, the acid gas adsorption apparatus 100 is a carbon dioxide adsorption apparatus 100, the acid gas adsorption layer 15 is a carbon dioxide adsorption layer 15, and the acid gas adsorption material is a carbon dioxide adsorption material. The carbon dioxide adsorbing device 100, which is an embodiment of the acid gas adsorbing device, will be described in detail below.
B. Carbon dioxide adsorption device
As described above, the carbon dioxide adsorbing device 100 includes the substrate 1 and the carbon dioxide adsorbing layer 15. The structure of the base material 1 is not particularly limited, and examples thereof include a filter structure such as a honeycomb structure and a filter cloth; particle structure, etc. The carbon dioxide adsorbing layer 15 is not particularly limited as long as it is disposed on the surface of the base material 1.
B-1. Substrate (Honeycomb substrate)
In one embodiment, the substrate 1 is a honeycomb substrate 10 having a plurality of cells 14.
The cells 14 extend in the longitudinal direction (axial direction) of the honeycomb substrate 10 from the first end face 1a (inflow end face) to the second end face 1b (outflow end face) of the honeycomb substrate 10 (see fig. 2). The cells 14 have any suitable shape in cross section in a direction orthogonal to the longitudinal direction of the honeycomb substrate 10. Examples of the cross-sectional shape of the cell include a triangle, a quadrangle, a pentagon, a polygon of hexagonal shape or more, a circle, and an ellipse. The cross-sectional shape and size of the cells may be all the same or may be at least partially different. Among the cross-sectional shapes of such cells, hexagonal shapes and tetragonal shapes are preferable, and square shapes, rectangular shapes and hexagonal shapes are more preferable.
The cell density (i.e., the number of cells 14 per unit area) in the cross section in the direction orthogonal to the longitudinal direction of the honeycomb substrate may be appropriately set according to the purpose. The unit density may be, for example, 4 units/cm 2 About 320 units/cm 2 . If the cell density is in such a range, the strength of the honeycomb substrate and the effective GSA (geometric surface area) can be sufficiently ensured.
The honeycomb substrate 10 has any suitable shape (overall shape). Examples of the shape of the honeycomb substrate include a cylindrical shape having a circular bottom surface, an elliptic cylindrical shape having an elliptic bottom surface, a polygonal prismatic shape having a polygonal bottom surface, and an amorphous cylindrical shape having an irregular bottom surface. The honeycomb substrate 10 illustrated in the drawing has a cylindrical shape. The outer diameter and length of the honeycomb substrate may be appropriately set according to the purpose. Although not shown, the honeycomb substrate may have a hollow region at its center portion in a cross section in a direction orthogonal to the longitudinal direction.
The honeycomb substrate 10 typically includes an outer peripheral wall 11 and a partition wall 13 located inside the outer peripheral wall 11. In the illustrated example, the outer peripheral wall 11 is integrally formed with the partition wall 13. The peripheral wall 11 and the partition wall 13 may also be independent.
The outer peripheral wall 11 has a cylindrical shape. The thickness of the outer peripheral wall 11 can be arbitrarily and appropriately set. The thickness of the outer peripheral wall 11 may be, for example, 0.1mm to 10mm.
The partition wall 13 defines a plurality of cells 14. More specifically, the partition wall 13 has a first partition wall 13a and a second partition wall 13b orthogonal to each other, and the first partition wall 13a and the second partition wall 13b define a plurality of cells 14. The cross-sectional shape of the unit 14 is quadrangular except for portions where the first partition wall 13a and the second partition wall 13b meet the outer peripheral wall 11. The structure of the partition wall is not limited to the partition wall 13 described above. The partition wall may also have a first partition wall extending in the radial direction and a second partition wall extending in the circumferential direction, which define a plurality of cells.
The thickness of the partition walls 13 may be appropriately set according to the use of the honeycomb substrate. The thickness of the partition wall 13 is typically thinner than the thickness of the outer peripheral wall 11. The thickness of the partition wall 13 may be, for example, 0.03mm to 0.6mm. The thickness of the partition wall is measured by, for example, cross-sectional observation using SEM (scanning electron microscope). If the thickness of the partition wall is in such a range, the mechanical strength of the honeycomb substrate can be made sufficient, and the opening area (the total area of the cells in the cross section) can be made sufficient.
The porosity of the partition wall 13 can be appropriately set according to the purpose. The porosity of the partition wall 13 is, for example, 15% or more, preferably 20% or more, for example, 70% or less, preferably 45% or less. The porosity can be measured by, for example, mercury porosimetry.
The density of the partition wall 13 may be appropriately set according to the purpose. Their density is, for example, 1.7g/cm 3 The above is preferably 1.8g/cm 3 Above, for example, 2.8g/cm 3 Hereinafter, it is preferably 2.6g/cm 3 The following is given. The density can be measured by, for example, mercury porosimetry.
As a material constituting the partition wall 13, ceramics are typically exemplified. Examples of the ceramics include silicon carbide, silicon-silicon carbide-based composites, cordierite, mullite, alumina, silicon nitride, spinel, silicon carbide-cordierite-based composites, lithium aluminosilicate, and aluminum titanate. The materials constituting the partition wall may be used alone or in combination. Among the materials constituting the partition walls, cordierite, alumina, mullite, silicon carbide, a silicon-silicon carbide-based composite material, and silicon nitride are preferable, and silicon carbide and a silicon-silicon carbide-based composite material are more preferable.
Such a honeycomb substrate 10 can be typically produced by the following method. First, a binder and water or an organic solvent are added to a material powder containing the ceramic powder as necessary, the resulting mixture is kneaded to prepare a green clay, the green clay is molded (typically, extrusion molded) into a desired shape, and then the green clay is dried and fired as necessary to produce the honeycomb substrate 10. In the firing, for example, the firing is performed at 1200 to 1500 ℃. The firing time is, for example, 1 to 20 hours.
B-2 carbon dioxide adsorption layer
In one embodiment, the carbon dioxide adsorbing layer 15 is formed on the surface of the partition wall 13. In the honeycomb substrate 10, a gas flow path 16 is formed in a portion (typically, a central portion) of the cross section of the cell 14 where the carbon dioxide adsorbing layer 15 is not formed. The carbon dioxide adsorbing layer 15 may be formed on the entire inner surface of the partition wall 13 (that is, so as to surround the gas flow path 16) as in the illustrated example, or may be formed on a part of the surface of the partition wall. If the carbon dioxide adsorbing layer 15 is formed on the entire inner surface of the partition wall 13, CO can be realized 2 Is improved in the removal efficiency.
The gas flow path 16 extends from the first end face 1a (inflow end face) to the second end face 1b (outflow end face) as in the case of the cell 14. The cross-sectional shape of the gas flow path 16 may be the same as that of the cell 14 described above, and may be a hexagon, a quadrangle, and more preferably a square, a rectangle, or a hexagon. The cross-sectional shape and size of the gas flow path 16 may be the same or may be at least partially different.
The carbon dioxide adsorbing layer 15 includes a porous support and a carbon dioxide adsorbing material. In the carbon dioxide adsorbing layer 15, the porous support forms mesopores.
Examples of the porous carrier include metal-organic frameworks (MOFs) such as MOF-74, MOF-200 and MOF-210; activated carbon; nitrogen-doped carbon; mesoporous silica; mesoporous alumina; a zeolite; the carbon nanotubes preferably include Metal Organic Frameworks (MOFs), mesoporous silica, and mesoporous alumina.
The BET specific surface area of the porous support is, for example, 50m 2 Preferably 500m or more per gram 2 And/g. If the surface area of the porous carrier is not less than the lower limit, the carbon dioxide adsorbent can be sufficiently supported, and CO can be realized 2 The absorption rate is improved. The upper limit of the BET specific surface area of the porous support is typically 2000m 2 And/g or less.
The content of the porous carrier in the carbon dioxide adsorbing layer 15 is, for example, 0.1 mass% or more, preferably 10 mass% or more, for example, 70 mass% or less, preferably 50 mass% or less.
The thickness of the carbon dioxide adsorbing layer 15 is not particularly limited, and is, for example, 10 μm or more, preferably 50 μm or more, for example, 1000 μm or less, preferably 500 μm or less.
The carbon dioxide adsorbent is typically supported on a porous support and is present facing the gas flow path 16.
As the carbon dioxide adsorbing material, a material capable of adsorbing and desorbing CO can be used 2 Any suitable compound of (a). Examples of the carbon dioxide adsorbent include: a nitrogen-containing compound described later; basic compounds such as sodium hydroxide and potassium hydroxide; carbonates such as calcium carbonate and potassium carbonate; bicarbonate salts such as calcium bicarbonate and potassium bicarbonate; metal Organic Frameworks (MOFs) such as MOF-74, MOF-200, MOF-210, etc.; a zeolite; activated carbon; nitrogen-doped carbon, and the like. The carbon dioxide adsorbing material is preferably a material different from the porous carrier.
Among the carbon dioxide adsorbing materials, nitrogen-containing compounds are more preferably exemplified. More specifically, examples of the nitrogen-containing compound include amine compounds such as monoethanolamine, diethanolamine, triethanolamine, N- (3-aminopropyl) diethanolamine, aminopropyl trimethoxysilane, polyvinylamine, methyldiethylamine, tetraethylenepentamine, and the like; piperazine compounds such as 1- (2-hydroxyethyl) piperazine; aminosilane coupling agents such as polyethylenimine-trimethoxysilane, aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, and N- (2-aminoethyl) -3-aminopropyl-trimethoxysilane; organic polymers having primary to tertiary amino groups such as polyamidoamine, polyethyleneimine, and polystyrene having amino groups; organic monomers having primary to tertiary amino groups such as ethyleneimine and amino-group-added styrene; an organic/inorganic compound having an amino group as a substituent. The carbon dioxide adsorbing materials may be used alone or in combination.
The content ratio of the carbon dioxide adsorbing material in the carbon dioxide adsorbing layer 15 is, for example, 0.1 mass% or more, and preferably 0.5 mass% or more. When the content ratio of the carbon dioxide adsorbent is not less than the lower limit, excellent CO can be stably ensured 2 Absorption rate. The upper limit of the content ratio of the carbon dioxide adsorbing material is typically 30 mass% or less.
Such a carbon dioxide adsorbing layer 15 can be typically produced by the following method. First, a dispersion liquid of the porous carrier is prepared by dispersing the porous carrier in a dispersion medium, and a carbon dioxide adsorbent is added to the dispersion liquid. Next, a dispersion liquid containing a porous support and a carbon dioxide adsorbing material is applied to the substrate 1 (specifically, the partition wall 13), and then the coating film is dried and, if necessary, sintered to form the carbon dioxide adsorbing layer 15. The method for forming the carbon dioxide adsorbing layer will be described in detail in the description of the reforming step in item E.
The method for producing the carbon dioxide adsorbing layer 15 is not limited to the above method. For example, a dispersion of the porous support in which the porous support is dispersed in a dispersion medium is prepared, and the dispersion is applied to the substrate 1 (specifically, the partition wall 13), and then the coated film is dried and sintered to form a support-containing film. Thereafter, the liquid carbon dioxide adsorbent or a solution of the carbon dioxide adsorbent is applied to the carrier-containing film at normal temperature and pressure. Thus, the carbon dioxide adsorbing material is impregnated into and supported by the porous support containing the support membrane. Thus, the carbon dioxide adsorbing layer 15 is formed.
In another embodiment, the carbon dioxide adsorbing layer 15 includes: particles comprising the carbon dioxide adsorbent and the porous carrier, and an organic binder. The particles having the carbon dioxide adsorbing material and the porous carrier have carbon dioxide adsorbing ability, and are hereinafter referred to as carbon dioxide adsorbing ability particles. The organic binder is capable of binding carbon dioxide adsorbing capacity particles, typically being fixed to the substrate 1. The organic binder is capable of being dissolved in an aprotic polar solvent and is substantially insoluble in a protic polar solvent. That is, the organic binder has resistance (water resistance) to water as a protic polar solvent. The organic binder is substantially insoluble in the polar aprotic solvent and has water resistance, and thus swelling of the organic binder due to, for example, water vapor in the atmosphere can be suppressed. Therefore, the volume expansion and/or the decrease in strength of the organic binder can be suppressed, and further, the change in the structure of the particles having carbon dioxide adsorption ability can be suppressed by the organic binder binding and retaining. As a result, the excellent carbon dioxide adsorption ability can be maintained regardless of the use environment.
The surface of the carbon dioxide adsorbing layer 15 opposite to the partition wall 13 preferably has a three-dimensional mesh structure or a porous layered structure. Therefore, the acid gas such as carbon dioxide can be efficiently diffused from the surface of the carbon dioxide adsorbing layer to the inside. In particular, since the organic binder has water resistance, such a microstructure can be stably maintained on a surface that can be brought into contact with an acid gas regardless of the use environment.
The carbon dioxide adsorbing capacity particles are typically in a solid state at normal temperature and normal pressure (23 ℃ C., 0.1 MPa). The carbon dioxide adsorbing layer 15 contains a plurality of carbon dioxide adsorbing capacity particles. The carbon dioxide adsorbing ability particles may be primary particles or secondary particles formed by agglomerating a plurality of primary particles in a state of being contained in the carbon dioxide adsorbing layer 15.
Among the carbon dioxide adsorbing materials contained in the carbon dioxide adsorbing capacity particles, the nitrogen-containing compound is preferable, and the organic monomer having a primary to tertiary amino group and the organic polymer having a primary to tertiary amino group are more preferable. The weight average molecular weight Mw (converted to polystyrene) of the organic polymer is, for example, 1000 or more, preferably 5 ten thousand or more, for example, 100 ten thousand or less, preferably 30 ten thousand or less.
In one embodiment, the carbon dioxide adsorbing material comprised by the carbon dioxide adsorbing capacity particles is substantially insoluble in a protic polar solvent (typically water) and an aprotic polar solvent.
The solubility of the carbon dioxide adsorbent material in water is, for example, 0.1g/100g-H 2 O or less, preferably 0.05g/100g-H 2 O is less than or equal to. When the solubility of the carbon dioxide adsorbent in water is not more than the upper limit, excellent water resistance can be stably imparted to the carbon dioxide adsorbent. In addition, the lower limit of the solubility of the carbon dioxide adsorbing material to water is typically 0.01g/100g-H 2 O or more.
The solubility of the carbon dioxide adsorbent in the aprotic polar solvent is, for example, 1g/100 g-aprotic polar solvent or less, and preferably 0.5g/100 g-aprotic polar solvent or less. If the solubility of the carbon dioxide adsorbent in the aprotic polar solvent is not more than the upper limit, the carbon dioxide adsorbent can be prevented from being dissolved in the aprotic polar solvent during the production of the acid gas adsorption device. The lower limit of the solubility of the carbon dioxide adsorbent in the aprotic polar solvent is typically 0.01g/100g or more of the aprotic polar solvent.
The solubility parameter of the carbon dioxide adsorbent is, for example, 7 or more, preferably 8 or more, for example, 20 or less, preferably 15 or less. The solubility parameter can be calculated by the Hildebrand method, for example.
As the organic binder, any suitable organic compound capable of binding carbon dioxide adsorption capacity particles may be used. The organic binder is capable of being dissolved in an aprotic polar solvent and is substantially insoluble in a protic polar solvent. Examples of the organic binder include fluoropolymers such as polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), perfluoroalkoxyalkane (PFA), perfluoroethylene propylene copolymer (FEP), and ethylene tetrafluoroethylene copolymer (ETFE); amorphous plastics such as Polyethersulfone (PES). The organic binders may be used alone or in combination.
Among the organic binders, at least water as a poor solvent (substantially water-insoluble organic binders) is preferable, fluoropolymers are more preferable, and polyvinylidene fluoride is even more preferable. If the organic binder contains a fluoropolymer (polyvinylidene fluoride), excellent heat resistance and water resistance can be imparted to the carbon dioxide adsorbing device.
The solubility of the organic binder in the protic polar solvent (typically water) is, for example, 0.1g/100 g-protic polar solvent or less, preferably 0.05g/100 g-protic polar solvent or less. If the solubility of the organic binder in the polar protic solvent (typically water) is not more than the upper limit, excellent water resistance can be stably imparted to the acid gas adsorption device. In addition, the lower limit of the solubility of the organic binder to the protic polar solvent (typically water) is typically 0.01g/100g-H 2 O or more.
The solubility parameter of the organic binder is, for example, 9 or more, preferably 10 or more, for example, 15 or less, preferably 13 or less.
The carbon dioxide adsorbing layer 15 may contain any suitable additive material in addition to the carbon dioxide adsorbing capacity particles and the organic binder.
The carbon dioxide adsorbing layer 15 contains, for example, 30% by volume or more, preferably 50% by volume or more, for example, 100% by volume or less, preferably 99% by volume or less of the total of the carbon dioxide adsorbing capacity particles and the organic binder. The volume% can be measured by, for example, microstructure observation and elemental analysis.
The content ratio of the carbon dioxide adsorbing capacity particles in the carbon dioxide adsorbing layer 15 is, for example, 5% by volume or more, and preferably 30% by volume or more. If the content ratio of the carbon dioxide adsorbing ability particles is not less than the lower limit, the carbon dioxide adsorbing performance of the carbon dioxide adsorbing device can be sufficiently ensured. The upper limit of the content ratio of the carbon dioxide adsorption capacity particles is typically 85% by volume or less.
The content of the organic binder in the carbon dioxide adsorbing layer 15 is, for example, 5% by volume or more, and preferably 15% by volume or more. If the content ratio of the organic binder is not less than the lower limit, the carbon dioxide adsorbing ability particles can be prevented from falling off from the carbon dioxide adsorbing layer in the adsorption step and/or the desorption step described later. The upper limit of the content ratio of the organic binder is typically 70% by volume or less.
The carbon dioxide adsorbing layer 15 typically has communicating pores. The porosity of the carbon dioxide adsorbing layer 15 is, for example, 10% to 90%, preferably 10% to 60%, more preferably 15% to 40%.
The carbon dioxide adsorbing layer 15 containing carbon dioxide adsorbing capacity particles and an organic binder can be typically produced by the following method. First, the organic binder is dissolved in an aprotic polar solvent to prepare a binder solution, the carbon dioxide adsorbent particles are dispersed in the binder solution, the binder solution is applied to the surface of the substrate 1 (specifically, the partition wall 13) to form a precursor film, and the aprotic polar solvent contained in the precursor film is replaced with a poor solvent for the organic binder to form the carbon dioxide adsorbent layer 15. The method for forming the carbon dioxide adsorbing layer will be described in detail in the description of the reforming step in item E.
The method for producing the carbon dioxide adsorbing layer 15 including the carbon dioxide adsorbing capability particles and the organic binder is not limited to the above method. For example, the above-mentioned porous support may be dispersed in the above-mentioned binder solution, the binder solution is applied to the surface of the substrate 1 (specifically, the partition wall 13) to form a precursor film, the aprotic polar solvent contained in the precursor film is replaced with a poor solvent for the organic binder to form a support-containing film containing the porous support and the organic binder, and then the carbon dioxide adsorbent is supported on the porous support contained in the support-containing film to form the carbon dioxide adsorbent layer 15.
C. Adsorption step and separation step
As described above, the method for regenerating the carbon dioxide adsorbing device according to one embodiment includes adsorbing CO with the carbon dioxide adsorbing material provided in the carbon dioxide adsorbing device 100 2 Adsorption step (2) and CO production 2 And a separation step of separating the carbon dioxide adsorbent.
In the adsorption step, typically, CO is contained 2 Is a gas (CO-containing) 2 Gas) flows through the gas flow path 16 of the honeycomb substrate, and contacts the carbon dioxide adsorbing layer 15. In one embodiment, the composition contains CO 2 The gas is air (atmosphere). Containing CO 2 CO in gas 2 The concentration is, for example, 100ppm or more and 2% by volume or less. Containing CO 2 Gases other than CO 2 In addition, nitrogen is typically included. CO-containing in the adsorption step 2 The temperature of the gas is, for example, 0 ℃ or higher and 40 ℃ or lower. CO-containing in the adsorption step 2 The pressure of the gas being, for example, 0.3X10 5 Pa or more and 2.0X10 5 Pa or below. CO-containing in the adsorption step 2 The relative humidity RH of the gas is, for example, 10% RH or more and 60% RH or less. The time for performing the adsorption step is, for example, 15 minutes to 3 hours. CO-containing in the adsorption step 2 The flow rate of the gas is, for example, 0.5 m/sec or more and 5 m/sec or less.
Thereby, the carbon dioxide adsorbent present facing the gas flow path 16 adsorbs CO 2 . CO in the adsorption step 2 Recovery rate (=100- (CO in gas having passed through the gas flow path) 2 concentration/CO in gas before flowing into gas flow path 2 Concentration×100)), for example, is 80% or more, preferably 85% or more, more preferably 90% or more, for example, 100% or less.
The desorption step (sometimes referred to as a desorption step) is performed after the adsorption step. In the desorption step, typically, a carbon dioxide adsorbent is heated, and the desorbed CO is sucked and recovered by a pump or the like 2 Or to recycle CO 2 Pumping into carbon dioxide adsorption device again, heating, and recovering separated CO 2 。
The temperature in the separation step is, for example, more than 40 ℃, preferably 70 ℃ or more, for example, 200 ℃ or less, preferably 110 ℃ or less. The release step is performed for 1 minute or more and 1 hour or less, for example.
Thereby, CO held by the carbon dioxide adsorbing material 2 From dioxygenThe carbon-adsorbing material is separated (released, desorbed). Thus, CO can be recovered 2 Can be used for various purposes (e.g., methanation).
These adsorption step and separation step are preferably repeated. In one embodiment, the cycle of the adsorption step and the desorption step may be performed, for example, 10 times or more, preferably 30 times or more, more preferably 50 times or more, and still more preferably 100 times or more.
D. Removal step
In one embodiment, the removal step is performed after the adsorption step and the desorption step are performed (preferably after the cycle of the adsorption step and the desorption step is performed within the above-described range).
In the removal step, the carbon dioxide adsorbing layer 15 of the carbon dioxide adsorbing device having undergone the adsorption step and the separation step is removed from the surface of the substrate 1 (typically, the partition wall 13).
The carbon dioxide adsorbing layer may be removed by any suitable method depending on the material of the substrate and the type of porous carrier. Examples of the removal method include: a method (burning-out method) of burning out the carbon dioxide adsorbing layer by heating the carbon dioxide adsorbing device; a method of bringing an acidic solution into contact with the carbon dioxide adsorbent layer to dissolve the carbon dioxide adsorbent layer (acid dissolution method); a method of bringing an alkaline solution into contact with the carbon dioxide adsorbent layer to dissolve the carbon dioxide adsorbent layer (alkali dissolution method). In the removal step, a method of bringing an organic solvent into contact with the carbon dioxide adsorbent layer and dissolving only the carbon dioxide adsorbent in the organic solvent to remove the carbon dioxide adsorbent has also been studied. However, in such a method, the carbon dioxide adsorbent cannot be sufficiently removed from the carbon dioxide adsorbent layer, and there is a possibility that the deteriorated carbon dioxide adsorbent remains. Therefore, if the carbon dioxide adsorbing layer is formed again by performing the reforming step after the removal step, the deteriorated carbon dioxide adsorbing material may adversely affect the newly formed carbon dioxide adsorbing layer. In addition, in the case where the porous support is fixed to the base material by drying and/or sintering, the porous support cannot be removed in the organic solvent, and therefore, if the reforming step is performed after the removal step, a carbon dioxide adsorbing layer is formed on the remaining porous support, and the gas flow path may be narrowed. Therefore, in a carbon dioxide adsorption device in which a carbon dioxide adsorption layer including a porous support and a carbon dioxide adsorbent and in which the porous support is fixed to a substrate is disposed on the substrate, the removal step using an organic solvent is not suitable. On the other hand, in the case where the carbon dioxide adsorbing layer contains carbon dioxide adsorbing ability particles and an organic binder, and the organic binder is fixed to the substrate, the carbon dioxide adsorbing layer can be removed by bringing an aprotic polar solvent into contact with the carbon dioxide adsorbing layer (aprotic polar solvent dissolution method).
D-1 burn-off method
When the material constituting the substrate 1 (honeycomb substrate 10) includes at least 1 selected from the group consisting of cordierite, alumina, mullite, silicon carbide, a silicon-silicon carbide composite material, and silicon nitride, and the porous support includes a metal-organic framework and/or activated carbon, the firing method is preferably selected in the removal step.
In the calcination method, a carbon dioxide adsorbing device having been subjected to the adsorption step and the desorption step is heated to burn off the carbon dioxide adsorbing layer (porous carrier and carbon dioxide adsorbent). The heating temperature is, for example, 400℃or more, preferably 500℃or more, for example, 700℃or less, preferably 650℃or less. The heating time is not particularly limited as long as the carbon dioxide adsorbing layer can be removed, and is, for example, 1 hour or more and 48 hours or less.
D-2 acid dissolution method
When the material constituting the substrate 1 (honeycomb substrate 10) contains at least 1 selected from the group consisting of alumina, silicon carbide and a silicon-silicon carbide composite material, and the porous support contains mesoporous silica and/or zeolite, an acid dissolution method is preferably selected in the removal step.
In the acid dissolution method, the acidic solution is circulated through the gas flow path 16 of the carbon dioxide adsorbing device 100 in which the adsorption step and the desorption step are performed, and the acidic solution is brought into contact with the carbon dioxide adsorbing layer 15. Thereby, the carbon dioxide adsorbing layer (porous carrier and carbon dioxide adsorbing material) is dissolved in the acidic solution and removed.
The acidic solution is typically an aqueous solution of an acid component. The acid dissociation constant pKa of the acid component in water is, for example, -4.0 or more, preferably, -3.7 or more. For example, 3 or less, preferably 2.7 or less. Specific examples of the acid component include hydrofluoric acid, sulfuric acid, nitric acid, hydrochloric acid, and phosphoric acid. The concentration of the acid component in the acidic solution is, for example, 30 mass% or more, preferably 70 mass% or more, for example, 100 mass% or less, preferably 90 mass% or less.
D-3 alkali dissolution
When the material constituting the substrate 1 (honeycomb substrate 10) includes silicon carbide and/or a silicon-silicon carbide composite material and the porous support includes mesoporous aluminum, alkali dissolution is preferably selected in the removal step.
In the alkali dissolution method, an alkaline solution is circulated through the gas flow path 16 of the carbon dioxide adsorbing device 100 in which the adsorption step and the desorption step are performed, and the alkaline solution is brought into contact with the carbon dioxide adsorbing layer 15. Thereby, the carbon dioxide adsorbing layer (porous carrier and carbon dioxide adsorbing material) is dissolved in the alkaline solution and removed.
The alkaline solution is typically an aqueous solution of an alkaline component. The alkali dissociation constant pKb of the alkali component in water is, for example, 0 or more, preferably 1 or more, for example, 3 or less, preferably 2.5 or less. The alkali component includes, specifically, sodium hydroxide and potassium hydroxide. The concentration of the alkali component in the alkaline solution is, for example, 10 mass% or more, preferably 20 mass% or more, for example, 100 mass% or less, preferably 90 mass% or less.
D-4 aprotic polar solvent dissolution method
In the case where the carbon dioxide adsorbing layer contains carbon dioxide adsorbing capability particles and an organic binder, an aprotic polar solvent dissolution method is preferably selected in the removal step. In the aprotic polar solvent dissolution method, the aprotic polar solvent is circulated through the gas flow path 16 of the carbon dioxide adsorbing device 100 in which the adsorption step and the desorption step are performed, and the aprotic polar solvent is brought into contact with the carbon dioxide adsorbing layer 15. Thus, the organic binder contained in the carbon dioxide adsorbing layer is dissolved in the aprotic polar solvent, and the carbon dioxide adsorbing ability particles are detached from the substrate. Thereby, the carbon dioxide adsorption layer is removed.
The aprotic polar solvent from which the carbon dioxide adsorbing layer is removed contains carbon dioxide adsorbing capacity particles and an organic binder. Therefore, after removing the carbon dioxide adsorbing ability particles from the aprotic polar solvent containing the carbon dioxide adsorbing ability particles and the organic binder by filtration or the like, only the organic binder may be precipitated and reused by adding the protic polar solvent to the aprotic polar solvent containing the organic binder.
As the aprotic polar solvent, any suitable organic solvent may be used. Examples of aprotic polar solvents include N-methyl-2-pyrrolidone (NMP), dimethylformamide (DMF), dimethylacetamide (DMA), dimethylsulfoxide (DMSO), and Tetrahydrofuran (THF). Aprotic polar solvents may be used alone or in combination. Among aprotic polar solvents, N-methyl-2-pyrrolidone (NMP) is preferable. If the aprotic polar solvent contains NMP, the organic binder (particularly PVDF) can be more smoothly dissolved, and the carbon dioxide adsorption layer can be smoothly removed with low energy.
As described above, as shown in fig. 3, the carbon dioxide adsorbing layer (porous support and carbon dioxide adsorbing material) is removed from the surface of the substrate 1 (typically, the partition wall 13). The surface of the substrate 1 (typically, the partition wall 13) is cleaned as needed.
E. Reforming step
In one embodiment, the reforming step is performed after the removal step. In the reforming step, the carbon dioxide adsorbing layer 15 is newly formed on the surface of the substrate 1 (typically, the partition wall 13) from which the carbon dioxide adsorbing layer 15 is removed.
In the reforming step, for example, first, a dispersion slurry of the porous support is prepared in which the porous support is dispersed in a dispersion medium. Examples of the dispersion medium include water, alcohols, and glycols. The dispersion medium may be used alone or in combination. Among the dispersion media, an aqueous solvent (a mixed solvent of water and water) is preferable.
The concentration of the porous carrier in the dispersion slurry is, for example, 10 mass% or more, preferably 15 mass% or more, for example, 50 mass% or less, preferably 30 mass% or less. By adjusting the concentration of the porous carrier to the above range, the carbon dioxide adsorbing layer can be stably formed on the substrate.
Next, a carbon dioxide adsorbing material is added to the dispersion slurry. The concentration of the carbon dioxide adsorbing material in the dispersion slurry is, for example, 5 mass% or more, preferably 10 mass% or more, for example, 30 mass% or less, preferably 20 mass% or less.
Next, the dispersion slurry containing the porous carrier and the carbon dioxide adsorbing material is applied to the substrate 1 (specifically, the partition wall 13) by any suitable method. In one embodiment, the dispersion is circulated within the cells 14 of the honeycomb substrate 10. This makes it possible to smoothly apply the dispersion liquid to the surface of the partition wall. The number of applications of the dispersion slurry is appropriately changed according to the thickness of the carbon dioxide adsorbing layer.
Subsequently, the honeycomb substrate coated with the dispersion slurry is heated to, for example, 50 to 200 ℃, and the coating film is dried and, if necessary, sintered. The drying time is, for example, 0.5 to 24 hours. In the sintering, for example, the sintering is performed at 80 to 300 ℃. The sintering time is, for example, 1 hour or more and 100 hours or less.
Thereby, a carbon dioxide adsorbing layer including the porous carrier and the carbon dioxide adsorbing material is formed again on the substrate 1 (specifically, the partition wall 13).
In another embodiment, for example, first, the dispersion slurry is applied to the substrate 1 (specifically, the partition wall 13) in the same manner as described above. Then, the coating film on the substrate coated with the dispersion slurry is dried, and then heated to, for example, 400 ℃ to 800 ℃ and below, and sintered. The sintering time is, for example, 1 hour or more and 100 hours or less. Thus, a carrier-containing film is formed. Next, the carbon dioxide adsorbent or a solution of the carbon dioxide adsorbent, which is liquid at normal temperature and pressure, is applied to the carrier-containing film in the same manner as described above. Thus, the carbon dioxide adsorbing material is impregnated into and supported by the porous support containing the support membrane. In this way, a carbon dioxide adsorbing layer including the porous carrier and the carbon dioxide adsorbing material may be formed again on the substrate 1 (specifically, the partition wall 13).
In yet another embodiment, first, the organic binder is dissolved in the aprotic polar solvent to prepare a binder solution. The aprotic polar solvent is capable of dissolving the organic binder, and the carbon dioxide adsorbing capacity particles (more specifically, carbon dioxide adsorbing materials) are insoluble.
The solubility parameter distance of the organic binder and the aprotic polar solvent is, for example, 3 or less, preferably 2 or less. If the solubility parameter distance of the organic binder to the aprotic polar solvent is equal to or less than the upper limit, the organic binder can be dissolved in the aprotic polar solvent smoothly. The lower limit of the solubility parameter distance of the organic binder from the aprotic polar solvent is typically 0 or more.
The solubility parameter distance of the carbon dioxide adsorbing material to the aprotic polar solvent is, for example, 2 or more, preferably 3 or more, and more preferably 4 or more. If the solubility parameter distance of the carbon dioxide adsorbing material to the aprotic polar solvent is not less than the above lower limit, the carbon dioxide adsorbing material can be inhibited from dissolving in the aprotic polar solvent. The upper limit of the solubility parameter distance of the carbon dioxide adsorbing material from the aprotic polar solvent is typically 10 or less.
Next, the carbon dioxide adsorbing ability particles are added to the binder solution and dispersed.
The solution of the organic binder (particle-dispersed binder solution) as the aprotic polar solvent and in which the carbon dioxide adsorbing ability particles are dispersed is applied to the surface of the substrate 1 by any suitable method as described above.
Thus, the particle-dispersed binder solution is applied to the surface of the substrate 1 (typically, the surface of the partition wall 13) to form a precursor film. The precursor film comprises the carbon dioxide adsorbing capacity particles, the organic binder, and the aprotic polar solvent.
Next, the aprotic polar solvent contained in the precursor film is replaced with a poor solvent for the organic binder.
The poor solvent is more difficult to dissolve the organic binder than the aprotic polar solvent (good solvent), and the organic binder is substantially insoluble in the poor solvent. The solubility parameter distance of the organic binder from the poor solvent is typically greater than the solubility parameter distance of the organic binder from the aprotic polar solvent (good solvent). The solubility parameter distance between the organic binder and the poor solvent is, for example, 2 or more, preferably 3 or more, and more preferably 4 or more.
Examples of the poor solvent include: polar solvents with protonic properties such as alcohols (e.g., water, ethanol, butanol, isopropyl alcohol (IPA)), etc.; freons such as Hydrochlorofluorocarbons (HCFCs), hydrofluorocarbons (HFCs), and Hydrofluoroolefins (HFOs). The poor solvents may be used alone or in combination. Among the poor solvents, water is preferable.
By displacement of the aprotic polar solvent, a membrane stable in the protic solvent can be obtained.
As a result, the carbon dioxide adsorbing layer 15 including the carbon dioxide adsorbing capability particles and the organic binder can be formed again on the surface of the substrate 1 (typically, the surface of the partition wall 13). After that, the carbon dioxide adsorbing layer 15 is dried as necessary.
The step of reforming the carbon dioxide adsorbing layer containing the carbon dioxide adsorbing capacity particles and the organic binder is not limited to the above embodiment. For example, first, a binder solution is prepared in the same manner as described above. Next, the porous support is added to the binder solution and dispersed.
Thus, the porous carrier is dispersed in the binder solution, and the binder solution in which the porous carrier is dispersed (carrier-dispersed binder solution) is prepared.
Next, the carrier dispersion binder solution is coated on the surface of the substrate 1 by the coating method described above.
Thus, a carrier dispersion binder solution is applied to the surface of the substrate 1 (typically, the surface of the partition wall 13) to form a precursor film. The precursor film comprises the porous support, the organic binder, and the aprotic polar solvent.
Next, the aprotic polar solvent contained in the precursor film is replaced with the poor solvent.
Thus, a carrier-containing film is formed on the surface of the substrate 1 (typically, the surface of the partition wall 13). The carrier-containing film is then dried as necessary. The carrier-containing film contains the porous carrier and the organic binder.
Next, the carbon dioxide adsorbing material is supported on a porous support contained in the support-containing film. The carbon dioxide adsorbent used in the present embodiment is preferably liquid at normal temperature and pressure. More specifically, by the above-described coating method, a liquid carbon dioxide adsorbing material is coated on a carrier-containing film at normal temperature and pressure. Thus, the carbon dioxide adsorbing material permeates into and is supported by the porous support containing the support membrane, thereby forming carbon dioxide adsorbing capacity particles composed of the acid gas adsorbing compound and the porous support. That is, the carbon dioxide adsorbing layer 15 is composed of carbon dioxide adsorbing capacity particles and an organic binder.
In accordance with the above, the carbon dioxide adsorbing layer 15 including the carbon dioxide adsorbing capability particles and the organic binder can be formed again.
In accordance with the above, the carbon dioxide adsorbing device 100 is regenerated. The method for regenerating such a carbon dioxide adsorbent (acid gas adsorbent) is, in other words, a method for producing a carbon dioxide adsorbent (acid gas adsorbent) having a new carbon dioxide adsorbent layer (acid gas adsorbent). The method for producing a carbon dioxide adsorption device (acid gas adsorption device) comprises: the adsorption step; the above-mentioned disengaging step; the removing step; and a reforming step. In the method for producing a carbon dioxide adsorption device, excellent CO can be produced 2 A carbon dioxide adsorption device with recovery performance.
Industrial applicability
The regeneration method of the acid gas adsorption apparatus according to the embodiment of the present invention can be used for regeneration of an acid gas adsorption apparatus used for separation and recovery of an acid gas, and is particularly suitable for regeneration of a carbon dioxide adsorption apparatus used for a carbon dioxide recovery, utilization and storage (CCUS) cycle.
Description of the reference numerals
10 honeycomb substrate
13 dividing wall
14 units
15 carbon dioxide adsorption layer
100 carbon dioxide adsorption device
Claims (16)
1. A method for regenerating an acid gas adsorption apparatus, comprising:
a step of supplying a gas containing an acid gas to an acid gas adsorption apparatus including a base material and an acid gas adsorption layer, the acid gas adsorption apparatus being configured to be in contact with the acid gas adsorption layer, and adsorbing the acid gas to an acid gas adsorption material, wherein the acid gas adsorption layer is disposed on the surface of the base material and contains a porous support and the acid gas adsorption material;
a step of separating the acid gas from the acid gas adsorbing material;
a step of removing the acid gas adsorption layer of an acid gas adsorption apparatus, which is subjected to the step of adsorbing the acid gas and the step of removing the acid gas, from the surface of the base material; and
and forming an acid gas adsorption layer containing a porous support and an acid gas adsorption material on the surface of the substrate from which the acid gas adsorption layer has been removed.
2. The method for regenerating an acid gas adsorption apparatus of claim 1, wherein the acid gas is carbon dioxide.
3. The method for regenerating an acid gas adsorption apparatus according to claim 1 or 2, wherein the substrate is a honeycomb substrate having partition walls defining a plurality of cells,
The acid gas adsorption layer is formed on the surface of the partition wall.
4. The method for regenerating an acid gas adsorption apparatus according to claim 1 or 2, wherein,
the material constituting the substrate contains at least 1 selected from the group consisting of cordierite, alumina, mullite, silicon carbide, a silicon-silicon carbide-based composite material, and silicon nitride,
the porous carrier comprises a metal-organic framework and/or activated carbon,
in the step of removing the acid gas adsorption layer from the surface of the substrate, the acid gas adsorption device is heated to burn off the acid gas adsorption layer.
5. The method for regenerating an acid gas adsorption apparatus according to claim 4, wherein in the step of removing the acid gas adsorption layer from the surface of the substrate, the acid gas adsorption apparatus is heated to 400 ℃ or higher.
6. The method for regenerating an acid gas adsorption apparatus according to claim 3, wherein,
the material constituting the substrate contains at least 1 selected from the group consisting of cordierite, alumina, mullite, silicon carbide, a silicon-silicon carbide-based composite material, and silicon nitride,
the porous carrier comprises a metal-organic framework and/or activated carbon,
In the step of removing the acid gas adsorption layer from the surface of the substrate, the acid gas adsorption device is heated to burn off the acid gas adsorption layer.
7. The method for regenerating an acid gas adsorption apparatus according to claim 1 or 2, wherein,
the material constituting the substrate contains at least 1 selected from the group consisting of alumina, silicon carbide, and silicon-silicon carbide-based composite materials,
the porous support comprises mesoporous silica and/or zeolite,
in the step of removing the acid gas adsorption layer from the surface of the substrate, an acid solution is brought into contact with the acid gas adsorption layer to dissolve the acid gas adsorption layer.
8. The method for regenerating an acid gas adsorption apparatus according to claim 7, wherein the acid solution contains at least 1 selected from hydrofluoric acid, sulfuric acid, nitric acid, hydrochloric acid, or phosphoric acid.
9. The method for regenerating an acid gas adsorption apparatus according to claim 3, wherein,
the material constituting the substrate contains at least 1 selected from the group consisting of alumina, silicon carbide, and silicon-silicon carbide-based composite materials,
the porous support comprises mesoporous silica and/or zeolite,
In the step of removing the acid gas adsorption layer from the surface of the substrate, an acid solution is brought into contact with the acid gas adsorption layer to dissolve the acid gas adsorption layer.
10. The method for regenerating an acid gas adsorption apparatus according to claim 1 or 2, wherein,
the material constituting the substrate comprises silicon carbide and/or a silicon-silicon carbide-based composite material,
the porous support comprises mesoporous alumina,
in the step of removing the acid gas adsorption layer from the surface of the substrate, an alkaline solution is brought into contact with the acid gas adsorption layer to dissolve the acid gas adsorption layer.
11. The method for regenerating an acid gas adsorption apparatus of claim 10, wherein the alkaline solution comprises at least 1 selected from sodium hydroxide or potassium hydroxide.
12. The method for regenerating an acid gas adsorption apparatus according to claim 3, wherein,
the material constituting the substrate comprises silicon carbide and/or a silicon-silicon carbide-based composite material,
the porous support comprises mesoporous alumina,
in the step of removing the acid gas adsorption layer from the surface of the substrate, an alkaline solution is brought into contact with the acid gas adsorption layer to dissolve the acid gas adsorption layer.
13. The method for regenerating an acid gas adsorption apparatus according to claim 3, wherein,
the acid gas adsorbing layer comprises particles comprising the porous support and the acid gas adsorbing material,
the organic binder is capable of being dissolved in an aprotic polar solvent and is substantially insoluble in a protic polar solvent,
in the step of removing the acid gas adsorption layer from the surface of the substrate, an aprotic polar solvent is brought into contact with the acid gas adsorption layer to dissolve the organic binder.
14. The method for regenerating an acid gas adsorption apparatus according to claim 1 or 2, wherein in the step of adsorbing an acid gas to the acid gas adsorption material, the gas containing the acid gas supplied to the acid gas adsorption apparatus is air.
15. The method for regenerating an acid gas adsorption apparatus according to claim 3, wherein in the step of adsorbing an acid gas to the acid gas adsorption material, the gas containing an acid gas supplied to the acid gas adsorption apparatus is air.
16. A method for manufacturing an acid gas adsorption apparatus, comprising:
A step of supplying a gas containing an acid gas to an acid gas adsorption apparatus including a base material and an acid gas adsorption layer, the acid gas adsorption apparatus being configured to be in contact with the acid gas adsorption layer, and adsorbing the acid gas to an acid gas adsorption material, wherein the acid gas adsorption layer is disposed on the surface of the base material and contains a porous support and the acid gas adsorption material;
a step of separating the acid gas from the acid gas adsorbing material;
a step of removing the acid gas adsorption layer of an acid gas adsorption apparatus, which is subjected to the step of adsorbing the acid gas and the step of removing the acid gas, from the surface of the base material; and
and forming an acid gas adsorption layer containing a porous support and an acid gas adsorption material on the surface of the substrate from which the acid gas adsorption layer has been removed.
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| JP2022-064097 | 2022-04-07 | ||
| JP2022-190911 | 2022-11-30 | ||
| JP2022190911 | 2022-11-30 | ||
| PCT/JP2023/012499 WO2023195388A1 (en) | 2022-04-07 | 2023-03-28 | Regeneration method for acid-gas adsorption device, and manufacturing method for acid-gas adsorption device |
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