JP2020529914A - アルカリ金属水酸化物を使用した酸化亜鉛系吸着剤、およびその調製と使用プロセス - Google Patents
アルカリ金属水酸化物を使用した酸化亜鉛系吸着剤、およびその調製と使用プロセス Download PDFInfo
- Publication number
- JP2020529914A JP2020529914A JP2019565372A JP2019565372A JP2020529914A JP 2020529914 A JP2020529914 A JP 2020529914A JP 2019565372 A JP2019565372 A JP 2019565372A JP 2019565372 A JP2019565372 A JP 2019565372A JP 2020529914 A JP2020529914 A JP 2020529914A
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- Prior art keywords
- zinc oxide
- weight
- phase
- slurry
- zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 296
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 145
- 239000003463 adsorbent Substances 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 72
- 230000008569 process Effects 0.000 title claims abstract description 64
- 150000008044 alkali metal hydroxides Chemical class 0.000 title claims description 9
- 238000002360 preparation method Methods 0.000 title description 6
- 239000002243 precursor Substances 0.000 claims abstract description 90
- 239000011701 zinc Substances 0.000 claims abstract description 74
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 70
- -1 zinc aluminate Chemical class 0.000 claims abstract description 38
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 36
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 36
- 239000011734 sodium Substances 0.000 claims abstract description 36
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 34
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 22
- 239000011593 sulfur Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000012071 phase Substances 0.000 claims description 73
- 239000002002 slurry Substances 0.000 claims description 57
- 239000002245 particle Substances 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 17
- 238000001694 spray drying Methods 0.000 claims description 16
- 239000007790 solid phase Substances 0.000 claims description 15
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000002441 X-ray diffraction Methods 0.000 claims description 9
- 238000005299 abrasion Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 8
- 239000012798 spherical particle Substances 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 4
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims 3
- 238000000926 separation method Methods 0.000 claims 3
- 239000011343 solid material Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 34
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 11
- 150000001340 alkali metals Chemical class 0.000 abstract description 10
- 239000002585 base Substances 0.000 abstract description 3
- 229910001676 gahnite Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 22
- 239000000243 solution Substances 0.000 description 16
- 239000000543 intermediate Substances 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000001354 calcination Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 11
- 238000001556 precipitation Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 10
- 238000000975 co-precipitation Methods 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 9
- 239000007921 spray Substances 0.000 description 9
- 230000009257 reactivity Effects 0.000 description 8
- 238000011069 regeneration method Methods 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 230000008929 regeneration Effects 0.000 description 7
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 150000004679 hydroxides Chemical class 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 4
- 238000009827 uniform distribution Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Chemical class 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical class [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
- 239000002594 sorbent Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910007541 Zn O Inorganic materials 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- KZNMRPQBBZBTSW-UHFFFAOYSA-N [Au]=O Chemical class [Au]=O KZNMRPQBBZBTSW-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical class [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000002051 biphasic effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 229910001922 gold oxide Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000005414 inactive ingredient Substances 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- GSWAOPJLTADLTN-UHFFFAOYSA-N oxidanimine Chemical compound [O-][NH3+] GSWAOPJLTADLTN-UHFFFAOYSA-N 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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-
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/024—Compounds of Zn, Cd, Hg
- B01J20/0244—Compounds of Zn
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- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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- B01D2257/304—Hydrogen sulfide
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Abstract
Description
サイズ(オングストローム)={0.9xW/[FWHM−(GW)2]1/2}/cosθ
Cu源のX線波長であるWが1.540562オングストロームである場合、FWHMはソフトウェアによって決定されるラジアンでの報告された半値のピーク幅であり、GWは、この機器に固有の拡大因子であり、シータは、報告されたピーク重心の半分である。各結晶相について最終的に報告される結晶子サイズは、酸化亜鉛相およびアルミン酸亜鉛相の最も強いピークについて、Jadeソフトウェアによって計算された結晶子サイズである。
共沈装置については図2を参照。
Zn(NO3)2・6H2O、試薬グレード>98%
Al(NO3)3・9H2O、ACS試薬グレード>98%
NaOHペレット、試薬グレード>98%
濃縮HNO3、65〜67%、ACS試薬
2つの4L容器
pHおよび導電率計、モデル:HACH、HQ40d
Easy−Load II ぜん動ポンプを備えた2つのMasterflex L/S
機械的ミキサー モデル:Aron750
溶液の調製
金属塩を秤量し(表中の量リスト)、それらを4Lビーカーに入れる。脱イオン(DI)水を加えて、約1500mlの総溶液量にする。
塩スラリーを機械的に混合して、すべての塩が溶解し、透明な溶液が得られることを確認する。
金属塩溶液を50〜70℃に加熱し、共沈反応の持続時間中この温度を維持する。
NaOHペレットと脱イオン水を混合して、10重量%のNaOH溶液を作成する。
濃縮HNO3酸溶液および脱イオン水を使用して5モルのHNO3溶液を作成する。濃硝酸と水との反応は非常に急速で発熱性であるため、この混合ステップでは細心の注意を払うこと。
図2に示すように、機械的撹拌機、較正されたpH計および2つのぜん動ポンプを備えた沈殿タンクを装備する。
約600mlの脱イオン水を4Lビーカーに加えて、その溶液を撹拌し、pH電極を浸漬してpHを適切に測定できるようにする。
沈殿タンクをガラスウールで断熱する。水を50〜70℃に加熱する。
両方のぜん動ポンプを同時にオンにする。約30〜35ml/分の速度で塩溶液を送り込み、NaOH溶液の流量(60〜70ml/分)を調節して、沈殿溶液の目標pHを5.5〜7.5に維持する。
撹拌し、沈殿した混合物の温度をさらに30分間、50〜70℃に維持し続ける。
圧力フィルターまたは真空フィルターを使用して沈殿物をろ過する。
ナトリウムレベルが所望の範囲になるまで、沈殿物を脱イオン水で洗浄する。
スラリー調製
湿潤ケーキ中の固体量を測定する。既知量(〜20g)の洗浄したケーキを小さなるつぼに入れ、空気中500℃で2時間か焼し、収集したサンプル(g)を計量する。
10重量%の固体量スラリーを作るために添加する水を計算する:金属酸化物(g)/(湿潤ケーキ重量(g)+X)=0.10、ここで、Xは必要とされる水の量である。
プラスチックビーカー内で少なくとも30分間、ケーキを水(X)と混合する。
混合中にスラリーにHNO3溶液をゆっくりと加える。
30分間混合し続ける。
スラリーをろ過して、噴霧乾燥中にブロッキングを引き起こす可能性のある潜在的な大きな粒子を除去する。
噴霧乾燥機を掃除する。
初期内気温と外気温をそれぞれ、320℃と125℃に設定する。
ノズル−08;圧力0.75bar、フロー25〜35%
スラリー流量=50ml/分
上記の条件でろ過されたスラリーを噴霧乾燥する。
噴霧乾燥粉末を120℃で一晩乾燥させる。
噴霧乾燥粉末を流動空気中で2時間か焼する。
ZnO(固)+H2S(気)=ZnS(固)+H2O(気)
Claims (30)
- 供給流から少なくとも1つの還元硫黄種を除去するための流動性耐摩耗性の吸着剤であって、
実質的に球状の粒子を含み、
前記粒子は、酸化亜鉛相およびアルミン酸亜鉛相から本質的になる活性亜鉛成分を少なくとも75重量%含み、前記相のそれぞれは、X線回折半価幅分析によって決定される約50nm未満の結晶子サイズを有し、
前記活性亜鉛成分は、前記酸化亜鉛相と前記アルミン酸亜鉛相の組み合わせた酸化亜鉛に基づいて計算される総酸化亜鉛量を、前記活性亜鉛成分の重量に基づいて、約50重量%〜約80重量%有し、前記固相中の残留ナトリウムレベルは、ナトリウムの重量で約25ppm〜ナトリウムの重量で約2500ppmである、流動性耐摩耗性の吸着剤。 - 前記固相中の残留ナトリウムレベルが、ナトリウムの重量で約50ppm〜ナトリウムの重量で約1000ppmである、請求項1に記載の流動性耐摩耗性の吸着剤。
- 前記固相中の残留ナトリウムレベルが、ナトリウムの重量で約75ppm〜ナトリウムの重量で約750ppmである、請求項1に記載の流動性耐摩耗性の吸着剤。
- 前記還元硫黄種が、H2Sである、請求項1〜3のいずれか一項に記載の流動性耐摩耗性の吸着剤。
- 供給流からCOSを除去するための流動性耐摩耗性の吸着剤であって、
実質的に球状の粒子を含み、
前記粒子は、酸化亜鉛相およびアルミン酸亜鉛相から本質的になる活性亜鉛成分を少なくとも75重量%含み、前記相のそれぞれは、X線回折半価幅分析によって決定される約50nm未満の結晶子サイズを有し、
前記活性亜鉛成分は、前記酸化亜鉛相と前記アルミン酸亜鉛相の組み合わせた酸化亜鉛に基づいて計算される総酸化亜鉛量を、前記活性亜鉛成分の重量に基づいて、約50重量%〜約80重量%有し、前記固相中の残留ナトリウムレベルは、ナトリウムの重量で約25ppm〜ナトリウムの重量で約2500ppmである、流動性耐摩耗性の吸着剤。 - 流動性耐摩耗性で、活性酸化亜鉛含有吸着剤を調製するためのプロセスであって、以下のステップ:
前記固形分が、沈殿酸化亜鉛前駆体および沈殿酸化アルミニウム前駆体を含み、前記沈殿酸化亜鉛前駆体および前記沈殿酸化アルミニウム前駆体は、それぞれ、ZnOおよびAl2O3として計算される量で存在するように、
前記沈殿酸化亜鉛前駆体が、前記スラリー中の前記沈殿酸化亜鉛前駆体および前記沈殿酸化アルミニウム前駆体の総固形分量の約50重量%〜約80重量%を構成するように、および、混合および組合せステップ中のこのスラリーのpHが5.5〜7.5に維持されるように、酸化亜鉛前駆体と酸化アルミニウム前駆体との水溶液をアルカリ金属水酸化物の水溶液と組み合わせて、第1のスラリーを形成すること;
分離手段によって、前記第1のスラリーの液相を前記固相から分離すること;
ろ過された固相を水、好ましくは脱イオン水で洗浄して、ナトリウムの重量で約25ppm〜ナトリウムの重量で約2500ppmの前記固相の残留ナトリウムレベルを達成すること;
前記第1のスラリーから分離された固体材料を水および濃酸で処理して、第2のスラリーを生成すること(ここで、前記第2のスラリーのpHは、酸で3.5〜5.0に調節される);
前記第2のスラリーを噴霧乾燥して、噴霧乾燥粒子を形成すること;および
前記噴霧乾燥粒子をか焼して、酸化亜鉛相とアルミン酸亜鉛相とから本質的になる二相成分を含む流動性耐摩耗性で、活性酸化亜鉛含有吸着剤粒子を提供すること、
を含む、流動性耐摩耗性で、活性酸化亜鉛含有吸着剤を調製するためのプロセス。 - 前記噴霧乾燥ステップが、35μm〜175μmのサイズ範囲を有するか焼粒子を提供するのに十分な条件下で実施される、請求項6に記載のプロセス。
- 前記酸化亜鉛が、前記スラリー中の前記酸化亜鉛前駆体および前記酸化アルミニウム前駆体の総固形分量の少なくとも約50重量%を構成する、請求項6または7に記載のプロセス。
- 前記活性酸化亜鉛含有吸着剤粒子が、直径50nm未満の酸化亜鉛粒子を含む、請求項6〜8のいずれか一項に記載のプロセス。
- 前記活性酸化亜鉛含有吸着剤粒子が、直径約10nm〜約40nmの酸化亜鉛粒子を含む、請求項6〜8のいずれか一項に記載のプロセス。
- 前記活性酸化亜鉛含有吸着剤粒子が、直径約12nm〜約30nmの酸化亜鉛粒子を含む、請求項6〜8のいずれか一項に記載のプロセス。
- 前記活性酸化亜鉛含有吸着剤粒子が、直径約13nm〜約20nmの酸化亜鉛粒子を含む、請求項6〜8のいずれか一項に記載のプロセス。
- 前記スラリーが、促進剤前駆体、バインダー前駆体、および耐火性酸化物前駆体からなる群より選択される少なくとも1つの追加材料をさらに含み、前記追加材料は、酸化亜鉛相とアルミン酸亜鉛相とから本質的になる前記二相成分を少なくとも約75重量%含む流動性耐摩耗性で、活性酸化亜鉛含有吸着剤粒子を提供するように選択された量で存在する、請求項6〜12のいずれか一項に記載のプロセス。
- 前記追加材料が、酸化亜鉛相とアルミン酸亜鉛相とから本質的になる前記二相成分を少なくとも約80重量%含む流動性耐摩耗性で、活性酸化亜鉛含有吸着剤粒子を提供するように選択された量で存在する、請求項13に記載のプロセス。
- 前記追加材料が、酸化亜鉛相とアルミン酸亜鉛相とから本質的になる前記二相成分を少なくとも約90重量%含む流動性耐摩耗性で、活性酸化亜鉛含有吸着剤粒子を提供するように選択された量で存在する、請求項14に記載のプロセス。
- 前記追加材料が、酸化亜鉛相とアルミン酸亜鉛相とから本質的になる前記二相成分を少なくとも約95重量%含む流動性耐摩耗性で、活性酸化亜鉛含有吸着剤粒子を提供するように選択された量で存在する、請求項15に記載のプロセス。
- 前記アルカリ金属水酸化物の全部または一部が、アルカリ金属炭酸塩で置き換えられる、請求項6〜16のいずれか一項に記載のプロセス。
- 前記アルカリ金属水酸化物が、水酸化ナトリウムである、請求項6〜16のいずれか一項に記載のプロセス。
- 前記水酸化ナトリウムの全部または一部が、炭酸ナトリウムで置き換えられる、請求項18に記載のプロセス。
- 前記固相の残留ナトリウムレベルが、ナトリウムの重量で50ppm〜ナトリウムの重量で1000ppmである、請求項6〜19のいずれか一項に記載のプロセス。
- 前記固相の残留ナトリウムレベルが、ナトリウムの重量で75ppm〜ナトリウムの重量で750ppmである、請求項20に記載のプロセス。
- 前記第2のスラリーの酸性化に使用される前記酸が、硝酸である、請求項6〜21のいずれか一項に記載のプロセス。
- 前記第2のスラリーのpH範囲が、4.0〜4.5の間に調節される、請求項6〜22のいずれか一項に記載のプロセス。
- 前記第1のスラリーの形成が、周囲温度〜約85℃の温度で実施される、請求項6〜23のいずれか一項に記載のプロセス。
- 前記第1のスラリーの形成が、約50℃〜約80℃の温度で実施される、請求項24に記載のプロセス。
- 前記第1のスラリーの形成が、約65℃〜約75℃の温度で実施される、請求項25に記載のプロセス。
- 前記固相からの前記第1のスラリーの前記液相の分離が、周囲温度〜約85℃の温度で行われる洗浄プロセスを含む、請求項6〜26のいずれか一項に記載のプロセス。
- 前記固相からの前記第1のスラリーの前記液相の分離が、約50℃〜約80℃の温度で行われる洗浄プロセスを含む、請求項6〜27のいずれか一項に記載のプロセス。
- 前記噴霧乾燥粒子が、約500℃〜約900℃でか焼される、請求項6〜28のいずれか一項に記載のプロセス。
- 前記噴霧乾燥粒子が、約600℃〜約800℃でか焼される、請求項29に記載のプロセス。
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ENERGY & FUELS, vol. 8, no. 3, JPN6022012236, 1994, pages 763 - 769, ISSN: 0005016625 * |
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CA3062639A1 (en) | 2019-02-07 |
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KR20200026820A (ko) | 2020-03-11 |
WO2019028127A1 (en) | 2019-02-07 |
AU2018312487B2 (en) | 2024-03-14 |
US20210121850A1 (en) | 2021-04-29 |
JP7299844B2 (ja) | 2023-06-28 |
US11491457B2 (en) | 2022-11-08 |
AU2018312487A1 (en) | 2019-11-28 |
KR102562687B1 (ko) | 2023-08-01 |
EP3661642A1 (en) | 2020-06-10 |
EP3661642A4 (en) | 2021-04-28 |
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