JP2023093977A - アルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法 - Google Patents
アルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 74
- 239000000843 powder Substances 0.000 title claims abstract description 64
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 50
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 48
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 26
- 238000004090 dissolution Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000000654 additive Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 23
- 230000002378 acidificating effect Effects 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- -1 4-dodecyl Chemical group 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000012266 salt solution Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000012670 alkaline solution Substances 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000005868 electrolysis reaction Methods 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- KWXICGTUELOLSQ-UHFFFAOYSA-N 4-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=C(S(O)(=O)=O)C=C1 KWXICGTUELOLSQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003929 acidic solution Substances 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- XPSMITSOZMLACW-UHFFFAOYSA-N 2-(4-aminophenyl)-n-(benzenesulfonyl)acetamide Chemical compound C1=CC(N)=CC=C1CC(=O)NS(=O)(=O)C1=CC=CC=C1 XPSMITSOZMLACW-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims 1
- 229940092714 benzenesulfonic acid Drugs 0.000 claims 1
- 230000009977 dual effect Effects 0.000 claims 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract description 17
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 239000007858 starting material Substances 0.000 abstract description 8
- 238000011978 dissolution method Methods 0.000 abstract description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- 229910018626 Al(OH) Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011946 reduction process Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 229910001593 boehmite Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Images
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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
2Al(s)+2KOH(aq)+6H2O→2K+ (aq)+2Al(OH)4 - (aq)+3H2(g)
Al(OH)4 - (aq)+H+ (aq)→Al(OH)3(s)+H2O
2Al(OH)3→Al2O3+3H2O
2Al+6HCl→2AlCl3+3H2(g)
AlCl3+3NH4OH→Al(OH)3↓+3NH4Cl
又は、
Al2(SO4)3+6NH4OH→2Al(OH)3↓+3(NH4)2SO4
2Al(OH)3→Al2O3+3H2O
Al+3i-C3H7OH→(i-C3H7O)3Al+3/2H2(g)
2(i-C3H7O)3Al+3H2O→2Al(OH)3(s)
2Al(OH)3→Al2O3+3H2O
Al+3i-C8H17OH→Al(OC8H17)3→Al(OH)3+3i-C8H17OH
2Al(OH)3→Al2O3+3H2O
Claims (10)
- アルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法であって、
電気化学装置を用意し、アルミニウム材料をアノード、酸性溶液を電解液とする工程(A)と、
電流パルス法で前記アルミニウム材料の溶解を加速して酸性アルミニウム塩溶液を形成する工程(B)と、
アルカリ性溶液で酸性アルミニウム塩溶液を中和して粒径範囲が1~10μmである水酸化アルミニウムゾルを形成する工程(C)と、
前記水酸化アルミニウムゾルの中に添加剤を加えて水酸化アルミニウムゾルの粒径をナノスケールに制御し、水酸化アルミニウムゾルをろ過して乾燥させた後、水酸化アルミニウム粉末(水酸化アルミニウム粉末の粒子径は30~300nmの範囲である)を得る工程(D)と、
前記水酸化アルミニウム粉末を高温で焙焼してミクロンオーダーのγ-アルミナ粉末を形成する工程(E)と、を含むアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。 - 前記工程(A)のアルミニウム材料は、純度3Nグレード以上のアルミニウムくず又はアルミニウム破砕片であり、前記電気化学装置は電気化学二重電極システムであり、カソード材料が白金、金、黒鉛のいずれかである請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(A)の酸性電解液は、塩酸(HCl)、硫酸(H2SO4)及び硝酸(HNO3)からなる群から選択される1つであり、前記酸性電解液の濃度は0.5M~3Mの範囲である請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(B)の電流パルス法は、電源供給装置により定電流パルスを設定し、定電流パルスが0.1~1.0A/cm2及び秒数10秒、0A/cm2及び秒数15秒を1サイクルとし、パルス電流サイクル数は20回以上、総電解時間は500秒以上である請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(C)のアルカリ性溶液は、水酸化ナトリウム(NaOH)、アンモニア(NH4OH)及び水酸化カリウム(KOH)からなる群から選択される1つであり、前記アルカリ性溶液で酸性アルミニウム塩溶液の酸とアルカリをpH6~8の範囲に中和させ、水酸化アルミニウム(Al(OH)3)ゾルを形成する請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(D)の添加剤は、塩化ナトリウム(NaCl)、塩化アンモニウム(NH4Cl)、3-メルカプト-1-プロパンスルホン酸ナトリウム塩(3-mercapto-1-propanesulfonicacisodiumsalt、MPS)及び4-ドデシルベンゼンスルホン酸(4-Dodecylbenzenesulfonic acid、DBSA)からなる群から選択される1つである請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記添加剤の濃度は0.01M~0.5Mの範囲であり、pH値をpH6~8の範囲に制御する請求項6に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(D)の濾過・乾燥手順は、水酸化アルミニウムゾルを吸引濾過した後、オーブン又はホットプレートを温度80~100℃に設定して低温で乾燥させてナノスケールの水酸化アルミニウム粉末を形成する請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(E)の高温焙焼温度は、600℃~1000℃で、温度保持時間は1~5時間である請求項1に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
- 前記工程(E)の高温焙焼温度は、600℃~900℃で、温度保持時間は1~5時間であり、高温焙焼後でミクロンオーダーのγ-アルミナ粉末を形成する請求項9に記載のアルミニウム塩を電気化学的に溶解する方法によるアルミナ粉末の調製方法。
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KR20210144561A (ko) * | 2020-05-21 | 2021-11-30 | 한국과학기술원 | 양극산화법을 이용한 베마이트 나노입자 또는 베이어라이트 나노입자 대량 제조방법 및 장치 |
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