JP2019512453A - 高アスペクト比層状複水酸化物材料及びその調製方法 - Google Patents
高アスペクト比層状複水酸化物材料及びその調製方法 Download PDFInfo
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- JP2019512453A JP2019512453A JP2018568161A JP2018568161A JP2019512453A JP 2019512453 A JP2019512453 A JP 2019512453A JP 2018568161 A JP2018568161 A JP 2018568161A JP 2018568161 A JP2018568161 A JP 2018568161A JP 2019512453 A JP2019512453 A JP 2019512453A
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- adamantane
- ldh
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- 238000000034 method Methods 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 title claims description 15
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000002245 particle Substances 0.000 claims abstract description 50
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000011541 reaction mixture Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- JIMXXGFJRDUSRO-UHFFFAOYSA-N adamantane-1-carboxylic acid Chemical compound C1C(C2)CC3CC2CC1(C(=O)O)C3 JIMXXGFJRDUSRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 11
- 150000001450 anions Chemical class 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 150000004692 metal hydroxides Chemical class 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 4
- 229910000000 metal hydroxide Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- -1 adamantane ions Chemical class 0.000 description 3
- 238000005349 anion exchange Methods 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000004922 13C solid-state nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 125000003821 2-(trimethylsilyl)ethoxymethyl group Chemical group [H]C([H])([H])[Si](C([H])([H])[H])(C([H])([H])[H])C([H])([H])C(OC([H])([H])[*])([H])[H] 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 102000040954 LDH family Human genes 0.000 description 1
- 108091077232 LDH family Proteins 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000001460 carbon-13 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 150000007942 carboxylates Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010412 oxide-supported catalyst Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
Description
層状複水酸化物の調製
1つの典型的な調製では、95gの脱イオン水に5グラム(g)のMg(OH)2を溶解することによって5重量%のMg(OH)2溶液を調製した。これに3.36gのAl(OH)3を加えて、Mg/Alモル比を2にした。次いで、9.31gのアダマンタンカルボン酸を同じ溶液(Al/アダマンタンモル比=1)に添加し、得られた反応混合物を、室温で1時間激しく撹拌した。その後、溶液をテフロン(登録商標)加工のオートクレーブに移し、150℃で24時間(h)加熱した。初期反応混合物及び最終濾液のpHを測定したところ、それぞれ9.5及び8.6であった。別の組の実験では、Mg/Alのモル比を5にして上記の手順を繰り返した。反応が終わった後、生成物を水で十分に洗浄し、65℃で乾燥させた。
Claims (18)
- アダマンタンインターカレート層状複水酸化物(LDH)粒子の調製方法であって、
第1の前駆体及び第2の前駆体を水溶液に添加し、初期混合物を形成する工程であって、
前記第1の前駆体は、Al(OH)3またはAl2O3であり、
前記第2の前駆体は、水酸化物M(OH)2または酸化物MOであり、ここで、Mは酸化状態+2の金属であり、
前記初期混合物は、1〜5のM/Alモル比を有し、
前記初期混合物は、前記初期水溶液の総重量を基準にして、10重量%未満の固形分を有する、形成する工程と、
前記初期混合物に、ある量のアダマンタンを添加して、0.5〜2のAl/アダマンタンモル比を有する反応混合物を形成する工程と、
前記反応混合物を加熱して、前記アダマンタンインターカレートLDH粒子を生成することであって、ここで、前記アダマンタンインターカレートLDH粒子は、100より大きいアスペクト比を有し、前記アスペクト比は、アダマンタンインターカレートLDH粒子の幅を、前記アダマンタンインターカレートLDH粒子の厚さで割ることにより定義される、生成する工程と、
を含む、調製方法。 - 前記反応混合物を撹拌する工程をさらに含む、請求項1に記載の方法。
- 前記アダマンタンが、カルボン酸として添加される、請求項1に記載の方法。
- 前記加熱工程が、110℃〜180℃の反応温度で、12時間〜48時間の反応時間行われる、請求項1に記載の方法。
- Mは、Mg、Ca、Co、Ni、Cu、またはZnから選択される、請求項1に記載の方法。
- 前記第2の前駆体が、Mg(OH)2、Ca(OH)2、Co(OH)2、Ni(OH)2、Cu(OH)2、またはZn(OH)2である、請求項1に記載の方法。
- 前記第2の前駆体が、Mg(OH)2またはMgOである、請求項1に記載の方法。
- 前記第2の前駆体が、Mg(OH)2であり、前記第1の前駆体が、Al(OH)3である、請求項1に記載の方法。
- 前記Al/アダマンタンモル比が、0.8〜1.2である、請求項1に記載の方法。
- 前記アダマンタンインターカレートLDH粒子が、一般式[M1−xAlx(OH)2](A)x・mH2Oを有し、式中、xは、0.14〜0.33であり、mは、0.33〜0.50であり、Mは、Mg、Ca、Co、Ni、Cu、またはZnから選択され、Aは、アダマンタンカルボキシレートである、請求項1に記載の方法。
- Mは、Mgである、請求項1に記載の方法。
- 前記初期混合物が、前記初期混合物の総重量を基準にして、5重量%未満の固形分を有する、請求項1に記載の方法。
- 前記アスペクト比が、125より大きい、請求項1に記載の方法。
- 前記アダマンタンインターカレートLDH粒子が、5〜10μmの粒径を有する、請求項1に記載の方法。
- アダマンタンインターカレートLDH粒子の形態のアダマンタンインターカレート層状複水酸化物(LDH)材料であって、前記アダマンタンインターカレートLDH粒子が、
[M1−xAlx(OH)2](A)x・mH2Oによって定義される一般式(式中、xは、0.14〜0.33であり、mは、0.33〜0.50であり、Mは、Mg、Ca、Co、Ni、Cu、またはZnから選択され、Aは、アダマンタンカルボキシレートである)と、
100より大きいアスペクト比であって、前記アスペクト比は、アダマンタンインターカレートLDH粒子の幅を、前記アダマンタンインターカレートLDH粒子の厚さで割ることにより定義される、アスペクト比と、を含む、材料。 - Mは、Mgである、請求項15に記載のアダマンタンインターカレートLDH材料。
- 前記アスペクト比が、125より大きい、請求項15に記載のアダマンタンインターカレートLDH材料。
- 前記アダマンタンインターカレートLDH粒子が、5〜10μmの粒径を有する、請求項15に記載のアダマンタンインターカレートLDH材料。
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US10906859B2 (en) | 2021-02-02 |
US10138199B2 (en) | 2018-11-27 |
SG11201807817SA (en) | 2018-10-30 |
JP6914282B2 (ja) | 2021-08-04 |
EP3429749A1 (en) | 2019-01-23 |
WO2017160965A1 (en) | 2017-09-21 |
KR102164758B1 (ko) | 2020-10-13 |
CN109414686B (zh) | 2021-09-28 |
US20170267623A1 (en) | 2017-09-21 |
KR20190049620A (ko) | 2019-05-09 |
US20190039988A1 (en) | 2019-02-07 |
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