RU2017100949A - Аморфный мезопористый оксид алюминия с высокой связностью и способ его производства - Google Patents
Аморфный мезопористый оксид алюминия с высокой связностью и способ его производства Download PDFInfo
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- RU2017100949A RU2017100949A RU2017100949A RU2017100949A RU2017100949A RU 2017100949 A RU2017100949 A RU 2017100949A RU 2017100949 A RU2017100949 A RU 2017100949A RU 2017100949 A RU2017100949 A RU 2017100949A RU 2017100949 A RU2017100949 A RU 2017100949A
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- Prior art keywords
- deposition
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- 238000004519 manufacturing process Methods 0.000 title claims 11
- 238000000034 method Methods 0.000 title claims 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims 4
- 239000002243 precursor Substances 0.000 claims 19
- 230000008021 deposition Effects 0.000 claims 15
- 230000002378 acidificating effect Effects 0.000 claims 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 6
- 239000000725 suspension Substances 0.000 claims 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 4
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims 4
- 238000010438 heat treatment Methods 0.000 claims 4
- 229910001388 sodium aluminate Inorganic materials 0.000 claims 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 3
- 229910052782 aluminium Inorganic materials 0.000 claims 3
- 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 claims 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 2
- WPUINVXKIPAAHK-UHFFFAOYSA-N aluminum;potassium;oxygen(2-) Chemical compound [O-2].[O-2].[Al+3].[K+] WPUINVXKIPAAHK-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 2
- 229910017604 nitric acid Inorganic materials 0.000 claims 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 2
- 239000000843 powder Substances 0.000 claims 2
- 239000012429 reaction media Substances 0.000 claims 2
- 239000012431 aqueous reaction media Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 claims 1
- 238000002336 sorption--desorption measurement Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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Claims (20)
1. Аморфный мезопористый оксид алюминия, характеризующийся связностью (Z) более 2,7, при этом, связность определяется на основании изотерм адсорбции/десорбции азота.
2. Оксид алюминия по п. 1, характеризующийся связностью от 3 до 7.
3. Оксид алюминия по одному из пп. 1 или 2, характеризующийся удельной площадью поверхности по ВЕТ от 50 до 450 м2/г.
4. Оксид алюминия по одному из пп. 1-3, характеризующийся объемом мезопор, большим или равным 0,5 мл/г, измеренным на основании изотермы адсорбции азота до насыщения.
5. Способ производства указанного оксида алюминия по одному из пп. 1-4, при этом, указанный способ включает, по меньшей мере, следующие стадии:
а) по меньшей мере, первая стадия осаждения оксида алюминия, включающая осаждение в водной реакционной среде, по меньшей мере, одного основного прекурсора, выбранного из алюмината натрия, алюмината калия, аммиака, гидроксида натрия и гидроксида калия, и, по меньшей мере, одного кислого прекурсора, выбранного из сульфата алюминия, хлорида алюминия, нитрата алюминия, серной кислоты, соляной кислоты и азотной кислоты, при этом, по меньшей мере, один из прекурсоров - основный или кислый - содержит алюминий, относительный расход кислого и основного прекурсоров выбран так, чтобы обеспечить рН реакционной среды от 8,5 до 10,5, и расход прекурсора или прекурсоров - кислого и основного, содержащих алюминий, выбран так, чтобы доля выхода указанной первой стадии составляла от 40 до 100%, при этом, доля выхода определяется как отношение количества оксида алюминия, в эквиваленте Al2O3, образовавшегося на указанной первой стадии осаждения, к общему количеству оксида алюминия, образовавшемуся по окончании стадии или стадий осаждения, при этом, указанную первую стадию осаждения осуществляют при температуре от 10 до 50°С, в течение периода времени от 2 минут до 30 минут,
b) стадия тепловой обработки суспензии, полученной по окончании стадии а), при температуре от 50 до 200°С в течение периода времени от 30 минут до 5 часов,
с) стадия фильтрации суспензии, полученной по окончании стадии b) тепловой обработки, сопровождаемая, по меньшей мере, одной стадией промывки полученного геля,
d) стадия сушки геля оксида алюминия, полученного по окончании стадии с), с целью получения порошка,
e) стадия формования порошка, полученного по окончании стадии d), с целью получения необработанного материала,
f) стадия тепловой обработки необработанного материала, полученного по окончании стадии е), при температуре от 500 до 1000°С в присутствии или в отсутствии потока воздуха, содержащего до 60 об.% воды.
6. Способ по п. 5, в котором основный прекурсор представляет собой алюминат натрия.
7. Способ производства по одному из пп. 5 или 6, в котором кислый прекурсор представляет собой сульфат алюминия.
8. Способ производства по одному из пп. 5-7, в котором массовое отношение указанного основного прекурсора к указанному кислому прекурсору составляет от 1,6 до 2,05.
9. Способ производства по одному из пп. 5-8, в котором доля выхода указанной стадии а) осаждения составляет от 45 до 90%.
10. Способ производства по одному из пп. 5-9, в котором в том случае, когда доля выхода, достигаемая на первой стадии а) осаждения, меньше 100%, указанный способ производства включает вторую стадию аʹ) осаждения после первой стадии осаждения.
11. Способ производства по п. 10, в котором стадию нагревания суспензии, полученной по окончании стадии а) осаждения, осуществляют между двумя стадиями а) и aʹ) осаждения, при этом, указанную стадию нагревания проводят при температуре от 20 до 90°С в течение периода времени от 7 до 45 минут.
12. Способ производства по одному из пп. 10 или 11, в котором указанную вторую стадию aʹ) осаждения суспензии, полученной по окончании стадии нагревания, проводят путем добавления в указанную суспензию, по меньшей мере, одного основного прекурсора, выбранного из алюмината натрия, алюмината калия, аммиака, гидроксида натрия и гидроксида калия, и, по меньшей мере, одного кислого прекурсора, выбранного из сульфата алюминия, хлорида алюминия, нитрата алюминия, серной кислоты, соляной кислоты и азотной кислоты, при этом, по меньшей мере, один из прекурсоров - основный или кислый - содержит алюминий, относительный расход кислого и основного прекурсоров выбран так, чтобы обеспечить рН реакционной среды от 8,5 до 10,5, и расход прекурсора или прекурсоров - кислого и основного, содержащих алюминий, выбран так, чтобы доля выхода второй стадии составляла от 0 до 60%, при этом, доля выхода второй стадии определяется как отношение количества оксида алюминия, в эквиваленте Al2O3, образовавшегося на указанной второй стадии аʹ) осаждения, к общему количеству оксида алюминия, образовавшемуся по окончании стадии аʹ) осаждения способа производства, при этом, указанную вторую стадию аʹ) осаждения осуществляют при температуре от 40 до 90°С, в течение периода времени от 2 минут до 50 минут.
13. Способ производства по п. 12, в котором массовое отношение указанного основного прекурсора к указанному кислому прекурсору составляет от 1,6 до 2,05, при этом, основным и кислым прекурсорами являются, соответственно, алюминат натрия и сульфат алюминия.
14. Способ производства по одному из пп. 12 или 13, в котором вторую стадию аʹ) осаждения осуществляют при температуре от 45 до 70°С.
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FR1455423A FR3022238B1 (fr) | 2014-06-13 | 2014-06-13 | Alumine mesoporeuse amorphe ayant une connectivite elevee et son procede de preparation |
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PCT/EP2015/062828 WO2015189202A1 (fr) | 2014-06-13 | 2015-06-09 | Alumine mesoporeuse amorphe ayant une connectivite elevee et son procede de preparation |
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