RU2009120540A - Формованные пористые элементы из альфа-оксида алюминия и способы их получения - Google Patents
Формованные пористые элементы из альфа-оксида алюминия и способы их получения Download PDFInfo
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- RU2009120540A RU2009120540A RU2009120540/04A RU2009120540A RU2009120540A RU 2009120540 A RU2009120540 A RU 2009120540A RU 2009120540/04 A RU2009120540/04 A RU 2009120540/04A RU 2009120540 A RU2009120540 A RU 2009120540A RU 2009120540 A RU2009120540 A RU 2009120540A
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- Prior art keywords
- alumina
- alpha
- fluorine
- reactor
- introducing
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract 20
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract 42
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract 27
- 229910052731 fluorine Inorganic materials 0.000 claims abstract 27
- 239000011737 fluorine Substances 0.000 claims abstract 27
- 239000002243 precursor Substances 0.000 claims abstract 23
- 150000001875 compounds Chemical class 0.000 claims abstract 20
- 238000010438 heat treatment Methods 0.000 claims abstract 6
- OFHCOWSQAMBJIW-AVJTYSNKSA-N alfacalcidol Chemical compound C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)CCCC(C)C)=C\C=C1\C[C@@H](O)C[C@H](O)C1=C OFHCOWSQAMBJIW-AVJTYSNKSA-N 0.000 claims abstract 5
- 238000002360 preparation method Methods 0.000 claims abstract 5
- 239000000203 mixture Substances 0.000 claims 9
- 239000007789 gas Substances 0.000 claims 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 6
- 150000001336 alkenes Chemical class 0.000 claims 4
- 239000003054 catalyst Substances 0.000 claims 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 2
- 229910016569 AlF 3 Inorganic materials 0.000 claims 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 claims 2
- 125000002947 alkylene group Chemical group 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 2
- 229910052796 boron Inorganic materials 0.000 claims 2
- 230000006835 compression Effects 0.000 claims 2
- 238000007906 compression Methods 0.000 claims 2
- 238000006735 epoxidation reaction Methods 0.000 claims 2
- 150000002222 fluorine compounds Chemical class 0.000 claims 2
- 239000003607 modifier Substances 0.000 claims 2
- 239000001301 oxygen Substances 0.000 claims 2
- 229910052760 oxygen Inorganic materials 0.000 claims 2
- 229910052710 silicon Inorganic materials 0.000 claims 2
- 239000010703 silicon Substances 0.000 claims 2
- 235000012431 wafers Nutrition 0.000 claims 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 239000012808 vapor phase Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
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Abstract
1. Способ получения формованного пористого элемента, содержащего перекрывающиеся пластинки альфа-оксида алюминия, включающий ! а. подготовку реактора, в котором общее давление можно менять и контролировать; ! b. введение в реактор формованного предшественника элемента, который содержит, по меньшей мере, один предшественник альфа-оксида алюминия; ! с. введение в реактор в качестве фторсодержащего газа в условиях введения фторсодержащего соединения; ! d. установление общего давления внутри реактора приблизительно от 1 до 100000 мм.рт.ст. (1,36·10-3-136 кг/м2); и ! е. контактирование фторсодержащего соединения, по меньшей мере, с частью формованного предшественника элемента при одной или нескольких температурах, при одном или нескольких давлениях в течение одного или нескольких периодов времени, достаточных для превращения, по меньшей мере, 50% предшественника альфа-оксида алюминия в пластинки альфа-оксида алюминия. ! 2. Способ получения формованного пористого элемента, содержащего перекрывающиеся пластинки альфа-оксида алюминия, включающий ! а. подготовку реактора; ! b. введение в реактор формованного предшественника элемента, который содержит, по меньшей мере, один предшественник альфа-оксида алюминия; ! с. нагревание реактора до температуры выше 700°С; ! d. введение в нагретый реактор в качестве фторсодержащего газа при условиях введения фторсодержащего соединения и ! е. контактирование введенного фторсодержащего соединения, по меньшей мере, с частью формованного предшественника элемента, по меньшей мере, при одной температуре выше 700°С, в течение одного или нескольких периодов времени, достаточных для превращения, по
Claims (19)
1. Способ получения формованного пористого элемента, содержащего перекрывающиеся пластинки альфа-оксида алюминия, включающий
а. подготовку реактора, в котором общее давление можно менять и контролировать;
b. введение в реактор формованного предшественника элемента, который содержит, по меньшей мере, один предшественник альфа-оксида алюминия;
с. введение в реактор в качестве фторсодержащего газа в условиях введения фторсодержащего соединения;
d. установление общего давления внутри реактора приблизительно от 1 до 100000 мм.рт.ст. (1,36·10-3-136 кг/м2); и
е. контактирование фторсодержащего соединения, по меньшей мере, с частью формованного предшественника элемента при одной или нескольких температурах, при одном или нескольких давлениях в течение одного или нескольких периодов времени, достаточных для превращения, по меньшей мере, 50% предшественника альфа-оксида алюминия в пластинки альфа-оксида алюминия.
2. Способ получения формованного пористого элемента, содержащего перекрывающиеся пластинки альфа-оксида алюминия, включающий
а. подготовку реактора;
b. введение в реактор формованного предшественника элемента, который содержит, по меньшей мере, один предшественник альфа-оксида алюминия;
с. нагревание реактора до температуры выше 700°С;
d. введение в нагретый реактор в качестве фторсодержащего газа при условиях введения фторсодержащего соединения и
е. контактирование введенного фторсодержащего соединения, по меньшей мере, с частью формованного предшественника элемента, по меньшей мере, при одной температуре выше 700°С, в течение одного или нескольких периодов времени, достаточных для превращения, по меньшей мере, 50% предшественника альфа-оксида алюминия в пластинки альфа-оксида алюминия.
3. Способ изготовления формованного пористого элемента, содержащего перекрывающиеся пластинки альфа-оксида алюминия, и этот способ включает
а. подготовку реактора;
b. введение в реактор формованного предшественника элемента, который содержит, по меньшей мере, один предшественник альфа-оксида алюминия;
с. введение в реактор в качестве фторсодержащего газа в условиях введения фторсодержащего соединения, по существу, не состоящего из фторида водорода и выбранного из группы, включающей (1) фторуглероды, SiF4, BF3, NF3, F2, XeF2, SF6, PF5, CF4, CHF3, C2H2F4 и AlF3; (2) смеси двух или нескольких таких газов; и (3) смеси HF и одного или нескольких из числа фторуглеродов, SiF4, BF3, NF3, F2, XeF2, SF6, PF5, CF4, CHF3, C2H2F4 и AlF3; и
d. контактирование введенного фторсодержащего соединения, по меньшей мере, с частью формованного предшественника элемента, при одной или нескольких температурах и в течение одного или нескольких периодов времени, достаточных для превращения, по меньшей мере, 50% предшественника альфа-оксида алюминия в пластинки альфа-оксида алюминия.
4. Способ модификации поверхностной композиции альфа-оксида алюминия, включающий
а. подготовку реактора;
b. введение в реактор альфа-оксида алюминия, имеющего поверхностную композицию;
с. введение в реактор в качестве фторсодержащего газа в условиях введения фторсодержащего соединения; и
d. контактирование введенного фторсодержащего соединения, по меньшей мере, с частью альфа-оксида алюминия в течение одного или нескольких периодов времени и при одной или нескольких температурах, достаточных для модификации поверхностной композиции альфа-оксида алюминия.
5. Способ модификации поверхностной композиции формованного пористого элемента, содержащего пластинки альфа-оксида алюминия, включающий
а. подготовку реактора;
b. подачу в реактор продукта одной или нескольких стадий е. по п.1 и/или 2, и/или стадии d. по п.3;
с. введение в реактор в качестве фторсодержащего газа в условиях введения фторсодержащего соединения и
d. контактирование введенного фторсодержащего соединения, по меньшей мере, с частью поверхности альфа-оксида алюминия в течение одного или нескольких периодов времени и при одной или нескольких температурах, достаточных для модификации поверхностной композиции альфа-оксида алюминия.
6. Носитель для катализатора эпоксидирования олефина, где носитель
а. содержит, по меньшей мере, 80 мас.% оксида алюминия, и из этого оксида алюминия, по меньшей мере, 90% представляют собой альфа-оксид алюминия, за исключением модификатора;
b. имеет площадь поверхности, по меньшей мере, 1,0 м2/г;
с. имеет пористость, по меньшей мере, 75%; и среднюю прочность при плоскостном сжатии, по меньшей мере, 1 фунт/мм (0,45 кг/мм), измеренную в виде полого цилиндра, имеющего аксиальное цилиндрическое отверстие по длине цилиндра, наружный диаметр 0,26 дюйма (6,60 мм), внутренний диаметр отверстия 0,1 дюйма (2,54 мм) и длину 0,25 дюйма (6,35 мм).
7. Носитель для катализатора эпоксидирования олефина, где носитель
а. содержит, по меньшей мере, 80 мас.% оксида алюминия, и из этого оксида алюминия, по меньшей мере, 90% представляют собой альфа-оксид алюминия, за исключением модификатора;
b. имеет площадь поверхности, по меньшей мере, 1,0 м2/г;
с. имеет пористость, по меньшей мере, 70%; и среднюю прочность при плоскостном сжатии, по меньшей мере, 3,5 фунт/мм (1,6 кг/мм), измеренную в виде полого цилиндра, имеющего аксиальное цилиндрическое отверстие по длине цилиндра, наружный диаметр 0,26 дюйма (6,60 мм), внутренний диаметр отверстия 0,1 дюйма (2,54 мм) и длину 0,25 дюйма (6,35 мм).
8. Перекрывающиеся пластинки альфа-оксида алюминия, имеющие поверхностную композицию, включающую кремнийсодержащие образцы с концентрацией приблизительно от 1 до 20 ат.% кремния, измеренную с помощью рентгеновской фотоэлектронной спектроскопии.
9. Перекрывающиеся пластинки альфа-оксида алюминия, имеющие поверхностную композицию, включающую борсодержащие образцы с концентрацией приблизительно от 1 до 20 ат.% бора, измеренную с помощью рентгеновской фотоэлектронной спектроскопии.
10. Способ по пп.1, 2, 3 или 5, в котором
а. температура, при которой фторсодержащее соединение вводят реактор, содержащий формованный предшественник элемента, является недостаточной, чтобы превратить предшественник альфа-оксида алюминия в пластинки альфа-оксида алюминия;
b. проконтактировавший с фторсодержащим соединением нагретый формованный предшественник элемента, затем нагревают до второй температуры в течение времени, достаточного для того, чтобы введенное фторсодержащее соединение превратило, по меньшей мере, 50% предшественника альфа-оксида алюминия в пластинки альфа-оксида алюминия.
11. Способ по п.1 или 2, также включающий удаление, по меньшей мере, части остающегося фторсодержащего соединения; и
нагревание продукта стадии е. в вакууме до второй температуры в интервале приблизительно от 1050 до 1600°С в течение приблизительно от 1 до 48 ч.
12. Способ по п.3, также включающий удаление, по меньшей мере, части остающегося фторсодержащего соединения; и
нагревание продукта стадии d. в вакууме до второй температуры в интервале приблизительно от 1050 до 1600°С в течение приблизительно от 1 до 48 ч.
13. Способ по любому из пп.1-5, дополнительно включающий удаление, по меньшей мере, части остающегося фторсодержащего соединения; и
введение в реактор в качестве фторсодержащего соединения в условиях введения второго фторсодержащего соединения.
14. Способ по п.4, где альфа-оксид алюминия находится в форме формованного элемента.
15. Способ по п.4 или 5, где альфа-оксид алюминия состоит из пластинок.
16. Способ повышения прочности при раздавливании формованного пористого элемента, состоящего из пластинок альфа-оксида алюминия, включающий способ по любому из пп.1-3 или 10-13, дополнительно включающий обработку формованного пористого элемента, содержащего альфа-оксид алюминия, путем нагревания при температуре выше чем 1000°С в атмосфере воздуха.
17. Катализатор для получения олефина, содержащий серебро и один или несколько промоторов, нанесенных на формованные пористые элементы по пп.1-3, модифицированный альфа-оксид алюминия по п.4 или 5, носитель по п.6 или 7 или подвергнутый тепловой обработке формованный пористый элемент по п.16.
18. Способ получения продуктов алкиленоксида, включающий контактирование в паровой фазе алкена с кислородом или кислородсодержащим газом в присутствии катализатора по п.17, причем контактирование проводят в технологических условиях, достаточных для производства алкиленоксида.
19. Способ получения этиленгликоля, этаноламина или простого эфира этиленгликоля, включающий превращение этиленоксида, полученного способом по п.18.
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-
2007
- 2007-07-20 WO PCT/US2007/016437 patent/WO2008054564A1/en active Application Filing
- 2007-07-20 CN CN201210567470.7A patent/CN103101943B/zh active Active
- 2007-07-20 CA CA2925267A patent/CA2925267A1/en not_active Abandoned
- 2007-07-20 US US12/446,127 patent/US20100056816A1/en not_active Abandoned
- 2007-07-20 CN CN2007800405792A patent/CN101534938B/zh active Active
- 2007-07-20 EP EP20158314.3A patent/EP3677334A1/en active Pending
- 2007-07-20 RU RU2009120540/04A patent/RU2009120540A/ru not_active Application Discontinuation
- 2007-07-20 MX MX2009004622A patent/MX2009004622A/es unknown
- 2007-07-20 EP EP13161427.3A patent/EP2620212A3/en active Pending
- 2007-07-20 CA CA2667980A patent/CA2667980C/en active Active
- 2007-07-20 EP EP07810638.2A patent/EP2089155B1/en active Active
- 2007-07-20 TW TW096126603A patent/TWI454427B/zh active
Also Published As
Publication number | Publication date |
---|---|
CN103101943A (zh) | 2013-05-15 |
CN101534938B (zh) | 2012-12-26 |
MX2009004622A (es) | 2009-05-15 |
TWI454427B (zh) | 2014-10-01 |
EP2620212A3 (en) | 2014-01-15 |
CA2667980C (en) | 2016-06-14 |
WO2008054564A1 (en) | 2008-05-08 |
CN103101943B (zh) | 2015-10-07 |
EP2089155B1 (en) | 2020-04-01 |
US20100056816A1 (en) | 2010-03-04 |
TW200821262A (en) | 2008-05-16 |
EP3677334A1 (en) | 2020-07-08 |
CA2667980A1 (en) | 2008-05-08 |
CA2925267A1 (en) | 2008-05-08 |
EP2089155A1 (en) | 2009-08-19 |
EP2620212A2 (en) | 2013-07-31 |
CN101534938A (zh) | 2009-09-16 |
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