DE10300094A1 - Zeolite having a lamellar aggregate structure, useful in ion exchange, catalysis, washing powder and gas separation is prepared from a layer silicate, intercalated with a template followed by direct hydrothermal recrystallization - Google Patents
Zeolite having a lamellar aggregate structure, useful in ion exchange, catalysis, washing powder and gas separation is prepared from a layer silicate, intercalated with a template followed by direct hydrothermal recrystallization Download PDFInfo
- Publication number
- DE10300094A1 DE10300094A1 DE2003100094 DE10300094A DE10300094A1 DE 10300094 A1 DE10300094 A1 DE 10300094A1 DE 2003100094 DE2003100094 DE 2003100094 DE 10300094 A DE10300094 A DE 10300094A DE 10300094 A1 DE10300094 A1 DE 10300094A1
- Authority
- DE
- Germany
- Prior art keywords
- zeolite
- bea
- zeolite according
- reaction mixture
- deionized water
- 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.)
- Withdrawn
Links
- 239000010457 zeolite Substances 0.000 title claims abstract description 48
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 44
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000005342 ion exchange Methods 0.000 title claims description 3
- 238000001953 recrystallisation Methods 0.000 title abstract 3
- 238000006555 catalytic reaction Methods 0.000 title 1
- 239000000843 powder Substances 0.000 title 1
- 238000000926 separation method Methods 0.000 title 1
- 238000005406 washing Methods 0.000 title 1
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000011541 reaction mixture Substances 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 11
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002086 nanomaterial Substances 0.000 claims description 6
- 238000004220 aggregation Methods 0.000 claims description 4
- 230000002776 aggregation Effects 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- PMYUVOOOQDGQNW-UHFFFAOYSA-N hexasodium;trioxido(trioxidosilyloxy)silane Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] PMYUVOOOQDGQNW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 6
- 230000009466 transformation Effects 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
Die Erfindung betrifft einen Zeolith,
dessen Kristallite schichtartig aggregiert sind, und ein Verfahren
zu seiner Herstellung, wobei der Zeolith direkt aus einem Schichtsilikat
erhalten wird nach Hauptpatent
Zeolithe sind poröse kristalline Alumosilikate mit hochgeordnetem kristallinen Aufbau. Sie bestehen aus SiO4- und AlO4-Tetraedern und werden von feinen Kanälen mit 0,3 bis 0,8 nm Durchmesser durchzogen. Die Porenöffnungsdurchmesser liegen zwischen 3 bis 14 Å (mikroporös), die spezifischen Oberflächen können größer als 1000 m2 g–1 sein. Zeolithe werden z. B. als Ionenaustauscher, als Katalysatoren und Trennmittel für Gasgemische in der Petrochemie und der Mineralölverarbeitung großtechnisch, aber auch in Bereichen des täglichen Lebens als Waschmittelzusatz eingesetzt.Zeolites are porous crystalline aluminosilicates with a highly ordered crystalline structure. They consist of SiO 4 and AlO 4 tetrahedra and are traversed by fine channels with a diameter of 0.3 to 0.8 nm. The pore opening diameters are between 3 and 14 Å (microporous), the specific surfaces can be larger than 1000 m 2 g -1 . Zeolites are e.g. B. as an ion exchanger, as catalysts and release agents for gas mixtures in petrochemicals and mineral oil processing on an industrial scale, but also in everyday life as a detergent additive.
Aufgrund der Größenverhältnisse zählen diese Materialien zu den nanostrukturierten Materialien bzw. sind die einzelnen Kristallite als Nanopartikel anzusehen.Due to the size relationships, these materials are among the nanostructured materials or are the individual crystallites to be regarded as nanoparticles.
Als Nanopartikel werden Partikel mit einer Größe von ca. 0,1 bis 100 Nanometern (nm) bezeichnet.Particles become nanoparticles with a size of approx. 0.1 to 100 nanometers (nm).
Die Erzeugung von Nanopartikeln und nanostrukturierten Materialien ist Gegenstand der Nanotechnik oder Nanostrukturtechnik, einem modernen Gebiet der physikalischen Grundlagenforschung und Halbleitertechnik, die die Manipulation von Materie im atomaren Maßstab erlaubt. Ziel der Nanotechnik sind präzise Strukturierungen in der Größenordnung von Nanometern zur Herstellung extrem kleiner Baueinheiten oder Strukturen mit gezielt einstellbaren Eigenschaften.The generation of nanoparticles and nanostructured materials is the subject of nanotechnology or Nanostructure technology, a modern field of basic physical research and Semiconductor technology that manipulates matter in the atomic scale allowed. The aim of nanotechnology is precise structuring in the Magnitude of nanometers for the manufacture of extremely small units or Structures with selectively adjustable properties.
Durch die Nanotechnik ergeben sich auch für Zeolithe neue Einsatzgebiete und -möglichkeiten. Zeolithkristallite sind letztlich Nanopartikel und Verbünde davon stellen nanoskopische Strukturen dar.The result of nanotechnology also for zeolites new fields of application and possibilities. zeolite crystallites are ultimately nanoparticles and composites of them make nanoscopic Structures.
Nanostrukturen werden auch als regelmäßige Anordnungen von Nanoteilchen auf geeigneten Substraten erzeugt. Für Zeolithe ergeben sich neue Einsatzgebiete und ein erweitertes Anwendungspotenzial.Nanostructures are also called regular arrangements generated by nanoparticles on suitable substrates. For zeolites there are new areas of application and an expanded application potential.
Hinzu tritt die Möglichkeit der gezielten Modifikation der Eigenschaften durch die Ausnutzung der Oberflächeneigenschaften und Phänomene der Zeolithpartikel und Strukturen, beispielsweise durch eine Beschichtung bzw. Imprägnierung.Added to this is the possibility of targeted modification the properties by utilizing the surface properties and phenomena the zeolite particles and structures, for example by a coating or impregnation.
Der Erfindung liegt die im Verhältnis zum Hauptpatent präzisierte Aufgabe zugrunde, einen Zeolith derart auszubilden, dass dieser eine hohe Kristallinität bei sehr geringen Teilchengrößen mit einer einheitlichen Morphologie und eine sehr gut zugängliche Oberfläche aufweist sowie ein Verfahren zu seiner Herstellung anzugeben, wobei als Schichtsilikat Kanemit Verwendung finden soll.The invention lies in relation to the main patent clarified Task to form a zeolite in such a way that this high crystallinity with very small particle sizes a uniform morphology and a very accessible one surface has and to specify a method for its production, wherein Kanemit should be used as layered silicate.
Erfindungsgemäß wird die Aufgabe durch einen
Zeolith mit einer lamellaren Aggregationsstruktur nach dem Gegenstand
des Hauptpatents
Aufgabengemäß soll der Zeolith aus Kanemit bzw. deren Precursor, dem Natriumdisilikat (SKS-6), gewonnen werden, wobei nach einer beispielhaften Ausgestaltung der Erfindung 50 g SKS-6 in 1000 ml deionisiertem Wasser dispergiert und über 90 min gerührt werden. Anschließend wird der Kanemit gefiltert, mit deionisiertem Wasser gewaschen und bei Raumtemperatur über 24 h getrocknet.According to the task, the zeolite from Kanemit or their precursor, the sodium disilicate (SKS-6), are obtained, whereby according to an exemplary embodiment of the invention 50 g SKS-6 dispersed in 1000 ml deionized water and over 90 min touched become. Subsequently the Kanemit is filtered, washed with deionized water and at room temperature above Dried for 24 hours.
Der Kanemit wird zu einer 10% bis 40%igen wässrigen Lösung von Tetraethylammoniumhydroxid (TEAOH) und Natriumaluminat mit einem Gehalt von 10% bis 25% Al2O3 und 10 % bis 30% Na2O sowie deionisiertem Wasser zugesetzt und über 45 min gerührt, wobei die chemische Komposition der entstehenden Reaktionsmischung bei 0,2 bis 0,3 Na2O : x Al2O3 : SiO2: 0,25 bis 0,5 TEAOH : 25 bis 40 H2O enthält, wobei x zwischen 0,000025 und 0,02 liegt.The kanemite is added to a 10% to 40% aqueous solution of tetraethylammonium hydroxide (TEAOH) and sodium aluminate containing 10% to 25% Al 2 O 3 and 10% to 30% Na 2 O and deionized water and over 45 min stirred, the chemical composition of the resulting reaction mixture at 0.2 to 0.3 Na 2 O: x Al 2 O 3 : SiO 2 : 0.25 to 0.5 TEAOH: 25 to 40 H 2 O, where x between 0.000025 and 0.02.
Das Reaktionsgemisch wird in einem Autoklaven auf 110 bis 150°C erhitzt und unter Eigendruck zwischen ca. 1,5 bis 10 bar über beispielsweise 10 h bis 96 h hydrothermal in beta Zeolith (BEA) umgewandelt.The reaction mixture is in one Autoclaves at 110 to 150 ° C heated and under autogenous pressure between about 1.5 to 10 bar, for example 10 h to 96 h hydrothermally converted to beta zeolite (BEA).
Das Reaktionsprodukt wird nachfolgend gefiltert, mit deionisiertem Wasser gewaschen und bei 550°C über 12 h kalziniert.The reaction product is as follows filtered, washed with deionized water and at 550 ° C for 12 h calcined.
Nach einer besonders vorteilhaften Ausgestaltung der Erfindung wird der beta Zeolith (BEA) zur Erreichung seiner katalytisch aktiven Protonendonator – Form (H-BEA) zweimal mit 1 M Ammoniumnitratlösung (NH4NO3) bei 70°C über 12 h zum Ionenaustausch geführt.According to a particularly advantageous embodiment of the invention, the beta zeolite (BEA) is carried out twice with 1 M ammonium nitrate solution (NH 4 NO 3 ) at 70 ° C. for 12 h to achieve its catalytically active proton donor form (H-BEA) for 12 hours for ion exchange.
In diesem Falle wird der beta Zeolith (BEA) anschließend erneut bei 550°C über 12 h kalziniert.In this case the beta zeolite (BEA) afterwards again at 550 ° C for 12 h calcined.
Es entsteht auf diese Weise ein Zeolith, der in besonderer Weise die typische BEA-Struktur aufweist und der darüber hinaus Einzelkristalle besitzt, die eine schichtartige Aggregationsstruktur aufweisen und damit die typischen Vorteile von Nanopartikeln besitzen, die durch die Aggregationsstruktur besonders gut einsetzbar sind.This creates a zeolite, which has the typical BEA structure in a special way and which about that also has single crystals that have a layer-like aggregation structure have the typical advantages of nanoparticles, which can be used particularly well due to the aggregation structure.
Weitere Einzelheiten, Merkmale und Vorteile der Erfindung ergeben sich aus der nachfolgenden Beschreibung von Ausführungsbeispielen mit Bezugnahme auf die zugehörigen Zeichnungen. Es zeigen:More details, features and Advantages of the invention result from the following description of embodiments with reference to the related Drawings. Show it:
In
Dieses Ausführungsbeispiel entspricht der Probe-Nr. st-307 mit einer Kristallinität von 97%.This embodiment corresponds to sample no. st-307 with a crystallinity of 97%.
Dieses Ausführungsbeispiel entspricht der Probe-Nr. st-306 mit einer maximalen Kristallinität von 100%.This embodiment corresponds to sample no. st-306 with a maximum crystallinity of 100%.
In
Deutlich zu erkennen ist, dass die Schichtstruktur in einen nanoskaligen feinteiligen Zeolith umgewandelt ist.It can be clearly seen that the layer structure is converted into a nanoscale fine-particle zeolite.
Die maximale Kristallinität erreichte dabei die Probe-Nr. st-306.The maximum crystallinity reached the sample no. st-306th
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2003100094 DE10300094A1 (en) | 2001-07-06 | 2003-01-03 | Zeolite having a lamellar aggregate structure, useful in ion exchange, catalysis, washing powder and gas separation is prepared from a layer silicate, intercalated with a template followed by direct hydrothermal recrystallization |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2001134022 DE10134022A1 (en) | 2001-07-06 | 2001-07-06 | Zeolites having improved crystallinity and catalytic properties at low particle size are obtained by intercalating a layered silicate and then recrystallizing by direct hydrothermal treatment |
| DE2003100094 DE10300094A1 (en) | 2001-07-06 | 2003-01-03 | Zeolite having a lamellar aggregate structure, useful in ion exchange, catalysis, washing powder and gas separation is prepared from a layer silicate, intercalated with a template followed by direct hydrothermal recrystallization |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE10300094A1 true DE10300094A1 (en) | 2004-07-15 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE2003100094 Withdrawn DE10300094A1 (en) | 2001-07-06 | 2003-01-03 | Zeolite having a lamellar aggregate structure, useful in ion exchange, catalysis, washing powder and gas separation is prepared from a layer silicate, intercalated with a template followed by direct hydrothermal recrystallization |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE10300094A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006054950A1 (en) * | 2004-11-19 | 2006-05-26 | Agency For Science, Technology And Research | Crystalline oxide material and its synthesis |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4318242A1 (en) * | 1993-06-02 | 1994-12-08 | Hoechst Ag | Process for the preparation of crystalline sodium layer silicate with kanemite structure |
| DE69512993T2 (en) * | 1994-06-10 | 2000-02-03 | Pq Holding, Inc. | SILICATE COMPOSITE MATERIAL |
| DE10046635A1 (en) * | 1999-09-20 | 2001-04-05 | Denso Corp | Porous metal oxide materials, useful for removing water in air conditioning plant, e.g. for vehicle, have water vapor adsorption capacity varying with relative water vapor pressure |
| DE69619821T2 (en) * | 1995-06-23 | 2002-11-28 | Reilly Industries, Inc. | Pyridine-SYNTHESIS |
| DE10134022A1 (en) * | 2001-07-06 | 2003-02-06 | Tricat Catalytic Products Gmbh | Zeolites having improved crystallinity and catalytic properties at low particle size are obtained by intercalating a layered silicate and then recrystallizing by direct hydrothermal treatment |
-
2003
- 2003-01-03 DE DE2003100094 patent/DE10300094A1/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4318242A1 (en) * | 1993-06-02 | 1994-12-08 | Hoechst Ag | Process for the preparation of crystalline sodium layer silicate with kanemite structure |
| DE69512993T2 (en) * | 1994-06-10 | 2000-02-03 | Pq Holding, Inc. | SILICATE COMPOSITE MATERIAL |
| DE69619821T2 (en) * | 1995-06-23 | 2002-11-28 | Reilly Industries, Inc. | Pyridine-SYNTHESIS |
| DE10046635A1 (en) * | 1999-09-20 | 2001-04-05 | Denso Corp | Porous metal oxide materials, useful for removing water in air conditioning plant, e.g. for vehicle, have water vapor adsorption capacity varying with relative water vapor pressure |
| DE10134022A1 (en) * | 2001-07-06 | 2003-02-06 | Tricat Catalytic Products Gmbh | Zeolites having improved crystallinity and catalytic properties at low particle size are obtained by intercalating a layered silicate and then recrystallizing by direct hydrothermal treatment |
Non-Patent Citations (2)
| Title |
|---|
| Baerlocher, C. et al.: Atlas of Zeolite Framework Types. 5. Aufl., Amsterdam: Elsevier, 2001, S. 76 u. 77, ISBN 0-444-50701-9 * |
| JP 06-48725 A (Ref. aus Pat. Abstr. of Jp.) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006054950A1 (en) * | 2004-11-19 | 2006-05-26 | Agency For Science, Technology And Research | Crystalline oxide material and its synthesis |
| US7976822B2 (en) | 2004-11-19 | 2011-07-12 | Agency For Science, Technology And Research | Crystalline oxide material and its synthesis |
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