DE69515235D1 - Verfahren zur Herstellung eines Katalysators, Katalysatorträgers oder Adsorbens mit hoher Widerstandskraft - Google Patents

Verfahren zur Herstellung eines Katalysators, Katalysatorträgers oder Adsorbens mit hoher Widerstandskraft

Info

Publication number
DE69515235D1
DE69515235D1 DE69515235T DE69515235T DE69515235D1 DE 69515235 D1 DE69515235 D1 DE 69515235D1 DE 69515235 T DE69515235 T DE 69515235T DE 69515235 T DE69515235 T DE 69515235T DE 69515235 D1 DE69515235 D1 DE 69515235D1
Authority
DE
Germany
Prior art keywords
catalyst
adsorbent
production
high resistance
catalyst carrier
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.)
Expired - Fee Related
Application number
DE69515235T
Other languages
English (en)
Other versions
DE69515235T2 (de
Inventor
Merrill Lynn
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Corning Inc
Original Assignee
Corning Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Corning Inc filed Critical Corning Inc
Publication of DE69515235D1 publication Critical patent/DE69515235D1/de
Application granted granted Critical
Publication of DE69515235T2 publication Critical patent/DE69515235T2/de
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28042—Shaped bodies; Monolithic structures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28042—Shaped bodies; Monolithic structures
    • B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/30—After treatment, characterised by the means used
    • B01J2229/42—Addition of matrix or binder particles
DE69515235T 1994-09-12 1995-07-31 Verfahren zur Herstellung eines Katalysators, Katalysatorträgers oder Adsorbens mit hoher Widerstandskraft Expired - Fee Related DE69515235T2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US30415794A 1994-09-12 1994-09-12
US08/486,477 US5633217A (en) 1994-09-12 1995-06-07 Method of making a high strength catalyst, catalyst support or adsorber

Publications (2)

Publication Number Publication Date
DE69515235D1 true DE69515235D1 (de) 2000-04-06
DE69515235T2 DE69515235T2 (de) 2000-09-07

Family

ID=26973840

Family Applications (1)

Application Number Title Priority Date Filing Date
DE69515235T Expired - Fee Related DE69515235T2 (de) 1994-09-12 1995-07-31 Verfahren zur Herstellung eines Katalysators, Katalysatorträgers oder Adsorbens mit hoher Widerstandskraft

Country Status (6)

Country Link
US (1) US5633217A (de)
EP (1) EP0700718B1 (de)
JP (1) JPH08253376A (de)
KR (1) KR100362495B1 (de)
BR (1) BR9503985A (de)
DE (1) DE69515235T2 (de)

Families Citing this family (65)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5565394A (en) * 1994-10-11 1996-10-15 Corning Incorporated Low expansion molecular sieves and method of making same
EP0756891A1 (de) * 1995-07-26 1997-02-05 Corning Incorporated Eisenzeolith zur NOx-Umsätzung
US6001320A (en) * 1995-10-12 1999-12-14 Corning Incorporated Method of adsorbing hydrocarbons
DE19607862C2 (de) * 1996-03-01 1998-10-29 Volkswagen Ag Verfahren und Vorrichtungen zur Abgasreinigung
JP2001503668A (ja) 1996-08-19 2001-03-21 フォルクスワーゲン・アクチェンゲゼルシャフト ＮＯ▲下ｘ▼吸収体
WO1998007497A1 (de) 1996-08-19 1998-02-26 Volkswagen Aktiengesellschaft FREMDGEZÜNDETE BRENNKRAFTMASCHINE MIT EINEM NOx-ADSORBER
US6004896A (en) * 1996-09-30 1999-12-21 Corning Incorporated Hydrocarbon adsorbers, method of making and use therefor
IN186651B (de) * 1997-03-10 2001-10-20 Indian Petrochemicals Corp Ltd
IN186652B (de) * 1997-03-10 2001-10-20 Indian Petrochemicals Corp Ltd
IN188725B (de) * 1997-03-10 2002-11-02 Indian Petrochemicals Corp Ltd
DE19723751A1 (de) * 1997-06-06 1998-12-10 Basf Ag Formkörper und Verfahren zu dessen Herstellung
DE19741201A1 (de) * 1997-09-18 1999-03-25 Wacker Chemie Gmbh Auf Organopolysiloxanmikrogelpartikeln immobilisierte Organoaluminiumverbindungen
WO1999017873A1 (en) * 1997-10-08 1999-04-15 Corning Incorporated Method of making small pore hydrophilic molecular sieve bodies
US5919724A (en) * 1998-03-05 1999-07-06 Aluminum Company Of America Process for making phosphate stabilized metal oxide particles
CA2326179C (en) * 1998-03-31 2009-01-27 Grace Gmbh & Co. Kg. Shaped body of zeolite, a process for its production and its use
US6117812A (en) 1998-10-06 2000-09-12 China Petro-Chemical Corporation Dual functional catalyst of packing type and the catalytic distillation equipment
US6548440B1 (en) * 1999-05-26 2003-04-15 Science & Technology Corporation @ Unm Synthesis of attrition-resistant heterogeneous catalysts using templated mesoporous silica
DE19924453A1 (de) * 1999-05-28 2001-01-18 Grace Gmbh & Co Kg Formkörper aus Silicagel und porösen amorphen Mischoxiden, Verfahren zu ihrer Herstellung und deren Verwendung
AUPQ219399A0 (en) * 1999-08-13 1999-09-02 Currumbin Sand & Gravel Pty Ltd Improvements to hydrated aluminosilicates
US6207101B1 (en) * 1999-09-30 2001-03-27 Corning Incorporated Method of making fired bodies
JP2003518434A (ja) 1999-12-28 2003-06-10 コーニング インコーポレイテッド ゼオライト／アルミナ触媒支持体組成物およびその製造方法
KR20020080357A (ko) * 1999-12-29 2002-10-23 코닝 인코포레이티드 고강도 및 고표면적 촉매, 촉매 지지체 또는 흡착제조성물
KR20020007021A (ko) * 2000-07-14 2002-01-26 신동우 세라믹스 촉매 담체의 제조 방법
JP4215936B2 (ja) * 2000-07-31 2009-01-28 日本碍子株式会社 ハニカム構造体の製造方法
JP2002228359A (ja) * 2001-02-02 2002-08-14 Ngk Insulators Ltd ハニカム構造体の乾燥方法
JP2003024777A (ja) * 2001-07-19 2003-01-28 Mitsubishi Electric Corp 窒素酸化物吸着体およびその製造方法
US6592651B2 (en) * 2001-11-02 2003-07-15 The Boc Group, Inc. Activation processes for monolith adsorbents
US6773580B2 (en) 2001-12-11 2004-08-10 Corning Incorporated Catalytic reforming system and process
DE10219879A1 (de) * 2002-05-03 2003-11-20 Basf Ag Katalysatorträger und Verfahren zu seiner Herstellung
US20040004031A1 (en) * 2002-06-26 2004-01-08 Boger Thorsten R. System and process for pyrolysis gasoline hydrotreatment
TW200507924A (en) 2003-02-17 2005-03-01 Getters Spa Composition and devices for gas sorption and process for their manufacturing
US7157013B2 (en) * 2003-09-17 2007-01-02 Mani Erfan Filtration method
US7572749B2 (en) * 2004-08-31 2009-08-11 Exxonmobil Research And Engineering Company Structured bodies with siliceous binder
DE102005059711A1 (de) * 2005-12-12 2007-06-14 Basf Ag Formkörper enthaltend ein mikroporöses Material und mindestens ein siliciumhaltiges Bindemittel, Verfahren zu seiner Herstellung und seine Verwendung als Katalysator, insbesondere in einem Verfahren zur kontinuierlichen Synthese von Methylaminen
EP2176188B1 (de) * 2007-07-31 2020-09-02 Corning Incorporated Verfahren zur herstellung von porösen keramischen filtern und zusammensetzungen zum auftragen auf keramische wabenkörper
US9828298B2 (en) 2007-11-30 2017-11-28 Corning Incorporated Cement compositions for applying to honeycomb bodies
US9174879B2 (en) 2007-11-30 2015-11-03 Corning Incorporated Ceramic precursor batch composition and method of increasing ceramic precursor batch extrusion rate
PL2485840T3 (pl) * 2009-10-08 2017-01-31 Basf Se SPOSÓB WYTWARZANIA ZWIĄZANEGO Si KATALIZATORA DO PROCESÓW W ZŁOŻU FLUIDALNYM
US20120046157A1 (en) * 2010-08-23 2012-02-23 Yanxia Lu Particulate Filter And Methods For Filter Strength And Pore Size Modification
WO2012063341A1 (ja) * 2010-11-10 2012-05-18 イビデン株式会社 ハニカム構造体の製造方法、およびハニカム成形体の脱脂処理装置
US9011583B2 (en) 2011-04-29 2015-04-21 Corning Incorporated Article for CO2 capture having heat exchange capability
US20120308439A1 (en) 2011-06-01 2012-12-06 Johnson Matthey Public Limited Company Cold start catalyst and its use in exhaust systems
JP2015514011A (ja) * 2012-04-05 2015-05-18 コーニング インコーポレイテッド 選択されたハニカムチャネル表面上の不透性ポリマー被覆
US9062586B2 (en) 2012-04-05 2015-06-23 Corning Incorporated Impermeable polymer coating on selected honeycomb channel surfaces
MX2014016112A (es) 2012-06-22 2015-09-21 Praxair Technology Inc Composiciones adsorbentes novedosas.
RU2670754C2 (ru) 2013-10-30 2018-10-25 Джонсон Мэтти Паблик Лимитед Компани Катализатор тройного действия и его использование в выхлопных системах
KR102383420B1 (ko) 2013-12-06 2022-04-07 존슨 맛쎄이 퍼블릭 리미티드 컴파니 귀금속 및 소기공 분자체를 포함하는 수동 NOx 흡착제
RU2692809C1 (ru) 2013-12-06 2019-06-27 Джонсон Мэтти Паблик Лимитед Компани Катализатор для холодного запуска и его применение в выхлопных системах
WO2015085305A1 (en) 2013-12-06 2015-06-11 Johnson Matthey Public Limited Company An exhaust gas catalyst containing two different noble metal-molecular sieve catalysts
FR3022800A1 (fr) * 2014-06-30 2016-01-01 IFP Energies Nouvelles Procede de preparation par extrusion reactive de materiaux inorganiques poreux mis en forme
FR3031915B1 (fr) * 2015-01-28 2018-11-30 Centre National De La Recherche Scientifique (C.N.R.S) Nouveau materiau comme adsorbant pour la decontamination moleculaire
JP6700290B2 (ja) 2015-02-06 2020-05-27 ジョンソン、マッセイ、パブリック、リミテッド、カンパニーＪｏｈｎｓｏｎ Ｍａｔｔｈｅｙ Ｐｕｂｌｉｃ Ｌｉｍｉｔｅｄ Ｃｏｍｐａｎｙ 三元触媒及び排気システムにおけるその使用
RU2017132853A (ru) 2015-02-26 2019-03-26 Джонсон Мэтти Паблик Лимитед Компани ПАССИВНЫЙ АДСОРБЕР NOx
KR20170132158A (ko) 2015-03-25 2017-12-01 존슨 맛쎄이 퍼블릭 리미티드 컴파니 귀금속 및 OFF 프레임워크 유형을 갖는 분자체를 포함하는 수동 NOx 흡착제
CN107847865A (zh) 2015-07-02 2018-03-27 庄信万丰股份有限公司 被动nox吸附剂
CN105622079B (zh) * 2015-12-25 2016-10-19 山东硅元新型材料有限责任公司 分子筛膜支撑体的制备方法
GB2551622A (en) 2016-04-22 2017-12-27 Johnson Matthey Plc STA-19, A new member of the GME family of molecular sieve zeotypes, methods of preparation and use
GB2551871A (en) 2016-04-22 2018-01-03 Johnson Matthey Plc STA-18, A new member of the SFW family of molecular sieve zeotypes, methods of preparation and use
GB2551885A (en) 2016-04-28 2018-01-03 Johnson Matthey Plc STA-20, a novel molecular sieve framework type, methods of preparation and use
US10717035B2 (en) * 2017-02-13 2020-07-21 Praxair Technology, Inc. Tunable adsorbents
CN111032595A (zh) * 2017-08-11 2020-04-17 康宁股份有限公司 包含反相乳液的生坯陶瓷批料混合物及形成陶瓷体的方法
CN111712474A (zh) 2017-12-19 2020-09-25 康宁股份有限公司 包含稳定化乳液的生坯陶瓷混合物及形成陶瓷体的方法
CN113474290B (zh) 2019-03-28 2023-12-29 庄信万丰股份有限公司 具有“sfw-GME尾部”的cha和aft的分子筛共生物、制备和使用方法
FR3108332B1 (fr) * 2020-03-23 2022-10-21 Centre Nat Etd Spatiales Suspension homogène pour peintures zéolithiques
WO2021198645A1 (en) 2020-03-31 2021-10-07 Johnson Matthey Public Limited Company Mixed oxide and its use as nox adsorber

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL6709949A (de) * 1966-07-22 1968-01-23
US4083905A (en) * 1975-04-25 1978-04-11 Champion Spark Plug Company Open mesh, random fiber, ceramic structure, monolithic catalyst support
US4239615A (en) * 1979-12-19 1980-12-16 Uop Inc. High octane FCC process
US4657880A (en) * 1985-03-18 1987-04-14 Corning Glass Works Preparation of high surface area agglomerates for catalyst support and preparation of monolithic support structures containing them
US4831267A (en) * 1987-02-16 1989-05-16 Siemens Aktiengesellschaft Detector for charged particles
US5074990A (en) * 1987-10-30 1991-12-24 Exxon Research And Engineering Company Fluid catalytic cracking using catalysts containing an alumina-on-silica component
US5520895A (en) * 1994-07-07 1996-05-28 Mobil Oil Corporation Method for the reduction of nitrogen oxides using iron impregnated zeolites

Also Published As

Publication number Publication date
BR9503985A (pt) 1996-09-24
JPH08253376A (ja) 1996-10-01
US5633217A (en) 1997-05-27
EP0700718A1 (de) 1996-03-13
KR960010079A (ko) 1996-04-20
EP0700718B1 (de) 2000-03-01
KR100362495B1 (ko) 2003-03-26
DE69515235T2 (de) 2000-09-07

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