JP6307074B2 - マグネシウム安定化超低ソーダ分解触媒 - Google Patents

マグネシウム安定化超低ソーダ分解触媒 Download PDF

Info

Publication number
JP6307074B2
JP6307074B2 JP2015524374A JP2015524374A JP6307074B2 JP 6307074 B2 JP6307074 B2 JP 6307074B2 JP 2015524374 A JP2015524374 A JP 2015524374A JP 2015524374 A JP2015524374 A JP 2015524374A JP 6307074 B2 JP6307074 B2 JP 6307074B2
Authority
JP
Japan
Prior art keywords
catalyst
zeolite
total weight
magnesium salt
present
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
JP2015524374A
Other languages
English (en)
Japanese (ja)
Other versions
JP2015528744A (ja
Inventor
シユー,ユイイン
チエン,ウー−チエン
ウオームスベヒヤー,リチヤード・エフ
ストビチ,ケビン・ジエイ
クマー,ランジト
ジーバース,マイケル・エス
Original Assignee
ダブリュー・アール・グレイス・アンド・カンパニー−コネチカット
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 ダブリュー・アール・グレイス・アンド・カンパニー−コネチカット filed Critical ダブリュー・アール・グレイス・アンド・カンパニー−コネチカット
Publication of JP2015528744A publication Critical patent/JP2015528744A/ja
Application granted granted Critical
Publication of JP6307074B2 publication Critical patent/JP6307074B2/ja
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • 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
    • B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
    • B01J29/084—Y-type faujasite
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/16—Clays or other mineral silicates
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06—Halogens; Compounds thereof
    • B01J27/125—Halogens; Compounds thereof with scandium, yttrium, aluminium, gallium, indium or thallium
    • 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
    • B01J29/061—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof containing metallic elements added to the zeolite
    • 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
    • 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
    • B01J37/0027—Powdering
    • B01J37/0045—Drying a slurry, e.g. spray drying
    • 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
    • B01J37/0072—Preparation of particles, e.g. dispersion of droplets in an oil bath
    • 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
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • 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
    • B01J37/06—Washing
    • 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
    • B01J37/08—Heat treatment
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
    • C10G11/04—Oxides
    • C10G11/05—Crystalline alumino-silicates, e.g. molecular sieves
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
    • C10G11/08—Halides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G11/14—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts
    • C10G11/18—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts according to the "fluidised-bed" technique
    • 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
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
    • B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
    • 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
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/20—After treatment, characterised by the effect to be obtained to introduce other elements in the catalyst composition comprising the molecular sieve, but not specially in or on the molecular sieve itself
    • 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
    • B01J2229/38—Base treatment
    • 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
    • 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
    • B01J29/80—Mixtures of different zeolites
    • 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
    • B01J29/90—Regeneration or reactivation
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/70—Catalysts, in general, characterised by their form or physical properties characterised by their crystalline properties, e.g. semi-crystalline

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
JP2015524374A 2012-07-23 2013-07-23 マグネシウム安定化超低ソーダ分解触媒 Expired - Fee Related JP6307074B2 (ja)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US201261674527P 2012-07-23 2012-07-23
US61/674,527 2012-07-23
PCT/US2013/051581 WO2014018484A1 (en) 2012-07-23 2013-07-23 Magnesium stabilized ultra low soda cracking catalysts

Publications (2)

Publication Number Publication Date
JP2015528744A JP2015528744A (ja) 2015-10-01
JP6307074B2 true JP6307074B2 (ja) 2018-04-04

Family

ID=49997766

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2015524374A Expired - Fee Related JP6307074B2 (ja) 2012-07-23 2013-07-23 マグネシウム安定化超低ソーダ分解触媒

Country Status (13)

Country Link
US (1) US20150202602A1 (enExample)
EP (1) EP2874744B1 (enExample)
JP (1) JP6307074B2 (enExample)
KR (1) KR102151830B1 (enExample)
CN (1) CN104487167B (enExample)
BR (1) BR112015001606A2 (enExample)
CA (1) CA2879527C (enExample)
IN (1) IN2015DN00101A (enExample)
MX (2) MX376692B (enExample)
RU (1) RU2700409C2 (enExample)
TW (1) TWI611014B (enExample)
WO (1) WO2014018484A1 (enExample)
ZA (1) ZA201500188B (enExample)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2599720C1 (ru) * 2015-07-08 2016-10-10 Акционерное общество "Газпромнефть - Омский НПЗ" Катализатор для осуществления реакций межмолекулярного переноса водорода и способ его приготовления
US11319265B2 (en) 2018-11-02 2022-05-03 Shell Usa, Inc. Separation of ethane oxidative dehydrogenation effluent
KR102134292B1 (ko) * 2020-02-11 2020-07-15 주식회사 에스엔텍솔루숀 플라즈마 저온산화 흡착촉매 탈취기 및 탈취방법
TWI888612B (zh) 2020-08-03 2025-07-01 荷蘭商蜆殼國際研究公司 整合乙烯生產方法

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4242237A (en) * 1979-05-31 1980-12-30 Exxon Research & Engineering Co. Hydrocarbon cracking catalyst and process utilizing the same
US4308129A (en) * 1979-09-28 1981-12-29 Exxon Research & Engineering Co. Octane improvement cracking catalyst
CA1194465A (en) * 1981-08-10 1985-10-01 William A. Welsh Zeolite catalyst manufacture
US4458023A (en) * 1981-08-10 1984-07-03 W. R. Grace & Co. Catalyst manufacture
MX156975A (es) * 1981-08-10 1988-10-18 Grace W R & Co Mejoras en metodo para preparar una composicion catalizadora
JPH01111446A (ja) * 1987-10-23 1989-04-28 Nippon Oil Co Ltd 炭化水素転化触媒
DE3867421D1 (de) * 1987-10-23 1992-02-13 Nippon Oil Co Ltd Katalysatoren zur umwandlung von kohlenwasserstoffen.
JP3383071B2 (ja) * 1994-05-18 2003-03-04 出光興産株式会社 新規ゼオライト触媒及びその製造方法
JP3586544B2 (ja) * 1997-06-04 2004-11-10 触媒化成工業株式会社 炭化水素接触分解用触媒組成物
US8084383B2 (en) * 2004-03-16 2011-12-27 W.R. Grace & Co.-Conn. Gasoline sulfur reduction catalyst for fluid catalytic cracking process
US9643166B2 (en) * 2004-12-21 2017-05-09 Albemarle Netherlands B.V. FCC catalyst, its preparation and use
TWI428180B (zh) * 2005-02-25 2014-03-01 W R 康格雷氏公司 適用於流體化觸媒裂解程序之汽油硫減量觸媒
CN101166574B (zh) * 2005-04-27 2011-09-21 格雷斯公司 用于减少流化催化裂化过程中的NOx排放物的组合物和方法
WO2011115745A1 (en) * 2010-03-18 2011-09-22 W. R. Grace & Co.-Conn. Process for making improved zeolite catalysts from peptized aluminas
CN103703105B (zh) * 2011-07-06 2016-05-18 瑞来斯实业有限公司 催化剂/添加剂的工艺和组成物,用于降低流化床催化裂化(fcc)过程中的燃料气收率

Also Published As

Publication number Publication date
MX2020004131A (es) 2020-08-13
WO2014018484A1 (en) 2014-01-30
TW201410861A (zh) 2014-03-16
CA2879527A1 (en) 2014-01-30
EP2874744A1 (en) 2015-05-27
MX376692B (es) 2025-03-07
KR20150036718A (ko) 2015-04-07
MX2015001077A (es) 2015-04-08
EP2874744A4 (en) 2016-03-30
EP2874744B1 (en) 2023-06-14
CN104487167B (zh) 2017-12-12
US20150202602A1 (en) 2015-07-23
RU2015105982A (ru) 2016-09-10
JP2015528744A (ja) 2015-10-01
IN2015DN00101A (enExample) 2015-05-29
CN104487167A (zh) 2015-04-01
TWI611014B (zh) 2018-01-11
KR102151830B1 (ko) 2020-09-03
RU2700409C2 (ru) 2019-09-17
ZA201500188B (en) 2020-02-26
CA2879527C (en) 2022-01-11
BR112015001606A2 (pt) 2017-07-04

Similar Documents

Publication Publication Date Title
JP6570530B2 (ja) ホウ素酸化物およびリンを含有するfcc触媒組成物
JP6584411B2 (ja) ホウ素酸化物を含有するfcc触媒組成物
TWI647011B (zh) 含磷fcc觸媒
JP5431167B2 (ja) 改善された残油(bottoms)転化率を有する接触分解用触媒組成物
CN103703105B (zh) 催化剂/添加剂的工艺和组成物,用于降低流化床催化裂化(fcc)过程中的燃料气收率
JP6615097B2 (ja) Fcc法におけるホウ素酸化物
US10005072B2 (en) High matrix surface area catalytic cracking catalyst stabilized with magnesium and silica
JP4463556B2 (ja) ニッケルとバナジウムを含有する供給材料用のfcc触媒
US9993810B2 (en) Silica sol bound catalytic cracking catalyst stabilized with magnesium
CN104487167B (zh) 镁稳定的超低苏打裂化催化剂
JP7123864B2 (ja) 炭化水素油用流動接触分解触媒
US20100264066A1 (en) Aluminum sulfate bound catalysts

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20160627

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20170426

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20170524

A601 Written request for extension of time

Free format text: JAPANESE INTERMEDIATE CODE: A601

Effective date: 20170824

A601 Written request for extension of time

Free format text: JAPANESE INTERMEDIATE CODE: A601

Effective date: 20171024

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20171124

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20180207

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20180309

R150 Certificate of patent or registration of utility model

Ref document number: 6307074

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

LAPS Cancellation because of no payment of annual fees