TWI648407B - 自粒狀含貴金屬耐火材料中分離貴金屬之方法 - Google Patents

自粒狀含貴金屬耐火材料中分離貴金屬之方法 Download PDF

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Publication number: TWI648407B
Authority: TW; Taiwan
Prior art keywords: refractory material; noble metal; weight; fluidized bed; containing refractory
Prior art date: 2016-10-07

Application number

TW106130339A

Other languages

English (en)

Chinese (zh)

Other versions

TW201814056A (zh

Inventor

荷傑溫克勒

克莉絲汀克勞斯哈爾

彼得史翠弗

簡羅德

克理斯多夫羅利奇

Original Assignee

德商賀利氏德國有限責任兩合公司

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.)

2016-10-07

Filing date

2017-09-05

Publication date

2019-01-21

2017-09-05 Application filed by 德商賀利氏德國有限責任兩合公司 filed Critical 德商賀利氏德國有限責任兩合公司

2018-04-16 Publication of TW201814056A publication Critical patent/TW201814056A/zh

2019-01-21 Application granted granted Critical

2019-01-21 Publication of TWI648407B publication Critical patent/TWI648407B/zh

Links

239000010970 precious metal Substances 0.000 title claims abstract description 95
239000011819 refractory material Substances 0.000 title claims abstract description 74
238000000034 method Methods 0.000 title claims abstract description 34
VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 72
239000007789 gas Substances 0.000 claims abstract description 61
229910000510 noble metal Inorganic materials 0.000 claims abstract description 57
ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 38
239000000460 chlorine Substances 0.000 claims abstract description 38
229910052801 chlorine Inorganic materials 0.000 claims abstract description 38
239000011261 inert gas Substances 0.000 claims abstract description 20
239000000203 mixture Substances 0.000 claims description 34
BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 26
KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 22
239000002699 waste material Substances 0.000 claims description 18
239000000463 material Substances 0.000 claims description 14
229910052697 platinum Inorganic materials 0.000 claims description 13
229910052763 palladium Inorganic materials 0.000 claims description 11
239000002893 slag Substances 0.000 claims description 11
238000005065 mining Methods 0.000 claims description 10
239000002638 heterogeneous catalyst Substances 0.000 claims description 9
229910001510 metal chloride Inorganic materials 0.000 claims description 6
239000012141 concentrate Substances 0.000 claims description 5
239000010802 sludge Substances 0.000 claims description 5
239000007787 solid Substances 0.000 claims description 4
BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
238000005243 fluidization Methods 0.000 claims description 3
229910052741 iridium Inorganic materials 0.000 claims description 3
GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
229910052762 osmium Inorganic materials 0.000 claims description 3
SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 3
229910052709 silver Inorganic materials 0.000 claims description 3
239000004332 silver Substances 0.000 claims description 3
KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
229910052737 gold Inorganic materials 0.000 claims description 2
239000010931 gold Substances 0.000 claims description 2
229910052707 ruthenium Inorganic materials 0.000 claims description 2
238000006243 chemical reaction Methods 0.000 description 35
239000003054 catalyst Substances 0.000 description 30
239000002245 particle Substances 0.000 description 14
238000000227 grinding Methods 0.000 description 13
IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
239000000306 component Substances 0.000 description 8
238000000576 coating method Methods 0.000 description 6
229910052757 nitrogen Inorganic materials 0.000 description 6
229910052782 aluminium Inorganic materials 0.000 description 5
XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
239000011248 coating agent Substances 0.000 description 5
GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
238000004182 chemical digestion Methods 0.000 description 4
239000008187 granular material Substances 0.000 description 4
238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 4
229910017604 nitric acid Inorganic materials 0.000 description 4
239000000126 substance Substances 0.000 description 4
101150003085 Pdcl gene Proteins 0.000 description 3
238000004380 ashing Methods 0.000 description 3
238000002485 combustion reaction Methods 0.000 description 3
238000010438 heat treatment Methods 0.000 description 3
229910052703 rhodium Inorganic materials 0.000 description 3
239000010948 rhodium Substances 0.000 description 3
MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
238000000926 separation method Methods 0.000 description 3
XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
150000001875 compounds Chemical class 0.000 description 2
238000000605 extraction Methods 0.000 description 2
239000012535 impurity Substances 0.000 description 2
238000004519 manufacturing process Methods 0.000 description 2
238000000746 purification Methods 0.000 description 2
238000000197 pyrolysis Methods 0.000 description 2
238000007670 refining Methods 0.000 description 2
238000012958 reprocessing Methods 0.000 description 2
230000003068 static effect Effects 0.000 description 2
ZUGAOYSWHHGDJY-UHFFFAOYSA-K 5-hydroxy-2,8,9-trioxa-1-aluminabicyclo[3.3.2]decane-3,7,10-trione Chemical compound [Al+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O ZUGAOYSWHHGDJY-UHFFFAOYSA-K 0.000 description 1
229910000505 Al2TiO5 Inorganic materials 0.000 description 1
OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
229910052684 Cerium Inorganic materials 0.000 description 1
150000000703 Cerium Chemical class 0.000 description 1
RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
229910021536 Zeolite Inorganic materials 0.000 description 1
QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
239000003570 air Substances 0.000 description 1
238000004887 air purification Methods 0.000 description 1
229910045601 alloy Inorganic materials 0.000 description 1
239000000956 alloy Substances 0.000 description 1
238000000137 annealing Methods 0.000 description 1
229910052786 argon Inorganic materials 0.000 description 1
239000002585 base Substances 0.000 description 1
238000010923 batch production Methods 0.000 description 1
230000015572 biosynthetic process Effects 0.000 description 1
238000001354 calcination Methods 0.000 description 1
229910002092 carbon dioxide Inorganic materials 0.000 description 1
239000001569 carbon dioxide Substances 0.000 description 1
229910002091 carbon monoxide Inorganic materials 0.000 description 1
239000012159 carrier gas Substances 0.000 description 1
239000000919 ceramic Substances 0.000 description 1
CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
239000007795 chemical reaction product Substances 0.000 description 1
238000005660 chlorination reaction Methods 0.000 description 1
150000001805 chlorine compounds Chemical class 0.000 description 1
239000006255 coating slurry Substances 0.000 description 1
229910052802 copper Inorganic materials 0.000 description 1
239000010949 copper Substances 0.000 description 1
229910052878 cordierite Inorganic materials 0.000 description 1
239000008358 core component Substances 0.000 description 1
230000008021 deposition Effects 0.000 description 1
JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
230000005611 electricity Effects 0.000 description 1
239000004744 fabric Substances 0.000 description 1
238000001914 filtration Methods 0.000 description 1
238000005188 flotation Methods 0.000 description 1
239000010439 graphite Substances 0.000 description 1
229910002804 graphite Inorganic materials 0.000 description 1
229910000856 hastalloy Inorganic materials 0.000 description 1
239000001307 helium Substances 0.000 description 1
229910052734 helium Inorganic materials 0.000 description 1
SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
238000005984 hydrogenation reaction Methods 0.000 description 1
238000009854 hydrometallurgy Methods 0.000 description 1
238000011065 in-situ storage Methods 0.000 description 1
230000002452 interceptive effect Effects 0.000 description 1
HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
239000000395 magnesium oxide Substances 0.000 description 1
238000010309 melting process Methods 0.000 description 1
229910052751 metal Inorganic materials 0.000 description 1
239000002184 metal Substances 0.000 description 1
239000007769 metal material Substances 0.000 description 1
150000004706 metal oxides Chemical class 0.000 description 1
150000002739 metals Chemical class 0.000 description 1
NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
229910052863 mullite Inorganic materials 0.000 description 1
229910052759 nickel Inorganic materials 0.000 description 1
229910052756 noble gas Inorganic materials 0.000 description 1
150000002835 noble gases Chemical class 0.000 description 1
239000011148 porous material Substances 0.000 description 1
AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
239000000376 reactant Substances 0.000 description 1
238000002407 reforming Methods 0.000 description 1
229910003468 tantalcarbide Inorganic materials 0.000 description 1
MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
239000004408 titanium dioxide Substances 0.000 description 1
239000010457 zeolite Substances 0.000 description 1
229910052726 zirconium Inorganic materials 0.000 description 1

Classifications

- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/06—Chloridising
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling

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Chemical & Material Sciences (AREA)
Engineering & Computer Science (AREA)
Manufacturing & Machinery (AREA)
Materials Engineering (AREA)
Mechanical Engineering (AREA)
Metallurgy (AREA)
Organic Chemistry (AREA)
Chemical Kinetics & Catalysis (AREA)
Catalysts (AREA)
Manufacture And Refinement Of Metals (AREA)

TW106130339A 2016-10-07 2017-09-05 自粒狀含貴金屬耐火材料中分離貴金屬之方法 TWI648407B (zh)

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
??16192809.8		2016-10-07
EP16192809		2016-10-07

Publications (2)

Publication Number	Publication Date
TW201814056A TW201814056A (zh)	2018-04-16
TWI648407B true TWI648407B (zh)	2019-01-21

Family

ID=57121100

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
TW106130339A TWI648407B (zh)	2016-10-07	2017-09-05	自粒狀含貴金屬耐火材料中分離貴金屬之方法

Country Status (2)

Country	Link
TW (1)	TWI648407B (de)
WO (1)	WO2018065127A1 (de)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
EP3763682A1 (de)	2019-07-12	2021-01-13	Heraeus Quarzglas GmbH & Co. KG	Reinigung von quarzpulvern durch entfernung von mikropartikeln aus feuerfesten materialien

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EP0612853A1 (de) *	1993-02-24	1994-08-31	Elektro-Chemie Ibbenbüren Gmbh	Verfahren zur Rückgewinnung von Wertmetallen aus gebrauchten Abgaskatalysatoren
WO2015193901A1 (en) *	2014-06-19	2015-12-23	Yeda Research And Development Co. Ltd.	Method for platinum group metals recovery from spent catalysts

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DE102007020142A1 (de) *	2007-04-26	2008-10-30	Bayer Materialscience Ag	Verfahren zur Rückgewinnung von Ruthenium aus einem rutheniumhaltigen geträgerten Katalysatormaterial
KR101663334B1 (ko) *	2008-12-30	2016-10-06	바스프 에스이	사용된 산화루테늄 포함 촉매로부터 루테늄을 회수하는 방법
CN102560128B (zh) *	2012-03-05	2013-10-09	武汉凯迪工程技术研究总院有限公司	氧化铝负载钌废催化剂中回收钌的方法

2017
- 2017-04-13 WO PCT/EP2017/058917 patent/WO2018065127A1/de not_active Ceased
- 2017-09-05 TW TW106130339A patent/TWI648407B/zh not_active IP Right Cessation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
US2860045A (en) *	1955-07-25	1958-11-11	Universal Oil Prod Co	Method of removing platinum from a composite containing platinum and alumina
EP0612853A1 (de) *	1993-02-24	1994-08-31	Elektro-Chemie Ibbenbüren Gmbh	Verfahren zur Rückgewinnung von Wertmetallen aus gebrauchten Abgaskatalysatoren
WO2015193901A1 (en) *	2014-06-19	2015-12-23	Yeda Research And Development Co. Ltd.	Method for platinum group metals recovery from spent catalysts

Also Published As

Publication number	Publication date
WO2018065127A1 (de)	2018-04-12
TW201814056A (zh)	2018-04-16

Publication	Publication Date	Title
US11898220B2 (en)	2024-02-13	Apparatus for platinum group metals recovery from spent catalysts
Jha et al.	2013	Hydrometallurgical recovery/recycling of platinum by the leaching of spent catalysts: A review
JP2010524672A (ja)	2010-07-22	ルテニウム含有担持触媒材料からルテニウムを回収する方法
KR102446605B1 (ko)	2022-09-22	귀금속 함유 촉매 성형체로부터 귀금속을 분리하기 위한 방법
CN104831071A (zh)	2015-08-12	一种水热法从废载体催化剂中回收铂钯的方法
TWI648407B (zh)	2019-01-21	自粒狀含貴金屬耐火材料中分離貴金屬之方法
CN113631740B (zh)	2023-06-23	生产pgm捕集剂合金的方法
EP3532646B1 (de)	2020-10-28	Verfahren zur metallrückgewinnung von platingruppenmetallen aus verbrauchten katalysatoren
JP7595305B2 (ja)	2024-12-06	Ｐｇｍの回収方法
TW201816128A (zh)	2018-05-01	自粒狀含貴金屬耐火材料中分離貴金屬之方法
US10612111B2 (en)	2020-04-07	Method and apparatus for extracting high-purity gold from ore
TW201814055A (zh)	2018-04-16	自含貴金屬耐火材料所製得之粗多孔成形體中分離貴金屬之方法
RU2094499C1 (ru)	1997-10-27	Способ переработки концентрата благородных металлов
JP4984123B2 (ja)	2012-07-25	ＳｉＣ系物質からの金または白金族元素の回収方法
WO2018219417A1 (ru)	2018-12-06	Способ и устройство для извлечения молибдена из низкосортного рудного сырья
US6045768A (en)	2000-04-04	Removal of carbon from particulate mixtures
TWI685571B (zh)	2020-02-21	貴重金屬-錫合金之濕式冶金加工的方法
RU2514554C2 (ru)	2014-04-27	Способ очистки серебросодержащего материала
RU2398900C1 (ru)	2010-09-10	Способ извлечения палладия из отходов электронного сырья
JPH0765122B2 (ja)	1995-07-12	貴金属の凝離方法
Devyatykh et al.	2019	Survey of Methods of Refining Catalysts for the Extraction of Platinum Group Metals
JPH01132723A (ja)	1989-05-25	合金成分の単離方法
JPS62280330A (ja)	1987-12-05	白金回収方法
HU194946B (en)	1988-03-28	Process for producing platinum of at least 99,9% purity from exhousted catalysts and/or other exhousted metal platinum
RO110055B1 (ro)	1995-09-29	Procedeu de recuperare a platinei și rodiului

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2020-10-21	MM4A	Annulment or lapse of patent due to non-payment of fees