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(12) United States Patent (10) Patent No.: US 6,524,737 B1 Tanii Et Al

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(12) United States Patent (10) Patent No.: US 6,524,737 B1 Tanii Et Al USOO6524737B1 (12) United States Patent (10) Patent No.: US 6,524,737 B1 Tanii et al. (45) Date of Patent: Feb. 25, 2003 (54) METHOD FOR CRUSHING CELL 5,478,664 A 12/1995 Kaneko et al. ............... 429/49 5,888,463 A * 3/1999 McLaughlin et al. ..... 429/49 X (75) Inventors: Tadaaki Tanii, Takasago (JP); Satoshi 6,150,050 A * 11/2000 Mathew et al. ............... 429/49 Tsuzuki, Takasago (JP); Shiro Honmura, Takasago (JP); Takeo FOREIGN PATENT DOCUMENTS Kamimura, Takasago (JP); Kenji Sasaki, Kobe (JP); Masakazu Yabuki, DE 4419.695 8/1995 ............ HO1M/6/52 Takasago (JP); Kiyonori Nishida, WO WO 94/25167 11/1994 ............ HO1M/6/52 Takasago (JP (JP) * cited by examiner (73) Assignee: Mitsubishi Heavy Industries, Ltd., Tokyo (JP) Primary Examiner Stephen Kalafut (*) Notice: Subject to any disclaimer, the term of this (74) Attorney, Agent, or Firm-Crowell & Moring LLP patent is extended or adjusted under 35 U.S.C. 154(b) by 0 days. (57) ABSTRACT This invention provides a safe and efficient method of (21) Appl. No.: 09/555,264 dismantling used lithium ion batteries. More Specifically, the (22) PCT Filed: Sep. 27, 1999 plastic cases which protect Sealed battery cells are removed from the system in a stable and reliable fashion. Valuable (86) PCT No.: PCT/JP99/05255 materials. Such as lithium cobalt oxide, an oxide of a lithium S371 (c)(1), tranStonition metal compound,COmpOund aluminum and copperCOoper must bbe (2), (4) Date: Jul. 25, 2000 Separated and recovered. The invention is distinguished by the fact that it entails the following processes. In the (87) PCT Pub. No.: WO00/19557 crushing process, the batteries are chilled to a temperature of PCT Pub. Date: ADr. 6, 2000 -50 C. or lower. In this state they are repeatedly subjected : Apr 0, to vibration and preSSure by a number of objects whose (30) Foreign Application Priority Data rigidity and Specific gravity are greater than those of the plastic. In this way the batteries are separated into Sealed Se2. SE - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - E. battery cells and plastic cases. In the heating process, the PI. ZO, 1999 () . Sealed battery cells Separated in the process are heated to a (51) Int. Cl." ............................................... HO1M 10/54 temperature of at least 200 C. in a non-oxidizing atmo (52) U.S. Cl. ......................................................... 429/49 Sphere to Separate mainly the organic materials. Finally, in (58) Field of Search ... ... 429/49 one or more Separation processes, the useleSS materials are removed and the targeted valuable materials are separated in (56) References Cited a Sequential fashion from the crushed fragments produced in the crushing process. U.S. PATENT DOCUMENTS 4,775,107 A * 10/1988 Heng et al. ................... 241/23 36 Claims, 27 Drawing Sheets - JSED BATTERY COPFR FOI ITUN COBA 6x3 &N CARBO U.S. Patent Feb. 25, 2003 Sheet 1 of 27 US 6,524,737 B1 Fig. 1 USED BATTERY SERENP- (S1) (S2) 2 HEATED (N2) (S3) (S4) 3. (S5) (S.11) SNEY (S15) recove the BALLS COPPER (S12)S12 Ca(OH)2 5 GAS OLUTION SEPARATR (S9) XHAUST CAS TREATMENT PROCESS 11 SpsPARATION PROCESS - Air o -1 g ~APSir (S10) solidCaF2, Ca3(PO4)waste 35EBrion 2 4)2 U.S. Patent Feb. 25, 2003 Sheet 2 of 27 US 6,524,737 B1 Fig. 2 1 2 (S3) (S4) t (S5) (S.11) 3 (S16) Espevide 4. (S7) (S12) gRATION SEER SOLID/ GAE LITHIUM COBALT SEPARATOR OXDE AND CARBO 5 OLUTIO re-season-issils8. (S9) (S8) EM SPSSES BAE 1 O 7 SOLUTION S10) HC SOLID WASTE 9 OLUTION CaF2, Ca.3(PO4)2 U.S. Patent Feb. 25, 2003 Sheet 3 of 27 US 6,524,737 B1 Fig. 3 USED BATTERY (S1) (S2) 2 (S3) 3 i S” (S.11) ) t (S16) striper HEAREEreas 4. (S22) (S12) S ( S31) 5TESLTEM COBAL SOLID/ CARBON GAS SEPARATOR Ca(OH)2 5 ON 8 y (S8) 1 EAEPE J is E 10 7 9 He arra SOLD WASTE OLUTION (S10) CaF2, Cas(PO4)2 U.S. Patent Feb. 25, 2003 Sheet 4 of 27 US 6,524,737 B1 Fig. 4 END - (S1) 2 (S2) (S3) (S4) 3 (SS) (S11) 16A 5 (S31) ission"--it as (S8) PROCESS 1 CharoxIDERM SEP I 7 E. E. Jo SOLID WASTE 9 CaF2, Ca.3(PO4)2 U.S. Patent Feb. 25, 2003 Sheet 5 of 27 US 6,524,737 B1 Fig. 5 ERP - (S1) (S2) 2 (S3) cause h- (S4) 3 16S (S26) HC SOLUTION ARATOR FOR UMCOBAL ALMNM st :Ens (SASEri. SEPARAF6i 17 S (S3i) SESSIONre -issile (S9) (S8) 11 8 7 so-E ESSE 10 SOLD WASTE 9 HCEurios CaF2, Ca.3(PO4)2 U.S. Patent Feb. 25, 2003 Sheet 6 of 27 US 6,524,737 B1 ESSEY (S3) railway(S4) 3 Ski ATInn (S 6) - RecoyiRECOWER TsTHE (S15)BALLS 4 S) Sierron (S7) (SAIF COPPER 6 (S12) SOLID/GAS LITHIUMTSE AN) COBAL Ca(OH)2 souri, SEPARATOR CARBON 50 8 (S9) SOLID WASTE 9 (S10) CaF2, Ca.3(PO4)2 U.S. Patent Feb. 25, 2003 Sheet 7 of 27 US 6,524,737 B1 Fig. 7 USED BATTERY ExN-1 (S1) 2 (S2) (S32) Eggs - (S3) (S4) 3 (S34)|COOLING (S5) (S.11) SNEELY (S 6) (S15) l (S7) in recove the balls E | | SETION 6 ea :EU:SOBALT 5 CARBON 50 (S33) (S9) (S8) 11 PARATI AS SOLUTSES HERE Do 9 SOLD WASTE SOLUTION (S10) CaF2, Cag (PO4)2 U.S. Patent Feb. 25, 2003 Sheet 8 of 27 US 6,524,737 B1 Fig. 8 4S. a ARROW A U.S. Patent Feb. 25, 2003 Sheet 9 of 27 US 6,524,737 B1 Fig. 9 SIDE VIEW FOMA U.S. Patent Feb. 25, 2003 Sheet 10 Of 27 US 6,524,737 B1 Fig. 10 SSTHOO?ANOILW?W?TI?OTOELANOWI?OJ. (GS) U.S. Patent Feb. 25, 2003 Sheet 11 of 27 US 6,524,737 B1 Fig.11 USED BATTERY (S ) ED AND BREAK OPEN (S2) MAGNETICALLY SEPARAT ESTICASE 2 (SAA) CHILLING AND CRUSHING (S 1) (S5) MAGNETICALLYSEPARATED BATEAER IRON 3 E.HEATING PROCESS (S 15) BALL E BALLS WIBRATION 4. SEE(ATION SEER FOIL 6 (S 1 2) LITHIUM COBALT OXIDE AND CARBON (S 13) f 8 GRANULATION - 5 3:SSION EEASENS (S 8) COBALT OXDE LITHIUM SEPARATION PROCESS OF WATER File: SOLID AND SOLUTION O 9 (S 1 0) SOLD WASTE SOLUTION CaF2,, CCa3 (PO4)2O4) U.S. Patent Feb. 25, 2003 Sheet 12 of 27 US 6,524,737 B1 Fig. 12 (#IS)SS300Hä9NILVAH | | | | | P (??S)SS300HäHIVAHALVM U.S. Patent Feb. 25, 2003 Sheet 13 Of 27 US 6,524,737 B1 SOLUTION 0, 1 O NO CHANGE NO CHANGE NO CHANGE NO CHANGE 8 BUBBLES TINY BUBBLES 5 SRFACE SSEE NO CHANGE NO CHANGE ROUGH, SMALL BUBBLES 10 MELFNC ON THE ENDS SURFACE NO CHANGE SMALL BUBBLESSMALL BUBBLES s 15 ARE NO CHANGE ON NO CHANGE PRODUCED THE SURFACE PARTIALLY SMALL BUBBLES TORN NO CHANGE ON NO C GE 20 OFF THE SURFACE HAN ROUGH SMALL BUBBLES 25 START MELTING THE SURFACE ROUGH SMAL BUBBLES START NO CHANGE ON NO CHANGE MELTING THE SURFACE SMALL BUBBLES NO CHANGE ON NO CHANGE END THE SURFACE no cases is so | | | | U.S. Patent Feb. 25, 2003 Sheet 14 of 27 US 6,524,737 B1 ig. 4 (O,G6)Å8CIELV?H 1870 (1HZ)OZ! U.S. Patent Feb. 25, 2003 Sheet 15 of 27 US 6,524,737 B1 Fig. 15 N. & a q : T Na d cd 3al E. s r Aa CN C e s S. S & 3 S 9 se & with (2) SNOI NINO?) is dO 3LWN NOILWIGNs) U.S. Patent Feb. 25, 2003 Sheet 16 of 27 US 6,524,737 B1 Fig. 16 NIII HSNTNN CS S C o O C e ad R es rN. SNJVo Le n (96 ) SNOI 3 NIYOnT. O ALVN NOILwala Nat) U.S. Patent Feb. 25, 2003 Sheet 17 of 27 US 6,524,737 B1 Fig. 17 U.S. Patent Feb. 25, 2003 Sheet 18 of 27 US 6,524,737 B1 Fig. 18 END -(S1) (S2) SSNLEY Plastic case heared (N)-(S3) S. (S11) 3 rs:SELY (S WATER BAT - (S15) FEEaton Eists12 S Ap OPPER re ARH, (S31) SENERSonSN R 4 LUM COBA S GASal Ens SEPARAT OCESS 11 EEREPARATIO to SOLD WASTE CaF2Ca(PO4)2 SOTTON (S10) 20 WA PRECIPITATION WATER SEPER WATER CONTAINING PHOR TER E"DE ("E" Efti. EAMOXIDE ANPESEQIS OMPOUND 7 (S41) 22 23 U.S. Patent Feb. 25, 2003 Sheet 19 of 27 US 6,524,737 B1 Fig. 19 ge:NP-(S) (S2) (S3) Er 7 (S4)(S5) (S11) 3 SEEDY 4 (S12) COPPER (ALUMINUM (S31) T 5 st St. Let E-2 SSESSION it. ocess, 8 (S8) FRESSEbst:RERSEPARATION 1. soleHC (sio Cafacis(Fo):SOLD WASTE 2O (S40) (S41) 1 O CPRAA9XIDE 22 7 22 U.S. Patent Feb. 25, 2003 Sheet 20 of 27 US 6,524,737 B1 Fig. 20 1 (S1) CHILLED AND BEE Š5 (S3) Out (S5)(S4) (S11) 3 MA EEEY EAR S ES 4. (S12) SEPARATORal ESSIC 8 (S8) 9 HC SO O (S10) CaF2, Cala(PO) O (S40) (S41) O 22 7 22 U.S. Patent Feb. 25, 2003 Sheet 21 of 27 US 6,524,737 B1 Fig. 21 1 (S1) EBSD (S2) 2 heared (n) --(S3) S: (S11) ) SESSEE2-ETER HC SOLUTIO e Sg/ SEPARäi DR (SOLID WASTE CaF2Ca(PO4)2 20 AOXID 22 7 22 U.S. Patent Feb. 25, 2003 Sheet 22 of 27 US 6,524,737 B1 Fig. 22 (S1) EiSPER AN (S2) 2 SNELLY (S3) ity (S4)(S5).
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