Source: http://www.google.com/patents/US5250112?dq=No.+6,411,949&ei=AUR7T-LGJqSr0AHy2aSiBg
Timestamp: 2017-06-25 22:12:31
Document Index: 365757947

Matched Legal Cases: ['art 1', 'art 1', 'art 2', 'art 2', 'art 3', 'art 3']

Patent US5250112 - Spinel black pigments based on copper-chromium-manganese mixed oxides, a ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsSpinel black pigments are prepared by annealing oxides, hydroxides or carbonates of copper, chromium and manganese and grinding the product. The manganese-yielding component is Mn3 O4....http://www.google.com/patents/US5250112?utm_source=gb-gplus-sharePatent US5250112 - Spinel black pigments based on copper-chromium-manganese mixed oxides, a process for their preparation and their useAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS5250112 APublication typeGrantApplication numberUS 07/979,769Publication dateOct 5, 1993Filing dateNov 20, 1992Priority dateDec 5, 1991Fee statusLapsedAlso published asDE4140118A1, EP0545205A1, EP0545205B1Publication number07979769, 979769, US 5250112 A, US 5250112A, US-A-5250112, US5250112 A, US5250112AInventorsKlaus Wussow, Peter Kuske, Manfred Mansmann, Dieter Messer, Dieter RadeOriginal AssigneeBayer AktiengesellschaftExport CitationBiBTeX, EndNote, RefManPatent Citations (6), Non-Patent Citations (16), Referenced by (19), Classifications (16), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetSpinel black pigments based on copper-chromium-manganese mixed oxides, a process for their preparation and their use
3. A process for the preparation of spinel black pigments, comprising annealing a mixture of oxides, hydroxides or carbonates of copper, chromium and manganese, optionally with the addition of mineralizing agents, at temperatures of from 750° to 900° C. and grinding and optionally washing and drying the furnace products, wherein the manganese yielding component is Mn3 O4.
Mixed phase pigments are normally produced by subjecting an intimate mixture of the metal oxides, or of compounds which form the metal oxides when heated, to a solid state reaction at temperatures of from 800° to 1400° C. and then grinding the product.
U.S. Pat. No. 2,248,021 describes ceramic colouring agents consisting of oxides of copper and chromium in a molar ratio of chromium to copper of from 1.5:1 to 2.5:1, optionally containing up to 5% of manganese dioxide. U.S. Pat. No. 2,309,173 discloses black pigments of the copper-chrome type which are obtained by adding up to 15% of the metal oxides of iron, nickel, cobalt, manganese, molybdenum, tungsten, vanadium and/or uranium to a mixture of copper oxide and chromium oxide and calcining the resulting mixture at temperatures of from 800° to 1100° C.
The present invention also relates to a process for the preparation of the black pigments according to the invention. This is a process for the preparation of spinel black pigments by annealing a mixture of oxides, hydroxides and/or carbonates of copper, chromium and manganese, optionally with the addition of mineralizing agents, at temperatures of from 750° to 900° C. and grinding the furnace products and optionally washing and drying, Mn3 O4 being the component which provides the manganese.
After the addition of the copper and chromium component, a homogeneous suspension is prepared with intensive stirring. Mixing apparatus operating on the rotor-stator principle are particularly suitable for this purpose. The suspension is then dewatered, for which purpose filter presses, decanting centrifuges or the like may be used. After the filter cake has been dewatered, it may be dried by conventional methods, preferably using hot gas driers such as spray driers or spin flash driers and contact driers. The filter cake or the dry substance is then calcined. Both directly heated and indirectly heated furnaces are suitable for calcining, e.g. continuously operating rotary furnaces, annular hearth furnaces, sliding bat furnaces, tunnel furnaces or intermittently operated rotary drum furnaces and chamber furnaces. Annealing temperatures of from 750° C. to 900° C. have proved to be suitable for the formation of copper-chromium-manganese mixed oxide. The reaction times are, of course, longer at low temperatures than at higher temperatures and vary from 8 hours to 30 minutes.
2 m3 of MnSO4 solution at a concentration of 600 g of MnSO4.H2 O/1 are diluted with 7.5 m3 of water in a heatable stirrer vessel with gas inlet. The pH is adjusted to 11 by the addition of 395 l of 45% sodium hydroxide solution. The resulting suspension of Mn(OH)2 is then heated to 80° C. and gassed with 70 m3 of air per hour for 6 hours. The solid substance obtained is filtered off and washed. According to X-ray diffraction analysis, the product is phase pure Mn3 O4 with Hausmannite structure. The manganese content of the moist filter cake is 40%. The specific surface area (determined according to BET-N2 -1-point method DIN 66131) of the material which has been dried at 130° C. is 10 m2 /g.
660 kg of the Mn3 O4 filter cake obtained as described above are worked up into a homogeneous suspension with 365 kg of Cr2 O3 GN (Product of Bayer AG), 332 kg of CuCO3.Cu(OH)2.xH2 O (46% Cu, Product of Th. Goldschmidt AG), 9 kg of Na2 B4 O7.5H2 O and 1000 l of water, using a rotor-stator mixer. The mixture is dried and calcined for 6 hours at 800° C. in an oxidizing atmosphere in a rotary drum furnace. The furnace clinker is first size reduced wet in a ball mill and then fine ground in a cascade of pearl mills. An intensely black pigment with high tinting strength, as indicated by a low CIELAB brightness L* of the mixture with the whit pigment (see Table 1), is obtained after drying and disagglomeration.
The suspension is filtered, dried and then annealed at 800° C. for one hour in a laboratory batch furnace. 80 g of the furnace product are size reduced in a laboratory ball mill with 140 ml of water for 30 minutes and the suspension thus obtained is then stirred for 10 minutes at 2000 revs/min in a laboratory ball mill equipped with stirrer containing 320 ml corresponding to 600 g of grinding media (average diameter 0.7 mm). The grinding media are separated off and the suspension is filtered, washed, dried and dis-agglomerated. A deep black pigment of high tinting strength (see Table 1) and spinel structure is obtained. The composition of this pigment is comparable to that of the product from Example 1.
The colour of the dried lacquer was measured according to DIN 5033, using a spectral colorimeter (Standard Illuminant C, measuring geometry d/8, 2° standard observer). The CIELAB colour system according to DIN 6174 was used for evaluating the result.
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A. Lewis, Pigment Handbook, John Wiley & Sons, New York 1988. 2nd Edition, vol. 1, pp. 777 784.14P. A. Lewis, Pigment Handbook, John Wiley & Sons, New York 1988. 2nd Edition, vol. 1, pp. 777-784.15 *Ullmanns Encyklop die der technischen Chemi, Verlag Chemie, Weinheim 1979, 4th Edition, vol. 18, pp. 607 608.16Ullmanns Encyklopadie der technischen Chemi, Verlag Chemie, Weinheim 1979, 4th Edition, vol. 18, pp. 607-608.* Cited by examinerReferenced byCiting PatentFiling datePublication dateApplicantTitleUS5693134 *Dec 29, 1994Dec 2, 1997Merck Patent Gesellschaft Mit Beschrankter HaftungGray interference pigment and process for producing the sameUS6235106Sep 28, 2000May 22, 2001Engelhard CorporationBlue shade Fe-Cr blackUS6416868Nov 23, 1999Jul 9, 2002Dmc2 Degussa Metals Catalysts Cerdec AgAlkaline earth-manganese oxide pigmentsUS6503316Sep 22, 2000Jan 7, 2003Dmc2 Degussa Metals Catalysts Cerdec AgBismuth-containing laser markable compositions and methods of making and using sameUS6579356Jul 17, 2001Jun 17, 2003Engelhard CorporationHigh strength Fe-Cr brown with excellent weatheringUS6680121Dec 18, 2002Jan 20, 2004Dmc2 Degussa Metals Catalysts Cerdec AgBismuth-containing laser markable compositions and methods of making and using sameUS6932862 *Nov 29, 2001Aug 23, 2005Maytag CorporationHigh temperature coating composition and method of applyingUS7619031 *Aug 6, 2003Nov 17, 2009Techno Polymer Co., Ltd.Low heat storing thermoplastic resin composition and molding thereofUS9115262Nov 2, 2012Aug 25, 2015Tokan Material Technology Co., Ltd.Complex inorganic colored pigment with reduced elution of hexavalent chromium therefromUS9276232 *Sep 11, 2013Mar 1, 2016Samsung Display Co., Ltd.Display apparatus and method of manufacturing the sameUS9574092Apr 17, 2012Feb 21, 2017Brightsource Industries (Israel), Ltd.Solar-radiation-absorbing formulations and related apparatus and methodsUS20030099775 *Nov 29, 2001May 29, 2003Maytag CorporationHigh temperature coating composition and method of applyingUS20060128862 *Aug 6, 2003Jun 15, 2006Yuuichi KanayamaLow heat storing thermoplastic resin composition and molding thereofUS20140339510 *Sep 11, 2013Nov 20, 2014Samsung Display Co., Ltd.Display apparatus and method of manufacturing the sameCN103958617A *Nov 2, 2012Jul 30, 2014东罐材料科技株式会社Composite oxide pigment having reduced elution of hexavalent chromium therefromCN103958617B *Nov 2, 2012Jan 6, 2016东罐材料科技株式会社减少六价铬溶出的复合氧化物颜料EP2774956A4 *Nov 2, 2012Sep 30, 2015Tokan Material Technology Co LtdComposite oxide pigment having reduced elution of hexavalent chromium therefromWO2000004101A1 *Jul 13, 1999Jan 27, 2000Inco Industria Colori S.R.L.Inorganic black pigments containing molybdenumWO2012145283A1 *Apr 17, 2012Oct 26, 2012Brightsource Industries (Israel) Ltd.Solar-radiation-absorbing formulations and related apparatus and methods* Cited by examinerClassifications U.S. Classification106/453, 106/480International ClassificationC01G45/00, C03C8/14, C08K3/22, C09C1/00, C09D17/00Cooperative ClassificationC01P2006/12, C01G45/006, C01P2002/32, C01P2006/80, C01P2006/60, C01P2006/62, C09C1/00European ClassificationC01G45/00D, C09C1/00Legal EventsDateCodeEventDescriptionNov 20, 1992ASAssignmentOwner name: BAYER AG, GERMANYFree format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNORS:WUSSOW, KLAUS;KUSKE, PETER;MANSMANN, MANFRED;AND OTHERS;REEL/FRAME:006342/0841;SIGNING DATES FROM 19920930 TO 19921012May 13, 1997REMIMaintenance fee reminder mailedOct 5, 1997LAPSLapse for failure to pay maintenance feesDec 16, 1997FPExpired due to failure to pay maintenance feeEffective date: 19971008RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services