Source: http://www.google.com/patents/US5807494?dq=5,664,133
Timestamp: 2014-07-14 16:33:02
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Matched Legal Cases: ['Application No. 272127', 'Application No. 272127', 'Application No. 410152', 'Application No. 433229', 'Application No. 410152', 'Application No. 433229', 'Application No. 92145679', 'Application No. 9295517', 'Application No. 92241473', 'Application No. 9133147', 'Application No. 92145679', 'Application No. 9295517', 'Application No. 92241473', 'Application No. 9133147', 'Application No. 636591', 'Application No. 636591', 'application No. 08', 'application No. 08']

Patent US5807494 - Gel compositions comprising silica and functionalized carbon products - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign in<nobr>Advanced Patent Search</nobr>PatentsNew gel compositions which comprise a carbonaceous component attached to a gel component. Preferably, the carbonaceous component is selected from the group consisting of: carbon blacks, carbon fibers, activated carbons and graphitic carbons; and the gel component is selected from the group consisting...http://www.google.com/patents/US5807494?utm_source=gb-gplus-sharePatent US5807494 - Gel compositions comprising silica and functionalized carbon productsAdvanced Patent SearchPublication numberUS5807494 APublication typeGrantApplication numberUS 08/356,849Publication dateSep 15, 1998Filing dateDec 15, 1994Priority dateDec 15, 1994Fee statusPaidAlso published asCA2207417A1, CN1096880C, CN1173144A, DE69515347D1, DE69515347T2, EP0871540A2, EP0871540B1, US6107350, WO1996018456A2, WO1996018456A3Publication number08356849, 356849, US 5807494 A, US 5807494A, US-A-5807494, US5807494 A, US5807494AInventorsRalph Ulrich Boes, James A. Belmont, David J. Kaul, Douglas M. Smith, William C. AckermanOriginal AssigneeBoes; Ralph Ulrich, Belmont; James A., Kaul; David J., Smith; Douglas M., Ackerman; William C.Export CitationBiBTeX, EndNote, RefManPatent Citations (100), Non-Patent Citations (127), Referenced by (12), Classifications (46), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetGel compositions comprising silica and functionalized carbon productsUS 5807494 AAbstract New gel compositions which comprise a carbonaceous component attached to a gel component. Preferably, the carbonaceous component is selected from the group consisting of: carbon blacks, carbon fibers, activated carbons and graphitic carbons; and the gel component is selected from the group consisting of: metal oxide gels and polymeric gels. □ Also disclosed are new gel compositions comprising: a gel component and a carbon black product having attached at least one organic group, the organic group comprising: a) at least one aromatic group, and b) at least one ionic group, at least one ionizable group, or a mixture of an ionic group and an ionizable group, wherein at least one aromatic group of the organic group is directly attached to the carbon black. Further disclosed are new gel compositions comprising: a gel component and a carbon black product having attached at least one organic group, the organic group comprising: a) at least one C1 -C12 alkyl group, and b) at least one ionic group, at least one ionizable group, or a mixture of an ionic group and an ionizable group, wherein at least one alkyl group of the organic group is directly attached to the carbon black. Uses for the gel compositions are also disclosed.
We claim: 1. A gel composition comprising:a gel component, wherein said gel comprises silica and a carbon black product having attached at least one organic group, the organic group comprising a) at least one aromatic group, and b) at least one ionic group, at least one ionizable group, or a mixture of an ionic group and an ionizable group, wherein at least one aromatic group of the organic group is directly attached to the carbon black. 2. The gel composition of claim 1 wherein the organic group comprises a sulfophenyl group or a salt thereof; a carboxyphenyl or a salt thereof; or mixtures thereof.
5. A gel composition comprising:a gel component, wherein said gel comprises silica and a carbon black product having attached at least one organic group, the organic group comprising: a) at least one C1 -C12 alkyl group, and b) at least one ionic group, at least one ionizable group, or a mixture of an ionic group and an ionizable group, wherein at least one alkyl group of the organic group is directly attached to the carbon black. 6. The gel composition of claim 5 wherein the ionic or the ionizable group comprises an ethane sulfonic acid or a salt thereof.
7. Thermal insulation comprising:a silica gel composition according to claim 1 or claim 5 comprising a carbon black produce attached to said gel component. 8. A gel composition according to claim 1 or claim 5 comprising:a carbonaceous component attached to a gel component wherein the carbonaceous component comprises: carbon black, carbon fiber, activated carbon, graphitic carbon or mixtures thereof. 9. The gel composition of claim 8 wherein the carbonaceous component comprises 1-50%, by weight of the composition.
6) Aging the resulting gel in a mold for approximately 24 hours at 50� C.;
7) Washing the resulting gel with water to replace the solvent component with water, and then aging the gel in water at elevated temperature (up to 100� C., preferably approximately 70� C.) for up to 24 hours;
______________________________________Metal Oxide      Form(s) as Gel Precursor______________________________________SiO2  Alkoxide, Sodium Si1icate, ColloidalTiO2  Alkoxide, ColloidalAl2 O3      Alkoxides, Colloidal, Sodium Aluminate, Salts______________________________________
TABLE 1______________________________________Carbon Black Analytical Properties                           Avg. Primary      N2 SA  DBP      Particle SizeCarbon Black      (m2 /g)                  (ml/100 g)                           (nm)______________________________________CB-A       24          132      130CB-B       230         70       16CB-C       560         120      16______________________________________
A solution prepared from 36.2 g sulfanilic acid, 8.76 g NaOH and 162 g of water was cooled in ice. Twenty grams of NO2 was added with stirring and the resulting suspension was warmed to 75 C. and added without delay to a pelletizer containing 300 g of CB-B. After pelletizing for three minutes, 35 g of additional water was added. After pelletizing for two additional minutes, the product was removed from the pelletizer and dried in an oven at approximately 125� C. The product had a 325 mesh residue of 0.14%, compared to 94% for the unreacted carbon black
Two hundred grams of CB-C was mixed into 2.8 L of water. Sulfanilic acid (42.4 g) was dissolved into the stirring mixture, and then a cold solution of 25.5 g NO2 in 100 g of water was added with rapid stirring. 4-Sulfobenzenediazonium hydroxide inner salt is formed in situ, which reacts with the carbon black. Bubbles were released. After stirring for one hour, 5 g of NO2 was introduced directly into the mixture. The dispersion was stirred for 15 minutes, left overnight and dried in an oven at 130� C.
Example 5 A concentrated silica sol was prepared by mixing 61 ml (milliliters) of tetraethyl orthosilicate (98% pure), 61 ml of ethyl alcohol, 4.87 ml deionized water, and 0.2 ml of 1M hydrochloric acid in a 500 ml round bottom flask with vigorous stirring. The flask was placed in a heating mantle and the mixture refluxed with the aid of a condenser at 70� C. for 2 hours. The resulting sol, which contained 15% SiO2 by weight, was cooled and stored at 5� C. until use.
Prior to gelation the sol was warmed to room temperature and the concentration was adjusted by dilution with ethyl alcohol such that the resulting mixture contained 11% SiO2 by weight. This was accomplished by combining 70% by volume original sol with 30% by volume ethyl alcohol. Gelation was initiated by addition of 0.5M NH4 OH in a volume ratio of 1:10 ammonia to sol. After the ammonia was added, the mixture was allowed to stir for 2-5 minutes and then cast into cylindrical tubes. Gelation occurred within 7-10 minutes. The gels were then sealed within the molds to prevent drying and aged at 50� C. for 24 hours. After the initial aging the gels were removed from the mold, placed in sealed tubes containing deionized water and aged further at 70� C. for an additional 24 hours. Upon removal from the oven the gels were rinsed several times with deionized water.
The gels were then placed in sealed tubes containing acetone and allowed to exchange pore fluid (primarily water) for 10 hours at 50� C. At the end of a 10 hour interval the gels were rinsed with acetone. This process was repeated a total of 3 times. After three such intervals a portion of the gels were then directly dried from acetone, first at 50� C. for 12 hours then at 140� C. for an additional 12 hours. The resulting gels showed some shrinkage and each had a measured bulk density of 0.5-0.6 g/cm3.
The remaining gels were placed in sealed tubes containing heptane and allowed to exchange pore fluid for 10 hours at 50� C. At the end of a 10 hour interval the gels were rinsed with heptane. This process was repeated three times. After three such intervals the gels were then directly dried from heptane, first at 70� C. for 12 hours then at 140� C. for an additional 12 hours. These gels retained their cylindrical shapes with the least amount of shrinkage and each had a bulk density of 0.4-0.44 g/cm3.
As in the previous Example, the ammonia was added, the CB-A was dispersed with vigorous stirring for 2-5 minutes and then cast into cylindrical tubes. Gelation occurred within 8-12 minutes. The gels were then aged for 24 hrs at 50� C., then removed from the casts and aged another 24 hours in deionized water at 70� C. The gels were then solvent exchanged and dried as outlined in Example 5, from acetone and heptane.
TABLE 2______________________________________Alkoxide Precursor Gels (&#8806;50% Carbon) Dried in Acetone              Carbon              Black              %, by           Bulk  Carbon      weight   Drying Density                                     RubExample  Black       (solids) Solvent                              (g/cm3)                                     Off______________________________________5      None        None     Acetone                              0.60   --6      CB-A         5%      Acetone                              0.55   17.57      CB-A        10%      Acetone                              0.45   238      CB-A        15%      Acetone                              0.48   359      CB-A        20%      Acetone                              0.43   4010     CB-A        30%      Acetone                              0.49   3511     CB-A        50%      Acetone                              0.51   4512     Modified CB-A               5%      Acetone                              0.45   7.513     Modified CB-A              10%      Acetone                              0.43   1514     Modified CB-A              15%      Acetone                              0.38   1515     Modified CB-A              20%      Acetone                              0.38   2516     Modified CB-A              30%      Acetone                              0.42   2517     Modified CB-A              50%      Acetone                              0.47   3018     CB-B        15%      Acetone                              0.45   2519     Modified CB-B              15%      Acetone                              0.44   1520     Phenolic CB-B              15%      Acetone                              0.35   1021     CB-C        15%      Acetone                              0.38   3522     Modified CB-C              15%      Acetone                              0.37   15______________________________________
TABLE 3__________________________________________________________________________Alkoxide Precursor Gels (&#8806;50% Carbon) Dried in Heptane         Carbon         Black         %, by       Bulk     SEM Carbon  weight               Drying                     Density                          Rub FIG.Example Black   (solids)               Solvent                     (g/cm3)                          Off #__________________________________________________________________________5     None    None  Heptane                     0.40 --  16     CB-A     5%   Heptane                     0.38 15  --7     CB-A    10%   Heptane                     0.37 20  --8     CB-A    15%   Heptane                     0.31 30  29     CB-A    20%   Heptane                     0.34 40  --10    CB-A    30%   Heptane                     0.36 35  --11    CB-A    50%   Heptane                     0.41 45  --12    Modified CB-A          5%   Heptane                     0.36  5  --13    Modified CB-A         10%   Heptane                     0.34 15  --14    Modified CB-A         15%   Heptane                     0.29 10  315    Modified CB-A         20%   Heptane                     0.30 25  --16    Modified CB-A         30%   Heptane                     0.31 20  --17    Modified CB-A         50%   Heptane                     0.33 30  --18    CB-B    15%   Heptane                     0.36 25  419    Modified CB-B         15%   Heptane                     0.31 10  520    Phenolic CB-B         15%   Heptane                     0.26 5   621    CB-C    15%   Heptane                     0.31 30  722    Modified CB-C         15%   Heptane                     0.30 10  8__________________________________________________________________________ SEM FIG. # = Scanning Electron Microscope Figure Number
Example 23 A silica stock solution was prepared by mixing commercially available sodium silicate (SiO2 /Na2 O molar ratio of 3.22:1) with deionized water in a volume ratio of 1.33:1 water to sodium silicate. The temperature of the mixture was maintained at 15� C. with vigorous stirring in a jacketed beaker. A separate solution comprising 2M H2 SO4 was prepared by diluting concentrated sulfuric acid (96%) with water. An aliquot of 104 ml of the sodium silicate stock solution was then slowly added to 50 ml of stirred 2M acid. The rate of silicate addition was kept constant at 1 ml/minute and the acid solution was maintained at 15� C. in a jacketed beaker. The resulting silica sol contained approximately 10 wt % silica in a salty solution.
The gels were allowed to age for 1-2 hours at 50� C. in the molds after which they were placed in sealed tubes containing deionized water and kept at room temperature. Fresh water was added every 3 hours for a total of 12 hours at which time it was determined (by insertion of a sodium electrode) that the sodium sulfate salt was completely removed from the gel.
The gels were then aged at 70� C. in deionized water for up to 24 hours. Upon removal from the oven the gels were rinsed several times with deionized water, placed in sealed tubes with acetone and allowed to exchange pore fluid for 10 hours at 50� C. At the end of 10 hours the gels were rinsed with acetone and stored in fresh acetone at 50� C. This procedure was repeated three times.
After three such intervals, the gels were placed in sealed tubes containing heptane and allowed to exchange pore fluid for 10 hours. At the end of 10 hours the gels were rinsed with heptane and stored in fresh heptane at 50� C. This procedure was repeated three times.
After three such intervals, the gels were dried directly from heptane, first at 70� C. for 12 hours then at 140� C. for an additional 12 hours. The resulting dried gels retained their cylindrical forms and exhibited minimal shrinkage.
After gelation the materials were aged at 50� C. for 1-2 hours, as in Example 23, removed from the molds, and then washed free of salt for 12 hours at room temperature. The loaded gels were then solvent exchanged and dried as outlined in Example 23, from heptane.
The Modified CB-A was dispersed in a beaker of acetone, vacuum filtered, and then rinsed repeatedly with deionized water until the pH of the wash water was close to neutral. The Modified CB-A was then dried at 140� C. for 12 hours.
After gelation the materials were aged at 50� C. for 1-2 hours as before, removed from the molds, and then washed free of salt for 12 hours at room temperature. The gel compositions were then aged up to 24 hours at 70� C. in deionized water. A portion of the gels were then solvent exchanged and dried from heptane as outlined in the prior Examples.
After gelation, the materials were aged at 50� C. for 1-2 hours as before, removed from the molds and then washed free of salt for 12 hours at room temperature. The gel compositions were then aged up to 24 hours at 70� C. in deionized water. A portion of the gel compositions were then solvent exchanged and dried from heptane as outlined in the prior examples.
The Modified CB-B was dispersed in a beaker of acetone, vacuum filtered, and then rinsed repeatedly with deionized water until the pH of the wash water was close to neutral. The Modified CB-B was then dried at 140� C. for 12 hours.
After gelation, the materials were aged at 50� C. for 1-2 hours as before, removed from the molds, and then washed free of salt for 12 hours at room temperature. The gel compositions were then aged up to 24 hours at 70� C. in deionized water. The gels were then solvent exchanged and dried from heptane as outlined in the prior Examples.
The Phenolic CB-B was dispersed in a beaker of acetone, vacuum filtered, and then rinsed repeatedly with deionized water until the pH of the wash water was close to neutral. The Phenolic CB-B was then dried at 140� C. for 12 hours.
Example 29 The steps from Example 11 were repeated with the exception that the amount of CB-A was increased to 60% of the total solids contents and the aging and drying steps were changed. As before, the appropriate amount of CB-A was added and the sol was diluted with ethyl alcohol to maintain a constant total solids content. Gelation was initiated in the same fashion as in previous examples 5-22. The gels were then aged for 24 hours at 50� C. in the sealed cylindrical molds. Instead of washing with water and aging at 70� C., these gels were then dried directly from the mother liquor, first at 50� C. for 10 hours, then at 140� C. for 10 hours.
As in previous examples, the Modified CB-A was washed and then dispersed into the partially hydrolyzed silica solution such that 60% of the total solids content was Modified CB-A and the balance was silica. As before, the sol was diluted with ethyl alcohol to maintain a constant total solids content and gelation was initiated in an analogous fashion. The gels were then dried directly from the mother liquor as in Example 29, by aging for 24 hours at 50� C. in the sealed cylindrical molds, then at 140� C. for 10 hours.
The steps from Example 30 were repeated with the exception that the amount of Modified CB-A was increased to 70% of the total solids, the balance being silica. As before, the sol was diluted with ethyl alcohol to maintain a constant total solids content and gelation was initiated in an analogous fashion. The gels were then aged for 24 hours at 50� C. in the sealed cylindrical molds and then dried directly from the mother liquor, first at 50� C. for 10 hours, then at 140� C. for 10 hours.
The CB-C was dispersed into the partially hydrolyzed silica solution such that 80% of the total solids content was CB-C and the balance was silica. As before, the sol was diluted with ethyl alcohol to maintain a constant total solids content and gelation was initiated in an analogous fashion. The gels were then aged for 24 hours at 50� C. in the sealed cylindrical molds and then dried directly from the mother liquor, first at 50� C. for 10 hours, then at 140� C. for 10 hours.
As in previous examples, the Modified CB-C was washed and then dispersed into the partially hydrolyzed silica solution such that 80% of the total solids content was Modified CB-C and the balance was silica. As before, the sol was diluted with ethyl alcohol to maintain a constant total solids content and gelation was initiated in an analogous fashion. The gels were then aged for 24 hours at 50� C. in the sealed cylindrical molds and then dried directly from the mother liquor, first at 50� C. for 10 hours, then at 140� C. for 10 hours.
The steps from Example 33 were repeated with the exception that the amount of Modified CB-C which was utilized in the gel composition was increased to 85% of the total solids content. As before, the appropriate amount of Modified CB-C was added, and the sol was diluted with ethyl alcohol to maintain a constant total solids content and gelation was initiated in an analogous fashion. The gels were then aged for 24 hours at 50� C. in the sealed cylindrical molds and then dried directly from the mother liquor, first at 50� C. for 10 hours, then at 140� C. for 10 hours.
The steps from Example 33 were repeated with the exception that the amount of Modified CB-C which was utilized in the gel composition was increased to 90% of the total solids content As before, the appropriate amount of Modified CB-C was added and the sol was diluted with ethyl alcohol to maintain a constant total solids content and gelation was initiated in an analogous fashion. The gels were then aged for 24 hours at 50� C. in the sealed cylindrical molds and then dried directly from the mother liquor, first at 50� C. for 10 hours, then at 140� C. for 10 hours.
TABLE 5__________________________________________________________________________Alkoxide Precursor Gels (&gt;50% Carbon)Carbon        Drying  BulkExampleBlack    Amount              Solvent Density                             Form__________________________________________________________________________29   CB-A     60%  Mother liquor                      0.53 g/cm3                             Fines30   Modified CB-A         60%  Mother liquor                      0.54 g/cm3                             Pellet31   Modified CB-A         70%  Mother liquor                      0.61 g/cm3                             Pellet32   CB-C     80%  Mother liquor                      0.66 g/cm3                             Fines33   Modified CB-C         80%  Mother liquor                      0.65 g/cm3                             Pellet34   Modified CB-C         85%  Mother liquor                      0.66 g/cm3                             Pellet35   Modified CB-C         90%  Mother liquor                      0.63 g/cm3                             Pellet__________________________________________________________________________
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May. 1989.126Zoheidi et al., "Role of Oxygen Surface Groups in Catalysis of Hydrogasification of Carbon Black by Potassium Carbonate," Carbon, vol. 25, No. 6, pp. 809-819, 1987.127 *Zoheidi et al., Role of Oxygen Surface Groups in Catalysis of Hydrogasification of Carbon Black by Potassium Carbonate, Carbon, vol. 25, No. 6, pp. 809 819, 1987.* Cited by examinerReferenced byCiting PatentFiling datePublication dateApplicantTitleUS6375735 *Mar 31, 2000Apr 23, 2002Agritec, Inc.Acidifying caustic silicate solution produced by caustic digestion of biomass ash containing silica and activated carbon, the ash being obtained from thermal pyrolysis of the biomassUS6458458May 24, 1999Oct 1, 2002Cabot CorporationCarbon modified with ionizable or polar group; shell-core polymers; tensile strengthUS6479571Apr 3, 2000Nov 12, 2002Cabot CorporationElastomeric compositions containing polymer coated carbon products and other pigmentsUS6527022Feb 27, 2001Mar 4, 2003The Goodyear Tire & Rubber CompanyPneumatic tire having a tread containing a metal oxide aerogelUS7222821Nov 21, 2002May 29, 2007Matos Jeffrey AMethod and apparatus for treating fuel to temporarily reduce its combustibilityUS7345099 *Jun 29, 2004Mar 18, 2008Kao CorporationAqueous ink for ink jet printer recordingUS7410718 *Mar 26, 2004Aug 12, 2008Lawrence Livermore National Security, LlcAerogel and xerogel composites for use as carbon anodesUS7968191Mar 15, 2005Jun 28, 2011Cabot CorporationModified carbon products and their applicationsUS8042771May 25, 2007Oct 25, 2011Karl F. Milde, Jr.Method and apparatus for treating fuel to temporarily reduce its combustibilityUS20120172195 *Mar 16, 2012Jul 5, 2012World Minerals, Inc.Composition for filtering and removing particles and/or constituents from a fluidWO2000022051A1 *Oct 8, 1999Apr 20, 2000Cabot CorpPolymer coated carbon products and other pigments and methods of making same by aqueous media polymerizations or solvent coating methodsWO2001074712A1 *Mar 30, 2001Oct 11, 2001AgritecPrecipitated silicas, silica gels with and free of deposited carbon from caustic biomass ash solutions and processes* Cited by examinerClassifications U.S. Classification252/62, 423/449.2, 106/472International ClassificationB01J20/32, C01B31/02, C08L61/28, B01D71/02, B01D69/14, B01J21/18, C09K3/00, B01J20/20, C09C1/56, C08K3/04, C04B30/00, B01J20/10, B01J13/00, C08L61/08, C08L61/12, F02B77/13, C09D17/00Cooperative ClassificationB01J20/324, C09D17/005, B01J21/18, C09C1/56, C04B30/00, B01J20/28047, B01D71/021, F02B77/13, B01J20/3204, C09K3/00, B01J20/103, B01D69/141, B01J20/20, B01J20/3251, B01J20/3253European ClassificationB01D71/02C, B01J21/18, B01D69/14B, C09C1/56, C09D17/00J2, B01J20/32, F02B77/13, C09K3/00, B01J20/20, C04B30/00, B01J20/10BLegal EventsDateCodeEventDescriptionFeb 19, 2010FPAYFee paymentYear of fee payment: 12Feb 28, 2006FPAYFee paymentYear of fee payment: 8Feb 26, 2002FPAYFee paymentYear of fee payment: 4May 9, 1995ASAssignmentOwner name: CABOT CORPORATION, MASSACHUSETTSFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:BOES, RALPH U.;BELMONT, JAMES A.;KAUL, DAVID J.;AND OTHERS;REEL/FRAME:007486/0275;SIGNING DATES FROM 19950427 TO 19950503RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services©2012 Google