Source: http://www.google.com/patents/US5919841?dq=5359317
Timestamp: 2014-08-29 21:16:02
Document Index: 602454651

Matched Legal Cases: ['Application No. 80', 'Application No. 80', 'Application No. 63', 'Application No. 63', 'Application No. 53', 'Application No. 53', 'Application No. 61', 'Application No. 61', 'Application No. 63', 'Application No. 63', 'Application No. 63', 'Application No. 63', 'Application No. 2', 'Application No. 2', 'Application No. 4', 'Application No. 4', 'Application No. 4', 'Application No. 4', 'Application No. 4', 'Application No. 4']

Patent US5919841 - Hysteresis-free at high temperature - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign in<nobr>Advanced Patent Search</nobr>PatentsDisclosed are elastomeric compounds including an elastomer and a silicon-treated carbon black, and optionally including a coupling agent. The elastomeric compound exhibits poorer abrasion resistance, lower hysterisis at high temperature and comparable or increased hysterisis at low temperature compared...http://www.google.com/patents/US5919841?utm_source=gb-gplus-sharePatent US5919841 - Hysteresis-free at high temperatureAdvanced Patent SearchPublication numberUS5919841 APublication typeGrantApplication numberUS 08/876,903Publication dateJul 6, 1999Filing dateJun 17, 1997Priority dateMay 22, 1995Fee statusPaidAlso published asUS5830930Publication number08876903, 876903, US 5919841 A, US 5919841A, US-A-5919841, US5919841 A, US5919841AInventorsKhaled Mahmud, Meng-Jiao Wang, Robert A. FrancisOriginal AssigneeCabot CorporationExport CitationBiBTeX, EndNote, RefManPatent Citations (58), Non-Patent Citations (54), Referenced by (27), Classifications (15), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetHysteresis-free at high temperatureUS 5919841 AAbstract Disclosed are elastomeric compounds including an elastomer and a silicon-treated carbon black, and optionally including a coupling agent. The elastomeric compound exhibits poorer abrasion resistance, lower hysterisis at high temperature and comparable or increased hysterisis at low temperature compared to an elastomer containing an untreated carbon black. Elastomeric compounds incorporating an elastomer and an oxidized, silicon-treated carbon black are also disclosed. Also disclosed are methods for preparing elastomers compounded with the treated carbon black.
What is claimed is: 1. A method of preparing an elastomeric compound, comprising:masticating in a mixer, an aggregate comprising a carbon phase and a silicon-containing species phase and an elastomer for a first predetermined amount of time until the temperature rises to a first predetermined point, to form a masterbatch; milling said masterbatch; cooling said masterbatch to a first predetermined temperature; masticating said masterbatch in said mixer for a second predetermined amount of time until the temperature rises to a second predetermined point, to form a second masterbatch; milling said second masterbatch; cooling said second masterbatch to a second predetermined temperature; masticating in said mixer said second masterbatch and a curing agent for a third predetermined amount of time until the temperature rises to a third predetermined point, to form said elastomeric compound; milling said elastomeric compound; and cooling said elastomeric compound. 2. The method of claim 1, wherein said silicon-containing species phase exists as regions primarily at the surface of the aggregate.
RELATED APPLICATIONS This application is related to the following applications identified by title and attorneys' docket number, filed on even date herewith, for which serial numbers have not yet been accorded: Mineral Binders Colored With Silicon-Containing Carbon Black (0639/0A991); Elastomeric Compounds Incorporating Partially Coated Carbon Blacks (0639/0B060); and Elastomeric Compounds Incorporating Silicon-Treated Carbon Blacks and Coupling Agents (0639/0B059). The disclosure of each of the foregoing applications is hereby incorporated by reference.
FIELD OF THE INVENTION The present invention relates to novel elastomeric compounds exhibiting improved hysterisis properties. More particularly, the invention relates to novel elastomeric compounds incorporating silicon-treated carbon blacks.
The hysterisis of an elastomeric compound relates to the energy dissipated under cyclic deformation. In other words, the hysterisis of an elastomeric composition relates to the difference between the energy applied to deform the elastomeric composition and the energy released as the elastomeric composition recovers to its initial undeformed state. Hysterisis is characterized by a loss tangent, tan δ, which is a ratio of the loss modulus to the storage modulus (that is, viscous modulus to elastic modulus). Tires made with a tire tread compound having a lower hysterisis measured at higher temperatures, such as 40� C. or higher, will have reduced rolling resistance, which in turn, results in reduced fuel consumption by the vehicle using the tire. At the same time, a tire tread with a higher hysterisis value measured at low temperature, such as 0� C. or lower, will result in a tire with high wet traction and skid resistance which will increase driving safety. Thus, a tire tread compound demonstrating low hysterisis at high temperatures and high hysterisis at low temperatures can be said to have a good hysterisis balance.
SUMMARY OF THE INVENTION The present invention is directed to an elastomeric compound including an elastomer and a silicon-treated carbon black, and optionally including a coupling agent. The silicon-treated carbon black imparts to the elastomer poorer abrasion resistance, lower hysterisis at high temperature and comparable or increased hysterisis at low temperature compared to an untreated carbon black. Elastomeric compounds incorporating an elastomer and an oxidized, silicon-treated carbon black are also disclosed. Also disclosed are methods for preparing elastomeric compounds with the silicon-treated carbon blacks.
DETAILED DESCRIPTION OF THE INVENTION The present inventors have discovered that elastomeric compounds having desirable hysterisis and other properties may be obtained by compounding an elastomer with a silicon-treated carbon black. In the silicon-treated carbon black a silicon-containing species, including but not limited to, oxides and carbides of silicon, may be distributed through at least a portion of the carbon black aggregate as an intrinsic part of the carbon black.
The elastomeric compounds of the present invention may be prepared from the treated carbon blacks by compounding with any elastomer including those useful for compounding a carbon black. Any suitable elastomer may be compounded with the treated carbon blacks to provide the elastomeric compounds of the present invention. Such elastomers include, but are not limited to, homo- or co-polymers of 1,3 butadiene, styrene, isoprene, isobutylene, 2,3-dimethyl-1,3-butadiene, acrylonitrile, ethylene, and propylene Preferably, the elastomer has a glass transition temperature (Tg) as measured by differential scanning colorimetry (DSC) ranging from about -120� C. to about 0� C. Examples include, but are not limited, styrene-butadiene rubber (SBR), natural rubber, polybutadiene, and polyisoprene. Blends of any of the foregoing may also be used.
Five mg of carbon black was dispersed into 20 ml of chloroform and subjected to ultrasonic energy using a probe sonicator (W-385 Heat Systems Ultra Sonicator). A 2 ml aliquot was then dispersed into 15 ml of chloroform using a probe sonicator for three minutes. The resulting dispersion was placed on a 200 mesh nickel grid with aluminum substrate. The grid was then placed under a Fisons HB501 Scanning Transmission Electron Microscope (Fisons, West Sussex, England) equipped with an Oxford Link AN10000 Energy Dispersive X-ray Analyzer (Oxford Link, Concord, Mass.). Initially the grid was scanned for potential silica aggregates at low magnification (less than 200,000�). This was done by searching for aggregates that had a Si/C count ratio greater than unity. After this initial scan, typically thirty aggregates were selected for detailed analysis at higher magnification (from between 200,000� and 2,000,000�). The selected aggregates included all of the aggregates which contained Si/C count ratios greater than unity, as identified by the initial scan. The highest ratios of Si/C counts thus determined are set forth in Table 3 for N234, OMTS-CB and a mixture of N234 and silica.
Example 3--HF Treatment Hydrofluoric acid (HF) is able to dissolve silicon compounds but does not react with carbon. Thus, if either a conventional (untreated) carbon black or a mixture of silica and carbon black is treated with HF, the surface and surface area of the carbon black will remain unchanged, because it is unaffected by the dissolution of the silicon compounds removed from the mixture. However, if silicon containing species are distributed throughout at least a portion, including the surface, of the carbon black aggregate, the surface area will markedly increase as micropores are formed as the silicon compound is dissolved out of the carbon black structure.
Example 4--Preparation of Elastomeric Compositions The carbon blacks of the previous Examples were used to make elastomeric compounds. Elastomeric compositions incorporating the silicon-treated carbon blacks discussed above, were prepared using the following elastomers: solution SBR (Duradene 715 and Cariflex S-1215, from Firestone Synthetic Rubber & Latex Co., Akron, Ohio), functionalized solution SBR (NS 114 and NS 116 from Nippon Zeon Co., SL 574 and TO589 from Japan Synthetic Rubber Co.), emulsion SBR (SBR 1500, from Copolymer Rubber & Chemicals, Corp., Baton Rouge, La.), and natural rubber (SMR5, from Malaysia).
Flexzone 7P�, N-(1,3-dimethyl butyl)-N'-phenyl-p-phenylene diamine, is an anti-oxidant available from Unroyal Chemical Co., Middlebury, Conn. Durax�, N-cyclohexane-2-benzothiazole sulphenamide, is an accelerator available from R. T. Vanderbilt Co., of Norwalk, Conn., and Captax�, 2-mercaptobenzothiazole, is an accelerator available from R. T. Vanderbilt Co.
The elastomeric compounds were prepared using a two-stage mixing procedure. The internal mixer used for preparing the compounds was a Plasti-Corder EPL-V (obtained from C. W. Brabender, South Hackensack, N.J.) equipped with a cam-type mixing head (capacity 600 ml). In the first stage, the mixer was set at 80� C., and the rotor speed was set at 60 rpm. After the mixer was conditioned to 100� C. by heating the chamber with a dummy mixture, the elastomer was loaded and masticated for 1 minute. Carbon black, pre-blended with zinc oxide (obtained from New Jersey Zinc Co., N.J.), and optionally a coupling agent, was then added. After three minutes, stearic acid (obtained from Emery Chemicals, Cincinnati, Ohio) and anti-oxidant were added. Mixing was continued for an additional two minutes. The stage 1 masterbatch was then dumped from the mixer at five minutes total. This was then passed through an open mill (four inch, two-roll mill, obtained from C. W. Brabender, South Hackensack, N.J.) three times and stored at room temperature for two hours.
Example 5--Bound Rubber Test The bound rubber content of an elastomeric compound incorporating carbon black can be taken as a measure of the surface activity of the carbon black. The higher the bound rubber content, the higher the surface activity of the carbon black. Bound rubber was determined by extraction of an elastomeric compound with toluene at room temperature. The bound rubber is the elastomer remaining after extraction by the solvent. The elastomer used was solution SBR (SSBR) Duradene 715 without a coupling agent, as described above in Example 4.
Example 6--Dynamic Hysterisis and Abrasion Resistance The dynamic hysterisis and abrasion resistance rates were measured for the elastomeric compositions produced according to Example 4 above.
Abrasion resistance was determined using an abrader, which is based on a Lambourn-type machine as described in U.S. Pat. No. 4,995,197, hereby incorporated by reference. The tests were carried out at 14% slip. The percentage slip is determined based on the relative velocities of a sample wheel and a grindstone wheel. The abrasion resistance index is calculated from the mass loss of the elastomeric compound. Dynamic properties were determined using a Rheometrics Dynamic Spectrometer II (RDS II, Rheometrics, Inc., N.J.) with strain sweep. The measurements were made at 0 and 70� C. with strain sweeps over a range of double strain amplitude (DSA) from 0.2 to 120%. The maximum tan δ values on the strain sweep curves were taken for comparing the hysterisis among elastomeric compounds as can be seen in FIGS. 3a and 3b. Alternatively, hysterisis measurements were made by means of temperature sweeps at a DSA of 5% and a frequency of 10 Hz. The temperature range was from -60� C. to 100� C., as seen in FIG. 3c.
TABLE 6______________________________________Dynamic Hysterisis Data               tan &#948;                        tan &#948;                                abrasion atSSBR Compositiona       Si-69   at 0� C.                        at 70� C.                                14% slip______________________________________N234        0       0.400    0.189   100N234        3       0.429    0.170   103.5OMTS-CB     0       0.391    0.175   84.4OMTS-CB     3       0.435    0.152   110.5TEOS-CB     0       0.400    0.167   78.1TEOS-CB     3       0.433    0.142   97.2______________________________________ a Duradene 715; two stage mixing.
Example 6A The dynamic hysterisis and abrasion properties of a black made by following the procedure of Example 3A (and containing 1.91% Si) were measured as in Example 6. As seen in Table 6A below, tan δ at 70� C. values were reduced by 14%, tan δ at 0� C. values were reduced by 6% and the wear resistance was reduced by 22%, for the SSBR samples when TEOS-CB' was substituted for N234. However, when Si69 coupling agent was incorporated into the composition, the wear resistance for the TEOS-CB sample improved to 108% of the value for N234. The tan δ at 70� C. values decreased by 18% compared to N234 without coupling agent and 7% compared to N234 with coupling agent. The tan δ at 0� C. values decreased by only 1.5% when the coupling agent was added to TEOS-CB', compared to N234 with coupling agent.
TABLE 6A______________________________________Dynamic Hysterisis DataSSBR              tan &#948; @                       tan &#948; @                               Abrasion @Compositiona     Si 69   0� C.                       70� C.                               14% Slip______________________________________N234      0       0.428     0.184   100N234      4       0.394     0.162   94TEOS-CB`  0       0.402     0.158   78TEOS-CB`  4       0.388     0.151   108______________________________________ a Cariflex S1215; two stage mixing
Example 7--Improvement in Hysterisis by Three Stage Compounding The beneficial properties obtained using the treated carbon blacks with the elastomeric compounds of the present invention may be further enhanced by using an additional mixing stage during the compounding process. The procedure for two stage mixing used in the previous compounding examples, is described above in Example 4.
Table 7 below compares hysterisis and abrasion characteristics for elastomers compounded with TEOS-CB using two and three stage mixing. As can be seen from the Table, three stage mixing results in higher tan δ at 0� C. and lower tan δ at 70� C.
TABLE 7______________________________________Dynamic Hysterisis Data - 2 Stage v. 3 Stage Mixing               tan &#948;                        tan &#948;                                abrasion atCarbon Black       Si-69   at 0� C.                        at 70� C.                                14% slip______________________________________Duradene 715Two Stage MixingN234        0       0.458    0.189   100N234        3       0.439    0.170   103.5TEOS-CB     0       0.434    0.150   78.1TEOS-CB     3       0.436    0.131   97.2Duradene 715Three Stage MixingN234        0       0.471    0.165   100N234        3       0.456    0.146   98.4TEOS-CB     0       0.446    0.139   57.6TEOS-CB     3       0.461    0.113   101.8______________________________________
Example 8--Oxidized Carbon Black In another aspect of the present invention, it was determined by the present inventors that oxidation of the silicon-treated carbon black can lead to elastomeric compositions with enhanced hysterisis. For a black made using the conditions of Table 1, but with OMTS as the volatilizable silicon-containing compound, and 2.74% silicon in the final black, the improvement obtained with oxidation is illustrated in the following Table. The hysterisis performance with the oxidized black is further enhanced by incorporating a coupling agent into the elastomeric compound.
The oxidized carbon black was prepared by treating the black with nitric acid. A small stainless steel drum was loaded with carbon black and rotated. During rotation a 65% nitric acid solution is sprayed onto the carbon black, until 15 parts per hundred carbon black had been added. After a soak period of 5 minutes, the drum was heated to about 80� C. to initiate the oxidation reaction. During the oxidation reaction, the temperature increased to about 100�-120� C. This temperature was held until the reaction was completed. The treated black was then heated to 200� C. to remove residual acid. The treated black was then dried overnight at 115� C. in a vacuum oven. Table 8 below compares hysterisis characteristics for elastomers compounded with OMTS-CB and oxidized OMTS-CB, with and without a coupling agent.
TABLE 8______________________________________Dynamic Hysterisis Data - oxidized, treated carbon blackCarbon Black             tan &#948;                            tan &#948;Duradene 715 - 2 stage         Si-69      at 0� C.                            at 70� C.______________________________________N234          0          0.513   0.186N234          3          0.463   0.176OMTS-CB       0          0.501   0.166OMTS-CB       3          0.467   0.135oxidized OMTS-CB         0          0.487   0.154oxidized OMTS-CB         3          0.467   0.133______________________________________
Example 9--Hysterisis and Abrasion Resistance for a Variety of Elastomers Hysterisis and abrasion resistance was compared for elastomeric compounds prepared with treated carbon blacks compounded with different elastomers, compounded with and without a coupling agent. Conventional carbon black was used as a control. The results are set forth in the Table 9 below.
These data show hysterisis improvement for all five elastomer systems tested. For example, the tan δ at 70� C. is reduced by between 10.5 and 38.3% without a coupling agent, and by between 11.7 and 28.2% with a coupling agent, compared to the corresponding control.
TABLE 9______________________________________Hysterisis and Abrasion Resistance - 3 Stage Mixing                 tan &#948;                          tan &#948;                                 wear atCarbon Black  Si-69   at 0� C.                          at 70� C.                                 14% slip______________________________________Solution SBR 116/NS 114 -80/20 blendN234          0       0.689    0.151  100.0N234          3       0.750    0.131  123.1TEOS-CB       0       0.721    0.115  86.3TEOS-CB       3       0.751    0.094  115.4Solution SBR SL 574N234          0       0.286    0.118  100.0N234          3       0.260    0.108  96.4TEOS-CB       0       0.246    0.101  58.0TEOS-CB       3       0.258    0.093  86.8Solution SBR PAT589N234          0       0.676    0.190  100.0N234          3       0.686    0.182  99.1TEOS-CB       0       0.698    0.170  82.4TEOS-CB       3       0.726    0.150  134.2Emulsion SBR 1500N234          0       0.299    0.176  100.0N234          3       0.285    0.137  87.9TEOS-CB       0       0.280    0.156  60.1TEOS-CB       3       0.270    0.121  88.1Natural Rubber SMR 5N234          0       0.253    0.128  100.0N234          3       0.202    0.088  85.8TEOS-CB       0       0.190    0.079  60.9TEOS-CB       3       0.173    0.069  88.6______________________________________
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ClassificationC08K9/06, C09C1/56, C09C1/50Legal EventsDateCodeEventDescriptionDec 28, 2010FPAYFee paymentYear of fee payment: 12Dec 18, 2006FPAYFee paymentYear of fee payment: 8Dec 30, 2002FPAYFee paymentYear of fee payment: 4Mar 23, 1998ASAssignmentOwner name: CABOT CORPORATION, MASSACHUSETTSFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:MAHMUD, KHALED;WANG, MENG-JIAO;FRANCIS, ROBERT A.;REEL/FRAME:009051/0879;SIGNING DATES FROM 19971028 TO 19971204RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services©2012 Google