Radiotracer Studies of Carbon Black Surface Interactions with Organic Systems. I. Experimental Approach and Initial Results from Chemisorption and Vinyl Polymerization Studies

1968 ◽  
Vol 41 (2) ◽  
pp. 382-399 ◽  
Author(s):  
Marvin L. Deviney ◽  
Lawrence E. Whittington

Abstract Radiotracer techniques have been applied to the study of interactions of carbon black surface functional groups with two chosen organic systems. The basic reaction mechanisms demonstrated in this study may have implications in elastomer reinforcement. Direct radiochemical evidence supports the conclusions of Hallum and Drushel (based on less direct polarographic data) that surface quinonic groups exhibit hydrogen abstraction activity toward tertiary hydrogens in paraffinic hydrocarbons. Studies on the system carbon black and styrene using tritium radiotracer have provided direct evidence that phenolic hydrogens participate in the polymerization acceleration and graft polymer formation reaction and are transferred to the growing polystyrene chains as postulated by Donnet. Several methods have been developed for specifically labelling certain oxygenated functional groups on the carbon surface with tritium and for tritium labelling carbon black in aromatic hydrogen positions. The techniques developed in this work and the basic reaction mechanisms derived will permit this investigation to be extended into a radiochemical study of carbon black surface interactions with elastomer related systems of interest to the rubber industry.

1956 ◽  
Vol 29 (1) ◽  
pp. 286-295
Author(s):  
W. D. Schaeffer ◽  
W. R. Smith

Abstract The high degree of stiffness or modulus which reinforcing carbon blacks impart to rubber has often been associated with reinforcement. Modulus appears to be associated with the chemical nature of the carbon black surface ; when the carbon black surface is cleaned of combined oxygen and hydrogen, a drastic drop in modulus occurs, and this is not accompanied by an equally drastic decrease in tire road wear. Reinforcing and semireinforcing carbon blacks have been heat-treated at successive increments through a temperature range of 1000° to 2700° C. Treatment up to 1500° results in removal of all combined oxygen and hydrogen, followed by an increasing degree of graphitization at higher temperatures. These carbon blacks have been compounded in a standard natural-rubber compound and properties evaluated. Modulus is profoundly altered by the chemistry of the carbon surface. Electrical resistivity passes through a minimum at 1500° C. Scorchiness or premature vulcanization improves with removal of volatile matter. The degree of graphitization of the carbon has only a minor effect on rubber properties. A highly graphitized carbon black still imparts a high degree of resistance to abrasive wear to tire treads.


1970 ◽  
Vol 43 (2) ◽  
pp. 449-463 ◽  
Author(s):  
J. E. Lewis ◽  
M. L. Deviney ◽  
C. F. McNabb

Abstract A broad investigation has been undertaken, using primarily radiochemical techniques, of the reactivity of the insoluble or “bound” sulfur on the surface of carbon blacks. The carbon black samples used in this study were prepared in small pilot plant reactors from sulfur-free commercial feedstocks to which had been added, in separate experiments, sulfur-35 tagged elemental sulfur, dibenzothiophene-S-35 and dibenzyl disulfide-S-35. After careful extraction-purification of the blacks, “chemical probe” studies were undertaken to gain knowledge of the nature of the surface sulfur complexes or functional groups, using reagents such as LiAlH4, trivalent phosphorus compounds, tetramethylthiuram disulfide, and hydrogen. These experiments demonstrated that bound surface sulfur possesses a considerable amount of chemical reactivity. Experiments were next designed to determine whether or not bound surface sulfur becomes involved in vulcanization reactions by, for example, exchange with added curing sulfur or accelerator. In radiotracer studies with SBR, natural rubber, and cis-polybutadiene vulcanizates, the results demonstrated that bound surface sulfur enters into the rubber phase during vulcanization. Finally, results from preliminary rubber physical testing and practical vulcanization studies involving pilot plant blacks (2% wt. sulfur) indicate that surface sulfur has little effect upon the vulcanization or final physical properties of SBR and NR.


Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 153
Author(s):  
Sang-Min Lee ◽  
Sang-Hye Lee ◽  
Jae-Seung Roh

In the present study, carbon black activated by CO2 gas was examined through XRD analysis, especially with regard to changes in its structural parameters. Based on the results, its activation process was thoroughly analyzed. The activation process was controlled by isothermally activating the carbon black inside a reaction tube through which CO2 gas flowed. With this approach, the degree of activation was varied as desired. At an early stage of the activation process, the amorphous fraction on the carbon black surface was preferentially activated, and later the less-developed crystalline carbon (LDCC) region inside the carbon black particles started to be activated. The latter process was attributable to the formation of pores inside the carbon black particles. As the activation process proceeded further, the more-developed crystalline carbon (MDCC) region started to be activated, thereby causing the pores inside the carbon black particles to grow larger. At the last stage of the activation process, La was found to be decreased to about 40 Å. This implied that the edges of the graphite crystals had been activated, thus causing the internal pores to grow and coalesce into larger pores. Activated conductive Super-P with enhanced pore properties is expected to have wide applications.


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