Accessibility of the Carbon Black Particle Surface to Elastomers

1970 ◽  
Vol 43 (2) ◽  
pp. 464-469 ◽  
Author(s):  
P. Aboytes ◽  
A. Voet
Keyword(s):  
Carbon Black ◽  
Particle Surface ◽  
Carbon Black Particle ◽  
Carbon Chain ◽  
Chain Structure ◽  
Inert Atmosphere ◽  
Chemical Surface ◽  
Molecular Weights ◽  
Surface Areas ◽  
Black Surface

Abstract Experimental carbon blacks were prepared with the generally encountered slit-shaped pores of discrete dimensions of 9,12.5, and 16 A˚ width in greatly differing size distribution. Equilibrium adsorption in the saturation range was determined in n-hexane for butadiene—styrene elastomers of the SBR type of average molecular weights of 1500; 2000; 15,000; and 300,000. In attempting to correlate the saturation adsorption values with carbon black surface areas, it was found that a simple linear relation in the range investigated could only be obtained by assuming that pores of 9 A˚ width were inaccessible to SBR of 1500 and 2000 MW; that pores of 9 and 12.5 A˚ width were inaccessible to SBR of 15,000 MW; and that all pores smaller than 20 A˚ width were inaccessible to SBR of 300,000 MW. The data indicated that there are no differences between high, regular and low structure blacks in saturation elastomer adsorption under conditions of equivalent dispersion. Equally, upon breaking the persistent carbon chain structure by dry ball milling in an inert atmosphere and equalizing the chemical surface properties by removal of surface oxides, no difference in elastomer adsorption from solution was observed. It must be concluded that commonly used high molecular elastomers do not have any access to smaller carbon black pores. Since access to the surface is a prerequisite for reinforcement, it is obvious that the surface in the pores of carbon black generally does not participate in reinforcing elastomers. The elastomer adsorbed per unit external black surface area appears to be independent of the carbon chain structure, indicating that the so called surface activity of the carbon black is independent of the chain length.

Immobilization of Elastomers at the Carbon Black Particle Surface

1970 ◽  
Vol 43 (5) ◽  
pp. 973-980 ◽  
Author(s):  
A. K. Sircar ◽  
A. Voet
Keyword(s):  
Carbon Black ◽  
Particle Surface ◽  
Carbon Black Particle ◽  
High Energy ◽  
Molecular Weights ◽  
Boiling Points ◽  
Furnace Black ◽  
Bound Rubber ◽  
Black Surface ◽  
Black Particle

Abstract Determinations have been made of the amount of elastomer unextractable from unvulcanized masticated mixes with carbon black by a given solvent at boil, expressed as immobilized elastomer. Saturated and unsaturated elastomers varying in molecular weights from 2000 to 325,000, were used, while solvents of greatly differing boiling points and solvent power were employed. It could be shown that the bonding between elastomers and carbon black is not a simple adsorption, but involves a higher energy interaction, defined as chemisorption. At successively higher temperatures elastomer is increasingly removed from the carbon black surface. The temperature Tm, obtained by extrapolation of the linear relationship between amounts immobilized and temperature of extraction, represents the temperature theoretically required to eliminate all bonds between carbon black and elastomer and is therefore indicative of the bond strength. Data suggest the existence of a bonding energy spectrum. Upon graphitization, blacks show a considerable decline in high energy bonding ability for elastomers. Saturated elastomers show less bonding than unsaturated elastomers with the same furnace black. “Bound rubber” represents the sum total of physically adsorbed, mechanically entangled, and chemisorbed elastomer. The actual values are greatly dependent upon the procedure used. “Immobilized rubber”, indicating chemisorbed elastomer, is easily determined, is not influenced by the method, and is more significant as an indicator of reinforcement.

scholarly journals Studies of Texaco Carbon Black Particle Surface by Polarography

1963 ◽  
Vol 84 (3) ◽  
pp. 212-214,A16 ◽  
Author(s):  
Shiro TAKASHIMA ◽  
Genzo HASHIZUME ◽  
Itaru MOTOOKA
Keyword(s):  
Carbon Black ◽  
Particle Surface ◽  
Carbon Black Particle ◽  
Black Particle

A Low-Cost, Rapid Method for Determining Carbon Black Surface Area

1983 ◽  
Vol 56 (2) ◽  
pp. 440-449 ◽  
Author(s):  
Jerry B. Pausch ◽  
Caroline A. McKalen
Keyword(s):  
Carbon Black ◽  
Surface Area ◽  
Low Cost ◽  
Control Procedure ◽  
Simple Method ◽  
Surface Areas ◽  
Measuring Surface ◽  
Headspace Gas ◽  
Black Surface ◽  
Area Data

Abstract For practical use of this method as a quality control procedure for carbon black, a combination of 4 mm3 and 6 mm octane doses appears to be the best compromise for a sample size of 0.1 g. These conditions cover well, a surface area range of 10–140 m2/g and surface areas up to 180 m2/g can be estimated. Larger doses of octane will extend the linear range on the high side, but the slope of the calibration curve is reduced significantly. A smaller slope yields lower precision. The regular testing of standards appears necessary to achieve optimum accuracy of surface area. At the present time, the method is calibrated against nitrogen surface area data, so the advantage of octane more closely simulating the rubber molecule is lost. We need to obtain adsorption isotherms that are better defined throughout the linear adsorption coefficient range for a number of carbon blacks, and thus become self-calibrated against octane. A more versatile dosing technique is preferred to enable these experiments to be run. An alternate approach is to correlate the headspace results with data obtained by other techniques such as CTAB. The advantages of automated headspace gas chromatography for measuring surface area have been outlined before . It is a rapid and simple method, which also exhibits relatively low labor involvement. The number of samples capable of being analyzed per day is significantly higher than by any other technique.

Carbon-Black-Elastomer Interaction II: Effects of Carbon Black Surface Activity and Loading

1993 ◽  
Vol 66 (5) ◽  
pp. 772-805 ◽  
Author(s):  
J. A. Ayala ◽  
W. M. Hess ◽  
G. A. Joyce ◽  
F. D. Kistler
Keyword(s):  
Surface Energy ◽  
Carbon Black ◽  
Surface Activity ◽  
Volume Fraction ◽  
Heat Treating ◽  
Inert Atmosphere ◽  
Morphological Properties ◽  
Rubber Compounds ◽  
Carbon Black Surface ◽  
Black Surface

Abstract Carbon black morphology, surface activity and loading have been varied systematically to study the effects on an SBR formulation. The surface activity of five commercial grades of carbon black was varied by heat treating the standard grade samples at 1100°C and 1500°C in an inert atmosphere. Measurements on carbon black-elastomer interaction were based on a parameter I, defined elsewhere. The parameter I exhibited the previously reported correlation with known indicators of the surface activity of carbon blacks. The heats of adsorption by inverse gas chromatography at infinite dilution have been found useful as a measure of the carbon-black surface energy related to rubber interaction. These measurements have been employed in conjunction with carbon-black morphology and loading to develop a surface-area-modified and a surface energy-modified effective volume fraction V′ and ψ, respectively. The parameter V′ was utilized to explain the variation of the dynamic elastic modulus E′ at 1 % double strain amplitude (DSA) for all rubber compounds. The parameter ψ was used to explain the variation of E′ at 25% DSA and the factor σ in the calculation of I. The parameters V′ and ψ provide a model for the estimation of I from fundamental carbon-black morphological properties and surface energy.

Determination of Carbon Black Particle Size by Reflectance

1967 ◽  
Vol 40 (5) ◽  
pp. 1319-1322 ◽  
Author(s):  
Merton L. Studebaker ◽  
Lester G. Nabors
Keyword(s):  
Particle Size ◽  
Carbon Black ◽  
Sample Preparation ◽  
Simple Technique ◽  
Carbon Black Particle ◽  
Carbon Black Surface ◽  
Reflectance Meter ◽  
Black Surface ◽  
Black Particle

Abstract A simple technique of sample preparation using dry carbon black samples has been developed which gives a carbon black surface of reasonably reproducible reflectance, using a commercially available and reasonably priced reflectance meter. The reflectance values were calibrated against particle size determined by Kraus and Rollmann using the calorimetric procedure of Harkins and Jura.

Identification of Carbon Black by Surface-Area Measurements

1943 ◽  
Vol 16 (3) ◽  
pp. 687-691
Author(s):  
F. H. Amon ◽  
W. R. Smith ◽  
F. S. Thornhill
Keyword(s):  
Carbon Black ◽  
Surface Area ◽  
Point Of View ◽  
Curing Temperature ◽  
Single Type ◽  
Surface Areas ◽  
Vulcanized Rubber ◽  
Chemical Combination ◽  
Black Surface ◽  
Rubber Stock

Abstract In general then, we may conclude that carbon black can be recovered from rubber stocks with unchanged surface-area. The nitric acid technique is the most effective method of effecting the separation. The digestion temperature must be controlled to between 60° and 70° C, for a total of not more than 3 to, 4 hours. This method of identifying the carbon black in an unknown rubber stock is directly applicable only in the presence of a single type of carbon black. If blends of blacks are employed in the material under investigation, some secondary identification is also required. The nonimpingement-type blacks, for example, are readily identified by microscopic observation. From the known surface-areas of these materials and the total per cent carbon present in the stock, a fairly positive identification of the blend can be made. The fact that carbon black can be recovered quantitatively and with unchanged surface-area from vulcanized rubber stocks appears to lend impetus to a physical concept of carbon black reinforcement. This point of view implies that any chemical combination between the ingredients of the rubber stock and the carbon black would be evidenced by some alteration in the surface of the latter. A few experiments were performed in an attempt to establish to what extent this concept was valid. One hundred grams of Grade-6 carbon black were intimately mixed with 6.6 grams of sulfur. This is about the ratio in which they are present in a standard rubber batch. Samples of this mixture were subjected to the standard curing temperature of 134° C for 30, 60, and 90 minutes. The free sulfur was then extracted for 40 hours with acetone ,and the combined sulfur on the carbon was determined. Values of 0.16, 0.21, and 0.4 per cent combined sulfur were obtained. The original sample of Grade-6 carbon black had a surface-area of 108 square meters per gram. The extracted sample of black containing 0.4 per cent of combined sulfur had a surface-area of 109 square meters per gram. These values are identical within experimental error. While unaltered surface-area need not necessarily be interpreted as evidence of complete lack of surface reactions, it is the authors' opinion that the extent of chemical combination at the carbon black surface is very small. This interpretation is in accord with the views expressed in a previous publication3, where it was suggested that the chief role of carbon black in rubber reinforcement may rest on its ability to orient the chains of rubber molecules and thus alter the extent and type of rubber-sulfur bonds normally formed in non-reinforced rubber stocks.

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
Keyword(s):  
Carbon Black ◽  
Functional Groups ◽  
Reaction Mechanisms ◽  
Hydrogen Abstraction ◽  
Surface Interactions ◽  
Carbon Surface ◽  
Organic Systems ◽  
Carbon Black Surface ◽  
Basic Reaction ◽  
Black Surface

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.

Research on Electrical Double Percolation of Carbon Black-Filled Cement-Based Composites

2011 ◽  
Vol 311-313 ◽  
pp. 201-204
Author(s):  
Hong Zhong Ru ◽  
Ran Ran Zhao
Keyword(s):  
Carbon Black ◽  
Cement Paste ◽  
Volume Fraction ◽  
Carbon Black Particle ◽  
Carbon Black Content ◽  
Percolation Behavior ◽  
Key Factor ◽  
Binder Ratio ◽  
Black Particle ◽  
Double Percolation

Electrical conductive carbon black-filled cement-based composites are significant as multifunctional structural materials. Double percolation in carbon black-filled cement-based composites involves both carbon black particle percolation and cement paste percolation, which has great effect on the resistivity of composites. Based on double percolation theory, the influences of sand-binder ratio and carbon black volume fraction on the resistivity of carbon black-filled cement-based composites are investigated. The results show that besides carbon black volume fraction, sand-binder ratio is a key factor affecting double percolation behavior in carbon black-filled cement-based composites. At a fixed carbon black content in overall mortar, with increasing sand-binder ratio, the cement paste percolation though aggregate phase increases due to high obstruction of aggregate but the carbon black particle percolation in cement paste decreases. This is because that the microstructure of aggregate is impenetrable so that the carbon black particles are limited in cement paste, that is, the carbon black content in paste is compacted and large amount of conductive paths are generated by lapped adjacent carbon black particles in paste. The double percolation in the electrical conduction in carbon black-filled cement-based composites is observed when the carbon black volume fraction is 7.5% and sand-binder ratio is 1.4, and its resistivity is only 3200 Ωcm, so that a sand-binder ratio of 1.4 and 7.5% carbon black volume fraction or more are recommended for attaining high conductivity with a compromise between workability and conductivity.

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