Carbon black compositions, polymer compositions including the carbon black compositions and articles of manufacture including the polymer compositions

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CARBON BLACK COMPOSITIONS, POLYMER COMPOSITIONSINCLUDING THE CARBON BLACK COMPOSITIONS AND ARTICLESOF MANUFACTURE INCLUDING THE POLYMER COMPOSITIONS 1

Carbon Black Compositions and Improved Polymer Compositions

Field of the Invention

The present invention relates to carbon black compositions comprising ethoxylated esters orpolyethers and carbon black. The compositions may be produced by incorporating ethoxylatedesters or polyethers onto fluffly carbon black in a pelletizing process to produce free flowing, lowdust, attrition resistant carbon black pellets which are easily dispersible in most polymeric systemsand provide enhanced rheological and mechanical properties.

The present invention also relates to polymer compositions which incorporate the carbonblack compositions of the present invention.

Background of the Art

Carbon blacks produced by a furnace process generally have bulk densities ranging from0.02 to 0.1 gram/cubic centimeter (g/cc) and are generally known as fluffy carbon blacks. Fluffycarbon blacks are generally easy to disperse in liquids, and in some polymeric systems. However,fluffy carbon blacks are generally cohesive and, hence difficult to handle for purposes such asconveying and weighing.

Fluffy carbon blacks are agglomerated by various types of mechanical processes, either inthe dry state, or with the aid of a liquid to produce pellets with improved handling characteristics.Common liquid pelletizing agents are oil and water. The process of agglomerating fluffy carbonblacks to form carbon black pellets is generally referred to as pelletizing.

Unfortunately, generally utilized densification or agglomeration (pelletizing) processes havedetrimental effects on the dispersion characteristics of the carbon black. Therefore it is recognizedin the art that in pelletizing carbon blacks there is a fine balance between acceptable handlingcharacteristics and ease of dispersion. A process for pelletizing carbon black is disclosed in U.S. Patent No. 2,065,371 whichdescribes a typical wet pelletization process whereby the fluffy carbon black and a liquid, typically 2 water, are combined and agitated until spherical beads are formed. These beads are then dried to reduce the water content preferably to below 1% to form carbon black pellets.

Prior art patents also disclose the use of binder additives in a wet pelletization process tofurther improve the pellet handling characteristics. U.S. Patent No. 2,850,403 discloses the use of carbohydrates e.g. sugar, molasses,soluble starches, saccharides and lignin derivatives as pellet binders in the range of 0.1% to 0.4%,by weight, based on the diy carbon black. The preferred drying temperature of the wet pellet isdisclosed as 150 to 425’ C which together with the residence time is sufficient to carbonize thebinder. U.S. Patent No. 2,908,586 discloses the use of a rosin emulsion as pellet binders as analternative to carbohydrates. The preferred level of rosin binder is in the range 0.5% to 2.0%, byweight, based on the dry carbon black. U.S. Patent No. 2,639,225 discloses the use of sulphonate and sulphate anionicsurfactants as pellet binders at levels of 0.1% to 0.5%, by weight, based on the dry carbon black. U.S. Patent No. 3,565,658 discloses the use of a fatty amine ethoxylate non-ionicsurfactant where the level of ethoxylation ranges from 2 to 50 moles of ethylene oxide per fattyamine group. The preferred level of surfactant in the pelletizing water is in the range 0.05% to 5%,by weight, based on the dry carbon black.

Similarly, U.S. Patent No. 3,645,765 discloses the use of a fatty acid or rosin acidethoxylate, non-ionic surfactant where the level of ethoxylation is 5 to 15 moles ethylene per acidgroup. The preferred level of addition on the carbon black is in the range 0.1% to 10%, byweight, based on the dry carbon black.

Soviet Union Patent No. 937,492 claims the benefits of using 0.1% to 5%, by weight,based on the dry carbon black, of an aqueous solution of a reaction product generated from ureaand an ethoxylated alkylolamide. The preferred level of ethoxylation is 1 to 7 moles of ethyleneoxide per alkylolamide molecule. 3 U.S. Patent No. 3,844,809 discloses the reduction in pellet dust levels by incorporating0.4% to 2.5%, by weight, based on the dry carbon black of an aqueous solution containing0.001% to 0.1%, by weight, of a nonionic surfactant containing randomly repeating poly(ethyleneoxide) and poly (dimethyl silicone) groups. Molasses is also included at substantially higherconcentration (up to 2%, by weight) as a co-binder and nitric acid (up to 15%, by weight) as anoxidizing source.

The use of carbohydrates, rosin or surface active agents as disclosed in the above patents isfocused towards improving pellet handling qualities. The patents do not disclose that thepelletizing treatments affected the performance properties of the carbon black in the final productapplications, which are typically rubber orientated.

Japanese Patent No. 1,201,369 discloses the use of a carboxylic acid type amphotericsurfactant in a concentration range 0.001% to 0.1%, by weight, in the pelletizing water to producecarbon black pellets with low adhesion and excellent dispersibility. U.S. Patent No. 3,014,810 discloses the benefits of wet pelletizing a range of pigments,including carbon blacks, with a blend of a quaternary ammonium compound and a bis(-2-hydroxyethyl)alkyl amine. Improvements in dispersion rate, viscosity stability and antistaticproperties are disclosed for the blend of surface active agents.

Pelletizing with oil, in the presence and absence of water is disclosed in U.S. Patent No.2,635,057, U.S. Patent No. 3,011,902 and U.S. Patent No. 4,102967 as beneficial in improvingthe handling properties of carbon black pellets.

Several patents, including U.S. Patent No. 2,511,901, U.S. Patent No. 2,457,962, U.S.Patent No. 4,440,807, U.S. Patent No. 4,569,834, U.S. Patent No. 5,168,012 and JapanesePatent No. 77,130,481 disclose polymers in emulsion, organic solvent solutions and in moltenform as means of modifying the pellet properties of carbon black. U.S. Patent No. 4,277,288 discloses a fluidised granulation process for producing free-flowing dustless pigment granules in the absence of water. The organic component required to 4 produce a dustless granule consists of two components, 5-20 phr of a non-aqueous granulating aid and a non-ionic surfactant for example sorbitan oleate ethoxylate as a second component The bulk of the disclosure relates to producing free-flowing organic and inorganic pigments, including carbon black. U.S. Patent No. 4,397,652 also discloses a process for producing negligible dustpreparations of organic dyes and optical brighteners. The process involves the dry blending,between 30 and 80' C, of the dye, or optical brightener, with 2-10%, by weight, of an adhesiveselected from the group consisting of polyhydric alcohol (e.g. sorbitol); manitol; manitose; lactose;hydrated dextrose; neopentyl glycol; and polyethylene glycol with a molar mass above 3,000.

Also included in the composition is 1-10% of a dusting aid selected from the group consisting offatty acid ethanolamide; fatty acid amide; alkyl alcohol; substituted phenol; and polyethylene glycolwith a molar mass between 200 and 1000. U.S. Patent No. 4,230,501 discloses a pigment concentrate, dispersible in plastics, whichis prepared by combining 51-85%, by weight, of a pigment and 14-49%, by weight, of a waxycomponent The waxy component is disclosed as being predominantly a natural, petroleum orsynthetic wax which has been blended with either polyethylene glycol or a hydrocarbon resin toreduce the melt viscosity and allow better incorporation of the pigment

Polyethylene glycol is previously known as an additive for direct compounding intothermoplastic compositions. U.S. Patent No. 4,013,622 discloses the incorporation of 100 to 600ppm of polyethyleneglycol in the molar mass range of 600 to 20,000 (preferably 1300 to 7500) to reduce thebreakdown of polyethylene during blown film operations which is observed as gel formation. U.S. Patent No. 4,812,505, U.S. Patent No. 4,440,671 and U.S. Patent No. 4,305,849 disclose the use of polyethylene glycols in the molar mass range 1,000 to 20,000 as beneficial for reducing the heat and water-treeing characteristics in polyolefin compositions for electrical insulation. Similarly U.S. Patent No. 4,612,139 extends this concept of water-tree reduction to 5 include the polyethylene glycol in semiconductive polyolefin compositions containing carbonblack.

Similar compositions are claimed in German Patent DE 27 23 488 where polyethyleneglycol and other mobile additives are disclosed as being beneficial to reduce the interlaminaradhesion between the insulation layer and outer conductive layer in an electric cable construction.

Polyethylene glycol and branched ethoxylate molecules are disclosed as plasticisers forethylene-acrylic acid copolymers in U.S. Patent No. 3,361,702.

United Kingdom Patent GB 975,847 discloses the use of polyethylene glycol, or analiphatic derivative, in an aqueous solution as a means of producing agglomerates of organicrubber chemicals. A dough is formed as an intermediate which is then converted into pellets anddried at low temperatures.

Summary of the Invention

The present invention comprises carbon black compositions that in their dry form haveimproved handling characteristics and that impart enhanced performance characteristics to polymercompositions. The carbon black compositions comprise: carbon black and 0.1% to 50%, preferably 1 to 20%, by weight, of at least one binder selected from at leastone of the following groups: i) an ethoxylated polyhydric alcohol having at least 3 hydroxyl groups per molecule prior to ethoxylation, where the total number of ethylene oxide molecules perpolyhydric alcohol is at least 3; preferably the polyhydric alcohol is selected fromthe group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan,sucrose or a polyglyceride and/or the total number of ethylene oxide molecules perpolyhydric alcohol varies from 3 to 500 and more preferably varies from 5 to 100; 6 ii) an alkyl carboxylic acid ester of an ethoxylated polyhydric alcohol having at least 3hydroxyl groups per molecule prior to ethoxylation, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selectedfrom the group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sucrose or a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; iii) an alkyl carboxylic acid ester of a polyhydric alcohol having at least 3 hydroxylgroups per molecule prior to esterification, where the alkyl carboxylic acid has from8 to 30 carbon atoms, and may be saturated or unsaturated, and further where themono-ester functionality is at least 80% with the remainder being a di-ester . functionality; preferably the polyhydric alcohol is selected from the groupconsisting of: triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan, sorbitoland a polyglyceride; iv) an ethoxylated alkyl carboxylic acid ester of a polyhydric alcohol having at least 3hydroxyl groups per molecule prior to esterification, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selected 7 from the group consisting of: triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sorbitol and a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; v) a polyethylene oxide - polypropylene oxide - polyethylene oxide block copolymer.

It is also preferred that the binders of groups i, ii, iii, iv and v have an HLB value of 8.0 to 30. HLB value refers to hydrophile-lipophile balance value which may be determined by themethod described in Non-Ionic Surfactants Volume 23. edited by Martin Schick (Marcel DekkerInc. (New York) 1987; ISBN 0-8247-7530-9), page 440. Non-Ionic Surfactants Volume 23provides equations relating the structure of the surfactant molecule to HLB value. HLB value isalso discussed in the following journal articles: Griffin W.C., J. Soc. Cosmetic Chemistt, Vol. 1,page 311 et seq. (1949) and Vol. 5, page 249 et seq. (1954). From data relating to the weightpercentage of ethylene oxide in the molecule, saponification number of the ester linkage and acidvalue of the “fatty” acid, HLB value may be directly calculated from one of the followingequations: for polyhydric fatty acid esters: HLB = 20 (1-S/A) where S = saponification number of the ester and A = acid number ofthe acid; and for ethoxylated polyhydric alcohols: HLB = (E + P)/5, where E = weight of percent ethylene oxide and P - weight pigment ofpolyhydric alcohol.

While any carbon black may be utilized in the compositions of the present invention,preferably the carbon black component of the carbon black composition has a nitrogen surface area(N2SA) of 15 to 1800 m2/g, a fluffy dibutyl· phthalate absorption value (DBP) of 50 to 350 8 cc/lOOg and a cetyl trimethylammonium bromide absorption value (CTAB) of 15 to 1500 m2/g.

The carbon black compositions may be produced in any manner known in the art, such asby physically blending the components, melt mixing the components or combining the componentswhile pelletizing the carbon black. Preferably the carbon black compositions are obtained bypretreating the carbon black with the binder.

The carbon black compositions may also be produced by a pelletizing process by:contacting a fluffy carbon black in a pin pelletizer with an aqueous solution containing a binder selected from the foregoing groups of compounds wherein the preferred level of binder inthe pelletizing water is from 0.5% to 50%; more preferably 20-40%, by weight; and heating the wet pellets under controlled temperature and time parameters such that the wateris removed from the pellets but the binder does not undergo substantial decomposition, and thefinal binder level on the dry carbon black is from 0.1% to 50%.

The present invention also includes new polymer compositions comprising:a polymer component and 0.1-65%, preferably 0.1-20%, by weight, of a composition comprising a carbon black and 0.1-50%, preferably 1-20%, of at least one binder componentselected from at least one of groups i, ii, iii, iv or v, set forth above. Preferably, the carbon blackis pretreated with the binder component The preferred carbon blacks, and binder components areas set forth above with respect to the carbon black compositions of the present invention. Thepolymer compositions may include other conventional additives such as pigments, reinforcingagents and the like.

While any polymer may be utilized in the polymer composition of the present invention,preferred polymers for use in the polymer compositions of the present invention include, but arenot limited to: a) homo or copolymers and graft polymers of ethylene where the co-monomers are selected from butene, hexene, propene, octene, vinyl acetate, acrylic acid, methacrylic acid, esters of acrylic acid, esters of methacrylic acid, maleic anhydride, half ester of maleic anhydride, and 9

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carbon monoxide; b) elastomers selected from natural rubber, polybutadiene, polyisoprene, random styrenebutadiene rubber (SBR), polychloroprene, acrylonitrile butadiene, ethylene propylene co andterpolymers; c) homo and copolymers of styrene, including styrene - butadiene - styrene linear and radialpolymer, acrylonitrile butadiene styrene (ABS) and styrene acrylonitrile (SAN); d) linear and branched polyether or polyester polyols; e) crystalline and amorphous polyesters and polyamides; f) alkyd resins, rosin acids or rosin esters, hydrocarbon resins produced from thermal orFriedel Crafts polymerization of cyclic diene monomers such as dicyclopentadiene, indene,cumene; and g) hydrocarbon oils such as parafinnic oil, naphthenic oil and hydrogenated naphthenic oil.

The polymer compositions of the present invention may be produced in any manner known to the art for combining polymers and dry or aqueous components.

The present invention further includes articles of manufacture produced from the polymercompositions of the present invention.

For use in semiconductive wire and cable applications, a typical formulation of the presentinvention preferably comprises: 25-55%, by weight, of a composition comprising carbon black and 0.5 to 10 parts per 100parts of carbon black of at least one binder component selected from at least one of groups i, ii, iii,iv or v, set forth above; 0 to 2%, by weight a stabilizer or antioxidant 0 to 5%, by weight an organic peroxide, preferably dicumyl peroxide; 0 to 10%, by weight a vinyl silane; the remainder being a polymer, or a blend of polymers, selected from the following group: ethylene homopolymer; 10 ethylene copolymerized with one or more alpha olefins, such as propylene, butene, or hexene; ethylene copolymerized with propylene and a diene monomer, preferably norbomene; andethylene copolymer with one or more monomers selected from vinyl acetate, acrylic acid, methacrylic acid, esters of acrylic or methacrylic acid containing 1 to 8 carbon atoms, maleicanhydride or a monoester derived from fumaric or maleic acid, vinyl chloride or vinylidenechloride.

The curable semi-conductive composition of the present invention may additionally include anadditive polymer such as acrylonitrile butadiene elastomer containing 25-55%, by weightacrylonitrile.

For use as a masterbatch composition, a typical formulation of the present inventionpreferably comprises: 30-60%, by weight, of a composition comprising a carbon black and 0.1 to 50%,preferably 1-20%, of at least one binder component selected from at least one of groups i, ii, iii, ivor v, set forth above; and 70-40%, by weight of an ethylene homopolymer or copolymer, where the comonomer ispreferably selected from hexene, propene, butene, octene or vinyl acetate.

Preferably, the polymer composition is polyethylene, low density polyethylene, linear low densitypolyethylene, high density polyethylene or a polyethylene wax. The masterbatch composition mayadditionally include antioxidants, peroxide decomposers, hindered amine light stabilizers,substituted benzophenone UV adsorbers or process aids.

An advantage of the carbon black compositions of the present invention is that in dry formthe carbon black compositions of the present invention have improved handling properties incomparison with conventional fluffy or pelleted carbon blacks.

An advantage of the polymer compositions of the present invention is that the polymercompositions exhibit enhanced rheological, processing or mechanical properties. 11

Further advantages of the carbon black compositions, and the polymer compositions, of thepresent invention will become apparent from the following detailed description.

Detailed Description of the Invention

The present invention includes carbon black compositions which in dry form haveimproved handling characteristics and impart enhanced performance characteristics to polymercompositions.

The carbon black compositions comprise:carbon black and 0.1% to 50%, preferably 1 to 20%, by weight, of at least one binder selected from at leastone of the following groups: i) an ethoxylated polyhydric alcohol having at least 3 hydroxyl groups per moleculeprior to ethoxylation, where the total number of ethylene oxide molecules perpolyhydric alcohol is at least 3; preferably the polyhydric alcohol is selected fromthe group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan,sucrose or a polyglyceride and/or the total number of ethylene oxide molecules perpolyhydric alcohol varies from 3 to 500 and more preferably varies from 5 to 100; ii) an alkyl carboxylic acid ester of an ethoxylated polyhydric alcohol having at least 3hydroxyl groups per molecule prior to ethoxylation, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selectedfrom the group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol, 12 sorbitan, sucrose or a polyglyceride and/or the total number of ethylene oxide molecules per polyhydric alcohol ester varies from 3 to 500 and more preferably varies from 5 to 100; iii) an alkyl carboxylic acid ester of a polyhydric alcohol having at least 3 hydroxylgroups per molecule prior to esterification, where the alkyl carboxylic acid has from8 to 30 carbon atoms, and may be saturated or unsaturated, and further where themono-ester functionality is at least 80% with the remainder being a di-esterfunctionality; preferably the polyhydric alcohol is selected from the groupconsisting of: triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan, sorbitoland a polyglyceride; iv) an ethoxylated alkyl carboxylic acid ester of a polyhydric alcohol having at least 3hydroxyl groups per molecule prior to esterification, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selectedfrom the group consisting of: triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sorbitol and a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; v) a polyethylene oxide - polypropylene oxide - polyethylene oxide block copolymer.

It is also preferred that the binders of groups i, ii, iii, iv and v have an HLB value of 8.0 to 30. 13 HLB value may be determined in the manner set forth above.

While any carbon black may be utilized in the compositions of the present invention,preferably the carbon black component of the carbon black composition has a nitrogen surface area(N2SA) of 15 to 1800 m2/g, a fluffy dibutyl phthalate absorption value (DBP) of 50 to 350cc/lOOg and a cetyl triamethylammonium bromide absorption value (CTAB) of 15 to 1500 m2/g.

The carbon black compositions may be produced by any conventional technique forcombining carbon black with dry or aqueous components. Preferably the carbon blackcompositions are produced by pretreating the carbon black with the binder. The carbon blackcompositions may be produced, in dry form, by a conventional pelletizing process. For example,the carbon black compositions of the present invention may be produced by contacting a fluffycarbon black in a pin pelletizer with an aqueous solution containing a binder selected from theforegoing groups of compounds wherein the level of binder in the pelletizing water is from 0.5%to 50%; and heating the wet pellets under controlled temperature and time parameters such that thewater is removed from the pellets but the binder does not undergo substantial decomposition, andthe final binder level on the dry carbon black is from 0.1% to 40%. The preparation of aqueoussolutions containing the binder compositions used in the present invention is within the skill of oneof ordinary skill in the art

Pin pelletizers which may be utilized to produce the compositions of the present inventionare known in the art and include the pin pelletizer described in U.S. Patent No. 3,528,785, thedisclosure of which is hereby incorporated by reference. U.S. Patent No. 3,528,785 alsodescribes a conventional pelletizing process which may be utilized to produce the compositions ofthe present invention.

The present invention also includes new polymer compositions comprising: a polymer component and 0.1-65%, preferably 0.1-20%, by weight, of a composition comprising a carbon black and 0.1-50%, preferably 1-20%, of at least one binder selected from at 14 least one of the following groups: i) an ethoxylated polyhydric alcohol having at least 3 hydroxyl groups per moleculeprior to ethoxylation, where the total number of ethylene oxide molecules perpolyhydric alcohol is at least 3; preferably the polyhydric alcohol is selected fromthe group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan,sucrose or a polyglyceride and/or the total number of ethylene oxide molecules perpolyhydric alcohol varies from 3 to 500 and more preferably varies from 5 to 100; ii) an alkyl carboxylic acid ester of an ethoxylated polyhydric alcohol having at least 3hydroxyl groups per molecule prior to ethoxylation, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selectedfrom the group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sucrose or a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; iii) an alkyl carboxylic acid ester of a polyhydric alcohol having at least 3 hydroxylgroups per molecule prior to esterification, where the alkyl carboxylic acid has from8 to 30 carbon atoms, and may be saturated or unsaturated, and further where themono-ester functionality is at least 80% with the remainder being a di-esterfunctionality; preferably the polyhydric alcohol is selected from the groupconsisting of: triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan, sorbitol 15 and a polyglyceride; iv) an ethoxylated alkyl carboxylic acid ester of a polyhydric alcohol having at least 3 hydroxyl groups per molecule prior to esterification, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selectedfrom the group consisting of: triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sorbitol and a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; • v) a polyethylene oxide - polypropylene oxide - polyethylene oxide block copolymer.Preferably, the carbon black is pretreated with the binder component The preferred carbon blacks,and binder components are as set forth above with respect to the carbon black compositions of thepresent invention. For example, it is preferred that the binder component have an HLB value of8.0 to 30. The polymer compositions may include other conventional additives such as pigments,reinforcing agents and the like.

While any polymer may be utilized in the polymer composition of the present invention,preferred polymers for use in the polymer compositions of the present invention include, but arenot limited to: a) homo or copolymers and graft polymers of ethylene where the co-monomers are selected from butene, hexene, propene, octene, vinyl acetate, acrylic acid, methacrylic acid, esters of acrylic acid, esters of methacrylic acid, maleic anhydride, half ester of maleic anhydride, and carbon monoxide; 16 b) elastomers selected from natural rubber, polybutadiene, polyisoprene, random styrenebutadiene rubber (SBR), polychloroprene, acrylonitrile butadiene, ethylene propylene co andterpolymers; c) homo and copolymers of styrene, including styrene - butadiene - styrene linear and radialpolymer, acrylonitrile butadiene styrene (ABS) and styrene acrylonitrile (SAN); d) linear and branched polyether or polyester polyols; e) crystalline and amorphous polyesters and polyamides; f) alkyd resins, rosin acids or rosin esters, hydrocarbon resins produced from thermal orFriedel Crafts polymerization of cyclic diene monomers such as dicyclopentadiene, indene,cumene; and g) hydrocarbon oils such as parafinic oil, naphthenic oil and hydrogenated naphthenic oil.

The polymer compositions of the present invention may be produced in any manner known to the art for combining polymers and dry or aqueous components.

The present invention further includes articles of manufacture produced from the polymercompositions of the present invention.

For use in semiconductive wire and cable applications, a typical formulation of the presentinvention comprises: 25-55%, by weight, of a composition comprising a carbon black and 0.5 to 10 parts, per100 parts of carbon black, of at least one binder selected from at least one of the following groups: i) an ethoxylated polyhydric alcohol having at least 3 hydroxyl groups per moleculeprior to ethoxylation, where the total number of ethylene oxide molecules perpolyhydric alcohol is at least 3; preferably the polyhydric alcohol is selected fromthe group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan,sucrose or a polyglyceride and/or the total number of ethylene oxide molecules perpolyhydric alcohol varies from 3 to 500 and more preferably varies from 5 to 100; 17 ii) an alkyl carboxylic acid ester of an ethoxylated polyhydric alcohol having at least 3hydroxyl groups per molecule prior to ethoxylation, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selectedfrom the group consisting of triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sucrose or a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; iii) an alkyl carboxylic acid ester of a polyhydric alcohol having at least 3 hydroxylgroups per molecule prior to esterification, where the alkyl carboxylic acid has from8 to 30 carbon atoms, and may be saturated or unsaturated, and further where themono-ester functionality is at least 80% with the remainder being a di-esterfunctionality; preferably the polyhydric alcohol is selected from the groupconsisting of: triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan, sorbitoland a polyglyceride; iv) an ethoxylated alkyl carboxylic acid ester of a polyhydric alcohol having at least 3hydroxyl groups per molecule prior to esterification, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3; preferably the polyhydric alcohol is selected 18 from the group consisting of: triethanolamine, glycerol, pentaerythritol, sorbitol,sorbitan, sorbitol and a polyglyceride and/or the total number of ethylene oxidemolecules per polyhydric alcohol ester varies from 3 to 500 and more preferablyvaries from 5 to 100; v) a polyethylene oxide - polypropylene oxide - polyethylene oxide block copolymer;0 to 2%, by weight a stabilizer or antioxidant; 0 to 5%, by weight an organic peroxide, preferably dicumyl peroxide; 0 to 10%, by weight a vinyl silane; the remainder being a polymer, or a blend of polymers, selected from the following group:ethylene homopolymer; ethylene copolymerized with one or more alpha olefins, such as propylene, butene, orhexene; ethylene copolymerized with propylene and a diene monomer, preferably norbomene; andethylene copolymer with one or more monomers selected from vinyl acetate, acrylic acid, methacrylic acid, esters of acrylic or methacrylic acid containing 1 to 8 carbon atoms, maleicanhydride or a monoester derived from fumaric or maleic acid, vinyl chloride or vinylidenechloride.

The curable semi-conductive composition of the present invention may additionally include anadditive polymer such as acrylonitrile butadiene elastomer containing 25-55%, by weightacrylonitrile.

For use as a masterbatch composition, a typical formulation of the present inventionpreferably comprises: 70-40%, by weight of an ethylene homopolymer or copolymer, where the comonomer ispreferably selected from hexene, propene, butene, octene or vinyl acetate; and 30-60%, by weight, of a composition comprising a carbon black and 0.1 to 50%, 19 preferably 1-20%, a binder component selected from at least one of the following groups: i) an ethoxylated polyhydric alcohol having at least 3 hydroxyl groups per moleculeprior to ethoxylation, where the polyhydric alcohol is preferably selected from thegroup consisting of triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan,sucrose or a polyglyceride and where the total number of ethylene oxide moleculesper polyhydric alcohol is at least 3, preferably varies from 3 to 500, morepreferably varies from 5 to 100; ii) an alkyl carboxylic acid ester of an ethoxylated polyhydric alcohol having at least 3hydroxyl groups per molecule prior to ethoxylation, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester f unctionality, and f urther where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3, preferably varies from 3 to 500, morepreferably varies from 5 to 100, and where the polyhydric alcohol is preferablyselected from the group consisting of triethanolamine, glycerol, pentaerythritol,sorbitol, sorbitan, sucrose or a polyglyceride; iii) an alkyl carboxylic acid ester of a polyhydric alcohol having at least 3 hydroxylgroups per molecule prior to esterification, where the alkyl carboxylic acid has from8 to 30 carbon atoms, and may be saturated or unsaturated, and further where themono-ester functionality is at least 80% with the remainder being a di-esterfunctionality, and where the polyhydric alcohol is preferably selected from thegroup consisting of: triethanolamine, glycerol, pentaerythritol, sorbitol, sorbitan,sorbitol and a polyglyceride; 20 iv) an ethoxylated alkyl carboxylic acid ester of a polyhydric alcohol having at least 3hydroxyl groups per molecule prior to esterification, where the alkyl carboxylic acidhas from 8 to 30 carbon atoms, and may be saturated or unsaturated, and furtherwhere the mono-ester functionality is at least 80% with the remainder being a di-ester functionality, and further where the number of ethylene oxide molecules perpolyhydric alcohol ester is at least 3, preferably varies from 3 to 500, morepreferably varies from 5 to 100, and where the polyhydric alcohol is preferablyselected from the group consisting of: triethanolamine, glycerol, pentaerythritol,sorbitol, sorbitan, sorbitol and a polyglyceride; v) a polyethylene oxide - polypropylene oxide - polyethylene oxide block copolymer.Preferably, the polymer composition is polyethylene, low density polyethylene, linear low densitypolyethylene, high density polyethylene or a polyethylene wax. The masterbatch composition mayadditionally include antioxidants, peroxide decomposers, hindered amine light stabilizers,substituted benzophenone UV adsorbers or process aids.

The effectiveness and advantages of various aspects and embodiments of the presentinvention will be further illustrated by the following examples wherein the following testingprocedures were utilized.

The following testing procedures were utilized in the determination and evaluation of theanalytical properties cf the carbon blacks utilized in the following examples. The DBP (dibutylphthalate adsorption value) of the carbon blacks utilized in the examples, expressed as cubiccentimeters DBP per 100 grams carbon black (cc/lOOg), was determined according to theprocedure set forth in ASTM D2414. The nitrogen surface area (N2SA) of the carbon blacksutilized in the examples, expressed as square meters per gram (m^/g), was determined according toASTM test procedure D3037 Method A.

The carbon blacks pellets described in the following examples were evaluated utilizing the 21

following testing procedures. The pellets were assessed for mass pellet strength using ASTM D1937. Pellet attrition was evaluated using a modified version of ASTM D 4324, wherein the ASTM test procedure was modified to generate the level of dust after shaking samples for 5 minutes.

The moisture content of the pellets was determined by drying the sample to constant massin an air circulating oven at 150’ C and then calculating moisture percentage by comparing theweight prior to drying to the weight after drying.

The polymer compositions, including the polymer masterbatch compositions, described inthe following examples were evaluated utilizing the following test procedures.

Melt index was determined by ASTM D1238.

Pressure rise of the masterbatch compositions was determined by introducing a 325 meshscreen pack behind the breaker plate of a 1 inch single screw extruder fitted with a pressuretransducer to measure the pressure change in the region of the screen pack.

Viscosity of the polymer compositions was measured utilizing a Carri-Med CS viscometer,produced and sold by TA Instruments of Wilmington, Delaware, at the temperature, and utilizingthe shear rate specified in the particular example.

Triple roll mill passes were evaluated by passing the polymer compositions through a tripleroll mill and recording the number of passes required to generate zero scratches on a Hegman•gauge, and also recording the residual background “sand” value.

Dispersion of the diluted samples in the following examples was determed by diluting themasterbatch composition down to a loading of 2%, by weight, carbon black with the EVA resin ina Brabender mixer operating at 85’ C and 50 rpm. The mixing time was 2 minutes. Samples werethen pressed between microscope slides and dispersion at 100X magnification was determined bythe Cabot Corporation rating method wherein the number (1-6) refers to the size of the undispersedparticles, with 1 being small and 6 being large; and the letter (A-E) refers to the number of particlesper field of view, with A being 1-2 particles and E being greater than 50 particles. Lower numbers \ 22

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and earlier letters indicate better dispersion, with a 1A rating indicating good dispersion and a 6Erating indication poor dispersion.

In Examples 18-26, dispersion of the carbon black pellets was determined by measuringthe number and size of surface imperfections in the tape formed from the compound incorporatingthe pellets using an optical microscope at lOOx magnification and a reflected light source.

The polymer compositions were evaluated for strippability utilizing the followingtechnique. The compositions containing 40% carbon black in the ethylene vinyl acetate resin werecompounded in a Brabender mixer with 1% dicumyl peroxide while maintaining the mixingtemperature below 150* C. The material was transferred to a heated hydraulic press (temperature130’ C) and a plaque 1.2 mm thick produced. A 2 mm polyethylene plaque containing 1%dicumyl peroxide was produced in a similar manner. The two plaques were laminated togetherunder a pressure of 100 psi and exposed to a curing cycle of 180* C for 15 minutes. The laminatewas allow to cool to ambient temperature under pressure. The delamination force under a peelingangle of 180 degrees and a separation speed of 3.94 inches/minute was recorded; the resultsprovided are an average of 28 peel tests.

The modulus, tensile and elongation of the polymer compositions were measured by theprocedure set forth in ASTM D 412.

The Shore A Hardness of the rubber compounds was determined according to theprocedure set forth in ASTM D-2240-86.

The maximum torque was determined from the peak of the motor load versus time profilefrom the Brabender mixer.

The dump torque (Nm) was determined from the final torque value at the end of the mixing cycle.

The total energy (Nm) was determined by calculating from the area under the full mixing curve.

The MDR @ 170’ C T50 (m.m), and T90 (m.m) was determined according to the 23 procedure set forth in ASTM 2084.

The Mooney viscosity (ML(l+4)@100* C (MU)) was determined according to the procedure set forth in ASTM 1646.

The IRHD (hardness) was determined according to the procedure set forth in ASTMD1415.

The effectiveness and advantages of the present invention will be further illustrated by thefollowing examples.

Examples 1-4

Examples 1-4 illustrate the use and advantages of carbon black compositions of the presentinvention, in comparison to conventional carbon black pellets, in polypropylene fiber applications.

Four carbon black pellet compositions, A, B, C and D were produced by introducing 400grams (g) of a fluffy carbon black, identified herein as CB-1, having a DBP of 60 cc/lOOg and anitrogen surface area of 112 m2/g, into a batch pin pelletizer together with a solution containing 20g of a binder and 300 g of water. The binder utilized in each pelleting composition was as shownin the Table below.

Binder

Pellet Composition

A

B

C

D water 5% sorbitan monostearate with 20 moles ethoxylate5% sorbitan monooleate with 5 moles ethoxylate5% sorbitan monooleate with 20 moles ethoxylate

Carbon black pellet composition A was a control composition, carbon black pellet compositions B,C and D were carbon black compositions of the present invention.

The carbon black/binder mixture was agitated for 5 minutes with a rotor speed of 800 rpm.The resultant pellets were dried at 120° C until the moisture content of the pellets was below 0.51.Pellet strength of each pellet composition was assessed qualitatively. The results are set forth in 24

Table 1 below.

The carbon black pellets were combined with a polypropylene homopolymer of melt index35 in a twin screw extruder to produce a masterbatch containing 35% by weight of the pelletedcarbon black, the remainder being polypropylene and binder.

The polypropylene composition was introduced into a 1 inch single screw extruder untilequilibrium pressure conditions. The masterbatch was introduced and the rate of pressure changerecorded according to the procedure described above. The results were as shown in Table 1below.

Table 1

Carbon Black PelletComposition pellet strength pressure risepsi/g A weak 4.86 B strong 4.34 C strong 4.25 D strong 2.97

These results indicate that carbon black compositions B, C and D of the present inventionhave improved pellet strength in comparison with the carbon black pellet composition A producedwith pelletizing water only. In addition, the reduction in pressure build-up in masterbatchcompositions containing carbon black compositions B, C and D of the present invention, incomparison to the masterbatch composition containing carbon black composition A, wouldtranslate to a reduction in the frequency of screen changes on a fiber production line, and thereforeimproved capacity and lower operating costs for the production line.

Examples 5-10

Examples 5-10 illustrate the use and advantages of carbon black compositions of the present invention, in comparison to conventional carbon black pellets, in polypropylene fiber i

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25 applications.

Two carbon black pellet compositions, E and F were produced in a continuous process bycombining a fluffy carbon black, identified herein as CB-2, having a DBP of 112 cc/lOOg and annitrogen surface area of 60 m2/g into a batch pin pelletizer together with a binder solution. Thepellets were produced in a continuous pin pelletizer operating with rotor speed of 800 rpm toprovide wet pellets with an average water content of 50%. The wet pellets were dried in a heatedrotating drum to provide dry pellets with a moisture content below 0.6%.

The binder utilized in each pelleting composition was as shown in the Table below.

Pellet Composition Binder water 2% sorbitan monooleate with 20 moles ethoxylate

Four runs of carbon black pellet composition E, and two runs of carbon black pellet compositionF were made. Carbon black pellet composition E was a control composition, and carbon blackpellet compositions F was a carbon black composition of the present invention.

The pellets were assessed for mass pellet strength and pellet attrition using the proceduresdescribed above. In addition, the pellets were used to produce a masterbatch, as in examples 1-4,and the pressure rise determined as described above. The results are set forth in Table 2 belQw. 26

Table 2

Carbon Black PelletComposition pellet strength pounds dust (%) 5 min. pressure rise psi/g E run 1 15 1.2 11.0 E run 2 14 1.2 11.4 E run 3 16 2.8 12.9 E run 4 18 1.6 9.1 F run 1 44 0.4 7.3 F run 2 58 0.2 5.3

These results illustrate the significant improvement in pellet strength and attrition resistance byincorporation of a binder of the type utilized in the present invention during the pelletizing processin preparing the carbon black pellet composition F of the present invention. Carbon black pelletcomposition F of the present invention also has improved dispersion, in comparison with aconventional water pelletized carbon black pellet composition E, as seen by the reduction inpressure build-up when extruded through a screen pack which would translate to improved outputat lower operating cost

Examples 11-14

Examples 11-14 illustrate the advantages of the carbon black pellet compositions of thepresent invention for use in polyurethane applications.

Two fluffy carbon blacks, identified herein as CB-3 and CB-4, were pelletized to produce carbon black pellet compositions. Carbon blacks CB-3 and CB-4 had the combination of analytical properties set forth below: 27

Fluffy Carbon Black CB-3 CB-4

DBP N,SA 112cc/100g 58m2/g 140 cc/lOOg 68 m2/g

Four carbon black pellet compositions, G, Η, I and J were produced in a continous processby combining the carbon blacks in a batch pin pelletizer together with a binder solution. The pelletswere produced in a continuous pin pelletizer operating with rotor speed of 1000 rpm and dried in aheated rotating drum to provide dry pellets with a moisture content below 0.3%. The binder andcarbon black utilized in each pelleting composition was as shown in the Table below.

Pellet Composition Carbon Black Binder G CB-3 water H CB-3 2% sorbitan monooleate with20 moles ethylene oxide I CB-4 water J CB-4 2% sorbitan, monooleate with 20 moles ethylene oxide

Carbon black pellet compositions G and I were control compositions, and carbon black pelletcompositions H and J were carbon black compositions of the present invention.

The pellets were assessed for mass pellet strength using the procedures described above.The results were as follows:

Pellet Composition mass pellet strength - pounds

G

H

I

J 14-16 51 10 26

The carbon black pellet compositions G, Η, I and J were compounded into a polyether polyol, having a viscosity of 150 mPa.s at 25’ C and a hydroxyl content of 3.4%, to produce a 30% carbon black content paste. In addition, a polyether polyol compositon was produced by 28 compounding carbon black CB-4 into the polyol and adding 2% sorbitan monooleate with 20 moles ethylene oxide binder directly to the polyol. Each compounding operation involved pre- dispersion under a high shear, Dispermat, mixer for 5 minutes at a speed of 2000 rpm.

The paste was then transferred to a triple roll mill for the final size reduction process. Thenumber of passes through the triple roll mill required to generate zero scratches on a Hegmangauge were noted together with the residual background "sand" value. The paste was then dilutedwith further polyol to produce a 15% carbon black loaded sample and the viscosity measured on aCarri-Med CS viscometer at a shear rate of 300 s-1. The results were as shown in Table 3:

Table 3

Carbon Black Numberof passes "sand" viscosityshear stress Pellet Composition triple roll (microns) (dvne/cm2) G 5 37 2800 H 5 19 1900 I 6 17 1860 J 5 17 1400 CB-4, with Binder Added 7 26 1790

Directly to Polyol

The above experiments illustrate the improved pellet strength and dispersion, and reducedcompound viscosity, of the carbon black pellet compositions H and J of the present invention incomparison to use of carbon black compositions G and H pelletized with water only. The data alsodemonstrates the benefits of incorporating a binder directly onto the carbon black (pretreating thecarbon black with a binder) in comparison to adding the binder to the polymer system.

This example is representative for polyurethane foam and sealant applications anddemonstrates improvement in dispersion and rheology of the polymer compositons incorporatingcarbon black compositions of the present invention. The reduction in viscosity would allow use oflow pressure to apply the polyurethane sealant in either automotive direct glazing or windowdouble/triple glazing unit operations. 29

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Example 15-17

This example illustrates the advantages of using the carbon black compositions of thepresent invention in ink formulations.

Carbon black compositions G and H from Examples 11-14 were evaluated in a typical oilbased gloss ink using the same process as outlined in examples 11-14. In this case the mill baseand letdown system were an oil (McGee 47) and a heatset resin (Lawter Vehicle 3477) used in aratio of 1:9 by weight A third ink formulation was produced by adding sorbitan monooleate with20 moles of ethylene oxide, to a composition of Carbon Black Composition G and the oil utilizedin the compounding process.

The compounding operation involved pre-dispersion under a high shear, Dispermat, mixerfor 5 minutes at a speed of 2000 rpm. The paste was then transferred to a triple roll mill for thefinal size reduction process. The number of passes through the triple roll mill required to generatezero scratches on a Hegman gauge were noted together with the residual background "sand" value.The paste was then diluted with further polyol to produce a 15% carbon black loaded sample andthe viscosity measured on a Carri-Med CS viscometer at a shear rate of300 s-1. The results wereas shown in Table 4:

Table 4 - Ink Formulation

Carbon Black Numberof passes "sand" viscosityshear stress Pellet Composition triple roll (microns) (dvne/cm2) G 5 18 330 H 4 15 165 G, with binder added to oil 4 17 240

These results demonstrate the improved dispersion and reduced viscosity obtained when the binder composition utilized in the carbon black compositions of the present invention is either incorporated onto the carbon black or with direct addition to the ink vehicle. Incorporating the binder onto the carbon black exhibits the most significant improvement The binder would potentially help to reduce the mixing time for the ink and the reduced viscosity and improved 30 dispersion would help to reduce wear in the application process.

Example 18-26

Examples 18-26 illustrate the use of carbon black compositions of the present invention insemiconductive compounds.

Three carbon black pellet compositions, K, L and M were produced by combining a fluffycarbon black, identified herein as CB-5, having a DBP of 140 cc/lOOg and a nitrogen surface areaof 70 m2/g, in a batch pin pelletizer together with a binder solution. The carbon black wascombined with various binder solutions in a continuous pin pelletizer operating at 1050 rpm toprovide wet pellets with levels of sorbitan monooleate with 20 moles ethylene oxide in amountsvarying from 0 to 4%. The pellets were dried in a heated rotating drum to provide dry pellets withmoisture content below 0.6%. The binder utilized in each pelleting composition was as shown inthe Table below.

Pellet Composition Binder water 2% sorbitan monooleate 20 moles ethylene oxide4% sorbitan monooleate 20 moles ethylene oxide

The carbon blacks were compounded into ethylene vinyl acetate resin (40% vinyl acetatecontent, melt index 3), using a twin screw extruder, to produce a 40% carbon black loadedcompound. The compound was subsequently extruded to form a tape and the level of carbon blackdispersion assessed by measuring the number and size of surface imperfections using an opticalmicroscope (magnification lOOx) with a reflected light source, by the procedures described herein.The results are shown below: EVA Composition area of un-dispersed carbon black

Carbon Black Composition 0.0470% 0.0056% 0.0067% 31

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The reduction in undispersed carbon black would be seen in the final cable compound as an improvement in surface smoothness of the extruded cable. Reduction in surface imperfections of the semi-conductive insulation shield is known to reduce the frequency of electrical breakdown dueto tree growth.

The EVA compositions containing carbon black compositions K and L disclosed abovewere evaluated for strippability onto a polyethylene substrate using the following technique: Thecompounds containing 40% carbon black in the ethylene vinyl acetate resin were compounded in aBrabender mixer with 1% dicumyl peroxide while maintaining the mixing temperature below 150*C. The material was transferred to a heated hydraulic press (temperature 130* C) and a plaque 1.2mm thick produced. A 2 mm polyethylene plaque containing 1% dicumyl peroxide was producedin a similar manner. The two plaques were laminated together under a pressure of 100 psi andexposed to a curing cycle of 180’ C for 15 minutes. The laminate was allow to cool to ambienttemperature under pressure. The delamination force under a peeling angle of 180 degrees and aseparation speed of 3.94 inches/minute was recorded; the results are an average of 28 peel tests:EVA Composition

Carbon Black Composition lb per 0.5 inch 6.55 +/- 0.465.12+/-0.44

The data shows a reduction in strip force required to remove the semi-conductive shieldcompound from the insulation layer. This is important in cable splicing operations or in makingterminal connections. The lower strip force will result in a faster operation and minimise voids/imperfections from high strip force systems and hence reduce the potential for electrical breakdown in use.

Examples 27-37

Examples 27-37 illustrate the use of carbon black compositions in polyolefin masterbatchcompositions. 32

Four carbon blacks were utilized to produce carbon black compositions of the presentinvention and control carbon black compositions. The carbon blacks utilized are designated hereinas CB-6, CB-7, CB-8 and CB-9 and had the combination of analytical properties set forth below:

Carbon Black DBP cc/lOOg N2SA m2/g CB-6 140 68 CB-7 135 180 CB-8 136 120 CB-9 168 53

The carbon blacks were were combined with either water or an aqueous solution ofsorbitan monooleate with 20 moles of ethylene oxide in a continuous pelletizer operating with arotor speed of 1000 rpm to produce wet pellets. The pellets were dried in an air circulating ovenoperating at 120* C to produce dry pellets with moisture content below 0.4%. In all 11 differentcarbon black compositions were produced as shown below:

Composition N O P Q R Carbon Black CB-6 CB-6 CB-6 CB-6 CB-6 Binder Water 0.5% sorbitan monooleate with 20 moles ethylene oxide1.0% sorbitan monooleate with 20 moles ethylene oxide2.0% sorbitan monooleate with 20 moles ethylene oxide4.0% sorbitan monooleate with 20 moles ethylene oxide S CB-7 Water T CB-7 2.0% sorbitan monooleate with 20 moles ethylene oxide U CB-8 Water V CB-8 2.0% sorbitan monooleate with 20 moles ethylene oxide W CB-9 Water X CB-9 2.0% sorbitan monooleate with 20 moles ethylene oxide

The carbon black compositions were assessed for pellet strength and attrition resistanceusing the procedures described herein. The results are shown below in Table 5. 33

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Table 5

Composition pellet strength(pounds) dust (%) 5’ io· N 25 4.4 5.0 0 61 0.5 1.1 P 49 0.6 1.5 Q 55 0.2 0.4 R 50 0.8 0.6 S 44 3.6 15.0 T 83 0.3 1.5 0 62 0.8 5.2 V 119 0.2 0.4 w 17 2.5 4.8 X 21 1.2 2.4

Each of the carbon black compositions was identically compounded into low density poly-ethylene having a melt index of 26 using a Brabender mixer to produce a masterbatch containing40% carbon black. The viscosity of the masterbatch was measured at 130* C and a shear rate of 50s-1. The results are set forth in Table 6 below. 34

Composition Ν'

S Τ

U

V

Table 6Viscosity (Pa.s) 5116 4045 3389 2873 2536 4329 3695 4591 3804 5487 4373

The data in Table 6 illustrates the reduction in viscosity obtained by using a carbon blacktreated with a binder composition of the present invention. This reduction in viscosity wouldfacilitate ease of dispersion of the masterbatch into further polyethylene in a typical extrusionblown film or profile extrusion application; and also improve output efficiency. One would alsoexpect an improvement in carbon black dispersion which would also provide an improvement inpigmentary effieciency, UV protection and mechanical performance (e.g. tensile or impactstrength).

Examples 38-49

This example illustrates the use of different binder compositions to produce carbon black compositions of the present invention, and the advantages of using the carbon black compositions of the present invention in ethyl vinyl acetate (EVA) applications.

Eleven carbon black compositions, HH, II, JJ, KK, LL, MM, NN, OO, PP, QQ and RR 35 were produced by combining 400 g of a fluffy carbon black having a DBP of 128 cc / lOOg and a nitrogen surface area of 68 m2 / g, designated herein as CB-12, together with 8 g of binder dissolved in 500 g of water, in a batch pin pelletizer. The binder utilized in each composition was as follows:

Composition Binder HH water II sucrose monoester of tallow fatty acid JJ sucrose monostearate KK sucrose distearate LL ethoxylated glyceride MM ethoxylated triglyceride NN SYNPERONIC PE/L61 surfactant OO SYNPERONIC PE/85 surfactant PP SYNPERONIC PE/F127E surfactant QQ SYNPERONIC PE/38E surfactant RR SYNPERONIC PE/108E surfactant * SYNPERONIC is a trade name for surfactants produced and sold by ICI Corporation andcomprise ethylene oxide - propylene oxide copolymers.

The mix was agitated at 800 rpm for 2 minutes to produce a pelletized carbon black. Thecarbon black pellets were dried at 125’ C until the moisture content was below 1%.

Mass pellet strength of the carbon black compositions was determined according to theprocedures described herein. The results are set forth in Table 7 below.

Each of the carbon black compositions was combined with an ethylene vinyl acetatecopolymer containing 40% vinyl acetate and a melt index of 3 in a Brabender mixer conditioned at65’ C. The compound was masticated for 6 minutes at 50 rpm to produce a fully dispersedcompound containing 40% carbon black. These compounds were assessed for melt index (MI) at 36 190* C using a 21.6 kg load, according to the procedures described herein. The results are also setforth in Table 9 below, which also shows the HLB of each binder.

Table 7

Comp Binder HLB MPS (pounds) MI (g/lOm) Disp. OfDil. Samples HH water 1.6 6.58 2C II sucrose monoester of tallow fatty acid 14.5 15.2 9.86 1C JJ sucrose monostearate 15.0 15.8 6.88 IB KK sucrose distearate 12.0 22.8 9.18 IB LL ethoxylate glyceride 15.7 4.9 8.84 1C MM ethoxylated triglyceride 14.4 6.7 14.00 ID NN SYNPERONIC PE/L61 surfactant 16.0 9.4 10.34 IB CO SYNPERONIC PE/85 surfactant 16.0 2.9 10.55 1C PP SYNPERONIC PE/F127E surfactant 22.0 2.6 6.70 IE QQ SYNPERONIC PE/38E surfactant 30.5 3.1 7.90 IB RR SYNPERONIC PE/108E surfactant 27.0 3.5 7.97 IE

Comp. = Composition; Disp. Of Dil. Samples = Dispersion of Diluted Samples.

These examples illustrate the improvement in dispersion quality and reduction in viscositywith improved pellet handling qualities, in a commercial system. These results would relate toshorter mixing cycles and improved extrusion characteristics.

Examples 50-52

These examples illustrates the production of carbon black compositions of the presentinvention, and the advantages of using the carbon black compositions of the present invention inethyl vinyl acetate (EVA) applications. 37

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Three carbon black compositions, SS, TT and UU were produced by combining a fluffycarbon black with a nitrogen surface area of 70 m2/g and a DBP of 140 cc/lOOg of carbon black,designated herein as CB-13, with a binder solution containing sorbitan monooleate in a continuouspin pelletiser operating at 1050 rpm to provide wet pellets. The resulting pellets containing either0%, 2% or 4% binder were dried in a heated rotating drum to provide dry pellets with moisturecontents below 0.6%. The percentage of the binder utilized in each composition was as follows:

Composition Binder (% by weight) SS 0.0 % sorbitan monooleate (water) TT 2% sorbitan monooleate UU 2% sorbitan monooleate

The treated carbon blacks where compounded into various polymers using a Brabendermixer operating at 50 rpm and with an initial chamber temperature of 85* C. The mixing cycle timewas 6 minutes. The compounds were assessed for melt viscosity at 130’ C and a shear rate of50s-l. polymer 0 Viscosity (Pa.s)percent binder 2 4 ethylene vinyl acetate(40% vinyl acetate, MI 3.0) 8155 3210 3080 ethylene vinyl acetate(18% vinyl acetate, MI 2.5) 7368 3564 3498 ethylene ethyl acrylate(18% ethyl acrylate, MI 6.0) 7018 3170 2558

The data illustrates a significant reduction in melt viscosity when using the designated binder, thiswould reflect in a reduction in die head pressure during the cable fabrication process. Visually thiswould be seen as an improvement is smoothness of the compound extrudate and also an increase inoutput rate. 38

The polymers utilized represent typical types of polymer used in wire and cableformulations used for conductor and semi-conductive shield applications. The polymerscontaining either 18% vinyl acetate or ethyl acrylate are typically used in conductor or bondedsemi-conductive shield applications while the polymer containing 40% vinyl acetate is moresuitable for a strippable semi-conductive shield type product

It should be clearly understood that the forms of the present invention herein described areillustrative only and are not intended to limit the scope of the invention.