Title of Invention	CARBON BLACK GRANULES
Abstract	Carbon black granules, characterised in that they contain a sorbitan triester.

Full Text

Carbon black granules The invention concerns carbon black granules, a process for their production and their use. Carbon blacks are preferably processed as granulated products, which are often referred to as carbon black granules, beaded carbon black or pelletised carbon black. The way in which the granulation is handled differs according to the structure and surface area of the carbon blacks. Thus, carbon blacks with a low structure agglomerate more easily than carbon blacks with a high structure. Inks containing a dye having a particle size of 0.01 pm to 25 µm, a hydrocarbon resin, an oxidised polyethylene and a resin as binder are known from US 5,981,625. In addition, a process is known from US 4,397,652 for the production of inks containing an adhesive, selected from the group consisting of sorbitol, hydrogenated dextrose, glucose, lactose, neopentyl glycol, mannitol, mannose and polyethylene glycol, and a dust binder. A carbon black composition containing carbon black and a binder selected from the group comprising ethoxylated esters and polyethers is known from. WO 96/21698. The known carbon black beads have the disadvantages that the carbon black beads are difficult to disperse and have a low gloss when incorporated into printing inks. In addition, such printing inks have poor flow properties, high water absorption and poor free running behaviour on the printing plate. The object of the present invention is to provide carbon black granules which when incorporated into printing inks display a good dispersion state, high gloss, good flow properties, low water absorption and good free running behaviour on the printing plate. The invention provides carbon black granules which are characterised in that they contain a triester of sorbitan. The carbon black granules can be in bead form. All triesters of saturated, unsaturated or polyunsaturated carboxylic acids can be used as sorbitan triester. The carboxylic acids can be branched or unbranched. Sorbitan trioleate, sorbitan trilaureate, sorbitan tristearate, sorbitan tripalmeate or sorbitan triricinoleate can preferably be used. The carbon black granules can contain 1 to 15 wt.%, preferably 3 to 7 wt.%, of the sorbitan triester, relative to the carbon black granules. The carbon black granules can have a BET surface area of 10 to 300 m2/g, preferably 45 to 110 m2/g. The invention also provides a process for the production of carbon black granules which is characterised in that a powdered carbon black or beaded carbon black is granulated with a sorbitan triester. Granulation can be performed in a ring-layer mix- pelletizer, a bead machine or a bead drum. Wet- or dry-beaded carbon black can be used as beaded carbon black. The carbon black granules can be dried after granulation. The dryer temperature can be between 100° and 250°C, preferably between 150° and 200°C. The temperature of the carbon black granules on leaving the dryer can be between 30° and 100°C, preferably between 40° and 70°C. The carbon black granules according to the invention can be post-beaded. All types of carbon black can in principle be granulated with the process according to the invention. Furnace blacks, lamp blacks, gas blacks, channel black, thermal black, acetylene black, plasma black, inversion black, known from DE 195 21 565, Si-containing carbon blacks, known from WO 98/45361 or DE 19613796, or metal-containing carbon blacks, known from WO 98/42778, arc blacks and carbon-containing materials that are secondary products of chemical production processes can be used. Carbon blacks having BET surface areas of between 10 and 300 m2/g can preferably be used. Printex 25, Printex 275, Printex 30, Printex 300, Printex 35 and Printex 45 from Degussa AG, for example, can be used as starting carbon black. The sorbitan triester can be dissolved, for example in mineral oils or vegetable oils, preferably in oils that can be used in printing inks. The sorbitan triester can. be used as a 10 and 90 wt. % solution. An additional binder can be added to the sorbitan triester. For example, resins or waxes, as well as numerous other substances, either alone or in combination with one another, can be added as additional binder. In a preferred embodiment, no additional binder can be added to the sorbitan triester. The carbon black granules according to the invention can be used in polymer blends, such as rubber and plastics for example, lacquers, inks, in particular printing inks, pigments and the many other application forms of carbon black. In a preferred application form the carbon black granules according to the invention can be used in oil- based offset printing inks. The invention also provides printing inks which are characterised in that they contain the carbon black granules according to the invention. The printing inks can contain conventional components, such as e.g. binders, solvents and diluents, as well as other auxiliary substances. The printing inks can contain 5 to 45 wt.%, preferably 10 to 25 wt.%, of carbon black granules according to the invention. The printing inks can be produced by premixing the carbon black granules according to the invention with printing ink binders and then dispersing and grinding them. The printing inks according to the invention can be used in offset printing. The carbon black granules according to the invention have the advantage that, when incorporated into printing inks, they display a good dispersion state, high gloss, good flow properties, low water absorption and good free running behaviour on the printing plate. Example 1-3 : Production of carbon black granules The carbon black granules according to the invention are produced by continuously feeding the starting carbon black to the heated ring-layer mix-pelletizer (RMG) by means of a gravimetric powder metering unit. The sorbitan trioleate is optionally heated to allow it to be pumped more readily and also to achieve better atomisation. The sorbitan trioleate is sprayed in with air by means of two-fluid atomisation using a feed nozzle which is 12.5 cm away from the centre of the carbon black filling nozzle. The partially granulated product discharged from the ring-layer mix- pelletizer is post-beaded in a granulating drum to round off the granules and to further reduce the fines. Printex 25 (Px25) is used as starting carbon black in Example 1, Printex 35 (Px35) in Example 2 and Printex 45 (Px45) in Example 3. In all three examples sorbitan trioleate (STO) is used as the sorbitan triester. The experimental conditions are described in Table 1. The analytical data for the carbon black beads is determined in accordance with the following standards: BET surface area ASTM 6556-0la, Fines: ASTM D-1508-01 Volatile matter 950 °C DIN 53552 Bead abrasion DIN 53583 Bulk density DIN 53600 The analytical data for examples 1 to 3 is set out in Table 2. Comparative example 4-6 The same starting carbon blacks as used in example 1-3, but without the addition of additive, are granulated as comparative examples. The experimental conditions are described in Table 3. The carbon black granules according to the invention (example 1-3) display a higher bulk density in comparison to the comparative examples 4-6. Example 7-9 For examples 7 to 9 the additive is applied to dry-beaded carbon black. To this end, dry-beaded carbon black from examples 4 to 6 is placed in the granulating drum. The sorbitan trioleate is heated to 80°C to allow it to be pumped more readily and also to achieve better atomisation. With the drum rotating, the sorbitan trioleate is sprayed with air onto the carbon black bed by means of two-fluid atomisation. When the addition is completed, the drum is allowed to run for a further 10 minutes. The experimental conditions are described in Table 5. The analytical data for comparative examples 7 to 9 is set out in Table 6. Example 10-12 Offset printing ink: The following components are mixed in a high-speed mixer: 12.8 % ER resin 125 12.0 % Necires LF 220/130 10.4 % Albertol KP 172 10.4 % Setalin V402 0.4 % Cycloxim FF 26.0 % Automotive oil F 4/7 8.0 % Automotive oil F 6/9 ER resin 125 is a hydrocarbon compound from American Gilsonite Company USA (supplied by Worlee Chemie GmbH Hamburg). Necires LF 220/130 is a hydrocarbon resin from Nevcin Polymers B.V. Holland. Albertol KP 172 is a phenolic resin-modified colophony resin from Solutia Germany GmbH & Co. KG Germany. Setalin V402 is an alkyd resin from Akzo Nobel Resins Holland. Cycloxim FF is a cyclohexanone oxime from Acima AG Switzerland. Automotive oil F 4/7 is an acid- treated petroleum distillate from Haltermann Products Hamburg. Automotive oil F 6/9 is an acid-treated petroleum distillate from Haltermann Products Hamburg. After the components have been intimately mixed, a further 20.0 % carbon black is added. After being predispersed for 15 minutes in the high-speed mixer (Getzmann), the mixture is then ground in a mill (Netzsch Attritor) with 3 mm steel balls until the grindometer fineness is below 5 µm. The carbon blacks used in the printing inks are listed in Table 7. The viscosity, yield point and flow behaviour of the printing ink is determined (Table 8). After de-aeration,using a triple roller mill, the printing ink is applied to paper in a test model printing device. The ink is applied in a 1.5 g/m2 layer onto APCO paper. After 24 h the optical density, gloss and yellow value b* in accordance with CieLab are determined on the dried print (Table 12) . The printing inks (example 10-12) with the carbon black granules according to the invention display an improved, lower viscosity, better flow and higher gloss than the printing inks (example 13-15) with the comparative examples. After de-aeration, using a triple roller mill, the printing ink is applied to paper in a test model printing device. The ink is applied in a 1.5 g/m2 layer onto APCO paper. After 24 h the optical density, gloss and yellow value b* in accordance with CieLab are determined on the dried print (Table 9). Comparative example 13-15 For the sake of comparison, the carbon black granules according to example 4 to 6 are likewise used in printing inks in an analogous way to example 10 to 12, and the inks are analysed (Table 10). The viscosity, yield point and flow behaviour of the printing ink is determined (Table 11). Example 16 In an analogous way to examples 7 to 9, Printex 275 (Px275, furnace black with a BET surface area of 53.3 m2/g) is used as the starting carbon black and a granulated carbon black is produced with sorbitan trioleate (Table 13). Example 17-18 As in examples 10-12, the Printex 275 granulated with sorbitan trioleate from Example 16 and conventionally dry- beaded starting carbon black Printex 275 are incorporated into printing inks (Table 15). The behaviour with regard to water is analysed using a Tack-O-Scope (Table 16). The printing ink (Example 17) with the carbon black granules according to the invention displays a higher tack after contact with water than the printing ink (Example 18) with the comparative carbon black. Example 19-20 Two printing inks are produced with commercial Printex 35 as described in example 10-12. 5% sorbitan trioleate (Example 19) and 5% sorbitan monooleate (Example 20), relative to carbon black, are used in the production. The behaviour of both inks with regard to water is analysed using a Tack-O-Scope (Table 17). The printing ink (Example 19) with the carbon black granules according to the invention displays a higher tack, which is also higher even after contact with water, as well as lower water absorption and better free running behaviour. WE CLAIM: 1. Carbon black granules, characterized in that they contain a sorbitan triester. 2. Carbon black granules as claimed in claim 1, wherein the sorbitan triester is a triester of saturated, unsaturated or polyunsaturated carboxylic acids. 3. Carbon black granules as claimed in claim 1, wherein the sorbitan triester is sorbitan trioleate, sorbitan, trilaureate, sorbitan tristearate, sorbitan tripalmeate or sorbitan triricinoleate, 4. Process for the production of carbon black granules as claimed in claim 1, wherein a powdered carbon black or beaded carbon black is granulated with a sorbitan triester. 5. Process for the production of carbon black granules as claimed in claim 4, wherein carbon black with BET surface areas of between 10 and 300 m2/g is used. 6. Process for the production of carbon black granules as claimed in claim 4, whererin sorbitan trioleate, sorbitan trilaureate, sorbitan tristearate, sorbitan tripalmeate or sorbitan triricinoleate is used as the sorbitan triester. 7. Process for the production of carbon black granules as claimed in claim 4, wherein the granulation is performed in a bead machine, ring-layer mix- pelletizer or bead drum. Carbon black granules, characterised in that they contain a sorbitan triester.

Documents:

666-KOL-2004-(01-10-2012)-CORRESPONDENCE.pdf

666-KOL-2004-(03-01-2013)-FORM-27.pdf

666-KOL-2004-ASSIGNMENT.pdf

666-KOL-2004-CERTIFIED COPIES(OTHER COUNTRIES).pdf

666-KOL-2004-CORRESPONDENCE.pdf

666-KOL-2004-FORM 16.pdf

666-KOL-2004-FORM 27.pdf

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666-kol-2004-granted-abstract.pdf

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666-kol-2004-granted-correspondence.pdf

666-kol-2004-granted-description (complete).pdf

666-kol-2004-granted-examination report.pdf

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666-KOL-2004-OTHER PATENT DOCUMENTS.pdf

666-KOL-2004-PA-1.1.pdf

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666-KOL-2004-PRIORITY DOCUMENT 1.1.pdf