Carbon black, methods for its production and its use

Abstract

Soot, characterized by the fact that the CTAB surface area is 100 - 160 m² 2 / g, the quartile ratio is 1.80-2.30 and the FP index is > 0, and that the ratio of the ΔD-50 value to the mode of the aggregate size distribution (ΔD-50 / mode) is greater than or equal to 1.10.

Description

[0001] The invention relates to a soot and its use.

[0002] Carbon blacks are commonly used as pigments, fillers, reinforcing fillers, and for a variety of other applications. For example, carbon blacks are used as reinforcing fillers in rubber compounds that can serve as the base material for vehicle tire treads.

[0003] It is well known that the specific surface area of ​​carbon black has a significant influence on its reinforcing properties in rubber compounds. The higher the specific surface area, the better the reinforcing properties and, in particular, the abrasion resistance of tire treads [G. Kraus, Applied Macromolecular Chemistry, Volume 60 / 61 (1977), page 215]. However, a high specific surface area has the disadvantage of high hysteresis in the rubber compound, resulting in increased rolling resistance of the tire treads [WM Hess et al., Rubber Chemistry and Technology, Volume 56, page 390]. Higher rolling resistance of tire treads leads to higher fuel consumption and thus higher energy consumption and carbon dioxide emissions. This is undesirable from both an economic and environmental perspective.

[0004] From an economic and ecological perspective, it is therefore desirable to further reduce the hysteresis of rubber compounds and thus the rolling resistance of tire treads for a given specific surface area. It is known that this can be achieved for a given specific surface area by broadening the aggregate size distribution [WM Hess et al., Rubber Chemistry and Technology, Volume 56, page 390]. However, broadening the aggregate size distribution also reduces the tint strength of the carbon black [CJ Stacy et al., Rubber Chemistry and Technology, Volume 48, page 538]. Furthermore, it is known that a broadened aggregate size distribution of carbon black, especially under high stress, leads to a reduction in the abrasion behavior of rubber compounds and thus to a reduction in the abrasion behavior of tire treads [WM Hess et al., Rubber Chemistry and Technology, Volume 56, page 390].A broadening of the aggregate size distribution is therefore favorable for rolling resistance, but is usually coupled with a deterioration in abrasion behavior.

[0005] From US 2005 / 0256249, a carbon material is known with a ΔD50 / M greater than 0.9 and a heterogeneity index greater than 2.3.

[0006] Furnace carbon blacks are known from EP 0754735 and DE 195 21 565 A1. When incorporated into SSBR / BR rubber compounds, these carbon blacks exhibit lower rolling resistance while maintaining the same or better wet slip resistance compared to similar carbon blacks with the same CTAB surface area. They can be produced in conventional carbon black reactors by controlling the combustion process in the combustion chamber to form carbon black nuclei that are brought into direct contact with the carbon black feedstock.

[0007] A disadvantage of the carbon blacks known from EP 0754735 and DE 195 21 565 A1 is their low abrasion resistance combined with low rolling resistance (loss factor tan δ) in rubber compounds.

[0008] From EP 0949303 and DE 198 39 925 A1, carbon blacks are known which, compared to the carbon blacks from EP 0754735, exhibit a particle size distribution with a lower proportion of large-diameter particles. This leads to improved abrasion resistance of rubber compounds. The carbon black reactors are operated in such a way that carbon black nuclei are formed, which are brought into direct contact with the carbon black feedstock, and the supply of combustion air and carbon black feedstock is increased accordingly.

[0009] The disadvantage of the carbon blacks known from EP 0949303 and DE 198 39 925 A1 is the reduced color strength and the improved abrasion resistance compared to the carbon blacks from EP 0754735 and DE 195 21 565 A1, while maintaining low rolling resistance (loss factor tan δ), but not an optimal balance between abrasion resistance and rolling resistance.

[0010] From EP 1783178, a furnace carbon black process is known in which a carbon black feedstock is supplied to a first stage and combined with a stream of hot gases to form a precursor, essentially consisting of carbon black in a reaction stream. Subsequently, further carbon black feedstock is supplied to this precursor to partially quench the reaction stream and then completely quench the entire reaction stream. The stream of hot gases in EP 1783178 can be generated as combustion gas from the reaction of a fuel with an oxidizing medium, for example, air, whereby the air-to-fuel ratio can be varied from 1:1 (stoichiometric) to infinity. The fuel can be solid, liquid, or gaseous.

[0011] US Patent No. 4,327,069 discloses another method for producing soot, using two reactors connected in series.

[0012] DE 691 04 191 T2 describes carbon blacks for use in rubber compositions, which have a CTAB of 120-160 m 2 / g, a specific N2 surface area of ​​125-180 m² 2 / g, a DBP absorption of 110-145 cm 3 / g, exhibiting a colour value / CTAB ratio of 0.8-1.10, a ΔD50 value of 70-100 nm and a ΔD50 / Dmode ratio of 0.80-1.05.

[0013] The object of the present invention is to provide a carbon black which has a good balance between high abrasion resistance (= low abrasion) and low rolling resistance in rubber compounds.

[0014] The invention relates to a carbon black as defined in independent claim 1. The carbon black is characterized, among other things, by the fact that the CTAB surface area is 100–160 m². 2 / g, preferably 100 - 149 m 2 / g, especially preferred 100 - 144 m 2 / g, especially preferred 105 - 140 m 2 / g, the quartile ratio is 1.80 - 2.30, preferably 1.85 - 2.25, and the FP index is > 0, preferably > 0.5, particularly preferably > 1.0, most preferably > 1.5.

[0015] The FP index is calculated according to the equation FP index = Tint strength - (65 + (1.057 g / m²) 2 ) * CTAB - (0.002745 g 2 / m 4 ) * CTAB * CTAB - (25.96 g / cm³) 3 ) * COAN - (0.201 g / m² 2 ) * (NSA - CTAB)) + 6.57502 - 847817 * EXP(-6.94397 * (quartile ratio)).

[0016] The CTAB value is measured according to ASTM D-3765-04.

[0017] The NSA value is measured according to ASTM D-6556-04, with the following parameters: relative pressures: section 10.4.4.

[0018] The COAN value is measured according to ASTM D-3493-06, with the following parameters: Oil: paraffin; method for end-point determination: procedure A.

[0019] The tint strength is measured according to ASTM D-3265-06, with the following parameters: Hoover Muller Paste Preparation, Erichsen tint tester - film drawdown method.

[0020] The quartile ratio is calculated from the aggregate size distribution.

[0021] The aggregate size distribution is determined according to the standard ISO 15825, first edition, 2004-11-01, with the following modifications applied: Addition to paragraph 4.6.3 of the ISO 15825 standard: The mode refers to the mass distribution curve.

[0022] Addition to paragraph 5.1 of the ISO 15825 standard: The BI-DCP Particle Sizer device and the associated evaluation software dcplw32, version 3.81, are used, all available from Brookhaven Instruments Corporation, 750 Blue Point Rd., Holtsville, NY, 11742.

[0023] Supplement to paragraph 5.2 of ISO 15825: The GM2200 ultrasonic control unit, the UW2200 transducer, and the DH13G sonotrode are used. The ultrasonic control unit, transducer, and sonotrode are available from Bandelin electronic GmbH & Co. KG, Heinrichstrasse 3-4, D-12207 Berlin, Germany. The following values ​​are set on the ultrasonic control unit: Power % = 50, Cycle = 8. This corresponds to a nominal power setting of 100 watts and a pulse setting of 80%.

[0024] Supplement to paragraph 5.2.1 of the standard ISO 15825: The ultrasound time is set at 4.5 minutes.

[0025] Contrary to the definition given in paragraph 6.3 of the ISO 15825 standard, “surfactant” is defined as follows: “surfactant” is an anionic surfactant of the type Nonidet P 40 Substitute from Fluka, available from Sigma-Aldrich Chemie GmbH, Industriestrasse 25, CH-9471 Buchs SG, Switzerland.

[0026] Contrary to the definition of spin liquid given in paragraph 6.5 of ISO 15825, the spin liquid is defined as follows: To prepare the spin liquid, 0.25 g of surfactant Nonidet P 40 Substitutes from Fluka (paragraph 6.3) are made up to 1000 ml with demineralized water (paragraph 6.1). The pH of the solution is then adjusted to 9-10 with 0.1 mol / l NaOH solution. The spin liquid may be used for a maximum of one week after its preparation.

[0027] Contrary to the definition of dispersion fluid given in paragraph 6.6 of ISO 15825, dispersion fluid is defined as follows: To prepare dispersion fluid, 200 ml of ethanol (paragraph 6.2) and 0.5 g of surfactant Nonidet P 40 Substitute from Fluka (paragraph 6.3) are made up to 1000 ml with demineralized water (paragraph 6.1). The pH of the solution is then adjusted to 9-10 using 0.1 mol / l NaOH solution. The dispersion fluid may be used for a maximum of one week after its preparation.

[0028] Supplement to paragraph 7 of the ISO 15825 standard: Only beaded carbon black is used.

[0029] The instructions in paragraphs 8.1, 8.2, and 8.3 of ISO 15825 are summarized and replaced by the following instructions: The granulated carbon black is lightly crushed in an agate mortar. 20 mg of carbon black is then mixed with 20 ml of dispersion solution (paragraph 6.6) in a 30 ml crimp-top vial (diameter 28 mm, height 75 mm, wall thickness 1.0 mm) and treated with ultrasound (paragraph 5.2) in a cooling bath (16°C ± 1°C) for 4.5 minutes (paragraph 5.2.1), thus suspending it in the dispersion solution. After the ultrasound treatment, the sample is measured in a centrifuge within 5 minutes.

[0030] Supplement to paragraph 9 of standard ISO 15825: The value for the density of carbon black to be entered is 1.86 g / cm³. 3The temperature to be entered is determined according to paragraph 10.11. The "Aqueous" option is selected for the spinning fluid type. This results in a spin fluid density of 0.997 g / cc and a spin fluid viscosity of 0.917 cP. Light scattering correction is performed using the options selectable in the dcplw 32 software: File = carbon.prm; Mie correction.

[0031] Supplement to paragraph 10.1 of the standard ISO 15825: The centrifuge speed is set at 11000 rpm.

[0032] Supplement to paragraph 10.2 of the ISO 15825 standard: Instead of 0.2 cm 3 Ethanol (paragraph 6.2) will be 0.85 cm 3 Ethanol (paragraph 6.2) is injected.

[0033] Supplement to paragraph 10.3 of the ISO 15825 standard: Exactly 15 cm 3 Spin fluid (paragraph 6.5) is injected. Then 0.15 cm 3 Ethanol (paragraph 6.2) is injected.

[0034] The instruction in paragraph 10.4 of the ISO 15825 standard is completely omitted.

[0035] Supplement to paragraph 10.7 of the ISO 15825 standard: Immediately after the start of data recording, the spin liquid in the centrifuge is overlaid with 0.1 cm. 3 Dodecane (paragraph 6.4).

[0036] Supplement to paragraph 10.10 of ISO 15825: If the measurement curve does not return to the baseline within one hour, the measurement is terminated after exactly one hour. A change in centrifuge speed does not restart the measurement.

[0037] Supplement to paragraph 10.11 of ISO 15825: Instead of the method described in the instruction for determining the measurement temperature, the measurement temperature T, which is to be entered into the computer program, is determined as follows: T=2 / 3(Te−Ta)+Ta, where Ta denotes the temperature of the measuring chamber before measurement and Te the temperature of the measuring chamber after measurement. The temperature difference should not exceed 4°C.

[0038] The fraction of particles > 150 nm of the aggregate size distribution can be less than 20 wt.%, preferably less than 14 wt.%, particularly preferably less than 10 wt.%.

[0039] The fraction > 150 nm denotes the weight fraction of the aggregates that have a Stokes diameter greater than 150 nm and is also obtained from the aggregate size distribution according to the ISO 15825 standard described above.

[0040] The ratio of the ΔD-50 value to the mode is greater than or equal to 1.10 for the carbon black according to the invention.

[0041] The ΔD-50 value and the mode are also obtained from the aggregate size distribution according to the ISO 15825 standard described above.

[0042] The tint strength can be greater than 110, preferably greater than 114, especially greater than 117, and most especially greater than 120.

[0043] The COAN value can be 90 - 130 cm 3 / 100g.

[0044] The soot can be gas, channel, flame or furnace soot.

[0045] The carbon black according to the invention cannot be surface-modified or post-treated.

[0046] The pH value of the soot according to the invention can be > 5.

[0047] Also described herein is a method for producing the carbon black according to the invention in a furnace carbon black reactor, which contains a combustion zone, a reaction zone and a termination zone along the reactor axis, by generating a stream of hot exhaust gas in the combustion zone by burning a fuel in an oxygen-containing gas and directing the exhaust gas from the combustion zone through the reaction zone into the termination zone, mixing a carbon black raw material into the hot exhaust gas in the reaction zone and stopping the carbon black formation in the termination zone by spraying water, which is characterized in that 60-90 wt.%, preferably 75-85 wt.%, of the carbon black raw material is injected in the first third of the reaction zone and the remaining amount of the carbon black raw material is injected upstream at at least one further point into the reactor and the fuel is guided in such a way that upon first impact on the carbon black raw material 90-100 wt.%, preferably 99-100 wt.%, is released.-% of the fuel has evaporated and 5 ms before impacting the soot raw material 80 - 99 wt.%, preferably 90 - 99 wt.%, particularly preferably 92 - 98 wt.% of the fuel has evaporated.

[0048] Both pure pressure atomizers (single-component atomizers) and dual-component atomizers with internal or external mixing can be used as fuel atomizers. The fuel guidance according to the invention can be achieved with both pure pressure atomizers (single-component atomizers) and dual-component atomizers with internal or external mixing by selecting the conditions such that the droplet size achieved during atomization, the residence time of these droplets until they impact the carbon black feedstock, and the reaction temperatures are coordinated. In particular, by using dual-component atomizers and liquid fuel, the droplet size can be controlled over a wide range independently of the throughput and thus coordinated with the residence time of the fuel until it impacts the carbon black feedstock and the reaction temperatures.

[0049] The droplet size distribution can be determined using optical methods. Several commercial nozzle manufacturers offer these measurements as a service, for example, Düsen-Schlick GmbH, Hutstraße 4, D-96253 Untersiemau / Coburg, Germany (www.duesen-schlick.de). The droplet residence time and the reaction temperatures in the process can be determined using computer-aided fluid mechanics simulations. For example, the commercial software "Fluent," version 6.3, from Fluent (Fluent Deutschland GmbH, Birkenweg 14a, 64295 Darmstadt, Germany) allows users to model the furnace reactor and, after inputting all supplied process flows, including the measured droplet size distribution, calculate the residence times and evaporation rates of the fuel droplets and the reaction temperatures using the integrated chemical models.

[0050] The fuel can be liquid or partly liquid and partly gaseous.

[0051] The carbon black raw materials can be injected using radial lances. Two to threeteen, preferably four to sixteen, and particularly preferably four to eight radial lances can be used.

[0052] The carbon black raw material can be liquid or gaseous, or partly liquid and partly gaseous.

[0053] The liquid carbon black raw material can be atomized by pressure, steam, compressed air or the gaseous carbon black raw material.

[0054] Liquid carbon black feedstock can be liquid aliphatic or aromatic, saturated or unsaturated hydrocarbons or mixtures thereof, distillates from coal tar or residual oils produced during the catalytic cracking of petroleum fractions or during olefin production by cracking naphtha or gas oil.

[0055] Gaseous aliphatic saturated or unsaturated hydrocarbons, mixtures thereof, or natural gas can be used as the gaseous raw material for soot.

[0056] The so-called K-factor is frequently used as a measure to characterize excess air. The K-factor is the ratio of the amount of air required for stoichiometric combustion of the fuel to the amount of air actually supplied to the combustion process. A K-factor of 1 therefore indicates stoichiometric combustion. With excess air, the K-factor is less than 1. As with conventional carbon blacks, K-factors between 0.2 and 0.9 can be used. Preferably, K-factors between 0.6 and 0.8 are employed.

[0057] The described method is not limited to a specific reactor geometry. Rather, it can be adapted to various reactor types and sizes.

[0058] Both pure pressure atomizers (single-component atomizers) and two-component atomizers with internal or external mixing can be used as carbon black raw material atomizers, whereby the gaseous carbon black raw material can be used as the atomizing medium.

[0059] Two-component atomizers can be used for atomizing liquid carbon black feedstock. While a change in throughput can also lead to a change in droplet size in single-component atomizers, the droplet size in two-component atomizers can be influenced largely independently of the throughput.

[0060] When using soot oil and gaseous hydrocarbons, such as methane, as soot feedstock, the gaseous hydrocarbons can be injected separately from the soot oil into the stream of hot exhaust gas via a separate set of gas lances.

[0061] The carbon blacks according to the invention can be used as fillers, enhancer fillers, UV stabilizers, conductivity carbon blacks, or pigments. The carbon blacks according to the invention can be used in rubber, plastics, printing inks, inks, inkjet inks, toners, varnishes, paints, paper, bitumen, concrete, and other building materials. The carbon blacks according to the invention can be used as reducing agents in metallurgy.

[0062] The carbon black according to the invention can be used as a reinforcing carbon black in rubber compounds.

[0063] Also described herein are rubber mixtures characterized in that they contain at least one rubber, preferably at least one diene rubber, particularly preferably at least natural rubber, and at least one carbon black according to the invention.

[0064] The carbon black according to the invention can be used in quantities of 10 to 150 phr (parts per hundred rubber), preferably 20 to 100 phr, particularly preferably 30 to 90 phr, and most preferably 30 to 80 phr, based on the amount of rubber used.

[0065] The rubber compound may contain silica, preferably precipitated silica. The rubber compound may contain organosilanes, for example bis(triethoxysilylpropyl)polysulfide or (mercaptoorganyl)alkoxysilanes.

[0066] The rubber compound may contain rubber additives.

[0067] In addition to natural rubber, synthetic rubbers are also suitable for the production of rubber compounds. Preferred synthetic rubbers are described, for example, in W. Hofmann, Kautschuktechnologie (Rubber Technology), Genter Verlag, Stuttgart 1980. These include, among others... - Polybutadiene (BR), - Polyisoprene (IR), - Styrene / butadiene copolymers, for example emulsion SBR (E-SBR) or solution SBR (L-SBR), preferably with a styrene content of 1 to 60 wt.%, particularly preferably 2 to 50 wt.%, based on the total polymer, - Chloroprene (CR), - Isobutylene / isoprene copolymers (IIR), - Butadiene / acrylonitrile copolymers, preferably with an acrylonitrile content of 5 to 60 wt.%, preferably 10 to 50 wt.%, based on the total polymer (NBR), - partially or fully hydrogenated NBR rubber (HNBR), - Ethylene / propylene / diene copolymers (EPDM) - Ethylene / propylene copolymers (EPM) or - the above-mentioned rubbers which additionally possess functional groups, such as carboxy, silanol or epoxy groups, for example epoxidized NR, carboxy-functionalized NBR or silanol- (-SiOH) or siloxy-functionalized (-Si-OR) SBR, as well as mixtures of these rubbers.

[0068] Natural rubber and its mixture with diene rubbers can be used in particular for the production of truck tire treads.

[0069] SBR rubber and its mixture with other diene rubbers can be used in particular for the production of car tire treads.

[0070] The rubber compounds may contain other rubber additives such as reaction accelerators, anti-aging agents, heat stabilizers, light stabilizers, ozone stabilizers, processing aids, plasticizers, tackifiers, blowing agents, dyes, pigments, waxes, extenders, organic acids, retarders, metal oxides, and activators such as diphenylguanidine, triethanolamine, polyethylene glycol, alkoxy-terminated polyethylene glycol, or hexanetriol, which are known to the rubber industry.

[0071] Rubber additives can be used in typical quantities, which depend, among other things, on the intended use. Typical quantities can range, for example, from 0.1 to 50 phr based on rubber.

[0072] Sulfur, organic sulfur donors, or radical initiators can serve as crosslinking agents. The rubber compounds according to the invention can also contain vulcanization accelerators.

[0073] Examples of suitable vulcanization accelerators include mercaptobenzthiazoles, sulfenamides, guanidines, thiurams, dithiocarbamates, thioureas and thiocarbonates.

[0074] The vulcanization accelerators and crosslinkers can be used in amounts of 0.1 to 10 phr, preferably 0.1 to 5 phr, based on rubber.

[0075] The mixing of the rubbers with the filler, optionally rubber additives, and optionally the organosilanes can be carried out in conventional mixing units such as rollers, internal mixers, and mixing extruders. Typically, such rubber mixtures can be produced in an internal mixer, whereby the rubbers, the carbon black according to the invention, optionally the silica, and optionally the organosilanes and the rubber additives are first mixed in one or more successive thermomechanical mixing stages at 100 to 170°C. The sequence and timing of the addition of the individual components can have a decisive influence on the resulting mixture properties.The rubber mixture thus obtained can then usually be mixed with the crosslinking chemicals in an internal mixer or on a roller at 40-130°C, preferably 50-120°C, and processed into the so-called raw mixture for the subsequent process steps, such as shaping and vulcanization.

[0076] The vulcanization of the rubber compounds according to the invention can be carried out at temperatures of 80 to 200°C, preferably 130 to 180°C, optionally under pressure of 10 to 200 bar.

[0077] The rubber compounds are suitable for the production of molded parts, for example for the production of pneumatic tires, tire treads, cable sheaths, hoses, drive belts, conveyor belts, roller coverings, tires, shoe soles, sealing rings, profiles and damping elements.

[0078] The carbon black according to the invention has the advantage of good abrasion resistance combined with good rolling resistance in rubber compounds. Examples Example 1 (soot production):

[0079] A number of carbon blacks according to the invention are used in the Fig. 1. Soot reactor shown.

[0080] Fig. Figure 1 shows a longitudinal section through the furnace reactor. The soot reactor has a combustion chamber 5 in which the hot process gas for the pyrolysis of the soot oil is generated by burning fuel with the supply of excess atmospheric oxygen. Soot oil is used as fuel for the production of the soots according to the invention. Natural gas is used as fuel for the production of the reference soot.

[0081] Combustion air is supplied through several openings 2, which are distributed concentrically around the circular end wall of the combustion chamber. The fuel is introduced into the combustion chamber via the axial burner lance 1. The burner lance can be moved axially to optimize the process according to the invention. The combustion chamber tapers conically towards the constriction 6. The carbon black feedstock is injected into or in front of the constriction via radial lances 3. After passing through the constriction, the reaction gas mixture expands into the reaction chamber 7.

[0082] A, B, and C designate different positions for injecting the carbon black oil into the hot process gas using oil lances 3. The oil lances are equipped with suitable spray nozzles at their heads. At least four injectors are distributed around the circumference of the reactor at each injection position.

[0083] Water is sprayed into the demolition zone using the quench water lance 4.

[0084] The combustion zone, reaction zone, and ablation zone are in Fig. 1. Designated by the Roman numerals I to III. Their exact axial extent depends on the respective positioning of the burner lance, the oil lances, and the quench water lance.

[0085] The dimensions of the reactor used can be found in the following table: Largest diameter of the combustion chamber: 930 mm Length of combustion chamber to narrowing: 1660 mm Length of the conical part of the combustion chamber: 1300 mm Diameter of the constriction: 114 mm Length of the bottleneck: 80 mm Diameter of the reaction chamber: 240 mm Position of the oil lances 1) A 40 mm B - 215 mm C - 500 mm Maximum position of the quench water lance(s) 1) 8250 mm 1) measured from the point of entry into the narrow passage (+: after entry -: before entry)

[0086] For the production of the carbon blacks according to the invention, a carbon black oil with a carbon content of 92 wt.% and a hydrogen content of 6 wt.% is used as fuel and raw material. For the production of the reference carbon black, natural gas is used as fuel and a carbon black oil with a carbon content of 92 wt.% and a hydrogen content of 6 wt.% is used as raw material.

[0087] The reactor parameters for the production of the carbon blacks according to the invention are listed in Table 1. Five different carbon blacks are produced (carbon blacks 1 to 4 according to the invention and comparison carbon black 5). The production conditions differ, in particular, with regard to the amount of carbon black raw material injected into or upstream of the constriction.

[0088] The carbon blacks produced are wet-beaded using standard procedures before characterization and incorporation into the rubber compounds. Table 1: Reactor parameters Unit Soot1 Soot2 Soot3 Soot4 Comparison soot 5 combustion air Nm 3 / h 2800 2800 2601 2803 3301 Temperature of the combustion air °C 620 620 620 620 620 Fuel (soot oil) kg / h 199 201 220 202 0 Fuel (natural gas) Nm 3 / h 0 00 0 0 238 atomizing air Nm 3 / h 190 190 190 190 0 Carbon black raw material Item A kg / h 600 610 454 455 0 Carbon black raw material Item B kg / h 140 140 115 105 570 Carbon black raw material Item C kg / h 0 0 0 0 0 Soot oil temperature °C 117 119 120 118 120 Additive (K2CO3) g / h 7 36 18 65 239 Quench position mm 1095 1960 1960 1095 1095 Vaporized fuel 5 ms before first impact on the soot feedstock % by weight 98 98 92 98 100 Vaporized fuel upon contact with the soot raw material % by weight 100 100 100 100 100 1) Measured from the beginning of the bottleneck

[0089] The proportion of evaporated fuel 5 ms before the first impact on the soot raw material and the proportion of evaporated fuel upon impact on the soot raw material are calculated using the program "Fluent", version 6.3, by computer-aided fluid mechanics simulation calculation.

[0090] The soot analytical characteristics of the produced soots are listed in Table 2: Table 2: Analytical Key data soot Group 1 Comparison soot 1 N 121 Comparison soot 2 Ecorax 1720 Soot 1 Group 2 Comparison soot 3 N 220 Soot 2 Group 3 Comparison soot 4 N 134 Soot 3 Group 4 Comparison soot 5 Soot 4 Analytical Data CTAB m 2 / g 119,1 117,1 120,9 110,0 111,6 129,3 134,5 146,7 152,4 COAN cm 3 / 100g 111,9 109,6 118,5 102,5 102,1 101,8 112,7 109,3 100,8 NSA m 2 / g 118,3 125,8 122,7 113,3 110,1 134,9 144,0 145,3 158,3 Quartile Ratio 1,60 2,01 1,91 1,49 1,98 1,55 1,95 1,59 2,19 Tint strength 120,7 107,6 121,5 122,5 120,8 131,9 129,4 136,3 130,4 FP Index -8,47 -7,49 5,06 -18,93 3,90 -7,69 8,52 -3,61 1,79 Fraction >150nm % 1,1 14,7 8,1 0,4 9,9 1,3 5,7 0,1 5,6 fashion nm 73 68 58 74 57 64 54 60 43 ΔD-50 nm 61 76 66 54 68 50 72 53 68 ΔD-50 / mode 0,84 1,12 1,14 0,73 1,19 0,78 1,33 0,88 1,58

[0091] The comparison carbon black 1 is Corax. ® N 121 from Evonik Degussa GmbH. The comparison carbon black 2 is Ecorax. ® 1720 from Evonik Degussa GmbH. Reference carbon black 2 is produced according to the process described in EP 0949303. Reference carbon black 3 is Corax. ® N 220 from Evonik Degussa GmbH. The comparison carbon black 4 is Corax. ® N 134 from Evonik Degussa GmbH. Example 2 (Rubber technology investigations in natural rubber):

[0092] The formulation used for the natural rubber compounds is given in Table 3 below. The unit phr represents parts by weight, based on 100 parts of the raw rubber used.

[0093] The general process for the production of rubber compounds and their vulcanizates is described in the book: “Rubber Technology Handbook”, W. Hofmann, Hanser Verlag 1994. Table 3: phr Level 1 SMR 10 ML4=60-70 100,0 soot 52,0 Stearic acid 3,0 ZnO 3,0 Vulkanox ® 4020 1,0 Vulkanox ® HS 1,0 Protector ® G3108 1,0 Level 2 Batch level sulfur 1,5 Rhenogran ® TBBS-80 1,2

[0094] The natural rubber SMR10 ML4 = 60-70 is SMR10 that is masticated on a rolling mill according to standard procedures before the mixing process and then stored at room temperature for at least 24 hours, but no more than one week. The ML1+4 (100°C) value of the masticated SMR10 is in the range of 60-70. The ML1+4 value is measured according to DIN 53523 / 3.

[0095] At Vulkanox ® 4020 refers to the antioxidant 6PPD from Lanxess AG. Vulkanox ® HS refers to the TMQ antioxidant from Lanxess AG. Protector ® G3108 is an ozone protection wax from Paramelt BV. ®TBBS-80 is a TBBS-type vulcanization accelerator containing 80% active ingredient, from Rhein-Chemie GmbH.

[0096] The rubber compounds are produced in an internal mixer according to the mixing instructions in Table 4. Table 4 Level 1 Settings Mixing unit Werner and Pfleiderer GK 1.5N speed 65 rpm Stamp print 5.5 bar Empty volume 1,6 I Fill level 0,70 Flow temperature 70 °C Mixing process 0 to 1 minute natural rubber 1 to 2 minutes 1 / 2 soot 2 to 5 minutes 1 / 2 Soot, stearic acid, ZnO, Vulkanox, protector 5 min clean 5 to 6 minutes mix and drive Batch temperature 145 - 155°C storage 24 hours at room temperature Level 2 Mixing unit settings Werner and Pfleiderer GK 1.5N speed 40 rpm Stamp print 5.5 bar Empty volume 1,6 I Fill level 0,68 Flow temperature 60 °C Mixing process: 0 to 2 minutes Batch Stage 1, Sulfur, TBBS-80 Batch temperature 100 - 110°C 2 min Extend and form skin on laboratory mixing roller mill Troester WNU 1 (diameter 150 mm, length 350 mm, flow temperature 40 / 50°C, RPM 17 / 21). Homogenize: Cut 3 times on the left, 3 times on the right and fold over, and invert 3 times with a wide roller gap (6 mm) and 3 times with a narrow roller gap (3 mm). Pull the skin out. Batch temperature < 110°C

[0097] Table 5 lists the methods for rubber testing. Table 5 Physical testing / conditions standard Tensile test on ring 1, 23°C DIN 53504, ISO 37 Tensile strength (MPa) Stress value at 100% elongation (MPa) Stress value at 300% elongation (MPa) Elongation at break (%) Goodrich flexometer test, 0.175 inch stroke, 2 h, 23 °C piercing temperature (°C) DIN 53533, ASTM D 623 A Shore hardness, 23°C Shore A DIN 53505 DIN abrasion, 10 N, 23 °C abrasion (mm*mm*mm) DIN 53 516

[0098] Table 6 shows the results of the rubber testing. The vulcanization time of the compounds is 17 minutes. Table 6 natural rubber compound Group 1 Group 2 Group 3 Group 4 Soot (52 phr) Mixture 1V comparison- ruß 1 Mixture 2 Comparison ruß 2 Mixture 3 Soot 1 Mixture 4 Comparison ruß 3 Mixture 5 Soot 2 Mixture 6 Comparison ruß 4 Mixture 7 Soot 3 8V mixture comparison- ruß 5 Mixture 9 Soot 4 Rubber technical data vulcanization time min 17 17 17 17 17 17 17 17 17 Tensile elongation properties Tensile strength MPa 23,6 21,8 21,6 23,8 23,6 25,6 24,0 25,7 24,7 Voltage value 100% MPa 2,7 2,4 2,8 2,3 2,4 2,3 2,4 2,6 2,4 Voltage value 300% MPa 15,0 13,6 15,5 12,3 13,6 12,9 13,2 14,0 12,6 Elongation at break % 440 430 390 490 460 510 480 480 490 Shore hardness Shore A 69 66 69 67 66 67 68 70 68 DIN abrasion mm 3 80 87 79 102 99 96 93 97 96 Abrasion resistance index 100 92 101 100 103 100 103 100 101 Viscoelastic Characteristics Goodrich Flexometer - Penetration Temperature °C 106 92 93 104 86 105 100 117 99 Rolling resistance index 100 115 114 100 121 100 105 100 118

[0099] The higher the value for DIN abrasion (mm) 3 The lower the carbon black content, the worse the abrasion resistance of the rubber compound. The abrasion resistance index is therefore calculated for each carbon black within the respective carbon black group as follows: Abrasion resistance index = (DIN abrasion of the reference carbon black in the group / DIN abrasion) * 100.

[0100] The reference soot in group 1 is comparison soot 1, the reference soot in group 2 is comparison soot 3, the reference soot in group 3 is comparison soot 4 and the reference soot in group 4 is comparison soot 5.

[0101] An abrasion resistance index > 100 therefore means improved abrasion resistance, values ​​< 100 mean worsened abrasion resistance, relative to the respective reference carbon black in the group.

[0102] The higher the value for the insertion temperature (°C), the greater the heat generation and thus the hysteresis under dynamic stress in the rubber compound, and consequently the worse the expected rolling resistance. The rolling resistance index is therefore calculated for each carbon black within the respective carbon black group as follows: Rolling resistance index = (Penetration temperature of the reference soot in the group / Penetration temperature) * 100.

[0103] A rolling resistance index > 100 therefore means improved and thus reduced rolling resistance, values ​​< 100 mean worsened rolling resistance, relative to the respective reference soot in the group.

[0104] The results in Table 6 show that the carbon blacks according to the invention with an FP index > 0 each exhibit a better balance with regard to abrasion resistance and rolling resistance than the comparison carbon blacks with an FP index < 0, with a balanced general rubber-technical value profile. Example 3 (Rubber technology investigations in E-SBR):

[0105] The formulation used for the E-SBR mixtures is given in Table 7 below. Table 7: phr Level 1 Krynol ® E-SBR 1712 137,5 soot 80,0 Stearic acid 2,0 ZnO 3,0 Vulkanox ® 4020 1,5 Protector ® G3108 1,0 Level 2 Batch Stage 1 Level 3 Batch Stage 2 sulfur 1,75 Vulkacit ® CZ / EG-C 1,50 Percazite TBZTD-PDR-D 0,20

[0106] In the case of the E-SBR Krynol ® 1712 is an E-SBR rubber from Lanxess AG, extended with 37.5 phr of oil.

[0107] The vulcanization accelerator Vulkacite ®CZ / EG-C is CBS from Lanxess AG. The vulcanization accelerator Perkacit TBZTD-PDR-D is TBZTD from Flexsys NV.

[0108] The rubber compounds are produced in an internal mixer according to the mixing instructions in Table 8. Table 8 Level 1 Settings Mixing unit Werner and Pfleiderer GK 1.5N speed 60 rpm Stamp print 5.5 bar Empty volume 1,6 I Fill level 0,70 Flow temperature 60 °C Mixing process 0 to 1 minute rubber 1 to 3 minutes 1 / 2 soot 3 to 4 minutes 1 / 2 carbon black, Vulkanox, protector, ZnO, stearic acid 4 min clean 4 to 5 minutes mix and drive Batch temperature 145 - 155 °C storage 24 hours at room temperature Level 2 Settings Mixing unit Werner and Pfleiderer GK 1.5N speed 70 rpm Stamp print 5.5 bar Empty volume 1,6 I Fill level 0,68 Flow temperature 80 °C Mixing process 0 to 2 minutes Batch Stage 1 2 to 5 minutes Batch temperature maintained at 150 °C by varying the rotational speed 5 min exit Batch temperature 145 - 155 °C storage 24 hours at room temperature Level 3 Mixing unit settings Werner and Pfleiderer GK 1.5N speed 30 rpm Stamp print 5.5 bar Empty volume 1,6 I Fill level 0,66 Flow temperature 40 °C Mixing process: 0 to 2 minutes Batch Stage 2, Volcacite, Percacite, Sulfur Batch temperature < 110°C 2 min Extend and form skin on laboratory mixing roller mill Troester WNU 1 (diameter 150 mm, length 350 mm, flow temperature 40 / 50°C, RPM 17 / 21). Homogenize: 3* cut on the left, 3* on the right and fold over, and 10* with wide roller gap (6 mm) pull out skin. Batch temperature < 110°C

[0109] Table 9 shows the results of the rubber testing. The vulcanization time of the compounds is 13 minutes. Table 9 E-SBR mixture Group 5 Group 8 Group 7 Group 8 Soot (80 phr) Mixture 10 Comparison ruß 1 Mixture 11 Comparison ruß 2 Mixture 12 Soot 1 Mixture 13 Comparison ruß 3 Mixture 14 Soot 2 Mixture 15 Comparison ruß 4 Mixture 16 Soot 3 Mixture 17 Comparison ruß 5 Mixture 18 Soot 4 Rubber technical data vulcanization time min 13 13 13 13 13 13 13 13 13 Tensile elongation properties ring Tensile strength MPa 18,8 19,6 19,8 16,9 18,0 17,9 19,4 18,5 20,5 Voltage value 100% MPa 2,3 2,0 2,1 1,8 2,0 1,9 2,0 2,1 1,8 Voltage value 300% MPa 12,3 11,6 11,7 9,6 10,8 10,0 10,3 10,4 9,0 Elongation at break % 410 450 440 450 440 440 480 450 520 Shore hardness Shore A 70 66 69 67 67 68 69 72 68 DIN abrasion mm 3 68 70 66 74 75 81 77 104 101 Abrasion resistance index 100 97 103 100 99 100 105 100 103 Viscoelastic Characteristics Goodrich Flexometer - Penetration Temperature °C 148 127 127 142 124 143 143 161 138 Rolling resistance index 100 117 117 100 115 100 100 100 117

[0110] The reference soot in group 5 is comparison soot 1, the reference soot in group 6 is comparison soot 3, the reference soot in group 7 is comparison soot 4 and the reference soot in group 8 is comparison soot 5.

[0111] The results in Table 9 show that the carbon blacks according to the invention with an FP index > 0 each exhibit a better balance with regard to abrasion resistance and rolling resistance than the comparison carbon blacks with an FP index < 0, with a balanced general rubber-technical value profile.

Claims

[1] soot, characterized by that the CTAB surface area is 100 - 160 m² 2 / g, the quartile ratio is 1.80-2.30 and the FP index is > 0, and that the ratio of the ΔD-50 value to the mode of the aggregate size distribution (ΔD-50 / mode) is greater than or equal to 1.

10. [2] Soot according to claim 1, characterized by that the FP index is > 0.

5. [3] Carbon black according to claim 1, characterized by , that the fraction of particles > 150 nm of the aggregate size distribution is less than 20 wt.%. [4] Use of the carbon black according to claim 1 as a filler, enhancer filler, UV stabilizer, conductivity carbon black or pigment. [5] Use of the carbon black according to claim 1 as a reinforcing carbon black in rubber compounds.

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