High-structure acetylene black, its manufacturing method, and its composition and use

Abstract

Oil absorption capacity (OAN) of 360 mL / 100 g or more, and 50 to 200 2 The present invention provides a high-structure acetylene black having a BET surface area of ​​1000 nm / g. Such high-structure carbon black exhibits excellent electrical conductivity and good processing properties, such as dispersibility, and has excellent ability to impart electrical and / or thermal conductivity to various materials, making it particularly useful in all kinds of applications where high electrical and / or thermal conductivity is desired or beneficial, such as electrodes and other components of energy storage and / or conversion devices, or in the manufacture of electrically and / or thermally conductive materials and articles made therefrom.

Description

[Technical Field]

[0001] The present invention relates to novel, highly structured acetylene blacks, their production, compositions comprising acetylene black, and articles produced therefrom, as well as uses and applications of acetylene black, for example, for the production of electrodes or other components of energy storage or conversion devices or in rubber or plastic articles. [Background technology]

[0002] Acetylene black is a specific type of carbon black. Acetylene black can generally be produced by the pyrolysis of acetylene gas or an acetylene-containing hydrocarbon feedstock, forming colloidal carbon black particles and hydrogen at high temperatures, as described, for example, in J.-B. Donnett et al., "Carbon Black: Science and Technology," 2nd Edition. Other production methods, such as those described in U.S. Patent Application Publication No. 4,013,759, are based on the incomplete combustion of the hydrocarbon feedstock. Acetylene black is generally very pure (carbon content typically exceeds 99% by weight) and exhibits good specific conductance. These characteristics make acetylene black particularly attractive compared to other types of carbon black, such as furnace black, for applications requiring high purity and good electrical or thermal conductivity. Thus, they are widely used, for example, in the manufacture of electrodes, batteries, fuel cells, capacitors, or heating elements, and to provide antistatic, heat-dissipating, or conductive properties to plastic or rubber materials and articles, such as tires and tire components such as bladders, cables, conveyor belts, rollers, hoses, floors, or shoes, or to provide electronic components, paints, ink coatings, and adhesives. However, the types of acetylene black available are limited. Furthermore, it can be difficult to incorporate them uniformly into materials such as plastic or rubber materials or liquid carrier media, for example, in the manufacture of plastic or rubber articles, or in the preparation of aqueous or solvent-based compositions for the manufacture of electrodes, coatings, paints, or inks. This can also adversely affect the achievable conductance of the resulting acetylene black-doped material.Thus, there is a continuing effort and need for acetylene black that exhibits improved conductance and good processing characteristics (e.g., dispersibility), which allows for achieving desired levels of material conductance at lower concentrations of, for example, acetylene black, thereby having excellent ability to impart electrical and / or thermal conductivity to a variety of materials, ideally without adversely affecting other properties of the acetylene black that are relevant to the intended application, and which can be achieved in a cost-effective manner using readily available raw materials and equipment.

[0003] It is therefore an object of the present invention to provide an acetylene black that overcomes or alleviates at least some of the above-mentioned deficiencies and limitations of the prior art. Specifically, it is an object of the present invention to provide an acetylene black that exhibits low conductance, can be efficiently incorporated into various materials, and can provide the desired conductance in relatively small amounts. Such acetylene black should be obtainable in an economical manner without adversely affecting other beneficial properties of acetylene black, such as high purity. Summary of the Invention

[0004] The above object has been achieved according to the present invention by providing a novel, high-structure acetylene black as defined in the attached independent claim 1.

[0005] The acetylene black of the present invention has an oil absorption (OAN) of 360 mL / 100 g or more and an OAN of 50 to 200 m 2 / g.

[0006] The present invention also relates to a method for producing acetylene black of the present invention. The method includes supplying a hydrocarbon feedstock containing acetylene to a reactor, supplying an oxygen-containing gas to the reactor, contacting the hydrocarbon feedstock containing acetylene with the oxygen-containing gas to incompletely combust the hydrocarbon feedstock containing acetylene, thereby forming acetylene black in the reactor, and recovering the formed acetylene black. The hydrocarbon feedstock containing acetylene and the oxygen-containing gas are introduced into the reactor so that the molar ratio of oxygen to acetylene is in the range of 0.30 to 0.80.

[0007] The present invention further relates to compositions comprising the inventive acetylene black materials disclosed herein, such as electrode compositions and rubber or plastic compositions.

[0008] The present invention also relates to articles made from the acetylene black or compositions of the present invention, in particular electrodes or other components of energy storage and / or conversion devices, and rubber or plastic articles. The present invention also relates to energy storage and / or conversion devices comprising electrodes or components made from the acetylene black or compositions of the present invention.

[0009] Furthermore, the present invention relates to the use of an acetylene black material as disclosed herein as an electrical conductor, antistatic agent, thermally conductive agent, reinforcing filler and / or colorant for the manufacture of electrodes and other components of energy storage and / or conversion devices (e.g., primary batteries, secondary batteries, fuel cells and capacitors); and / or for the manufacture of plastic articles made with a matrix of thermoplastic or thermoset polymer or rubber (e.g., tires or components thereof, wires, cables and their sheaths, belts, hoses, shoe soles, rollers, heaters, or bladders, e.g., tire bladders, thermally conductive materials, heat transfer materials); and / or in coatings, paints or inks.

[0010] The acetylene blacks according to the present invention exhibit extremely high intrinsic conductance and are highly potent for imparting electrical and / or thermal conductivity to various materials, making it possible, for example, to achieve desired levels of material conductance at relatively low concentrations of acetylene black. They can be efficiently incorporated into materials to provide compositions with good processability and application performance, including, for example, electrode compositions. The acetylene blacks according to the present invention further maintain or even enhance other beneficial properties of acetylene black, such as high purity, and can be obtained in an economical manner using readily available raw materials and equipment.

[0011] These and other optional features and advantages of the present invention are explained in more detail in the following description. [Brief explanation of the drawings]

[0012] [Figure 1] A reactor for producing the acetylene black of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0013] As used herein, the term "comprising" is to be understood as open-ended and as not excluding the presence of additional, undescribed or unlisted elements, materials, components, or method steps, etc. The terms "including," "containing," and similar terms are understood to be synonymous with "comprise." As used herein, the term "consisting of" is to be understood as excluding the presence of any unspecified elements, components, or method steps, etc.

[0014] As used herein, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise.

[0015] Unless otherwise noted, the numerical parameters and ranges set forth in the following specification and appended claims are approximations. Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values ​​set forth in the specific examples are reported as precisely as possible. Any numerical values, however, contain errors necessarily resulting from the standard deviation in their respective measurements.

[0016] It should also be understood that any numerical range recited herein is intended to encompass all subranges therein. For example, a range of "1 to 10" is intended to encompass any and all subranges between and including the recited minimum value of 1 and the recited maximum value of 10, i.e., all subranges beginning with a minimum value of 1 or greater and ending with a maximum value of 10 or less, for example, all subranges between 1 to 6.3, or 5.5 to 10, or 2.7 to 6.1.

[0017] All parts, amounts, concentrations, etc. referred to herein are by weight unless otherwise specified.

[0018] As described above, the acetylene black of the present invention has a medium BET surface area, i.e., 50 to 200 m 2 The acetylene black of the present invention is characterized by having a BET surface area of ​​50 m / g. 2 / g or more, e.g., 60m 2 / g or more, or 70m 2 / g or more, or 80m 2 / g or more, or 90m 2 / g or more, or 100m 2 / g or more, or 110m 2 / g or more, or 120m 2 / g or more, or 130m 2 The acetylene black of the present invention can have a BET surface area of ​​200 m / g or more. 2 / g or less, e.g., 190m 2 / g or less, or 180m 2 / g or less, or 170m 2 / g or less, or 160m2 / g or less, or 150m 2 / g or less, or 140m 2 The BET surface area of ​​the acetylene black of the present invention can range between any of the recited values, for example, 50 m / g or less. 2 / g~200m 2 / g, or 60m 2 / g~180m 2 / g, or 80m 2 / g~160m 2 / g. Preferably, the acetylene black of the present invention has a viscosity of 100 to 200 m 2 / g, more preferably 120 to 200m 2 / g, and even more preferably 130-180m 2 / g, and even more preferably 130-160m 2 / g. As used herein, "BET surface area," as used in the examples, refers to the BET surface area that can be measured by nitrogen adsorption according to ASTM D6556-19a.

[0019] As mentioned above, the acetylene black of the present invention is further characterized by having a high structure. In the field of carbon black materials, structure refers to the degree to which individual primary particles of carbon black fuse to form larger aggregates composed of multiple primary particles of carbon black. Oil absorption can serve as an indicator of structure. Thus, the acetylene black of the present invention has a high oil absorption (OAN), which indicates the high structure of the acetylene black. The acetylene black of the present invention has an OAN of 360 mL / 100 g or more. The acetylene black of the present invention can have, for example, an OAN of 370 mL / 100 g or more, e.g., 380 mL / 100 g or more, or 390 mL / 100 g or more, or 400 mL / 100 g or more, or 410 mL / 100 g or more. The acetylene black of the present invention can have an OAN of, for example, up to 600 mL / 100 g, e.g., 550 mL / 100 g or less, or 500 mL / 100 g or less, or 490 mL / 100 g or less, or 480 mL / 100 g or less, or 470 mL / 100 g or less, or 460 mL / 100 g or less, or 450 mL / 100 g or less. The OAN of the acetylene black can range between any of the recited values, e.g., 360 mL / 100 g to 600 mL / 100 g, or 380 mL / g to 500 mL / 100 g, or 410 mL / 100 g to 450 mL / 100 g. Preferably, the OAN is in the range of 380 to 500 mL / 100 g, more preferably 410 to 450 mL / 100 g. As used herein, "oil absorption number (OAN)," as used in the examples, refers to oil absorption that can be measured according to ASTM D2414-19.

[0020] As mentioned above, the acetylene black according to the present invention exhibits a very high specific conductance, can be efficiently incorporated into various materials, and is extremely powerful in imparting electrical and / or thermal conductivity. Without intending to be bound by any theory, it is believed that the properties of the acetylene black according to the present invention, such as its high structure and moderate specific surface area, may be particularly beneficial for the formation of conductive pathways and networks, and may promote interactions involving more or less polar components, such as aqueous or organic solvent-based carrier media, plastic materials, or electrolytes.

[0021] In addition to the structure and BET surface area described above, the acetylene black of the present invention may have one or more or all of the properties described below.

[0022] Thus, acetylene black according to the present invention can be characterized, for example, by its oil absorption number (COAN) of a pressed sample, as measured according to ASTM D3493-19a. The COAN can range, for example, from 30 percent or more (e.g., 40 percent or more) of the OAN value of the acetylene black to the OAN value. The acetylene black can have a COAN of, for example, 150 mL / 100 g or more, e.g., 170 mL / 100 g or more, or 180 mL / 100 g or more. The acetylene black can have a COAN of, for example, 300 mL / 100 g or less, e.g., 250 mL / 100 g or less, or 200 mL / 100 g or less. The COAN of the acetylene black can range between any of the listed values, for example, 150 mL / 100 g to 300 mL / 100 g, or 170 mL / 100 g to 250 mL / 100 g.

[0023] Furthermore, as mentioned above, acetylene black generally contains agglomerates of multiple smaller particles, referred to as "primary particles." Agglomerates can be, for example, collections of multiple primary acetylene black particles fused together at their contact points and unable to be easily separated. The size of the primary particles in acetylene black can vary. The average primary particle size of the acetylene black material can be measured by TEM image analysis in accordance with ASTM D3849-07. The acetylene black of the present invention can have an average primary particle size of, for example, 10 nm or more, e.g., 12 nm or more, or 14 nm or more, or 16 nm or more, or 18 nm or more. The average primary particle size of the acetylene black of the present invention can be, for example, 30 nm or less, e.g., 28 nm or less, or 26 nm or less, or 24 nm or less. The average primary particle size of the acetylene black of the present invention can range between any of the recited values, e.g., 10 nm to 30 nm, or 14 nm to 28 nm, or 16 nm to 24 nm.

[0024] The acetylene black of the present invention can contain aggregates that may have irregular or non-spherical shapes. The shape can be characterized, for example, by the aspect ratio, which is defined as the ratio of the smallest ferret diameter to the largest ferret diameter. The powdered acetylene black particles of the present invention can have an aspect ratio of, for example, less than 0.8, e.g., less than 0.6, less than 0.5, or less than 0.3. The aspect ratio can be measured by averaging over at least 50 particles from electron microscope images. The irregular or non-spherical shape of the particles can be beneficial in forming conductive pathways and networks.

[0025] Additionally or alternatively, the acetylene black according to the present invention can be characterized in terms of void volume. The void volume can be measured in accordance with ASTM D7854-18a as the compressed volume of a weighed sample of acetylene black in a cylindrical chamber as a function of the pressure applied by a moving piston. The measurement method is explained in more detail in the experimental section below. The void volume provides a means for assessing the structure of acetylene black at various concentrations and degrees of agglomerate reduction. Increased aggregate irregularity and non-sphericity cause resistance to compression and are thereby generally reflected by higher void volume values. The void volume is typically reported in terms of void volume values ​​obtained at a constant mean geometric pressure, such as 50 MPa, 75 MPa, or 125 MPa. For example, acetylene black according to the present invention has a void volume of 60 cm3 measured at a mean geometric pressure of 50 MPa. 3 / 100g or more, e.g. 70cm 3 / 100g or more or 75cm 3 / 100g or more or 80cm 3 The acetylene black according to the present invention may have a void volume of 120 cm3 / 100 g or more, measured at a mean geometric pressure of 50 MPa. 3 / 100g or less, e.g. 100cm 3 / 100g or less, or 90cm 3 The void volume (@50 MPa) can range between any of the recited values, e.g., 60 to 120 cm 3 / 100g or 75-100cm 3 Additionally or alternatively, the acetylene black according to the present invention has a viscosity of 50 cm / 100 g, measured at a mean geometric pressure of 75 MPa. 3 / 100g or more, e.g. 60cm 3 / 100g or more or 65cm 3 The acetylene black according to the present invention may have a void volume of 100 cm3 or more, measured at a mean geometric pressure of 75 MPa. 3 / 100g or less, e.g. 90cm 3 / 100g or less, or 80cm 3 The void volume (@75 MPa) can range between any of the recited values, e.g., 50 to 100 cm 3 / 100g or 65-80cm 3 Further, additionally or alternatively, the acetylene black according to the present invention has a viscosity of 40 cm / 100 g, measured at a mean geometric pressure of 125 MPa. 3 / 100g or more, e.g. 45cm 3 / 100g or more or 50cm 3 The acetylene black according to the present invention may have a void volume of 80 cm3 / 100 g or more, measured at a mean geometric pressure of 125 MPa. 3 / 100g or less, e.g. 70cm 3 / 100g or less or 60cm 3 The void volume (@125 MPa) can range between any of the recited values, e.g., 40 to 80 cm 3 / 100g or 50-60cm 3 / 100g.

[0026] Additionally or alternatively, the acetylene black material according to the present invention can be characterized by its aggregate size distribution. The aggregate size distribution can be measured using a disc centrifugal photosedimentometer (DCP) in accordance with ISO 15825:2017. The aggregate size distribution can be determined in particular by the mode (D mode ), i.e., the particle size of the most frequently occurring aggregates, which appears as the peak of the mass distribution curve. The aggregate size distribution can be further described by the width of the mass distribution curve measured at half the mode (ΔD50), which is a measure of the width of the aggregate size distribution. For example, acetylene black according to the present invention has a D mode The acetylene black according to the present invention may have an aggregate particle size distribution in which D is 50 nm or more, for example, 60 nm or more, 70 nm or more, or 80 nm or more. modeD may have an aggregate size distribution in which D is 200 nm or less, for example 150 nm or less, or 130 nm or less, or 120 nm or less. mode can range between any of the recited values, for example, from 50 nm to 200 nm, or from 70 nm to 150 nm. Alternatively or additionally, the aggregate particle size distribution of the acetylene black according to the present invention has a ratio ΔD50 / D of 0.5 or more, for example, 0.6 or more, or 0.7 or more, or 0.8 or more, or 0.9 or more, or 1.0 or more, or 1.2 or more, or 1.5 or more. mode The aggregate size distribution of the acetylene black can, for example, have a ratio ΔD50 / D of 2.5 or less, e.g., 2.2 or less, 2.0 or less, or 1.8 or less, or 1.7 or less. mode ΔD50 / D mode can range between any of the recited values, such as 0.5 to 2.5, or 1.0 to 2.0, or 1.5 to 2.0.

[0027] The acetylene black according to the present invention can further be characterized by a certain amount of grit. Grit typically refers to undesirable coarse particles that can adversely affect the application properties of the acetylene black material. The acetylene black according to the present invention can have a small amount of grit. For example, the grit can be less than 100 ppm, more preferably less than 50 ppm, or even less than 10 ppm, of residue that does not pass through an ASTM sieve having a mesh opening size of 45 μm (ASTM E11-17, sieve designation: #325), based on the total weight of the acetylene black.

[0028] Additionally or alternatively, the acetylene black according to the present invention may exhibit a relatively high degree of crystallinity and / or a proportion of graphitic domains, which may be demonstrated by Raman spectroscopy. The Raman spectrum of carbon black materials exhibits a band around 1,360 cm, designated as the "D band" and the "G band", respectively. -1 and approximately 1,580 cm -1 Includes two bands. Approx. 1,360cm -1The "D band" in the 2 Attributable to carbon atoms, on the other hand, approximately 1,580 cm -1 The "G band" in 2 The D / G ratio is attributed to carbon atoms. The ratio of the integrated area of ​​the "D band" to the integrated area of ​​the "G band" (D / G ratio) therefore provides a measure of the degree of crystallinity and / or proportion of graphitic domains, with lower values ​​of the D / G ratio indicating higher order / crystallinity and / or a higher proportion of graphitic domains in the carbon black material investigated. The acetylene black of the present invention can have a D / G ratio of 1.5 or less, preferably 1.4 or less, and more preferably 1.3 or less, as measured by Raman spectroscopy. The acetylene black of the present invention can have a low D / G ratio of 0.8, for example, 0.9 or more, or 1.0 or more. The acetylene black of the present invention can have a D / G ratio ranging between any of the recited values, for example, 0.8 to 1.5, or 0.9 to 1.4, or 1.0 to 1.3.

[0029] Additionally or alternatively, the acetylene black according to the present invention can be characterized by its crystallite size. c The acetylene black of the present invention can be characterized by its crystallite size, for example, an L of 26 Å or more, such as 28 Å or more, or 30 Å or more, or 32 Å or more. c The acetylene black can have a crystallite size of, for example, 50 Å or less, e.g., 45 Å or less, or 40 Å or less, or 38 Å or less, or 35 Å or less. c The acetylene black of the present invention may have a crystallite size L ranging between any of the recited values. c The acetylene black may have a crystallite size of, for example, 26 Å to 50 Å, 28 Å to 40 Å, or 30 Å to 38 Å. Alternatively or additionally, the acetylene black may have a crystallite size of, for example, 26 Å to 50 Å, 28 Å to 40 Å, or 30 Å to 38 Å. a Acetylene black can be characterized by its crystallite size, for example, an L of 60 Å or more, e.g., 65 Å or more, or 70 Å or more, or 75 Å or more. aAcetylene black can have a crystallite size of, for example, 100 Å or less, e.g., 95 Å or less, or 90 Å or less. a The acetylene black of the present invention may have a crystallite size L ranging between any of the recited values. a The crystallite size may be, for example, 60 Å to 100 Å, or 70 Å to 90 Å. c Crystallite size and L a The crystallite size can be determined by X-ray diffraction, as described, for example, in "Autodecomposition of Hydrogen Peroxide on the Surface of Dispersed Carbon Black," G. I Razdyakonova, VALikholobov, Nanosystems, RENSIT, 2015, 7(2):180-190.

[0030] Additionally or alternatively, the acetylene black of the present invention can be characterized by its chemical composition or purity, for example, by one or more or all of its carbon content, oxygen content, hydrogen content, sulfur content, nitrogen content, total metal content, and / or ash content. Typically, acetylene black is essentially composed of carbon and has a high carbon content. Thus, the acetylene black of the present invention can have a carbon content of 98.5% by weight or more, preferably 99.0% by weight or more, or 99.2% by weight or more, or 99.4% by weight or more, or 99.5% by weight or more, or 99.6% by weight or more, for example, up to about 100% by weight, based on the total weight of the acetylene black. The content of non-carbonaceous impurities, if any, can be low as a result. The acetylene black can, for example, have a hydrogen content of less than 1.0% by weight, for example, less than 0.5% by weight, or less than 0.3% by weight, based on the total weight of the acetylene black. The acetylene black of the present invention may have an oxygen content of less than 0.1 wt.%, for example, less than 0.05 wt.%, or less than 0.03 wt.%, based on the total weight of the acetylene black. The nitrogen content of the acetylene black of the present invention may be less than 0.2 wt.%, for example, less than 0.1 wt.%, based on the total weight of the acetylene black. The sulfur content of the acetylene black of the present invention may be less than 0.1 wt.%, for example, less than 0.05 wt.%, or less than 0.01 wt.%, based on the total weight of the acetylene black. The carbon content, oxygen content, hydrogen content, sulfur content, and nitrogen content of the acetylene black can be measured by quantitative elemental analysis. Additionally or alternatively, the acetylene black of the present invention may have a low content of metals. For example, the acetylene black may have a metal content of less than 1,000 ppm, for example, less than 100 ppm, or less than 50 ppm, or less than 20 ppm, or less than 10 ppm, based on the total weight of the acetylene black. The metals in acetylene black can be measured, for example, by inductively coupled plasma optical emission spectroscopy (ICP-OES), for example using a Prodigy7 instrument from TELEDYNE LEEMAN LABS, Masson, USA.The acetylene black of the present invention may have an ash content of 1% by weight or less, for example, 0.5% by weight or less, or 0.2% by weight or less, or preferably 0.1% by weight or less, or more preferably 0.05% by weight or less, based on the total weight of the acetylene black. The ash content can be measured in accordance with ASTM D1506-15.

[0031] The acetylene black according to the present invention has been found to be exceptionally conductive. For example, the acetylene black according to the present invention can exhibit low powder resistivity. Powder resistivity can be measured by measuring the electrical resistance of a powder sample of acetylene black subjected to compression in a chamber at a defined mean geometric pressure, such as using a void volume tester equipped for simultaneous measurement of electrical resistivity as described in the Examples. The acetylene black according to the present invention can have, for example, a powder resistivity of less than 1.0 Ω·cm, e.g., 0.5 Ω·cm or less, 0.3 Ω·cm or less, or 0.2 Ω·cm or less, or 0.1 Ω·cm or less, or 0.08 Ω·cm or less, or 0.06 Ω·cm or less, when measured under a pressure of 50 MPa. It can have, for example, a powder resistivity of 0.005 Ω·cm or more, e.g., 0.01 Ω·cm or more, 0.02 Ω·cm or more, or 0.03 Ω·cm or more, when measured under a pressure of 50 MPa. The acetylene black of the present invention can have a powder resistivity (@50 MPa) ranging between any of the recited values, for example, 0.005 to 1.0 Ω·cm, 0.01 to 0.1 Ω·cm, 0.02 to 0.06 Ω·cm.

[0032] Acetylene black according to the present invention can be produced based on the incomplete combustion of an acetylene-containing hydrocarbon feedstock with an oxygen-containing gas, as described herein. Such an incomplete combustion reaction can be represented schematically by the following equation: C2H2+ xO2→ 2(1-x)C + 2xCO + H2 wherein x is a number greater than 0 and less than 1. Thus, as noted above, the present invention also relates to a method for producing acetylene black. The method includes feeding a hydrocarbon feedstock containing acetylene to a reactor; feeding an oxygen-containing gas to the reactor; contacting the hydrocarbon feedstock containing acetylene with the oxygen-containing gas to incompletely combust the hydrocarbon feedstock containing acetylene, thereby forming acetylene black in the reactor; and recovering the formed acetylene black. The amounts of the hydrocarbon feedstock containing acetylene and the oxygen-containing gas introduced into the reactor are controlled so that the molar ratio of oxygen to acetylene (represented by x in the above formula) is in the range of 0.30 to 0.80. Preferably, the molar ratio of oxygen to acetylene can be in the range of 0.30 to 0.60, more preferably 0.32 to 0.50, e.g., 0.35 to 0.45, or 0.37 to 0.42.

[0033] The hydrocarbon feedstock used in the process according to the present invention comprises acetylene. It may optionally further comprise one or more hydrocarbons other than acetylene. Such optional additional hydrocarbons may be exemplified by, but not limited to, ethylenically unsaturated hydrocarbons (e.g., alkylenes such as ethylene or propylene), aromatic hydrocarbons (e.g., benzene, toluene, or xylene), and aliphatic hydrocarbons (alkanes such as methane, ethane, or propane), or any mixture or combination thereof. Typically, the hydrocarbon feedstock comprises at least 50% by weight, e.g., 70% by weight or more, or 80% by weight or more, or 90% by weight or more, or 95% by weight or more, or 98% by weight or more, or 99% by weight or more, of acetylene, based on the total weight of the hydrocarbon feedstock. Preferably, the hydrocarbon feedstock consists of acetylene. For clarity, a hydrocarbon feedstock consisting of acetylene may still contain impurities commonly present in industrial acetylene gas, e.g., impurities in a total amount of up to 2% by weight, based on the total weight of the hydrocarbon feedstock. Acetylene from the steam cracker acetylene recovery unit is typically recovered at a purity of ≥ 99 wt%. The acetylene-containing hydrocarbon feed is typically fed to the reactor in gaseous form. Optionally, the hydrocarbon feed can be preheated before contacting with the oxygen-containing gas. If preheated, the acetylene-containing hydrocarbon feed is typically preheated to a temperature of ≤ 150°C for safety reasons.

[0034] The oxygen-containing gas can be any oxygen-containing gas, including, but not limited to, air, oxygen-enriched air, nitrogen-enriched air, oxygen-containing technical gas mixtures such as exhaust gas from carbon black production, or oxygen gas itself. The oxygen-containing gas can contain, for example, 1% by volume or more, or 5% by volume or more, e.g., 10% by volume or more, or 15% by volume or more, or 20% by volume or more, based on the total volume of the oxygen-containing gas. The oxygen-containing gas can contain, for example, up to 100% by volume, e.g., 99% by volume or less, or 95% by volume or less, or 90% by volume or less, or 80% by volume or less, or 60% by volume or less, or 50% by volume or less, or 40% by volume or less, or 30% by volume or less, based on the total volume of the oxygen-containing gas. The oxygen-containing gas can have an oxygen content ranging between any of the listed values, e.g., 1% by volume to 100% by volume, e.g., 10% by volume to 80% by volume, or 20% by volume to 30% by volume, based on the total volume of the oxygen-containing gas. For economic reasons, air is preferably used as the oxygen-containing gas in the process according to the invention. The oxygen-containing gas can optionally be preheated before contacting with the hydrocarbon feedstock. For example, the oxygen-containing gas can be preheated to a temperature of 200°C or higher, for example 300°C or higher, or 500°C or higher, or 700°C or higher. For practical reasons, the oxygen-containing gas is typically not preheated to a temperature above 850°C.

[0035] The oxygen-containing gas and the hydrocarbon feedstock are optionally preheated and then fed to the reactor by an introduction means such as a burner, where they are contacted with each other to cause incomplete combustion of the hydrocarbon feedstock, thereby causing the formation of acetylene black in the reactor, as described, for example, in U.S. Patent Application Publication No. 4,013,759. In the process disclosed herein, the rates at which the oxygen-containing gas and the hydrocarbon feedstock are fed to the reactor are generally controlled so that the molar ratio of oxygen to acetylene is in the ranges described above. The rates at which the oxygen-containing gas and the hydrocarbon feedstock are fed to the reactor are, for example, independently, between 5 and 500 Nm 3 / h, e.g., 10 to 300 Nm 3 / h, or 20 to 200 Nm 3 / h, or 30 to 150 Nm 3 / h. Due to the incomplete combustion of the hydrocarbon feedstock, high temperatures of the order of 2,000°C can be achieved in the reactor. Typically, acetylene black is formed in the reactor at temperatures of at least 1,700°C, e.g., 1,800°C or higher, or 1,900°C or higher, or 2,000°C or higher.

[0036] The pressure in the reactor can be controlled during operation for safety and process control reasons. For example, the pressure in the reactor can exceed atmospheric pressure (101.3 kPa) to prevent air ingress. For example, the pressure in the reactor can be in the range of 0.01 to 1 MPa above atmospheric pressure. Alternatively, the reactor can be operated under vacuum, i.e., at a pressure below atmospheric pressure, for example, in the range of 1 to 100 kPa.

[0037] The method for producing acetylene black according to the present invention can be carried out in a reactor as shown schematically in FIG. 1. The reactor includes a vertical furnace (1). The vertical furnace (1) may be, for example, a vertical cylindrical furnace having an overall height of 7.4 m and an inner diameter of 300 mm. A burner (2) is provided at the top of the vertical furnace. An oxygen-containing gas, such as air, can be supplied from a source (not shown) via a supply line (9) to an optional preheater (5), where it can be optionally preheated, and then passed to the burner (2) via a line (11). An acetylene-containing hydrocarbon feedstock can be supplied from a source (not shown) via a supply line (8) to an optional preheater (4), where it can be preheated if necessary, and then passed to the burner (2) via a line (10). Optionally, means can be provided for measuring the respective temperatures of the oxygen-containing gas (13) and the hydrocarbon feedstock (12) supplied to the burner. During operation, oxygen-containing gas and hydrocarbon feedstock are introduced into a vertical furnace (1) by a burner (2). The amounts of oxygen-containing gas and hydrocarbon feedstock are adjusted to achieve a desired molar ratio of oxygen to acetylene. The burner (2) can be configured so that the oxygen-containing gas stream is introduced into the furnace (1) in a zone immediately adjacent to the introduction zone of the hydrocarbon feedstock stream, e.g., peripherally and approximately tangentially to the hydrocarbon feedstock stream. The burner (2) can, for example, comprise an axial nozzle with a cylindrical internal passage for introducing the acetylene-containing hydrocarbon feedstock, the internal passage being surrounded by a hollow annular zone for introducing the oxygen-containing gas. Such burners are described in more detail, for example, in U.S. Pat. No. 4,013,759. The burner may include cooling means, such as water cooling of the acetylene inlet tube, which can minimize acetylene polymerization and resulting coking, as described, for example, in a paper by E. J. Klassen, Jr., Austin, Texas, May 1948, entitled "The Production of Carbon Black by Pyrolysis of Acetylene and Acetylene-Hydrocarbon Mixtures." Incomplete combustion of the hydrocarbon feedstock occurs in the combustion zone at the top of the vertical furnace (1).As described in the aforementioned paper by EJ Klassen, unwanted coking can be delayed by premixing acetylene with hydrogen and / or ensuring a sharp jet of acetylene from the burner nozzle. The walls of the vertical furnace, or parts thereof, such as the upper walls, may be protected from the high temperatures generated inside the furnace by lining them with a refractory material such as graphite and / or by providing cooling means such as a water-cooled jacket (14). This may also increase the reaction temperature and / or yield. A pressure gradient is generated within the furnace by a pump or exhaust system (3). The aerosol formed by the reaction, containing the formed acetylene black particles and residual gases, is drawn through a circuit (17) at the bottom of the vertical furnace (1), along which it cools by natural convection. A means (16) for measuring the temperature of the aerosol drawn from the vertical furnace may be installed along the circuit (17). The cooled aerosol is conducted through a circuit (17) to one or more separating cyclones (7) to separate the formed acetylene black from the gases of the aerosol. The separated acetylene black is then collected in a container such as a hopper (15), while the gases separated by the cyclones are discharged.

[0038] During operation, the flow of hydrocarbon feedstock may be interrupted from time to time for short periods (e.g., a few seconds to a minute), during which time pressurized gas such as compressed air is pumped into the furnace to dislodge any carbon black that may have adhered to the burners or furnace walls. A disintegration mill (6) may be provided at the bottom of the vertical furnace to break up any agglomerates of carbon black that have dislodged from the burners or furnace walls.

[0039] From time to time (e.g., days to weeks), once the reactor has cooled, it can be removed from production for a short time and cleaned. This cleaning removes all deposits and is more aggressive than the on-stream cleaning described above. Cleaning can be accomplished with pressurized air, brushes, ultrasonic cleaners, and other commonly known cleaning aids.

[0040] Optionally, the reactor can further include means for separating grit from the aerosol, such as a wire grid filter made from a material that can withstand high temperatures, e.g., a nickel-based alloy. As a further option, the reactor can be equipped with one or more purification means, e.g., a magnetic filter, for removing impurities, such as metal or metal-rich particles, from the aerosol. Any grit separation means and / or purification means can be provided, for example, along circuit (17).

[0041] Acetylene black formed according to the above-described manufacturing method is typically obtained in the form of a fluffy powder. The as-obtained powder can be subjected to further processing, such as size classification (e.g., by using a sieve) and / or densification, if necessary. For example, the as-obtained acetylene black in the form of a fluffy powder can be densified to form a derivable compacted entity therefrom, such as a pellet, granule, or the like. Densification can be carried out by any method known in the art for densifying powder materials, such as, but not limited to, applying a vacuum, compacting, rolling, pelletizing, granulation, briquetting, or a combination thereof. Densification of acetylene black can be carried out using conventional techniques and equipment, including, for example, fluidized bed spray granulation, fluidized bed spray drying, agitation granulation, dry pelletizing, wet pelletizing, or a combination thereof. Pelletization of the initial acetylene black can be carried out, for example, as described in EP 2913368 B1. The acetylene black can optionally be further dried, especially if the acetylene black has been contacted with a wet medium, for example, in a wet pelletizing step. Drying can be carried out by drying means commonly used in the art, for example, by applying heat and / or reduced pressure. For example, the acetylene black can be dried so that the residual moisture content of the acetylene black, e.g., densified acetylene black, after drying is less than 0.1 wt. %, for example, less than 0.05 wt. %, based on the total weight of the acetylene black. The moisture content can be measured according to ASTM D1509-95.

[0042] The acetylene black according to the present invention can be obtained, for example, as described above and can be utilized in a variety of technical applications, including all types of applications in which acetylene black is typically used. For application, the acetylene black can be compounded with one or more other components, such as binders and / or solvents, as described in more detail below. Accordingly, the present invention also relates to compositions comprising the acetylene black described herein, wherein the acetylene black according to the present invention can impart exceptionally high electrical and / or thermal conductivity to a composition or article made therefrom and / or can impart a desired level of electrical and / or thermal conductivity thereto at a relatively low concentration of acetylene black.

[0043] The acetylene black of the present invention can be advantageously processed using conventional powder processing techniques and equipment and can be easily incorporated into compositions. The compositions can be provided, for example, in the form of a dispersion, dry powder, paste, or solid mass. The acetylene black material of the present invention can be blended or dispersed with a carrier medium, such as an aqueous or organic solvent-based carrier medium, or with a plastic material. For this purpose, conventional mixing and blending equipment, such as a blender, mixer, kneader, or single- or twin-screw extruder, can be used. The acetylene black of the present invention typically exhibits good dispersibility in various carrier media, resulting in compositions with suitable and stable processing and application properties. The amount of powdered acetylene black material used largely depends on the type of composition and intended use and can be selected by those skilled in the art according to their respective needs, based on formulations similar to those for conventional acetylene black.

[0044] As used herein, an aqueous carrier medium refers to a carrier medium containing more than 50% by weight, e.g., 70% by weight or more, 80% by weight or more, 90% by weight or more, or up to 100% by weight, of water, based on the total weight of the carrier medium. An organic solvent-based carrier medium refers to a carrier medium containing more than 50% by weight, e.g., 70% by weight or more, 80% by weight or more, 90% by weight or more, or up to 100% by weight, of an organic solvent, based on the total weight of the carrier medium. The type of carrier medium used depends on the type of application and can vary widely. The carrier medium may contain water and / or one or more organic solvents. Examples of organic solvents that can be used include, but are not limited to, alcohols, ketones, aldehydes, amines, esters, ethers, carboxylic acids, hydrocarbons, or mixtures or combinations thereof.

[0045] Similarly, all types of polymer or resin material can be used as plastic material or binder in the composition according to the present invention, depending on intended use.Non-limiting examples of useful resin and polymer that can be used in the present invention include: olefin polymers such as polypropylene, polyethylene, ethylene-vinyl acetate copolymer, ethylene-vinyl alcohol resin, cyclic olefin copolymer, natural rubber, styrene-butadiene rubber, acrylonitrile-butadiene rubber, butyl rubber, acrylic rubber, ethylene-propylene rubber, ethylene-propylene terpolymer, ethylene-α-olefin copolymer rubber, silicone rubber, fluororubber, chloroprene rubber, hydrin rubber, chlorosulfonated polyethylene rubber, vinyl chloride polymers such as polyvinyl chloride, ethylene-vinyl chloride copolymer, polystyrene, styrene-acrylonitrile copolymer, Examples of suitable acetylene black resins include styrene-based polymers such as acrylonitrile-butadiene-styrene copolymers, acrylic polymers such as polymethyl methacrylate, polyesters such as polyethylene terephthalate, polybutylene terephthalate, polyamides, polyacetals, and polycarbonates, fluororesins such as polyphenylene ethers, polytetrafluoroethylene, and polyvinylidene fluoride, polyphenylene sulfide, liquid crystal polymers, thermoplastic polyamides, ketone-type resins, sulfone resins, phenyl resins, urea resins, melamine resins, alkyd resins, silicone resins, epoxy resins, urethane resins, polyvinyl esters, polyimides, furan resins, and quinine resins, as well as mixtures, blends, and combinations thereof. Accordingly, the present invention also relates to rubber or plastic compositions comprising the acetylene black disclosed herein and a rubber or polymer, such as those described above. The present invention also relates to rubber and plastic articles made from such rubber or plastic compositions.

[0046] Depending on the type of application, additional components can be used when formulating the composition according to the present invention. Those skilled in the art will select any such additional components and their respective amounts according to the desired properties and / or application of the composition. Examples of such additional components include oils and waxes, processing aids, rheology modifiers, pH adjusters, fillers, pigments, dyes, coupling agents, catalysts, accelerators, vulcanizing agents, activators, sulfur curing agents, antidegradants, antioxidants, stabilizers, biocides, and plasticizers. As described in more detail below, the compositions according to the present invention are useful for electrochemical applications, such as battery applications. Therefore, for such applications, they may further comprise one or more electrochemically active components. The electrochemically active components may be, for example, a common anode material, a cathode material, or an electrocatalyst.

[0047] As will be appreciated, the acetylene black of the present invention, as well as compositions containing it and articles made therefrom, are particularly useful in applications where high electrical and / or thermal conductivity is desirable or beneficial. The acetylene black material of the present invention can, for example, impart electrical conductivity to compositions containing it and articles made therefrom. Therefore, the acetylene carbon black material of the present invention is particularly useful, for example, for electrodes, conductive catalyst supports, and electrical conductors (including high-voltage cables), as well as for power and battery applications (including primary batteries, secondary batteries, fuel cells, and capacitors). Accordingly, the present invention is also directed to electrodes or other components of energy storage and / or conversion devices made from acetylene black or the present invention or compositions containing it. The present invention also relates to energy storage and / or conversion devices comprising such electrodes or components. The energy storage and / or conversion device can be, for example, a primary battery, a secondary battery, a fuel cell, or a capacitor. The acetylene black material of the present invention, compositions containing it, and articles made therefrom can also be used as or for the manufacture of thermally conductive or heat transfer materials.

[0048] Additionally, acetylene black materials can also be used as antistatic or conductive agents, for example, in rubber or plastic materials and articles (such as bladders for tire manufacturing).

[0049] The acetylene black described herein can be used, for example, as an electrical conductor, antistatic agent, thermally conductive agent, reinforcing filler and / or colorant for the manufacture of electrodes and other components of energy storage and / or conversion devices (e.g., primary batteries, secondary batteries, fuel cells and capacitors), and / or for the manufacture of plastic articles made of a thermoplastic or thermoset polymer or rubber matrix (e.g., tires or components thereof, wires, cables and their sheaths, belts, hoses, shoe soles, rollers, heaters, or bladders, e.g., tire bladders, heat conducting materials, heat transfer materials), and / or in coatings, paints or inks.

[0050] Having generally described the invention above, a further understanding can be obtained by reference to the following specific examples, which are provided herein for illustrative purposes only and are not intended to limit the invention, which rather is to be accorded the full scope of the appended claims, including any equivalents thereof. [Example]

[0051] [Preparation of acetylene black] Acetylene black was produced in a reactor as described above and shown schematically in Figure 1 of the present application. The reactor included a vertical furnace (1) with a burner (2) extending into the furnace at its upper end. Acetylene and air were supplied to the axial nozzle of the burner via supply lines (8) and (9), respectively. A preheater (5) was installed in the air supply line to preheat the air supply. A preheater (4) was not used on the acetylene supply line. Incomplete combustion of the acetylene supply with the supply air occurred in the vertical furnace, resulting in the formation of acetylene black. The furnace walls were protected from the high temperatures inside the furnace by a double water-cooled jacket (14). An exhauster (3) fluidly connected to the bottom of the furnace reduced the pressure in the furnace to prevent blockage of the burners and directed the formed aerosol containing acetylene black, via a circuit (17), while being cooled there by natural convection, to a set of cyclones (7), where the acetylene black was separated from the gases and collected in a tank.

[0052] Example 1 Using the above reactor, 42 Nm 3 / h acetylene (not preheated) and 75Nm preheated to 300°C 3 / h of air was introduced into the vertical furnace via a burner to produce acetylene black. Every 60 minutes, the flow of acetylene was interrupted and a cleaning cycle using room temperature air compressed to 2 bar was initiated for approximately 2 minutes. The flow of acetylene was then resumed. The acetylene black thus obtained was collected in the reactor hopper (15). The stoichiometric yield was 58%.

[0053] Example 2 (Comparative Example) Using the above reactor, another acetylene black was produced. The operation was the same as in Example 1, but with a flow rate of 55 Nm 3 / h acetylene (not preheated) and 75Nm preheated to 300°C 3 / h of air was introduced into the vertical furnace via a burner. Every 60 minutes, the acetylene flow was interrupted and a cleaning cycle using ambient air compressed to 2 bar was initiated for approximately 2 minutes. The acetylene flow was then resumed. The acetylene black thus obtained was collected in the reactor hopper (15). The stoichiometric yield was 66%.

[0054] [Characteristics of acetylene black] The properties of the acetylene black obtained in Examples 1 and 2 were measured by the property evaluation methods described below, and are summarized in Table 1, in comparison with acetylene black manufactured by Denka Co., Ltd. under the trade name "Li-435," which is used as a conductive agent in the technical field, as a reference material.

[0055] As can be seen from Table 1, the acetylene black material according to the invention (Example 1) inter alia had a significantly higher structure (as indicated by a higher OAN and void volume) and exhibited a significantly lower volume resistivity, i.e., a higher conductivity, than the comparative acetylene black material according to Example 2 or the commercial reference material Li-435.

[0056] Table 1: Properties of acetylene black [Table 1]

[0057] BET specific surface area was measured by nitrogen adsorption according to ASTM D6556-19a. Applied pressure points were 0.05, 0.075 and 0.1 p / p. 0The sample mass ranged from 0.15 to 0.4 g. The powdered carbon black samples were compressed before BET analysis. For this purpose, 5 g of powdered carbon black sample was added to a paper bag. The closed paper bag was then inserted into a plastic Ziploc bag. The Ziploc bag was then closed, leaving a small opening, through which a fitting tube connected to a vacuum pump was inserted. The vacuum pump was then turned on, and the tube was placed around the edge of the paper bag inside the plastic Ziploc bag. The Ziploc bag was then tightly closed, and any trapped air pockets were manually removed. Compression was then continued under vacuum for an additional 60 seconds. The vacuum was then turned off, and the compressed carbon black sample was removed from the paper bag.

[0058] Oil absorption number (OAN) was measured according to ASTM D2414-19 procedure B. The mass of carbon black samples used ranged from 6 to 12 g.

[0059] The carbon, hydrogen, oxygen, nitrogen, and sulfur contents were determined by quantitative elemental analysis using an automatic elemental analyzer (Vario EL cube elemental analyzer manufactured by Elementor Analysis Systems) according to DIN 51732-2014-07. The acetylene black material under analysis was dried at 125 °C for 2 h before quantitative elemental analysis.

[0060] The particle size, shape, and morphology of acetylene black were investigated by TEM analysis. 20 mg of the acetylene black material to be analyzed was transferred to a 5 mL polyethylene laboratory tube and dispersed in 2 mL of chloroform in an ultrasonic bath for 3 min using an ultrasonic stick immersed in the bath, operated at 100 W power to provide good dispersion of the acetylene black powder. A drop of the dispersion was then transferred onto a carbon-coated copper TEM holder (200 mesh) using an Eppendorf microliter pipette. The loaded grid was then transferred to the high vacuum of a Hitachi H-7500 TEM instrument (100 kV) for examination. The average primary particle size was determined from a representative set of TEM images containing approximately 2,000 well-dispersed, isolated particles by automated image analysis according to ASTM D3849-07.

[0061] Additionally, aggregate particle size distribution was measured for the investigated acetylene blacks by disc centrifuge photosedimentation (DCP) according to ISO15825:2017 using a Brookhaven BI-DCP particle size analyzer.

[0062] The acetylene black material was further analyzed by Raman spectroscopy. For this purpose, a powder sample of the acetylene black material to be analyzed was placed on a microscope slide and flattened by gently pressing it down from the top edge with a second slide. Raman spectra were then recorded for the thus prepared sample using a Thermo Scientific DXR Raman microscope (Thermo Fisher Scientific) at 50x magnification and 0.5 mW power of the laser operating at a wavelength of 532 nm, with an acquisition time of 2 seconds and an exposure rate of 32. Measurements were performed at 10 different locations for each sample to confirm reproducibility. Peak fitting analysis revealed a peak at approximately 1,360 cm. -1 Defect band (D band) at approximately 1,580 cm -1The intensity of the graphite band (G band) at 1000 K was determined from the recorded Raman spectra. The reported (D / G) ratio corresponds to the arithmetic mean of the ratio of the intensity of the D band to the intensity of the G band over the 10 measurements performed. Lower values ​​of the (D / G) ratio indicate a relatively high proportion of graphitic domains, i.e., a higher degree of order / crystallinity.

[0063] Additionally, the acetylene black materials were analyzed by X-ray diffraction (XRD) to determine their crystallite size, L a , L c was measured using the procedure described in "Autodecomposition of hydrogen peroxide on the surface of dispersed carbon black", G.I Razdyakonova, VALikholobov, Nanosystems, RENSIT, 2015, 7(2):180-190.

[0064] The void volume was measured according to ASTM D7854-18a. For this purpose, the acetylene black sample to be analyzed was provided on a tray and dried for at least 1 hour in a convection oven set at 125 ± 5 °C. The dried material was then cooled to ambient temperature and stored in a desiccator before use. Using a scale, a 1.000 g sample was weighed to the nearest 0.1 mg into the sample pan. The weighed sample was then transferred using a funnel into the cylindrical sample chamber (1-inch diameter) of a void volume tester (Hitec, Luxembourg). The sample pan and funnel were carefully brushed to ensure the entire sample was introduced into the cylindrical sample chamber. The test was then initiated by closing the cylindrical sample chamber, applying pressure to the movable piston of the cylindrical sample chamber, and measuring the compressed volume of the weighed sample in the cylindrical chamber as a function of the pressure applied by the movable piston. The pressure was increased from 0 to 125 MPa geometric mean pressure and then decreased back to 125 to 0 MPa geometric mean pressure at a compression / decompression rate of 2 MPa / s. Both compression and decompression curves were recorded, and the void volume was calculated from the measured volumes as a function of the pressure exerted by the moving piston and the weight of the sample. The values ​​reported in Table 1 correspond to the arithmetic mean of the void volumes measured from the pressure and decompression curves at geometric mean pressures of 50 MPa, 75 MPa, or 125 MPa, respectively.

[0065] The powder resistivity of acetylene black was measured simultaneously with the above-described void volume test using a void volume tester (Hitec Luxembourg) with a ceramic cylindrical sample chamber, according to the manufacturer's instructions. The electrical resistance of the analyzed sample was recorded over both compression and decompression scans as a function of the pressure applied by the moving piston and the resistivity calculated therefrom. The values ​​reported in Table 1 correspond to the arithmetic mean of the resistivity measured at a geometric mean pressure of 50 MPa from the compression and decompression curves.

[0066] [Preparation of electrode slurry] A dry premix was prepared by adding 4.5 g of Solef5130 (Solvay) PVDF polymer, 291 g of lithium-nickel-manganese-cobalt-oxide NMC532 (BASF), and 4.5 g of either acetylene black or Li-435 according to Example 1 to the mixing vessel of a double planetary mixer (FMPE HM2P-03 from Bühler Technology GmbH, Ratingen, Germany). The dry composition was mixed in the double planetary mixer at room temperature and a rotation speed of 20 rpm for 15 minutes.

[0067] The premixes were then dispersed in an organic solvent in a two-step procedure. First, 80 g of N-methyl-2-pyrrolidone (NMP, analytical purity ≥ 99.5% provided by VWR Chemicals) and 1.125 g of dispersant (BYK 40% LPN24711) were added to each premix, followed by mixing in a double planetary mixer at 40 rpm for 10 minutes, followed by mixing at 80 rpm for 50 minutes. An additional 15 g of NMP was then added to the mixture, and the composition was mixed in a double planetary mixer at 80 rpm for an additional 20 minutes to obtain an electrode slurry. The fineness of the slurries, as measured by a Hegman gauge, was less than 20 μm.

[0068] [Preparation of electrode film and measurement of electrical resistivity] Within 4 hours after preparation, electrode films were prepared from the prepared electrode slurries. Cathode films were prepared according to the following procedure: 20 μm-thick aluminum foil used as a current collector was placed smoothly and firmly on a coater (TQC Sheen K-Control Coater). Each electrode slurry was then cast onto one side of the aluminum foil, and the coater's doctor blade was used to adjust the layer thickness with a 200 μm gap. The coated electrodes were then dried in a vacuum oven at 100°C for 3 hours.

[0069] The electrical resistance of the resulting electrode films was measured using a HIOKI 4-terminal probe of a HIOKI RM3543-01 Resistivity HiTESTER. For this purpose, each coated aluminum foil was cut into a disk with a diameter of 14 mm, and the front and back surfaces were fitted with two flat plated metering electrodes (10 mm diameter, 0.7854 cm area). 2 ) and centered. A preliminary test was performed during warm-up of the instrument and zero calibration was performed using a copper disk. The measurement range was set to 1000 mΩ. After conditioning for 40 seconds under an applied pressure of 0.4 MPa, the resistance was automatically read from the HIOKI device. Volume resistivity was calculated by multiplying the obtained resistance by the measured area of ​​the plated metering electrode (0.7854 cm). 2 ) and divided by the measured thickness of the electrode coating. The tabulated results, shown in Table 2 below, represent the arithmetic mean of six disk samples from the same respective coating.

[0070] Table 2: Average electrode volume resistivity of electrodes prepared from electrode slurries containing different acetylene blacks [Table 2]

[0071] As can be seen from Table 2, the electrode formed from the slurry containing the acetylene black material according to the present invention (Example 1) exhibited significantly lower volume resistivity than the electrode derived from the commercially available reference material Li-435. [Explanation of symbols]

[0072] 1 vertical furnace 2 Burner 3 Exhaust system 4,5 Preheater 6. Collapse Mill 7 Separation cyclone 8,9 Supply lines 10 lines 12 Hydrocarbon feedstock 13 Oxygen-containing gases 14 Water cooling jacket 15 Hopper 16. Means for measuring the temperature of aerosols 17 circuits

Claims

1. (a) an oil absorption capacity (OAN) of 360 mL / 100 g or more as measured according to ASTM D2414-19, and (b) 50 to 200 m as measured according to ASTM D6556-19a ２ Acetylene black having a BET surface area in the range of / g.

2. The acetylene black according to claim 1, wherein the acetylene black has an OAN of 380 mL / 100 g or more.

3. Acetylene black, 80-160m ２ Acetylene black according to claim 1, having a BET surface area of ​​1 / g.

4. L values ​​greater than 26 Å measured by X-ray diffraction ｃ A crystallite size and / or L of 60 Å or greater, as measured by X-ray diffraction. ａ Acetylene black according to claim 1, having crystallite size.

5. The acetylene black according to claim 1, having a D / G ratio of less than 1.5 as measured by Raman spectroscopy.

6. D in the range of 50 nm to 200 nm ｍｏｄｅ and / or ratio ΔD50 / D in the range of 0.5 to 2.5 ｍｏｄｅ Acetylene black according to claim 1, having an aggregate particle size distribution having the following characteristics.

7. The acetylene black according to claim 1, having one or more or all of the following: - Carbon content of at least 99.0% by weight, - Oxygen content of less than 0.1% by weight, - Hydrogen content of less than 0.5% by weight, - Sulfur content of less than 0.1% by weight, - Nitrogen content of less than 0.2% by weight, - Metal content of less than 1,000 ppm.

8. 70 cm² measured at a pressure of 50 MPa according to ASTM D7854-18a ３ The acetylene black according to claim 1, having a void volume of 100 g or more, and / or a powder resistivity of less than 0.1 Ω·cm as measured at a pressure of 50 MPa.

9. A method for producing acetylene black according to any one of claims 1 to 8: To supply hydrocarbon raw materials containing acetylene to the reactor, Supplying oxygen-containing gas to the reactor, The process involves contacting a hydrocarbon raw material containing acetylene with an oxygen-containing gas to cause incomplete combustion of the hydrocarbon raw material containing acetylene, thereby forming acetylene black in the reactor, and This includes recovering the formed acetylene black, In this production method, the hydrocarbon raw material containing acetylene and the oxygen-containing gas are introduced into the reactor such that the molar ratio of oxygen to acetylene is in the range of 0.30 to 0.

80.

10. A composition comprising acetylene black according to any one of claims 1 to 8.

11. The composition according to claim 10, further comprising at least one of an electrochemically active component, a binder, and a solvent.

12. An electrode or other component of an energy storage and / or conversion device, made from acetylene black or a composition containing the acetylene black as described in any one of claims 1 to 8.

13. An energy storage and / or conversion device comprising an electrode or component as described in claim 12.

14. A rubber article or plastic article made from a composition comprising acetylene black according to any one of claims 1 to 8, and at least rubber or a polymer.

15. Use of the acetylene black material according to any one of claims 1 to 8 as a conductive agent, antistatic agent, thermal conductive agent, reinforcing filler and / or colorant.

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