Recycled carbon black powder having specific surface area increased through steam activation treatment, manufacturing method thereof, and rubber composite including same

Abstract

Disclosed are a recycled carbon black powder having a specific surface area increased through a steam activation treatment, a manufacturing method thereof, and a rubber composite including same, wherein the specific surface area is increased through a steam activation treatment via a steam activation treatment process, and steam-activated recycled carbon black having an increased specific surface area is used as an additive for a rubber composite, thereby enhancing physical properties such as mechanical strength, wear resistance, and durability.

Description

Regenerated carbon black powder with increased specific surface area through steam activation treatment, method for manufacturing the same, and a rubber composite containing the same

[0001] The present invention relates to recycled carbon black powder with an increased specific surface area through steam activation treatment, a method for manufacturing the same, and a rubber composite containing the same. More specifically, the invention relates to recycled carbon black powder with an increased specific surface area through steam activation treatment, a method for manufacturing the same, and a rubber composite containing the same, wherein the specific surface area is increased through steam activation treatment via a steam activation treatment process, and the steam-activated recycled carbon black with an increased specific surface area is utilized as an additive to the rubber composite to realize enhanced physical properties such as mechanical strength, wear resistance, and durability.

[0002]

[0003] Carbon black refers to an aggregate of very fine spherical particles obtained by the incomplete combustion of hydrocarbons or compounds containing carbon. Carbon black forms primary particles in a reactor, and these primary particles fuse together to form grape-cluster-shaped aggregates. Meanwhile, carbon black can be broadly classified into acetylene black and furnace black. Among these, furnace black has the advantage of being inexpensive, but it has the disadvantage that it is difficult to achieve high crystallinity compared to acetylene black.

[0004] Carbon black influences the quality of materials used based on its inherent physical properties, which include crystallinity, specific surface area, structure, and particle size. These properties can be controlled through various post-treatments. Carbon black is used in diverse fields, such as industrial additives, industrial paints, coating compositions, and various printed materials.

[0005] In particular, carbon black used in the manufacture of tires is an essential additive that increases the bonding strength of rubber, the main component of tires, and requires a purity of over 99%. In addition, pyrolysis is widely used as a method to recover carbon black from waste tires.

[0006] As such, research on carbon black recycling methods is being conducted to establish a circular economy for waste tires. Recovered carbon black (r-CB) is a product made by processing char obtained after the pyrolysis of waste tires, and is currently used by tire companies as a simple input during the manufacture of some tire compounds at a content ratio of about 1 to 5 wt%.

[0007] Recently, with the increasing demand for the use of sustainable materials and compliance with ESG regulations, the use of recovered carbon black (rCB), obtained from the pyrolysis of waste tires, is gradually expanding. However, conventional recovered carbon black has limitations in meeting the requirements of high-performance rubber composites due to its low specific surface area and activity. In particular, the low specific surface area and activity of recovered carbon black lead to reduced bonding strength in rubber composites, which can consequently result in a degradation of physical properties. Accordingly, post-processing technologies are required to enhance the performance of recovered carbon black.

[0008]

[0009] Based on the aforementioned technical problems, the present invention aims to provide a recycled carbon black powder with an increased specific surface area through steam activation treatment, a method for manufacturing the same, and a rubber composite containing the same, wherein the specific surface area is increased through steam activation treatment via a steam activation treatment process, and the steam-activated recycled carbon black with an increased specific surface area is utilized as an additive to a rubber composite, thereby realizing enhanced physical properties such as mechanical strength, wear resistance, and durability.

[0010]

[0011] A method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention for achieving the above objective comprises: (a) a step of transferring recycled carbon black recovered by a pyrolysis process of waste tires to a reactor in a nitrogen atmosphere; (b) a step of increasing the specific surface area of ​​recycled carbon black by performing steam activation treatment on the recycled carbon black transferred to the reactor in a nitrogen atmosphere by steam heat treatment; and (c) a step of obtaining recycled carbon black powder by cooling, drying, and grinding the steam-activated recycled carbon black.

[0012] In step (b) above, during the steam activation treatment, steam is supplied into the reactor in the nitrogen atmosphere at a rate of 10 to 1,000 ml / min.

[0013] In step (b) above, the steam activation treatment is carried out at 900 to 1,000°C for 1 to 9 hours.

[0014] The above steam activation treatment is carried out at 900 to 1,000℃ for 2 to 4 hours.

[0015] The above steam-activated recycled carbon black powder is used as an additive to rubber composites.

[0016]

[0017] The regenerated carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention for achieving the above objective is a regenerated carbon black powder manufactured by a method for manufacturing regenerated carbon black powder with increased specific surface area through steam activation treatment, wherein the regenerated carbon black powder is characterized by having an IA value of 100 to 550 g / kg, an N2SA value of 100 to 380 m² / g, an OAN value of 100 to 200 ml / 100g, and a Tint value of 45 to 55% ITRB.

[0018]

[0019] A rubber composite comprising recycled carbon black powder with an increased specific surface area through steam activation treatment according to an embodiment of the present invention for achieving the above objective is a rubber composite comprising recycled carbon black powder manufactured by a method for manufacturing recycled carbon black powder with an increased specific surface area through steam activation treatment, wherein the recycled carbon black powder is characterized by having an IA value of 100 to 550 g / kg, an N2SA value of 100 to 380 m² / g, an OAN value of 100 to 200 ml / 100g, and a Tint value of 45 to 55% ITRB.

[0020] The above rubber composite comprises the above recycled carbon black powder and the rubber composition, and the above recycled carbon black powder comprises 1 to 30 parts by weight per 100 parts by weight of the rubber composition.

[0021] The above rubber composite has a tensile strength (TB) of 210 to 230 kgf / ㎠, a tensile modulus (M300) of 100 to 120 kgf / ㎠, and an elongation (EB) of 500 to 530%.

[0022]

[0023] High-quality carbon black powder using steam-activated recycled carbon black according to the present invention, the method for manufacturing the same, and the rubber composite containing the same achieve high performance by increasing the surface area of ​​the recycled carbon black through a steam activation treatment process and applying it to a rubber composite.

[0024] To this end, the high-quality carbon black powder using steam-activated recycled carbon black according to the present invention, the method for manufacturing the same, and the rubber composite including the same are manufactured by thoroughly controlling the steam activation treatment temperature, time, and amount of steam injection to optimize the economic efficiency and physical properties of recycled carbon black (rCB), by performing steam activation treatment at 900 to 1,000°C for 1 to 9 hours, most preferably at 900 to 1,000°C for 2 to 4 hours, thereby producing high-quality recycled carbon black (rCB) with an increased specific surface area.

[0025] As such, the high-quality carbon black powder using steam-activated recycled carbon black according to the present invention, the method for manufacturing the same, and the rubber composite containing the same have significantly improved the bonding strength with the rubber composition and durability. This is achieved by effectively increasing the specific surface area of ​​the recycled carbon black through steam activation treatment, whereas recycled carbon black without steam activation treatment had low specific surface area and activity, which limited the improvement of physical properties when applied to rubber composites.

[0026] As a result, the high-quality carbon black powder using steam-activated recycled carbon black according to the present invention, the method for manufacturing the same, and the rubber composite containing the same allow for the application of recycled carbon black to rubber composites at a higher proportion and lay the foundation for the economical production of high-quality rubber products, thereby enabling the simultaneous securing of eco-friendliness and economic efficiency for tire manufacturing and other industrial rubber products.

[0027] In addition, the high-quality carbon black powder using steam-activated recycled carbon black according to the present invention, the method for manufacturing the same, and the rubber composite containing the same improve the specific surface area and structural characteristics of the recycled carbon black (rCB) through a steam activation treatment process, thereby increasing the specific surface area and oil absorption capacity (OAN) of the recycled carbon black and enhancing the interaction with the rubber composition.

[0028] Accordingly, the high-quality carbon black powder using steam-activated recycled carbon black according to the present invention, the method for manufacturing the same, and the rubber composite containing the same have improved tensile strength (TB), tensile modulus (M300), etc., thereby increasing the mechanical strength of the rubber composite. This ultimately contributes to increasing the wear resistance of the rubber composite, making it possible to secure physical properties suitable for high-durability products such as tires.

[0029] In addition to the effects described above, the specific effects of the present invention are described together with the specific details for implementing the invention below.

[0030]

[0031] FIG. 1 is a process flowchart showing a method for manufacturing regenerated carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention.

[0032]

[0033] The aforementioned objectives, features, and advantages are described in detail below with reference to the attached drawings, thereby enabling those skilled in the art to easily implement the technical concept of the present invention. In describing the present invention, detailed descriptions of known technologies related to the present invention are omitted if it is determined that such descriptions would unnecessarily obscure the essence of the invention. Hereinafter, preferred embodiments according to the present invention will be described in detail with reference to the attached drawings. In the drawings, the same reference numerals are used to indicate the same or similar components.

[0034] Details not described in this specification that can be sufficiently technically inferred by a person skilled in the art are to be omitted.

[0035] In this specification, the statement that any component is disposed on the "upper (or lower)" of a component or on the "upper (or lower)" of a component may mean not only that any component is disposed in contact with the upper (or lower) surface of said component, but also that another component may be interposed between said component and any component disposed on (or below) said component.

[0036] Singular expressions used in this specification include plural expressions unless the context clearly indicates otherwise. In this application, terms such as "contains," "has," or "includes" should not be interpreted as necessarily including all of the various components described in the specification, and should be interpreted as meaning that some of the components may not be included or that additional components may be included.

[0037] With reference to the attached drawings, the regenerated carbon black powder with increased specific surface area through steam activation treatment according to a preferred embodiment of the present invention, the method for manufacturing the same, and the rubber composite containing the same will be described in detail as follows.

[0038]

[0039] FIG. 1 is a process flowchart illustrating a method for manufacturing regenerated carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention.

[0040] As illustrated in FIG. 1, a method for manufacturing regenerated carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention includes a regenerated carbon black transfer step (S110), a steam activation treatment step (S120), and a regenerated carbon black powder obtaining step (S130).

[0041]

[0042] Recycled carbon black transfer

[0043] In the recycled carbon black transfer step (S110), the recycled carbon black recovered by the pyrolysis process of waste tires is transferred to a reactor in a nitrogen atmosphere.

[0044] In the present invention, the term recycled carbon black may be referred to as recovered carbon black, recycle carbon black, recycled CB, RCB, rCB, and r-CB, respectively, and these are all defined as corresponding to synonyms.

[0045] In this way, in the recycled carbon black transfer step (S110), the recycled carbon black recovered by the pyrolysis process of waste tires is transferred into the reactor of a steam activation treatment device maintained in a nitrogen atmosphere for steam activation treatment. At this time, it is desirable to maintain a clean state so that impurities that may occur during the process do not enter the reactor of the steam activation device.

[0046] Here, creating a nitrogen atmosphere inside the reactor of the steam activation treatment device is intended to control the process so that oxidation reactions do not occur at high temperatures by removing oxygen.

[0047]

[0048] Steam activation processing

[0049] In the steam activation treatment step (S120), steam activation treatment is performed on the regenerated carbon black transferred to a reactor in a nitrogen atmosphere to increase the specific surface area of ​​the regenerated carbon black.

[0050] This steam activation treatment process is carried out for the purpose of improving the specific surface area and structural characteristics of recycled carbon black (rCB) to enhance the physical properties of the rubber composite through mixing with the rubber composition.

[0051] In this step, it is preferable to perform the steam activation treatment at 900 to 1,000°C for 1 to 9 hours. More preferably, it is preferable to perform the steam activation treatment at 900 to 1,000°C for 2 to 6 hours, and most preferably, it is preferable to perform the steam activation treatment at 900 to 1,000°C for 2 to 4 hours.

[0052] In this way, the steam activation treatment is performed by heating the inside of the reactor of the steam activation treatment device to 900 to 1,000°C and maintaining a high temperature state, and then reacting the regenerated carbon black (rCB) with steam for 1 to 9 hours to activate it.

[0053] At this time, the steam injected into the reactor of the steam activation treatment device acts as an activator to expand the pores on the surface of the regenerated carbon black (rCB) and increase the specific surface area. To this end, during the steam activation treatment, it is desirable to supply steam at a rate of 10 to 1,000 ml / min into the reactor under a nitrogen atmosphere.

[0054] Here, if the steam activation treatment temperature is below 900°C or the steam activation treatment time is less than 1 hour, the activation treatment is not properly performed, and the effect of increasing the specific surface area of ​​the regenerated carbon black (rCB) may be negligible. Conversely, if the steam activation treatment temperature exceeds 1,000°C or the steam activation treatment time exceeds 9 hours, additional improvement in physical properties is possible, but it is not desirable because the longer the process time, the higher the energy consumption and cost, and the limited effect of performance improvement.

[0055] Accordingly, in the present invention, it was confirmed through experiments that maintaining the steam activation treatment at 900 to 1,000°C for 2 to 4 hours is a condition that can optimize the economic efficiency and physical properties of regenerated carbon black (rCB). As such, in the present invention, high-quality regenerated carbon black (rCB) with an increased specific surface area was produced by thoroughly controlling the steam activation treatment temperature, time, and steam injection amount.

[0056] In this way, the present invention increases the surface area of ​​recycled carbon black by performing steam activation treatment, and thereby improves the physical properties of the rubber composite when used as an additive to the rubber composite.

[0057] To this end, the present invention allows for the effective increase in the specific surface area of ​​recycled carbon black by performing steam activation treatment on recycled carbon black recovered by the pyrolysis process of waste tires under a nitrogen atmosphere at a high temperature of 900 to 1,000°C for 1 to 9 hours. When used as an additive to rubber composites, the physical properties of the rubber composite can be significantly improved compared to recycled carbon black that has not undergone steam activation treatment, even within a short steam activation treatment time. As a result, high-quality, eco-friendly recycled carbon black powder applicable to tires and other rubber products can be provided, thereby contributing to the circular economy and increasing resource efficiency.

[0058]

[0059] Obtaining recycled carbon black powder

[0060] In the step of obtaining regenerated carbon black powder (S130), the regenerated carbon black treated with steam activation is cooled, then dried and ground to obtain regenerated carbon black powder.

[0061] In this step, the steam-activated regenerated carbon black passes through a cooling section to maintain its activated state and prevent damage to the micropore structure. At this time, cooling may be performed by air cooling or water cooling, but is not limited thereto.

[0062] Subsequently, the cooled regenerated carbon black passes through a drying section to be dried, and then is ground to optimize particle size and distribution. This drying can be performed by residence drying at 150 to 250°C for 1 to 6 hours, but is not limited thereto. At this time, a rotary cylinder type dryer may be used for drying.

[0063] In addition, grinding can be performed using any one selected from a hammer mill, a high-speed mixer, a ball mill, and an air jet mill, and among these, it is preferable to grind using a high-speed rotating hammer mill. After such grinding, the steam-activated regenerated carbon black can be ground into a fine powder having an average diameter of 500 μm or less.

[0064] In this step, the steam-activated recycled carbon black powder has an IA value of 100 to 550 g / kg and an N2SA value of 100 to 380 m² / g.

[0065] In addition, steam-activated regenerated carbon black powder has an OAN value of 100 to 200 ml / 100g and a Tint value of 45 to 55% ITRB.

[0066] For the above, a method for manufacturing regenerated carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention may be concluded.

[0067]

[0068] The regenerated carbon black powder with increased specific surface area through steam activation treatment according to an embodiment of the present invention, manufactured by the above-described process, has an IA value of 100 to 550 g / kg and an N2SA value of 100 to 380 m² / g.

[0069] In addition, steam-activated regenerated carbon black powder has an OAN value of 100 to 200 ml / 100g and a Tint value of 45 to 55% ITRB.

[0070]

[0071] Meanwhile, a rubber composite comprising recycled carbon black powder with an increased specific surface area through steam activation treatment according to an embodiment of the present invention comprises recycled carbon black powder produced by a method for producing recycled carbon black powder with an increased specific surface area through steam activation treatment.

[0072] In addition, a rubber composite comprising recycled carbon black powder with an increased specific surface area through steam activation treatment according to an embodiment of the present invention comprises recycled carbon black powder and a rubber composition, wherein the recycled carbon black powder comprises 1 to 30 parts by weight per 100 parts by weight of the rubber composition.

[0073] Here, if recycled carbon black powder is added in an amount of less than 1 part by weight per 100 parts by weight of the rubber composition, the effect of improving mechanical properties such as tensile strength (TB), tensile modulus (M300), and elongation (EB) of the rubber composite may be negligible. Conversely, if recycled carbon black powder is added in excess of 30 parts by weight per 100 parts by weight of the rubber composition, the viscosity increases, which leads to increased energy consumption during the mixing process with the rubber composition and may have a somewhat adverse effect on processability, so it is not desirable.

[0074] In order to optimize the bonding strength with the rubber composition by considering the specific surface area characteristics of steam-activated recycled carbon black, it is desirable to apply a method of maintaining conditions of a low temperature of 130°C or lower and a low mixing speed of 40 to 60 RPM during the mixing process between the rubber composition and the recycled carbon black powder.

[0075] A rubber composite comprising recycled carbon black powder with an increased specific surface area through steam activation treatment according to an embodiment of the present invention has a tensile strength (TB) of 210 to 230 kgf / ㎠, a tensile modulus (M300) of 100 to 120 kgf / ㎠, and an elongation (EB) of 500 to 530%.

[0076]

[0077] As described above, the high-quality carbon black powder using steam-activated regenerated carbon black according to the embodiment of the present invention, the method for manufacturing the same, and the rubber composite containing the same achieve high performance by increasing the surface area of ​​the regenerated carbon black through a steam activation process and applying it to a rubber composite.

[0078] To this end, the high-quality carbon black powder using steam-activated recycled carbon black according to an embodiment of the present invention, the method for manufacturing the same, and the rubber composite including the same are manufactured by thoroughly controlling the steam activation treatment temperature, time, and amount of steam injection to optimize the economic efficiency and physical properties of the recycled carbon black (rCB), by performing steam activation treatment at 900 to 1,000°C for 1 to 9 hours, most preferably at 900 to 1,000°C for 2 to 4 hours, thereby producing high-quality recycled carbon black (rCB) with an increased specific surface area.

[0079] As such, the high-quality carbon black powder using steam-activated recycled carbon black according to the embodiment of the present invention, the method for manufacturing the same, and the rubber composite containing the same have significantly improved the bonding strength with the rubber composition and durability by effectively increasing the specific surface area of ​​the recycled carbon black through steam activation treatment, whereas recycled carbon black without steam activation treatment had low specific surface area and activity, which limited the improvement of physical properties when applied to rubber composites.

[0080] As a result, the high-quality carbon black powder using steam-activated recycled carbon black according to the embodiment of the present invention, the method for manufacturing the same, and the rubber composite containing the same allow for the application of recycled carbon black to the rubber composite at a higher proportion and establish a foundation for the economical production of high-quality rubber products, thereby enabling the simultaneous securing of eco-friendliness and economic efficiency for tire manufacturing and other industrial rubber products.

[0081] In addition, the high-quality carbon black powder using steam-activated recycled carbon black according to an embodiment of the present invention, the method for manufacturing the same, and the rubber composite containing the same improve the specific surface area and structural characteristics of the recycled carbon black (rCB) through a steam activation treatment process, thereby increasing the specific surface area and oil absorption capacity (OAN) of the recycled carbon black and enhancing the interaction with the rubber composition.

[0082] Accordingly, the high-quality carbon black powder using steam-activated recycled carbon black according to an embodiment of the present invention, the method for manufacturing the same, and the rubber composite containing the same have improved tensile strength (TB), tensile modulus (M300), etc., thereby increasing the mechanical strength of the rubber composite. This ultimately contributes to increasing the wear resistance of the rubber composite, thereby enabling the securing of physical properties suitable for high-durability products such as tires.

[0083]

[0084] Examples

[0085] Hereinafter, the structure and operation of the present invention will be explained in more detail through preferred embodiments of the present invention. However, these are presented as preferred examples of the present invention and should not be interpreted in any way as limiting the present invention.

[0086] Details not listed here can be sufficiently technically inferred by a person skilled in this field, so their explanation will be omitted.

[0087]

[0088] 1. Evaluation of Physical Properties of Recycled Carbon Black

[0089] Table 1 shows the results of the physical property evaluation of recycled carbon black prepared according to Examples 1 to 9 and Comparative Examples 1 to 2. In this case, Table 1 shows the results of the physical property evaluation of recycled carbon black according to the steam activation treatment time. To evaluate the physical properties of recycled carbon black according to the steam activation treatment time, recycled carbon black recovered from a waste tire pyrolysis process was subjected to steam activation treatment for 1 to 10 hours under a nitrogen atmosphere at a high temperature of 950°C, respectively.

[0090]

[0091] (1) Uncured properties

[0092] 1) IA (Iodine Adsorption Number)

[0093] This is a method for analyzing the specific surface area of ​​carbon black based on the amount of iodine adsorbed. It was measured according to ASTM-D1510 standards. The higher the amount of iodine adsorbed, the smaller the particle size of the carbon black becomes, and conversely, the lower the amount of iodine adsorbed, the larger the particle size becomes.

[0094]

[0095] 2) N2SA (Nitrogen Surface Area, BET, ㎡ / g)

[0096] N2SA is a value representing the specific surface area of ​​carbon black measured using nitrogen gas in accordance with ASTM D-6556 standards. It is expressed in units of m² / g by measuring the area where nitrogen is adsorbed onto the carbon black surface through BET analysis. A higher BET surface area indicates smaller carbon black particle sizes and a larger surface area.

[0097]

[0098] 3) OAN (Oil Absorption number)

[0099] The OAN value is a value representing the amount of dibutyl phthalate (DBP) oil absorbed that can be contained in 100g of carbon black. OAN was measured according to the analysis method based on ASTM D2414 {measuring the amount of dibutyl phthalate oil adsorbed in 100g of carbon black (ml / 100g)}. A higher OAN value indicates that the structure of the carbon black is more complex and developed.

[0100]

[0101] 4)COAN (Compressed Oil Absorption Number, ㎖ / 100g)

[0102] COAN is a value that measures the amount of oil carbon black can absorb under compressed conditions according to ASTM D-3493, and indicates the bonding strength between particles. It measures the amount of oil absorbed per 100g of carbon black under compressed conditions (ml / 100g) and generally has a lower value than OAN.

[0103]

[0104] 5) Tint

[0105] Tint was measured according to ASTM-D3265 standards. As a value (% ITRB) representing the color of carbon black, a higher tint value indicates that the carbon black has a smaller particle size and a simpler structure. Conversely, a lower tint value indicates that the carbon black has a larger particle size and a more complex structure.

[0106]

[0107] [Table 1]

[0108]

[0109] As shown in Table 1, for the regenerated carbon black according to Examples 1 to 9, it was confirmed that the IA value (Iodine Adsorption), specific surface area (N2SA), and oil absorption amount (OAN) of the regenerated carbon black gradually increased as the steam activation treatment time increased.

[0110] More specifically, it was confirmed that the recycled carbon black according to Examples 1 to 9 satisfied all of the following values: an IA value of 100 to 550 g / kg, an N2SA value of 100 to 380 m² / g, an OAN value of 100 to 200 ml / 100g, and a Tint value of 45 to 55% ITRB. At this time, it was confirmed that Examples 2 to 6, in which steam activation treatment was performed for 2 to 6 hours, and especially Example 3, in which steam activation treatment was performed for 3 hours, exhibited the most ideal physical properties.

[0111] On the other hand, in the case of the regenerated carbon black according to Comparative Example 1, it was confirmed that the IA value (Iodine Adsorption), specific surface area (N2SA), and oil absorption amount (OAN) did not satisfy all target values ​​due to the fact that steam activation treatment was not performed.

[0112] In addition, it was confirmed that in the case of the recycled carbon black prepared according to Comparative Example 2, the IA value, OAN value, and Tint value deviated from the target values ​​due to the steam activation treatment being performed excessively for 10 hours.

[0113] As can be seen from the experimental results above, when recycled carbon black prepared according to Examples 1 to 9 is applied as an additive to a rubber composite, the bonding strength with the rubber composition is increased, and it is believed that this can contribute to the improvement of key physical properties such as wear resistance, heat resistance, and mechanical strength.

[0114]

[0115] 2. Evaluation of Rubber Composite Properties

[0116] Table 2 shows the results of the physical property evaluation of rubber composites prepared according to Examples 1 to 5 and Comparative Example 1, and Table 3 shows the results of the physical property evaluation of rubber composites prepared according to Examples 6 to 9 and Comparative Example 2. In this case, Tables 2 and 3 show the results of the physical property evaluation of rubber composites when carbon black powder mixed with 25 wt% of recycled carbon black (rCB) and 75 wt% of ordinary carbon black (nCB: N660) is added, which is subjected to steam activation treatment for 0 to 10 hours. Here, a rubber composite was prepared by adding recycled carbon black powder, ordinary carbon black powder, zinc oxide, stearic acid, TDAE (Treated Distillate Aromatic Extracted) oil, and 6PPD and RD (2,2,4-Trimethyl-1,2-dihydroquinoline (TMQ)) as additives to raw rubber, respectively, and stirring at 150°C for 5 minutes to prepare a master batch. Subsequently, S (Sulfur) and NS (rubber vulcanization accelerator, TBBS) were added to the master batch, and the mixture was prepared by stirring at 110°C for 2 minutes.

[0117]

[0118] 1) Mooney viscosity (ML1+4, 100℃)

[0119] Mooney viscosity (MV) was measured for each rubber composite according to ASTM D 1646: RUBBER FROM NATURAL OR SYNTHETIC SOURCES-VISCOSITY AND VULCANIZATION CHARACTERISTICS (MOONEY VISCOMETER). 50-ML1+4(100℃), where 50-M is the viscosity number, L indicates the use of a large rotor, 1 means the motor was preheated for 1 minute before operation, 4 means the specified measurement time, and 100℃ means the measurement temperature. A higher Mooney viscosity indicates poorer dispersibility of the components within the rubber composite. Mooney viscosity was measured at 50-ML1+4 (100°C) for each rubber composite according to ASTM D 1646. This measurement reflects the dispersibility of each component, and the MV value increases as the steam activation treatment time increases. This was determined to be because the interaction with the rubber composition was strengthened as the specific surface area and structure of the recycled carbon black (rCB) changed due to the steam activation treatment.

[0120]

[0121] 2) Vulcanization properties

[0122] Hardness was measured according to ASTM D-2240, and tensile modulus (M300), elongation break (EB), and tensile break (TB) were measured according to ASTM 412-98a.

[0123]

[0124] [Table 2]

[0125]

[0126]

[0127] [Table 3]

[0128]

[0129] As shown in Tables 2 and 3, for the rubber composites according to Examples 1 to 9, the hardness increases as the specific surface area (N2SA) and IA (Iodine Adsorption) of the recycled carbon black increase, thereby increasing the contact surface with the rubber composition. Consequently, the physical bonding force between the rubber composite and the recycled carbon black is strengthened. This causes the rubber composite to become harder. Additionally, as the oil absorption amount (OAN) increases, the structure of the carbon black develops. The carbon black with a developed structure adsorbs more rubber, strengthening the interaction between the carbon black and the rubber, and tends to be dispersed more uniformly within the rubber composite. As a result, the density of the rubber composite increases, and the hardness also increases.

[0130] In addition, for the rubber composites according to Examples 1 to 9, the tensile modulus (M300) and elongation (EB) are strengthened as the specific surface area and structural properties of the recycled carbon black change with increasing steam activation treatment time, thereby increasing the bonding strength with the rubber composition. As a result, the recycled carbon black bonds more strongly with the rubber molecules within the rubber composite, increasing the resistance of the rubber composite. However, the tensile modulus (M300) is influenced by the interaction and strength between the carbon black and the rubber matrix. Initially, as the dispersion and stiffness of the carbon black increase, the tensile modulus (M300) also rises.

[0131] However, as with the rubber composite according to Comparative Example 2, when a certain level is exceeded, the stress distribution ability within the compound decreases, and a phenomenon occurs in which the stiffness actually decreases. This is because excessive carbon black dispersion causes aggregation, which disrupts the flexibility and balance of the rubber composite. Conversely, when the tensile modulus (M300) increases, the strength of the polymer composite increases, but the flexibility decreases, resulting in a lower elongation (EB) value. When the tensile modulus (M300) begins to decrease, the flexibility recovers, and the elongation (EB) value tends to rise.

[0132] In addition, for the rubber composites according to Examples 1 to 9, as the steam activation treatment time increases, the specific surface area (N2SA) and oil absorption amount (OAN) of the carbon black increase, thereby further strengthening the bonding force between the rubber composition and the carbon black. As a result, a higher tensile strength (TB) can be achieved within the rubber composite. Tensile strength (TB) is influenced by the stiffness of the compound and the balanced elongation rate. While tensile strength (TB) increases when the tensile modulus (M300) increases, excessive stiffness can actually impede the flexibility of the compound and cause a decrease in tensile strength (TB). Therefore, when the tensile modulus (M300) decreases after exceeding a certain range, tensile strength (TB) also decreases.

[0133]

[0134] 3. Conclusion

[0135] In this experiment, changes in the physical properties of a rubber composite were analyzed when 25 wt% of recycled carbon black (rCB), which had been steam-activated for 0 to 10 hours, was mixed with 75 wt% of ordinary carbon black.

[0136] Through this experiment, it was found that the content of recycled carbon black as a high-quality carbon black additive can be added at a constant level of 25 wt% or less, and as can be seen in Tables 2 and 3, it was confirmed that the physical properties of the rubber composite, such as tensile strength (TB), tensile modulus (M300), and elongation (EB), were generally improved.

[0137] In particular, for the rubber composites according to Examples 1 to 9, it was confirmed that as the steam activation treatment time increased, the tensile modulus (M300) and elongation (EB) were strengthened as the specific surface area and structural properties of the recycled carbon black changed, and the bonding strength with the rubber composition was enhanced. As a result, for the rubber composites according to Examples 1 to 9, it was confirmed that the resistance of the rubber composite increased as the recycled carbon black bonded more strongly with the rubber molecules within the rubber composite.

[0138] However, as the steam activation treatment time increases, the physical property values ​​of the rubber composite, such as MV (Mooney Viscosity), also increase; yet, when the steam activation treatment is performed for a long period exceeding 9 hours, it was found to have a negative effect on the heat resistance and durability of the rubber composite. Therefore, when recycled carbon black that has undergone steam activation treatment for 1 to 9 hours is used, it was found that the physical properties of the rubber composite, such as tensile strength (TB), tensile modulus (M300), and elongation (EB), are improved.

[0139] As with the rubber composite according to Comparative Example 2, it was confirmed that when the steam activation treatment time exceeds a certain level of 10 hours, the stress distribution ability within the compound decreases, and the stiffness actually decreases. This is because excessive carbon black dispersion causes aggregation, which disrupts the flexibility and balance of the rubber composite. Conversely, when the tensile modulus (M300) increases, the strength of the polymer composite increases, but the flexibility decreases, resulting in a lower elongation (EB) value. When the tensile modulus (M300) begins to decrease, the flexibility recovers, and the elongation (EB) value tends to rise.

[0140] In addition, it was confirmed that the rubber composite according to Comparative Example 1 did not satisfy the target values ​​for hardness, tensile strength (TB), and tensile modulus (M300).

[0141] Therefore, in this experiment, it was confirmed that in the case of a rubber composite in which 25 wt% of recycled carbon black, which has been steam-activated at 900 to 1,000°C for 1 to 9 hours, most preferably at 900 to 1,000°C for 2 to 4 hours, is added in combination with general carbon black, the tensile strength (TB), tensile modulus (M300), etc. are improved, thereby increasing the mechanical strength of the rubber composite, which ultimately contributes to increasing the wear resistance of the rubber composite, thereby enabling the securing of physical properties suitable for high-durability products such as tires.

[0142]

[0143] Although the present invention has been described above with reference to embodiments, various changes and modifications can be made by those skilled in the art to which the present invention pertains. Such changes and modifications are considered to be within the scope of the present invention as long as they do not depart from the technical concept provided by the present invention. Accordingly, the scope of rights of the present invention should be determined by the claims set forth below.

[0144]

[0145] [Explanation of the symbol]

[0146] S110: Recycled Carbon Black Transfer Step

[0147] S120: Steam activation processing step

[0148] S130: Step to obtain recycled carbon black powder

Claims

1. (a) A step of transferring recycled carbon black recovered by the pyrolysis process of waste tires to a reactor in a nitrogen atmosphere; (b) a step of increasing the specific surface area of ​​the regenerated carbon black by performing a steam activation treatment that steam heat-treats the regenerated carbon black transferred to the above-mentioned nitrogen atmosphere reactor; and (c) a step of cooling the steam-activated regenerated carbon black, then drying and grinding it to obtain regenerated carbon black powder; Characterized by including, Method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment.

2. In Paragraph 1, In step (b) above, When performing the above steam activation process, Characterized by supplying steam at a rate of 10 to 1,000 ml / min into the above-mentioned nitrogen atmosphere reactor, Method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment.

3. In Paragraph 1, In step (b) above, The above steam activation process is Characterized by being carried out at 900 to 1,000℃ for 1 to 9 hours, Method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment.

4. In Paragraph 3, The above steam activation process is Characterized by being carried out at 900 to 1,000℃ for 2 to 4 hours, Method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment.

5. In Paragraph 1, The above steam-activated recycled carbon black powder is Characterized by being used as an additive to rubber composites, Method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment.

6. Recycled carbon black powder manufactured by a method for manufacturing recycled carbon black powder with increased specific surface area through steam activation treatment according to any one of claims 1 to 4, wherein The above recycled carbon black powder is Characterized by having an IA value of 100 to 550 g / kg, an N2SA value of 100 to 380 m² / g, an OAN value of 100 to 200 ml / 100g, and a Tint value of 45 to 55% ITRB, Regenerated carbon black powder with increased specific surface area through steam activation treatment.

7. A rubber composite comprising recycled carbon black powder manufactured by a method for manufacturing recycled carbon black powder with an increased specific surface area through steam activation treatment according to any one of claims 1 to 4, The above recycled carbon black powder is Characterized by having an IA value of 100 to 550 g / kg, an N2SA value of 100 to 380 m² / g, an OAN value of 100 to 200 ml / 100g, and a Tint value of 45 to 55% ITRB, A rubber composite containing recycled carbon black powder with increased specific surface area through steam activation treatment.

8. In Paragraph 7, The above rubber composite is, The above-mentioned recycled carbon black powder and rubber composition, characterized in that the recycled carbon black powder comprises 1 to 30 parts by weight per 100 parts by weight of the rubber composition. A rubber composite containing recycled carbon black powder with increased specific surface area through steam activation treatment.

9. In Paragraph 7, The above rubber composite is Characterized by having a tensile strength (TB) of 210 to 230 kgf / ㎠, a tensile modulus (M300) of 100 to 120 kgf / ㎠, and an elongation (EB) of 500 to 530%. A rubber composite containing recycled carbon black powder with increased specific surface area through steam activation treatment.

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