Method of preparing activated carbon using waste marine bio-resources and activated carbon prepared thereby

KR103020596B1Active Publication Date: 2026-09-22IKSUNG CO LTD +1
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Application Number
KR1020250045960
Authority / Receiving Office
KR · KR
Patent Type
Patents
Current Assignee / Owner
Filing Date
2025-04-09
Publication Date
2026-09-22
Estimated Expiration
2045-04-09

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Abstract

The present invention relates to a method for producing activated carbon using marine biological resources, comprising the steps of: crushing marine biological resources; pre-treating the crushed marine biological resources; carbonizing the pre-treated marine biological resources at low temperature; and activating the low-temperature carbonized marine biological resources, and to activated carbon produced therefrom.
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Description

Technology Field

[0001] The present invention relates to a method for producing activated carbon using marine biological resources and activated carbon produced therefrom. Background Technology

[0003] In general, activated carbon is a material that plays a crucial role in various industrial fields due to its excellent adsorption performance. It is widely used primarily in water and air purification, establishing itself as an essential material for environmental protection and pollutant removal. Additionally, it is utilized as a material in diverse areas such as industrial gas treatment, catalysts for chemical reactions, purification of food and beverages, pharmaceuticals, electronic devices, and batteries.

[0004] In particular, activated carbon possesses excellent adsorption capabilities for harmful substances, playing a crucial role in removing harmful gases from the air and heavy metals and organic compounds from water. It is also used as an essential material in incinerators, exhaust gas treatment systems, and wastewater treatment systems. Furthermore, as an industrial adsorbent, it plays an important role in fine chemical and petrochemical processes and is utilized in fertilizer manufacturing and drinking water treatment.

[0005] Currently, there is a high degree of dependence on overseas technology for most raw materials and manufacturing processes of activated carbon. Domestic production of the raw materials required for manufacturing activated carbon is virtually non-existent, and all raw materials are imported. In particular, raw materials are imported in a form where grinding and carbonization processes have already been completed, and only a portion undergoes an activation process domestically to meet customer requirements before being supplied to the market as a final product.

[0006] As such, if both the raw materials and processes required to manufacture activated carbon are entirely dependent on foreign sources, various problems may arise, such as price fluctuations, supply instability, and differences in raw material quality. Furthermore, there may be difficulties in producing activated carbon that reflects the unique requirements tailored to the characteristics of the domestic industry.

[0007] Therefore, as the demand for activated carbon increases, localization is becoming increasingly necessary. Prior art literature

[0009] Republic of Korea Published Patent Application No. 10-2025-0010440 The problem to be solved

[0010] The present invention aims to provide a method for producing activated carbon with a high specific surface area and excellent yield using marine biological resources, and in particular, to provide activated carbon with excellent gas adsorption effect.

[0011] The present invention aims to provide activated carbon produced from the above method for producing activated carbon. means of solving the problem

[0013] The present invention, for solving the problems described above, provides a method for producing activated carbon using marine biological resources, comprising the steps of: crushing marine biological resources; pre-treating the crushed marine biological resources; carbonizing the pre-treated marine biological resources at low temperature; and activating the low-temperature carbonized marine biological resources.

[0014] The above marine biological resources are of the genus Sargassum ( Sargassum It could be a bird.

[0015] The above marine biological resource is a type of snail ( Sargassum thunbergii ), Sargassum ( Sargassum horneri ), Alssongi Sargassum ( Sargassum confusum ), twisted seaweed ( Sargassum siliquastrum ), large-leaved Sargassum ( Sargassum coreanum ), paired-leaf Sargassum ( Sargassum hemiphyllum ) and double-stemmed Sargassum ( Sargassum patens It may be one or more selected from ). Specifically, it may be Sargassum horneri.

[0016] The grinding step described above can be performed under conditions of 10,000 RPM to 50,000 RPM.

[0017] The average particle size (D50) of the above-mentioned crushed marine biological resources may be 15 μm to 60 μm.

[0018] It may be that a washing step is not performed prior to the grinding step mentioned above.

[0019] The above pretreatment step may be performed by mixing the crushed marine biological resources with one or more selected from the group consisting of an aqueous phosphate solution and an aqueous alkali compound solution.

[0020] The above phosphate is one or more selected from the group consisting of ammonium phosphate, potassium phosphate, and sodium phosphate, and the above alkali compound may be one or more selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetrahydroxymethylammonium, and tetrahydroxyethylammonium.

[0021] The above-mentioned crushed marine biological resources and one or more of the above-mentioned aqueous phosphate solution and aqueous alkali compound solution may be mixed in a weight ratio of 1:1 to 1:10.

[0022] The above low-temperature carbonization step can be performed under temperature conditions of 200 ℃ to 400 ℃.

[0023] The above-mentioned activating step can be performed under temperature conditions of 500 ℃ to 1,200 ℃.

[0024] In addition, the present invention, for solving the problems described above, provides activated carbon produced from a manufacturing method using the marine biological resources described above.

[0025] The carbon content of the above activated carbon may be 82% by weight to 99% by weight.

[0026] The BET specific surface area of ​​the above activated carbon is 500 m² 2 / g to 2,000 m 2 It can be / g. Effects of the invention

[0028] Activated carbon produced by the method using marine biological resources according to the present invention has a high yield and BET specific surface area, and can have an excellent gas adsorption effect.

[0029] The effects of the present invention are not limited to those mentioned above, and other unmentioned effects will be clearly understood by a person skilled in the art from the description below. Brief explanation of the drawing

[0031] Figure 1 is a graph showing the yield according to the carbonization temperature of Sargassum horneri according to one embodiment of the present invention. Figure 2 is a graph showing the BET specific surface area according to the carbonization temperature of Sargassum horneri according to one embodiment of the present invention. Figure 3 is the result of analyzing the thermal decomposition characteristics of Sargassum horneri according to one embodiment of the present invention. Figure 4 is an SEM image of crushed Sargassum horneri according to one embodiment of the present invention. Figure 5 is a particle size distribution of crushed Sargassum horneri according to one embodiment of the present invention. Figure 6 is an SEM image of activated carbon according to one embodiment of the present invention. Specific details for implementing the invention

[0032] The advantages and features of the present invention and the methods for achieving them will become clear by referring to the embodiments described in detail below. However, the present invention is not limited to the embodiments disclosed below but can be implemented in various different forms. These embodiments are provided merely to ensure that the disclosure of the present invention is complete and to fully inform those skilled in the art of the scope of the present invention, and the present invention is defined only by the scope of the claims.

[0033] The terms used herein are for describing the embodiments and are not intended to limit the invention. In this specification, the singular form includes the plural form unless specifically stated otherwise in the text. As used herein, "comprises" and / or "comprising" do not exclude the presence or addition of one or more other components in addition to the components mentioned. Throughout the specification, "and / or" includes each of the components mentioned and all combinations of one or more.

[0034] Units used in this specification without special notation are based on weight, and, for example, units of % or ratio mean weight % or weight ratio.

[0035] Unless otherwise defined, all terms used herein (including technical and scientific terms) may be used in a meaning commonly understood by those skilled in the art to which the present invention pertains. Additionally, terms defined in commonly used dictionaries are not to be interpreted ideally or excessively unless explicitly and specifically defined otherwise.

[0037] The present invention will be described in detail below.

[0038] The present invention provides a method for producing activated carbon using marine biological resources, comprising the steps of: crushing marine biological resources; pre-treating the crushed marine biological resources; carbonizing the pre-treated marine biological resources at low temperature; and activating the low-temperature carbonized marine biological resources. Through this, activated carbon with excellent BET specific surface area and superior gas adsorption effect can be provided from marine biological resources with a high yield.

[0039] In one embodiment, the marine biological resource is of the genus Sargassum ( Sargassum It could be a bird.

[0040] Sargassum is a member of the Sargassum genus ( Sargassum It is a general term for birds. Specific species Sargassum fulvellum It is also used as a general term for large brown algae. The body is outwardly distinct in terms of roots, stems, and leaves; the roots are disc-shaped and grow to over 1–3 meters in height by producing a single central branch. The stems are triangular or triangular and twisted. The leaves grow from the stem toward the base, curve, and are spatula-shaped or oval, with a midrib extending to the center. The upper leaves are lanceolate with serrated projections along the margins, and air bubbles form all over the body, extending from the stem. It is dark yellowish-brown in color and can be found along the entire coast of Korea. As a representative species of Sargassum used for food, it is commonly sold in markets. The genus Sargassum is a warm-water plant that is perennial and is a representative species that forms underwater forests along the Korean coast.

[0041] In one embodiment, the marine biological resource is a snail ( Sargassum thunbergii ), Sargassum ( Sargassum horneri ), Alssongi Sargassum ( Sargassum confusum ), twisted seaweed ( Sargassum siliquastrum ), large-leaved Sargassum ( Sargassum coreanum ), paired-leaf Sargassum ( Sargassum hemiphyllum ) and double-stemmed Sargassum ( Sargassum patens It may be one or more selected from ). Specifically, it may be Sargassum horneri.

[0042] The aforementioned *Jichungi* has a dark brown plant body. A single, short stem emerges from a button-shaped appressor, and this stem produces several cord-like central branches. Many very short branches grow from the central branch, and since these short branches are covered by numerous thorn-like leaves and awl-shaped air sacs, it appears as if there are no branches and the leaves and air sacs grow directly on the central branch. The reproductive branches are small, slender, and rod-shaped, growing on the short branches.

[0043] The aforementioned *Alssongi* (Sargassum) grows from the lower intertidal zone to the intertidal zone. The plant body grows to a height of 0.6–2 m, producing one or two to three short central branches from a disc-shaped root. The central branches are cylindrical and have small spines. The lower leaves are oval or spatulate, 7 cm long, with a buried midrib. The leaf margins are serrated, though sometimes they are absent. The upper leaves are highly variable but are usually long lanceolate, 3–5 cm long, tapering at both ends. Air sacs usually form at the base of small branches and are spherical; young ones are obovate and have a tibial tip. It is distributed in Korea, Sakhalin, the Kuril Islands, China, and other regions.

[0044] The above-mentioned Sargassum siliquastrum lives attached to rocks in the intertidal zone, extending from near the low tide line to the intertidal zone. Its length is usually 2 to 3 meters, but some reach tens of meters. Although it varies in unique shape depending on the season and habitat, generally, the leaves at the base are wide and lack double serrations; the branches are triangular and twisted in a pretzel shape. It stands upright underwater due to the air bubbles covering the upper part. It is mainly distributed in Korea (including Bijindo, Yokjido, Eocheongdo, and Jeju Island) and Japan.

[0045] The aforementioned *Sargassum gigantea* is distributed along the east and south coasts of Korea and Jeju Island. It is an edible brown algae belonging to the family Sargassumidae; its young stems and leaves are eaten, while the entire plant is dried and used as animal feed. *Sargassum gigantea* has a conical root 5–8 cm in length and a cylindrical central stem 5–7 mm in thickness emerging from the root, which branches out to produce leaves and branches.

[0046] The above-mentioned *Sargassum fusiformis* is a marine algae belonging to the family *Sargassum* in the order *Pucales*. It grows to a height of 30–50 cm, has thread-like roots, and has multiple stems emerging from a single point that branch out alternately. The leaves appear as if about half of them have been torn off vertically. The species name is derived from the fact that the leaf shape is not bilaterally symmetrical. The air sacs are egg-shaped or spindle-shaped, with some having rounded tips and others having pointed tips. It grows on rocks below the intertidal zone and is distributed along the east coast of Korea, Jeju Island, Japan, and the Pacific Ocean.

[0047] The aforementioned *Sargassum fusiforme* grows epiphytically in the lower intertidal zone, with stems rising upright from large discoid roots to a height of 1 meter or more. The stems are usually flattened, with thin margins, and branch into many central branches, which further branch in a feather-like fashion. The leaves at the base are elongated and bamboo-leaf-like, measuring 5–10 mm in width and 2–5 cm in length; they have flattened petioles and sometimes divide to form multiple alternate or feather-like leaves. The upper leaves are slender and linear, constricted at the base, and generally alternate. The air sacs are elliptical or obovate with flattened petioles, and there are crown leaves. In Korea, it grows in areas such as Ulleungdo, Yeosu, Wando, and Jeju.

[0048] In particular, the aforementioned Sargassum horneri washes ashore near the coastal waters of the southwestern region of Korea, including Jeju Island, from autumn to the following spring, obstructing ship navigation, damaging lifting facilities, and causing environmental pollution due to decay. Consequently, significant resources, including manpower, equipment, and collection sites, are allocated to the collection and disposal process to prevent marine pollution. As a result, floating Sargassum horneri flowing into nearshore waters is classified and managed as a harmful marine organism.

[0049] Currently, most Sargassum is utilized as compost for farms; however, processing Sargassum requires significant effort and labor, as it must be sorted and provided to farmers to be used as compost due to foreign substances such as marine debris and sand entangled within it, as well as salt and heavy metals. Furthermore, as there are almost no other treatment methods besides composting, problems are expected to worsen due to the ever-increasing influx of Sargassum.

[0050] In particular, this invention not only manufactures activated carbon by utilizing marine biological resources, but also produces high-value-added activated carbon that is highly useful industrially by using Sargassum horneri, which is classified as a waste marine organism, as a raw material, enabling its use in various industrial fields such as air purification, water purification, and chemical removal. Furthermore, producing activated carbon using Sargassum horneri is more affordable than using conventional activated carbon raw materials, and simultaneously allows for the recycling of marine biological resources, resulting in high economic value.

[0051] As such, producing high-value activated carbon by utilizing various marine biological resources, particularly waste marine biological resources such as Sargassum horneri, offers advantages in various aspects such as environmental protection, resource recycling, and the creation of industrial value, and can play an important role in reducing marine pollution and promoting sustainable economic activities.

[0052] In one embodiment, the grinding step may be performed under conditions of 10,000 RPM to 50,000 RPM, 15,000 RPM to 40,000 RPM, or 20,000 RPM to 30,000 RPM. Additionally, the grinding step may be performed for 30 seconds to 5 minutes, or 1 minute to 3 minutes.

[0053] When marine biological resources are ground under the above conditions, the grinding efficiency is maximized, and the particle size can be maintained small and consistent. Through this, the ground particles can exhibit a uniform reaction during subsequent pretreatment and low-temperature carbonization processes, and the adsorption capacity and BET surface area of ​​activated carbon can be improved with excellent yield.

[0054] In one embodiment, the average particle size (D50) of the crushed marine biological resource may be 15 μm to 60 μm, 10 μm to 40 μm, or 15 μm to 30 μm. When producing activated carbon through low-temperature carbonization and activation steps from a marine biological resource having an average particle size within the above range, the surface area can be optimized, which is advantageous for increasing the BET specific surface area, and the crushed particles thus can induce a uniform reaction during the activation and carbonization process to produce activated carbon of uniform quality.

[0055] The above average particle size (D50) can be measured, for example, using a laser diffraction method or a scanning electron microscope (SEM) image, and the average particle size (D50) of the particle can be defined as the particle size at the 50% standard of the particle size distribution (the particle size corresponding to the volume cumulative 50% of the particle size distribution).

[0056] In one embodiment, a washing step may not be performed prior to the grinding step. If a washing step is not performed prior to the grinding step, it may be more advantageous in terms of yield and BET specific surface area. Specifically, the yield may be higher if washing is not performed.

[0057] In one embodiment, the pretreatment step may be performed by mixing the crushed marine biological resources with one or more selected from the group consisting of an aqueous phosphate solution and an aqueous alkali compound solution. By pretreating through chemical treatment under the above conditions, a structure more favorable for activation during the low-temperature carbonization process can be created, and the surface of the activated carbon can be roughened to increase the BET specific surface area.

[0058] In the above pretreatment step, the phosphate and alkali compounds may be mixed in an aqueous solution. The phosphate and alkali compounds may each be included in the aqueous solution at a concentration of 10% to 30% by weight, or 15% to 25% by weight.

[0059] In one embodiment, the phosphate is one or more selected from the group consisting of ammonium phosphate, potassium phosphate, and sodium phosphate, and the alkali compound may be one or more selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetrahydroxymethylammonium, and tetrahydroxyethylammonium.

[0060] In one embodiment, the crushed marine biological resource and one or more of the aqueous phosphate solution and the aqueous alkali compound solution may be mixed in a weight ratio of 1:1 to 1:10, 1:1 to 1:8, 1:1 to 1:5, or 1:1 to 1:2. By pre-treating by mixing the crushed marine biological resource with the alkali compound in a weight ratio within the above range, the crushed marine biological resource and the alkali compound are uniformly distributed on the surface of the marine biological resource, thereby imparting excellent activated carbon characteristics during the activation process, which can improve the BET specific surface area and gas adsorption effect of the activated carbon.

[0061] In one embodiment, the low-temperature carbonization step may be performed under temperature conditions of 200 ℃ to 400 ℃, 200 ℃ to 350 ℃, or 250 ℃ to 300 ℃.

[0062] The above low-temperature carbonization step can be performed for a holding time of 30 minutes to 3 hours, 40 minutes to 2 hours, or 50 minutes to 1 hour and 20 minutes.

[0063] The above low-temperature carbonization step can be maintained after reaching the desired temperature at a heating rate of 0.1 ℃ / min to 5 ℃ / min, 0.5 ℃ / min to 3 ℃ / min, or 1 ℃ / min to 2 ℃ / min.

[0064] The low-temperature carbonization step described above can be performed under an atmospheric atmosphere, a CO2 atmosphere, a nitrogen atmosphere, or a mixed gas atmosphere of CO2 and nitrogen. For example, the low-temperature carbonization step may be performed under a mixed gas atmosphere of CO2 and nitrogen. As a specific example, in the low-temperature carbonization step, the heating phase may be performed under a nitrogen atmosphere, and the temperature maintenance phase may be performed under a CO2 atmosphere. By controlling the gas atmosphere during low-temperature carbonization in this manner, the BET specific surface area of ​​marine biological resources can be further improved.

[0065] When pulverized marine biological resources are carbonized under the above conditions, carbonization reactions caused by excessive heat can be prevented, carbon content can be increased, and heat resistance can be improved. In addition, activated carbon with an excellent BET specific surface area can be formed by exhibiting higher efficiency during the activation stage.

[0066] The above-mentioned activating step may be performed under temperature conditions of 500 ℃ to 1,200 ℃, 500 ℃ to 1,100 ℃, 600 ℃ to 1,000 ℃, or 700 ℃ to 1,000 ℃.

[0067] In addition, the activation step may be performed for a maintenance time of 30 minutes to 3 hours, 40 minutes to 2 hours, or 50 minutes to 1 hour and 20 minutes.

[0068] In addition, the above-mentioned activating step may maintain the temperature after reaching the desired temperature at a heating rate of 3 ℃ / min to 10 ℃ / min, 4 ℃ / min to 8 ℃ / min, or 5 ℃ / min to 8 ℃ / min.

[0069] Activating low-temperature carbonized marine biological resources under the above conditions provides optimal activation conditions, and in this process, the adsorption capacity and specific surface area of ​​the activated carbon can be significantly enhanced. Meanwhile, while higher activation temperatures open the surface more, increasing the volume of micropores and enhancing oxidation prevention and adsorption capabilities, excessively high temperatures can lead to a loss of structural stability; therefore, activation within an appropriate temperature range is crucial.

[0070] In one embodiment, after the step of activating the low-temperature carbonized marine biological resource, the step of washing and / or drying the activated marine biological resource may be further included. In the washing step, water at least twice the weight of the activated marine biological resource, for example, distilled water, may be used for washing.

[0071] The drying step may be performed for 5 to 24 hours, 8 to 20 hours, or 8 to 15 hours under temperature conditions of 80 ℃ to 200 ℃, 100 ℃ to 200 ℃ to 120 ℃ to 200 ℃, or 130 ℃ to 170 ℃.

[0072] In this way, by further including a step of washing and / or drying the activated marine biological resources after the step of activating the low-temperature carbonized marine biological resources, the phosphate and alkali compounds used in the pretreatment step can be effectively removed, thereby improving the quality of the finally produced activated carbon.

[0074] The present invention provides activated carbon produced by a manufacturing method using the above-described marine biological resources. Currently, activated carbon is manufactured using coconut shells or coal as raw materials and relies entirely on imports. In contrast, the present invention enables the localization of activated carbon by manufacturing it using marine biological resources as raw materials.

[0075] The carbon content of the above activated carbon may be 82% to 99% by weight, 85% to 95% by weight, or 90% to 95% by weight. If the holding time in the low-temperature carbonization process is increased, the oxygen content may decrease and the carbon content may be further increased. In the case of general-purpose activated carbon, the carbon content is generally 80% by weight and the oxygen content is 20% by weight; it can be seen that the carbon content of the activated carbon produced by the method according to the present invention is superior to this. The activated carbon according to the present invention, which has such a high carbon content, has a finer and more complex pore structure, resulting in excellent adsorption performance. The adsorption efficiency for various gases or harmful substances is significantly improved, allowing it to be used efficiently in various industrial fields.

[0076] The BET specific surface area of ​​the above activated carbon is 500 m² 2 / g to 2,000 m 2 / g, 1,000 m 2 / g to 2,000 m 2 / g, or 1,200 m 2 / g to 1,600 m 2 It can be / g. By having a high BET specific surface area within the above range, the adsorption efficiency for various gases or hazardous substances is significantly improved, allowing it to be used efficiently in various industrial fields.

[0078] Specific embodiments of the present invention are presented below. However, the embodiments described below are merely for the purpose of specifically illustrating or explaining the present invention and should not be limited thereby. Furthermore, details not described herein can be sufficiently technically inferred by a person skilled in the art, so such description is omitted.

[0080] [Preparation Example]

[0081] Preparation Examples 1-1 to 1-4

[0082] As shown in Table 1 below, the yield and BET specific surface area of ​​Sargassum horneri were measured according to whether or not it was washed and pretreated.

[0083] Preparation Example 1-1 involved drying the Sargassum horneri raw material at 80°C for 12 hours without washing or pretreatment.

[0084] Preparation Example 1-2 involved washing the Sargassum horneri raw material by repeating washing and rinsing five times with water, and drying it at 80°C for 12 hours.

[0085] Preparation Example 1-3 was pretreated by soaking the Sargassum horneri raw material in a mixture of 100 g of ammonium phosphate and 5 L of water for 5 minutes, and then drying it at 80 ℃ for 12 hours.

[0086] Preparation Example 1-4 involved washing the Sargassum horneri raw material by repeating washing and rinsing 5 times with water, then pretreating it by soaking it in a mixture of 100 g of ammonium phosphate and 5 L of water for 5 minutes, and drying it at 80 ℃ for 12 hours.

[0087] transference number

[0088] The weight ratio of the Sargassum obtained after drying to the weight of the Sargassum raw material was calculated.

[0089] BET specific surface area

[0090] Nitrogen adsorption experiments at 77K were conducted using a Belsorp max instrument, and the specific surface area (SBET) was derived using the Brunauer-Emmett-Teller (BET) equation. Additionally, the total pore volume (V Total ) was obtained using the adsorption curve up to a relative pressure of 0.990.

[0091] Preparation Example 1-1 Preparation Example 1-2 Preparation Example 1-3 Preparation Example 1-4 purifying X ○ X ○ Preprocessing X X ○ ○ transference number 87.7 53.5 66 46.9 BET 191 153 363 320

[0092] Looking at Table 1 above, it was confirmed that the yield and BET specific surface area values ​​were relatively low when the washing process was performed. In the case of Preparation Example 1-3, which performed only pretreatment without washing, the yield and BET specific surface area were the highest, excluding Preparation Example 1-1, which did not perform either washing or pretreatment.

[0093] Preparation Examples 2-1 to 2-4

[0094] The Sargassum horneri according to Preparation Examples 1-1 to 1-4 above were each placed on a zirconia crucible and carbonized in a hot air oven at a temperature of 400°C to 800°C. As a result, the measured yield is shown in Fig. 1 below.

[0095] Here, the carbonization was performed by injecting nitrogen at 5 ℃ / min and maintaining the temperature for 30 minutes.

[0096] transference number

[0097] The weight ratio of Sargassum horneri obtained after carbonization compared to before carbonization was calculated.

[0098] Looking at Figure 1, it was confirmed that the yield decreased as the temperature increased due to carbonization results at different temperatures. Specifically, while there were differences in yield due to washing and / or pretreatment, the trend of yield reduction due to temperature was confirmed to be distinct.

[0100] In addition, when the Sargassum horneri according to Preparation Example 1-3 was placed on a zirconia crucible and carbonized in a hot air oven at a temperature of 400°C to 800°C, the BET specific surface area was confirmed, and the results are shown in Fig. 2 below.

[0101] Referring to Fig. 2, the BET specific surface area value according to the carbonization temperature is 200 m² 2 / g to 400 m 2 It was confirmed at the / g level.

[0103] In addition, the Sargassum horneri according to Preparation Examples 1-3 above was placed on a zirconia crucible and its thermal decomposition characteristics were analyzed in a hot air oven under a nitrogen atmosphere at a temperature of 200 ℃ to 1,000 ℃, and the results are shown in Fig. 3 below.

[0104] Looking at Fig. 3(a), it was observed that weight loss began around 450 ℃, and a yield of approximately 25% was confirmed when the temperature was raised to 1,000 ℃. Additionally, looking at Fig. 3(b), it was impossible to confirm crystallization and melting temperatures based on DSC analysis results, which can be attributed to the high carbon temperature.

[0106] [Examples and Comparative Examples]

[0107] Example 1

[0108] The Sargassum horneri raw material was ground at 25,000 RPM for 2 minutes and classified to obtain ground Sargassum horneri with an average particle size (D50) of 15 μm to 30 μm. Here, a scanning electron microscope (SEM) image of the ground Sargassum horneri is shown in Fig. 4 below, and a particle size distribution is shown in Fig. 5 below.

[0109] The above-mentioned crushed Sargassum horneri was pretreated by mixing it with an aqueous potassium hydroxide solution (potassium hydroxide concentration of 20 wt%) in a weight ratio of 1:1 and drying it at 150°C for 10 hours.

[0110] The above-mentioned pre-treated Sargassum horneri was placed on a zirconia crucible and low-temperature carbonized at 280°C in a hot air oven. Here, low-temperature carbonization was performed under a CO2 atmosphere with a temperature increase of 1°C / min and a temperature holding time of 1 hour under a nitrogen atmosphere.

[0111] The above low-temperature carbonized Sargassum horneri was placed on a zirconia crucible and activated at 700 ℃ in a tube carbonization furnace. Here, the activation was performed under a nitrogen atmosphere with a temperature increase of 5 ℃ / min and a temperature holding time of 1 hour.

[0112] After activation, potassium hydroxide was removed by washing with distilled water weighing more than twice the weight of Sargassum horneri using an aspirator, and the product was dried at 150°C for 10 hours to obtain activated carbon prepared using Sargassum horneri.

[0114] Example 2

[0115] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that the weight ratio of potassium hydroxide aqueous solution to crushed Sargassum horneri was adjusted to 1:3 instead of 1:1 in the pretreatment step.

[0117] Example 3

[0118] Activated carbon was obtained by preparing it in the same manner as in Example 1, except that in the pretreatment step, the weight ratio of potassium hydroxide aqueous solution to crushed Sargassum horneri was adjusted to 1:5 instead of 1:1.

[0120] Example 4

[0121] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that the temperature in the activation step was controlled to 600°C instead of 700°C.

[0123] Example 5

[0124] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that the temperature in the activation step was adjusted to 800°C instead of 700°C.

[0126] Example 6

[0127] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that the temperature in the activation step was adjusted to 900°C instead of 700°C.

[0129] Example 7

[0130] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that the temperature was controlled to 1,000 ℃ instead of 700 ℃ during the activation step.

[0132] Example 8

[0133] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that the crushed Sargassum horneri was washed by repeating washing and rinsing five times with water before pretreatment.

[0135] Comparative Example 1

[0136] In the above Example 1, activated carbon was obtained by manufacturing in the same manner as in Example 1, except that the Sargassum horneri raw material was not crushed.

[0138] Comparative Example 2

[0139] Activated carbon was obtained by preparing it in the same manner as in Example 1, except that in Example 1, washing was performed by repeating washing and rinsing five times using water instead of pretreatment.

[0141] Comparative Example 3

[0142] In the above Example 1, activated carbon was obtained by preparing it in the same manner as in Example 1, except that no pretreatment was performed.

[0144] [Experimental Example]

[0145] Experimental Example 1: Yield and BET Specific Surface Area Measurement

[0146] The yield and BET specific surface area of ​​the activated carbon prepared in Examples 1 to 8 and Comparative Examples 1 to 3 were measured and are shown in Table 2 below. The yield was measured by the method described below, and the BET specific surface area was measured by the method described above.

[0147] transference number

[0148] The weight ratio of the finally obtained activated carbon to the weight of the Sargassum horneri raw material was calculated.

[0149] transference number(%) BET specific surface area (m 2 / g) Example 1 25.0 1,411 Example 2 8.5 746 Example 3 5.6 605 Example 4 38.0 706 Example 5 19.6 1,267 Example 6 17.3 1,264 Example 7 11.5 986 Example 8 24.8 1,301 Comparative Example 1 31.2 853 Comparative Example 2 49.9 218 Comparative Example 3 67.3 30

[0150] Referring to Table 2 above, it was confirmed through the results of Examples 1 to 3 that the yield and BET specific surface area of ​​activated carbon can be controlled by adjusting the weight ratio of marine biological resources and potassium hydroxide aqueous solution during the pretreatment step. In addition, looking at the results of Examples 1 and 4 to 7, it was confirmed that the yield and BET specific surface area of ​​activated carbon can be controlled according to the activation temperature.

[0151] In addition, looking at the results of Examples 1 and 8, it was possible to confirm the changes in the yield and BET specific surface area of ​​activated carbon depending on whether a washing step was added before the pretreatment step.

[0152] In addition, looking at the results of Example 1 and Comparative Example 1, it was confirmed that the BET specific surface area of ​​the activated carbon decreased when unground Sargassum raw material was used.

[0153] In addition, looking at the results of Example 1 and Comparative Example 2, it was confirmed that the BET specific surface area of ​​activated carbon decreased when the Sargassum horneri raw material was washed instead of pretreated.

[0154] In addition, looking at the results of Example 1 and Comparative Example 3, it was confirmed that the BET specific surface area of ​​activated carbon decreased when the Sargassum horneri raw material was not pretreated.

[0156] Experimental Example 2: Structural Analysis of Activated Carbon

[0157] In Example 1 above, the content of functional groups was confirmed by elemental analysis of the Sargassum horneri raw material, after low-temperature carbonization, and after activation, and the results are shown in Table 3 below. In addition, an SEM image of the activated carbon prepared in Example 1 above can be seen in Figure 6 below.

[0158] C H N S O raw material 39.11 6.03 1.93 0.71 52.23 Low-temperature carbonization 57.91 2.7 1.79 0.70 36.9 activate 91.79 0.61 2.03 0.67 4.9

[0159] Referring to Table 3 above, the elemental analysis results show that the carbon content is high, at approximately 92%, after the low-temperature carbonization and activation process. Here, it can be expected that if the holding time in the low-temperature carbonization process increases, the oxygen content will decrease and the carbon content will increase. For reference, general-purpose activated carbon generally has a carbon content of 80% and an oxygen content of 20%.

[0160] Although preferred embodiments of the present invention have been described above, the present invention is not limited thereto and can be implemented with various modifications within the scope of the claims, the detailed description of the invention, and the attached drawings, and it is obvious that such modifications also fall within the scope of the present invention.

Claims

Claim 1 A method for manufacturing activated carbon using marine biological resources, comprising the steps of: crushing marine biological resources; pre-treating the crushed marine biological resources; carbonizing the pre-treated marine biological resources at a temperature of 200 ℃ to 350 ℃; and activating the carbonized marine biological resources, wherein a washing step is not performed prior to the crushing step, and the marine biological resources are of the genus Sargassum ( Sargassum Method for manufacturing activated carbon using marine biological resources, specifically algae. Claim 2 delete Claim 3 In paragraph 1, the above marine biological resource is a type of snail ( Sargassum thunbergii ), Sargassum ( Sargassum horneri ), Alssongi Sargassum ( Sargassum confusum ), twisted seaweed ( Sargassum siliquastrum ), large-leaved Sargassum ( Sargassum coreanum ), paired-leaf Sargassum ( Sargassum hemiphyllum ) and double-stemmed Sargassum ( Sargassum patens A method for producing activated carbon using one or more marine biological resources selected from ). Claim 4 A method for producing activated carbon using marine biological resources, wherein the grinding step in claim 1 is performed under conditions of 10,000 RPM to 50,000 RPM. Claim 5 A method for producing activated carbon using marine biological resources, wherein, in claim 1, the average particle size (D50) of the crushed marine biological resources is 15 μm to 60 μm. Claim 6 delete Claim 7 A method for producing activated carbon using marine biological resources, wherein the pretreatment step is performed by mixing the crushed marine biological resources with one or more selected from the group consisting of an aqueous phosphate solution and an aqueous alkali compound solution. Claim 8 A method for producing activated carbon using marine biological resources, wherein, in claim 7, the phosphate is one or more selected from the group consisting of ammonium phosphate, potassium phosphate, and sodium phosphate, and the alkali compound is one or more selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetrahydroxymethylammonium, and tetrahydroxyethylammonium. Claim 9 A method for producing activated carbon using marine biological resources according to claim 7, wherein one or more of the crushed marine biological resources and the aqueous phosphate solution and the aqueous alkali compound solution are mixed in a weight ratio of 1:1 to 1:

10. Claim 10 delete Claim 11 A method for producing activated carbon using marine biological resources, wherein the activating step is performed under temperature conditions of 500 ℃ to 1,200 ℃ in accordance with claim 1. Claim 12 Activated carbon produced from a method of manufacturing using marine biological resources according to any one of paragraphs 1, 3 to 5, 7 to 9, and 11. Claim 13 In claim 12, the activated carbon has a carbon content of 82% to 99% by weight. Claim 14 In Clause 12, the BET specific surface area of ​​the activated carbon is 500 m² 2 / g to 2,000 m 2 Activated carbon in g.

Citation Information

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