KR20240107612A - Producing method of spherical activated carbon - Google Patents
Producing method of spherical activated carbon Download PDFInfo
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- KR20240107612A KR20240107612A KR1020220190398A KR20220190398A KR20240107612A KR 20240107612 A KR20240107612 A KR 20240107612A KR 1020220190398 A KR1020220190398 A KR 1020220190398A KR 20220190398 A KR20220190398 A KR 20220190398A KR 20240107612 A KR20240107612 A KR 20240107612A
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- activated carbon
- spherical activated
- organic binder
- weight
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 238000000034 method Methods 0.000 title description 4
- 239000011230 binding agent Substances 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 5
- 244000060011 Cocos nucifera Species 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 239000003245 coal Substances 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- -1 first Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3035—Compressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3042—Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/382—Making shaped products, e.g. fibres, spheres, membranes or foam
Abstract
본 발명은 구형활성탄의 제조방법에 관한 것으로, 더욱 상세하게는 저가의 활성탄소 원료로 내구도와 비표면적이 큰 구형활성탄을 제조할 수 있고, 유기계 바인더를 혼합하여 흡착도 및 입도 균일성이 우수한 구형활성탄을 제조할 수 있다.The present invention relates to a method for producing spherical activated carbon. More specifically, spherical activated carbon with high durability and specific surface area can be manufactured from low-cost activated carbon raw materials, and spherical activated carbon with excellent adsorption and particle size uniformity can be produced by mixing an organic binder. Activated carbon can be manufactured.
Description
본 발명은 구형 활성탄을 제조하는 방법에 대한 것이다. 보다 상세하게는 코코넛, 석탄계 또는 석유계 활성탄소 분말에 바인더 용액을 혼합하여 직경 크기가 작아 충진밀도가 높으면서도 내마모도 등 기계적 강도가 우수하며 기상 또는 수상에서의 오염 및 유해물질의 흡착, 제거 성능이 우수한 구형활성탄을 제조하는 방법에 대한 것이다. The present invention relates to a method for producing spherical activated carbon. More specifically, by mixing a binder solution with coconut, coal-based or petroleum-based activated carbon powder, the diameter size is small, so the filling density is high, but the mechanical strength such as abrasion resistance is excellent, and the performance of adsorption and removal of pollutants and harmful substances in the gas or water phase is excellent. This is about a method of producing excellent spherical activated carbon.
활성탄은 뛰어난 흡착특성을 지니고 있어 액상이나 기상에서 불순물을 제거하는 용도로 널리 사용되고 있다. 특히 활성탄은 미세 망 평면 구조의 물리 흡착을 일으키는 흡착제로서 활성탄 자체가 가지고 있는 고기공도, 내열성, 내화학성 등의 장점으로 오염물질 제거, 탈취, 유해기체 제거, 수처리, 촉매담채 등 광범위한 분야에 사용되고 있다.Activated carbon has excellent adsorption properties and is widely used to remove impurities from liquid or gas phase. In particular, activated carbon is an adsorbent that causes physical adsorption with a fine mesh planar structure. Due to the advantages of activated carbon itself, such as high porosity, heat resistance, and chemical resistance, it is used in a wide range of fields such as pollutant removal, deodorization, harmful gas removal, water treatment, and catalytic tinting. .
활성탄은 분말상과 입상으로 구분되는데, 분말상 활성탄의 경우 흡착 조작이 이루어지는 과정에서 분진이 발생하거나 불순물을 제거하는 용액을 탄분으로 검게 오염시키는 문제가 있고, 분말상 활성탄의 문제를 해결하기 위해 입상 활성탄이 개발되었으나 점결제를 사용하는 경우 분말상 활성탄과 마찬가지로 이차적인 오염이 발생하는 문제가 있다.Activated carbon is divided into powder and granular. In the case of powder activated carbon, there is a problem of generating dust during the adsorption process or contaminating the solution to remove impurities with carbon dust. To solve the problem of powder activated carbon, granular activated carbon was developed. However, when using a binder, like powdered activated carbon, there is a problem of secondary contamination occurring.
구형활성탄은 구형으로 제작된 입상 활성탄으로 분말상 활성탄 대비 분진의 발생이 적고, 제조 후 운송 및 후속처리가 용이하며, 압력손실이 적다는 장점이 있다. 특히, 직경이 작은 구형활성탄은 공극이 작아져 충진밀도가 높아 흡착 및 제거 성능이 우수하고, 기상 또는 수상에서의 오염 및 유해물질을 흡착, 제거할 수 있어 활용도가 높은 장점이 있다. Spherical activated carbon is a granular activated carbon manufactured in a spherical shape and has the advantages of generating less dust compared to powdered activated carbon, making it easier to transport and follow-up after manufacturing, and reducing pressure loss. In particular, spherical activated carbon with a small diameter has small pores and a high packing density, so it has excellent adsorption and removal performance, and has the advantage of being highly useful as it can adsorb and remove pollutants and harmful substances in the gas or water phase.
종래 피치를 원료로 하여 구형활성탄을 제조하는 방법이 대한민국등록특허 10-0146503호에 개시되어 있는데 제올라이트 분말과 활성탄 분말을 혼합하고 금속 실리케이트 수용액을 배합하여 입상화한 후 알칼리 토금속염 수용액 처리 후 건조시켜 제조함에 따라 구형활성탄의 입도제어가 어렵고 제조원가가 높아 군사, 의료와 같은 특수한 상황에서만 활용이 가능한 문제가 있다.A conventional method of producing spherical activated carbon using pitch as a raw material is disclosed in Korean Patent No. 10-0146503, which involves mixing zeolite powder and activated carbon powder and mixing them with an aqueous metal silicate solution to form granules, followed by treatment with an aqueous alkaline earth metal salt solution and drying. Due to manufacturing, it is difficult to control the particle size of spherical activated carbon and the manufacturing cost is high, so it can only be used in special situations such as military and medical.
본 발명은 상기와 같은 문제점을 해결하기 위한 것으로, 저렴하면서도 손쉽게 조달할 수 있는 석탄, 석유계 활성탄소 분말을 원료로 하여 유기계 바인더를 혼합하여 입도제어가 가능하면서도 비표면적과 경고가 우수한 구형활성탄을 제조하는 방법을 제공함에 있다.The present invention is intended to solve the above problems, using inexpensive and easily procurable coal and petroleum-based activated carbon powder as raw materials and mixing an organic binder to produce spherical activated carbon that can control particle size and has excellent specific surface area and warning. To provide a manufacturing method.
상기와 같은 목적을 달성하기 위해 본 발명의 구형활성탄의 제조방법은 (1) 유기계 바인더와 용매를 혼합하여 바인더 용액을 제조하는 단계; (2) 코코넛계, 석탄계 또는 석유계 중 어느 하나를 원재료로 하는 활성탄소와 바인더 용액을 회전식 교반기를 이용하여 혼합하여 활성탄소 혼합물을 제조하는 단계; (3) 활성탄소 혼합물을 금속 몰드에 주입하고 압축기를 이용하여 구형활성탄을 제조하는 단계; (4) (3) 단계에서 제조된 구형활성탄을 건조 후 소성하는 단계를 포함한다.In order to achieve the above object, the method for producing spherical activated carbon of the present invention includes the steps of (1) mixing an organic binder and a solvent to prepare a binder solution; (2) preparing an activated carbon mixture by mixing activated carbon using any one of coconut-based, coal-based, or petroleum-based raw materials and a binder solution using a rotary stirrer; (3) injecting the activated carbon mixture into a metal mold and producing spherical activated carbon using a compressor; (4) It includes the step of drying and then calcining the spherical activated carbon prepared in step (3).
또한, 상기 단계 (1)에서 유기계 바인더는 아크릴, 파라핀, 폴리비닐알코올(PVA), 이소불화비닐(PVDF) 또는 폴리 아크릴릭산(PAA) 중 어느 하나인 것을 특징으로 한다.In addition, the organic binder in step (1) is characterized in that it is one of acrylic, paraffin, polyvinyl alcohol (PVA), vinyl isofluoride (PVDF), or polyacrylic acid (PAA).
또한, 상기 단계 (1)에서 용매는 증류수, 에탄올, 이소프로판올, 아세톤 또는 톨루엔 중 어느 하나이고, 상기 단계 (1)에서 혼합되는 유기계 바인더는 50~80 중량%, 용매는 20~50 중량%인 것을 특징으로 한다.In addition, in step (1), the solvent is any one of distilled water, ethanol, isopropanol, acetone, or toluene, the organic binder mixed in step (1) is 50 to 80% by weight, and the solvent is 20 to 50% by weight. It is characterized by
또한, 상기 활성탄소는 비표면적이 1000~2000 m2/g이고, 상기 단계 (2)의 활성탄소 혼합물에서 활성탄소는 40~60 중량%, 바인더 용액은 40~60 중량%인 것을 특징으로 한다.In addition, the activated carbon has a specific surface area of 1000 to 2000 m2/g, and the activated carbon mixture in step (2) contains 40 to 60% by weight of activated carbon and 40 to 60% by weight of the binder solution.
또한, 상기 단계 (2)에서 활성탄소 혼합물은 회전식 교반기의 속도를 100~500 RPM으로 하여 교반하는 것을 특징으로 한다.Additionally, in step (2), the activated carbon mixture is stirred using a rotary stirrer at a speed of 100 to 500 RPM.
또한, 상기 단계 (4)에서 구형활성탄은 100 내지 200도에서 1~5 시간동안 건조하고, 100~300도에서 30분 내지 2시간 동안 소성하는 것을 특징으로 한다.In addition, in step (4), the spherical activated carbon is dried at 100 to 200 degrees for 1 to 5 hours and calcined at 100 to 300 degrees for 30 minutes to 2 hours.
이상과 같은 구성의 본 발명은 저가의 활성탄소 원료로 내구도와 비표면적이 큰 구형활성탄을 제조할 수 있고, 유기계 바인더를 혼합하여 흡착도 및 입도 균일성이 우수한 구형활성탄을 제조할 수 있다.The present invention with the above configuration can produce spherical activated carbon with high durability and specific surface area using low-cost activated carbon raw materials, and can produce spherical activated carbon with excellent adsorption and particle size uniformity by mixing an organic binder.
도 1은 본 발명의 일실시예에 따른 구형활성탄 제조방법의 순서도이고,
도 2는 본 발명의 일실시예에 따라 제작된 구형활성탄의 흡착등온선에 대한 데이터이고,
도 3은 본 발명의 일실시예에 따라 제작된 구형활성탄의 기공크기 분포이고,
도 4는 본 발명의 일실시예에 따라 제작된 구형활성탄의 SEM 사진이다.1 is a flowchart of a method for producing spherical activated carbon according to an embodiment of the present invention;
Figure 2 is data on the adsorption isotherm of spherical activated carbon produced according to an embodiment of the present invention,
Figure 3 is a pore size distribution of spherical activated carbon produced according to an embodiment of the present invention;
Figure 4 is an SEM photograph of spherical activated carbon produced according to an embodiment of the present invention.
이하에서 도면을 참조하여 본 발명에 따른 구형활성탄의 제조방법에 대해 상세히 설명한다.Hereinafter, the method for producing spherical activated carbon according to the present invention will be described in detail with reference to the drawings.
실시예1Example 1
활성탄소의 원료로는 코코넛 전구체로 제조된 코코넛계 활성탄소 분말, 석탄계 피치 분말 또는 석유계 활성탄 분말을 활용한다. As raw materials for activated carbon, coconut-based activated carbon powder, coal-based pitch powder, or petroleum-based activated carbon powder manufactured from coconut precursors are used.
활성탄소의 비표면적의 경우 1000~2000 m2/g를 사용하는 것이 바람직한데, 이는 본 발명에서 구형활성탄 제조 시 바인더를 사용하므로 수지가 흡착되어 기공을 막게 되어 구형활성탄의 흡착도를 양호하게 유지하기 위함이다. 활성탄소의 비표면적이 1,000 m2/g보다 작을 경우 흡착도가 떨어지고, 비표면적이 2,000 m2/g보다 클 경우 활성탄소 원료의 가격이 높아 제조원가가 상승하는 문제가 있다.In the case of the specific surface area of activated carbon, it is preferable to use 1000 to 2000 m2/g. This is because a binder is used when producing spherical activated carbon in the present invention, so that the resin is adsorbed and blocks the pores to maintain good adsorption of the spherical activated carbon. am. If the specific surface area of activated carbon is less than 1,000 m2/g, the adsorption degree decreases, and if the specific surface area is larger than 2,000 m2/g, the price of activated carbon raw materials is high, leading to an increase in manufacturing costs.
실시예2Example 2
바인더 용액의 제조과정을 설명하면 우선 유기계 바인더인 폴리비닐알코올(PVA)과 용매인 증류수를 50대 50 중량%로 혼합한다. 유기계 바인더와 증류수 혼합 시 25 내지 50° C의 온도 조건에서 2시간 이상 교반기를 이용하여 혼합을 수행한다. 완성된 유기계 바인더 용액에 침전물이 생기지 않도록 사용 전까지 계속 교반기를 이용하여 혼합하는 것이 바람직하다. 유기계 바인더는 PVA 외에도 아크릴, PVDF, 파라핀, PAA를 사용할 수 있다. 바인더 용액을 제조하기 위한 용매로는 증류수 외에 에탄올, 이소프로판올, 아세톤, 톨루엘을 사용할 수 있다. 유기계 바인도와의 효율적인 혼합을 위해서는 증류수, 에탄올, 이소프로판올이 바람직하다. 또한, 바인더 용액 내 유기계 바인더의 비율을 매우 중요한데 유기계 바인더의 비율이 높거나 낮으면 제조된 구형활성탄의 구형도를 균일하게 유지할 수 없기 때문이다.To explain the manufacturing process of the binder solution, first, polyvinyl alcohol (PVA), an organic binder, and distilled water, a solvent, are mixed in a ratio of 50 to 50% by weight. When mixing the organic binder and distilled water, mixing is performed using a stirrer for more than 2 hours at a temperature of 25 to 50 ° C. It is advisable to continue mixing using a stirrer until use to prevent sediment from forming in the completed organic binder solution. In addition to PVA, organic binders can use acrylic, PVDF, paraffin, and PAA. In addition to distilled water, ethanol, isopropanol, acetone, and toluel can be used as solvents for preparing the binder solution. For efficient mixing with organic binders, distilled water, ethanol, and isopropanol are preferred. In addition, the ratio of the organic binder in the binder solution is very important, because if the ratio of the organic binder is high or low, the sphericity of the manufactured spherical activated carbon cannot be maintained uniformly.
실시예3Example 3
활성탄소 혼합물을 제조하기 위해서는 실시예 1에서 준비된 활성탄소 원료분말 100 g과 유기계 바인더 용액 120g을 비커에 넣는다. 이때 활성탄소 분말이 날리지 않도록 천천히 비커에 넣어주며, 유기계 바인더의 경우 처음 미립자 활성탄소와 혼합이 잘 되지 않기 때문에 회전식 교반기를 이용하여 혼합을 수행하는 것이 바람직하다.To prepare an activated carbon mixture, 100 g of the activated carbon raw material powder prepared in Example 1 and 120 g of the organic binder solution were placed in a beaker. At this time, slowly add the activated carbon powder to the beaker to prevent it from flying away. In the case of organic binders, it is difficult to mix well with the initial particulate activated carbon, so it is preferable to mix using a rotary stirrer.
회전식 교반기의 속도는 250 RPM으로 설정하여 수행하였으며, 약 30분 내지 1시간 교반을 수행하는 것이 바람직하다.The speed of the rotary stirrer was set to 250 RPM, and it is desirable to stir for about 30 minutes to 1 hour.
제조된 슬러리 형태의 활성탄소 혼합물(활성탄소 + 유기계 바인더 용액)을 금속 몰드에 천천히 채워준 후, 금속 몰드를 결합한 후 프레스기를 이용하여 1~10 bar 정도의 압력을 가하여 구형활성탄을 제조한다.The prepared slurry-type activated carbon mixture (activated carbon + organic binder solution) is slowly filled into a metal mold, the metal molds are combined, and a pressure of 1 to 10 bar is applied using a press to produce spherical activated carbon.
실시예4Example 4
금속 몰드에 압력을 가하여 제조된 구형활성탄을 건조 및 소성하는 과정에 대해 설명하면 우선 금속 몰드 안의 구형활성탄소는 금속 몰드를 천천히 분해하여 획득한다. 이때 금속 몰드를 빠르게 제거할 경우 구형활성탄소의 성형이 무너질 수 있기 때문에 천천히 몰드를 분해 및 제거하는 것이 중요하다. 완성된 구형 활성탄을 서스용기에 넣고 오븐을 활용하여 100도에서 1시간 내지 2시간 건조를 수행한다.When explaining the process of drying and firing spherical activated carbon manufactured by applying pressure to a metal mold, first, the spherical activated carbon in the metal mold is obtained by slowly decomposing the metal mold. At this time, it is important to disassemble and remove the mold slowly because the molding of the spherical activated carbon may collapse if the metal mold is quickly removed. The completed spherical activated carbon is placed in a suspension container and dried at 100 degrees for 1 to 2 hours using an oven.
건조된 구형 활성탄을 열처리로를 활용하여 200도에서 1시간 소성을 수행한다. 이때 소성은 질소분위기에서 수행한다.The dried spherical activated carbon is fired at 200 degrees for 1 hour using a heat treatment furnace. At this time, firing is performed in a nitrogen atmosphere.
아래 표 1은 열처리 온도, 열처리 시간 및 제조된 구형활성탄의 비표면적을 나타낸 데이터이다.Table 1 below shows data showing heat treatment temperature, heat treatment time, and specific surface area of the manufactured spherical activated carbon.
<표 1. 열처리 조건 별 비표면적 데이터><Table 1. Specific surface area data by heat treatment conditions>
샘플명sample name
열처리 온도heat treatment temperature
열처리 시간heat treatment time
비표면적(m2/g)Specific surface area (m2/g)
샘플 1sample 1
100도 열처리100 degree heat treatment
3시간3 hours
552552
샘플 2sample 2
200도 열처리200 degree heat treatment
1시간1 hours
755755
샘플 3sample 3
200도 열처리200 degree heat treatment
2시간2 hours
685685
샘플 4sample 4
300도 열처리300 degree heat treatment
1시간1 hours
551551
비교예 1Comparative Example 1
900도 열처리900 degree heat treatment
1시간1 hours
194194
건조 및 소성 조건을 달리한 샘플에 대해 비표면적 분석장비의 분석결과를 도 2, 3에 나타내었다. 도 2 분석결과를 보면 샘플 1, 2, 3, 4는 비교예 1번과 비교하였을 때 상대압력(Relative Pressure) 0.1 이하에서 높은 흡착량을 보이는 것을 확인할 수 있는데 이는 2 nm이하의 미세기공이 많다는 것을 의미한다. 또한 샘플 1, 2, 3, 4과 비교예 1의 상대압력(Relative Pressure) 0.7~1 부근을 비교하였을 때 흡착과 탈착의 히스테리시스가 크게 발달 된 것을 확인할 수 있는데 이는 2 nm이상의 기공이 발달했다는 것을 확인할 수 있으며, 이는 수질용 흡착소재로 활용이 용이하다는 것을 의미한다.The analysis results of the specific surface area analysis equipment for samples under different drying and firing conditions are shown in Figures 2 and 3. Looking at the analysis results in Figure 2, it can be seen that Samples 1, 2, 3, and 4 show high adsorption amount at a relative pressure of 0.1 or less when compared to Comparative Example No. 1, which means that there are many micropores of 2 nm or less. means that In addition, when comparing the relative pressure of Samples 1, 2, 3, and 4 with Comparative Example 1 around 0.7 to 1, it can be seen that the hysteresis of adsorption and desorption has developed significantly, which means that pores of 2 nm or more have developed. This can be confirmed, which means that it is easy to use as an adsorption material for water quality.
도면 3은 샘플 1과 샘플 3의 기공크기분포를 비교한 것으로 샘플 1과 샘플 3 모두 미세기공(2 nm 이하) 및 중기공(2 ~ 50 nm)가 발달된 것을 확인 할 수 있다. 특히 샘플 3번의 경우 중기공이 많이 발달되어 있는 것을 확인할 수 있다.Figure 3 compares the pore size distribution of Sample 1 and Sample 3. It can be seen that both Sample 1 and Sample 3 have developed micropores (2 nm or less) and mesopores (2 to 50 nm). In particular, in the case of sample No. 3, it can be seen that the mesopores are highly developed.
Claims (7)
(2) 코코넛계, 석탄계 또는 석유계 중 어느 하나를 원재료로 하는 활성탄소와 바인더 용액을 회전식 교반기를 이용하여 혼합하여 활성탄소 혼합물을 제조하는 단계;
(3) 활성탄소 혼합물을 금속 몰드에 주입하고 압축기를 이용하여 구형활성탄을 제조하는 단계;
(4) (3) 단계에서 제조된 구형활성탄을 건조 후 소성하는 단계를 포함하는 구형활성탄의 제조방법.
(1) preparing a binder solution by mixing an organic binder and a solvent;
(2) preparing an activated carbon mixture by mixing activated carbon using any one of coconut-based, coal-based, or petroleum-based raw materials and a binder solution using a rotary stirrer;
(3) injecting the activated carbon mixture into a metal mold and producing spherical activated carbon using a compressor;
(4) A method for producing spherical activated carbon comprising the step of drying and then calcining the spherical activated carbon prepared in step (3).
상기 단계 (1)에서 유기계 바인더는 아크릴, 파라핀, 폴리비닐알코올(PVA), 이소불화비닐(PVDF) 또는 폴리 아크릴릭산(PAA) 중 어느 하나인 것을 특징으로 하는 구형활성탄의 제조방법.
In claim 1,
In step (1), the organic binder is any one of acrylic, paraffin, polyvinyl alcohol (PVA), vinyl isofluoride (PVDF), or polyacrylic acid (PAA).
상기 단계 (1)에서 용매는 증류수, 에탄올, 이소프로판올, 아세톤 또는 톨루엔 중 어느 하나이고,
상기 단계 (1)에서 혼합되는 유기계 바인더는 50~80 중량%, 용매는 20~50 중량%인 것을 특징으로 하는 구형활성탄의 제조방법.
In claim 1,
In step (1), the solvent is any one of distilled water, ethanol, isopropanol, acetone, or toluene,
A method for producing spherical activated carbon, characterized in that the organic binder mixed in step (1) is 50 to 80% by weight and the solvent is 20 to 50% by weight.
상기 활성탄소는 비표면적이 1000~2000 m2/g이고,
상기 단계 (2)의 활성탄소 혼합물에서 활성탄소는 40~60 중량%, 바인더 용액은 40~60 중량%인 것을 특징으로 하는 구형활성탄의 제조방법.
In claim 2,
The activated carbon has a specific surface area of 1000 to 2000 m2/g,
A method for producing spherical activated carbon, characterized in that the activated carbon is 40 to 60% by weight and the binder solution is 40 to 60% by weight in the activated carbon mixture of step (2).
상기 단계 (2)에서 활성탄소 혼합물은 회전식 교반기의 속도를 100~500 RPM으로 하여 교반하는 것을 특징으로 하는 구형활성탄의 제조방법.
In claim 1,
In step (2), the activated carbon mixture is stirred with a rotary stirrer at a speed of 100 to 500 RPM.
상기 단계 (4)에서 구형활성탄은 100 내지 200도에서 1~5 시간동안 건조하고, 100~300도에서 30분 내지 2시간 동안 소성하는 것을 특징으로 하는 구형활성탄의 제조방법.
In claim 1,
In step (4), the spherical activated carbon is dried at 100 to 200 degrees for 1 to 5 hours and calcined at 100 to 300 degrees for 30 minutes to 2 hours.
Publications (1)
| Publication Number | Publication Date |
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| KR20240107612A true KR20240107612A (en) | 2024-07-09 |
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