KR101008684B1 - Spherical activated carbon manufacturing method - Google Patents
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- KR101008684B1 KR101008684B1 KR1020100001526A KR20100001526A KR101008684B1 KR 101008684 B1 KR101008684 B1 KR 101008684B1 KR 1020100001526 A KR1020100001526 A KR 1020100001526A KR 20100001526 A KR20100001526 A KR 20100001526A KR 101008684 B1 KR101008684 B1 KR 101008684B1
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- titanium dioxide
- activated carbon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 35
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011941 photocatalyst Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 244000060011 Cocos nucifera Species 0.000 claims abstract description 16
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- 102000011782 Keratins Human genes 0.000 claims description 22
- 108010076876 Keratins Proteins 0.000 claims description 22
- 235000013399 edible fruits Nutrition 0.000 claims description 16
- 239000005751 Copper oxide Substances 0.000 claims description 12
- 229910000431 copper oxide Inorganic materials 0.000 claims description 12
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- 244000025254 Cannabis sativa Species 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 5
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- 229910052802 copper Inorganic materials 0.000 abstract description 20
- 239000010949 copper Substances 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 7
- 230000004913 activation Effects 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract description 2
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- 238000006303 photolysis reaction Methods 0.000 description 6
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- 239000002105 nanoparticle Substances 0.000 description 5
- 238000013032 photocatalytic reaction Methods 0.000 description 5
- 230000015843 photosynthesis, light reaction Effects 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 4
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- 239000000356 contaminant Substances 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- 229920006395 saturated elastomer Polymers 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000000417 fungicide Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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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
- B01J20/02—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
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
Description
본 발명은 높은 광분해 반응 및 효과적인 제균 작용을 위하여 흡착, 광분해 및 제균 기능이 강화된 구형 활성탄을 제조하는 방법에 관한 것으로서, 더욱 상세하게는 졸-겔 공법을 이용하여, 구리가 도핑된 이산화티타늄 나노 입자를 야자 열매 각질 분말에 합성시킨(TiO2 with Coconut Shell Powder and Copper; 이하 'TCSPC'라 함) 후, 성형 및 탄화 그리고 활성 단계를 거쳐 흡착, 광분해 및 제균 기능이 강화된 새로운 구리가 합성된 구형 활성탄의 제조 방법에 관한 것이다.The present invention relates to a method for producing spherical activated carbon having enhanced adsorption, photolysis, and sterilization functions for high photolysis reaction and effective bactericidal action, and more specifically, copper-doped titanium dioxide nanoparticles using a sol-gel method. The particles were synthesized into coconut keratin powder (TiO 2 with Coconut Shell Powder and Copper; hereinafter referred to as 'TCSPC'), and then formed, carbonized, and activated to synthesize new copper with enhanced adsorption, photolysis and bactericidal functions. A method for producing spherical activated carbon.
수처리 및 대기 정화 또는 토양 개량, 방습 등의 목적으로 종래의 활성탄은 흡착재로서 널리 사용되어 왔다. 그러나 이러한 기존의 활성탄은 다공질의 흡착력만을 이용한 것으로 제조원가가 매우 높고, 장시간 통수하면 활성탄 내·외부의 기공이 오염물질에 의해 포화가 된다. 이렇게 포화된 활성탄은 수처리 능력이 현저히 떨어지는, 파과(***)에 도달하게 되어, 정화 능력이나 방습의 효과가 급격히 감소하므로 주기적으로 교체해야 하는 단점이 있다. 또한 재생 처리 시에 발생하는 슬러지를 매립 또는 소각해야 하는 등의 2차 처리 필요성과 그 비용이 처리 효율에 비해 높다는 경제적인 문제점이 있다. 이러한 단점들을 극복하기 위해서 최근에는 이산화티타늄과 같은 광 촉매를 활성탄에 직접 합성하여 광분해 활성도를 가진 활성탄을 제조하여 사용하고 있다. 종래의 활성탄에 합성된 이산화티타늄의 특징은 일정한 영역의 빛 에너지(일반적으로 380nm 이하의 파장을 가지는 자외선)가 가해지면 전자(e-)가 가전자대(valence band)에서 전도대(conduction band)로 여기되어지고, 이때 전도대에는 전자들이 생성되고, 가전자대에는 정공(h+)이 형성된다. 즉, 종래의 활성탄에 합성된 이산화티타늄은 항상 일정한 양의 강한 빛을 흡수해야만 강한 환원력과 산화력을 가진 이온이 생성되어 여러 가지 화학작용에 의해 활성탄 내·외부에 포화된 오염물질을 제거할 수 있으나 빛은 항상 이산화티타늄 표면에 닿고 있는 것은 아니다. 때로는 어둡게 되기도 하고, 항상 약한 빛만이 닿는 곳도 있다. 또한, 한번 생성된 전자와 정공은 아주 빠른 속도로 다시 재결합되므로, 광분해 효율이 감소하는 문제점이 있다.Conventional activated carbon has been widely used as an adsorbent for the purpose of water treatment and air purification or soil improvement and moisture proofing. However, these existing activated carbons use only porous adsorption power, and the manufacturing cost is very high, and when water is passed for a long time, pores inside and outside the activated carbon become saturated by contaminants. Such saturated activated carbon reaches a breakthrough, in which water treatment capacity is remarkably decreased, and thus, the effect of purification and moisture proofing is sharply reduced, and thus it has to be replaced periodically. In addition, there is an economic problem that the secondary treatment necessitates the landfill or incineration of sludge generated during the regeneration treatment, and the cost thereof is higher than the treatment efficiency. In order to overcome these disadvantages, recently, a photocatalyst such as titanium dioxide is synthesized directly on activated carbon to produce and use activated carbon having photodegradation activity. Characteristics of the titanium dioxide synthesized with the conventional activated carbon is light energy of a constant region (generally ultraviolet light having a wavelength below 380nm) are ground electron (e -) applied to the conduction band (conduction band) in the valence band (valence band) where At this time, electrons are generated in the conduction band, and holes (h + ) are formed in the valence band. That is, titanium dioxide synthesized in conventional activated carbon always absorbs a certain amount of strong light to generate ions having strong reducing power and oxidizing power, and thus it is possible to remove saturated contaminants inside and outside activated carbon by various chemical reactions. Light does not always reach the surface of titanium dioxide. Sometimes it gets dark, and there are always places where only weak light hits. In addition, since once generated electrons and holes are recombined again at a very high speed, there is a problem that the photolysis efficiency is reduced.
종래의 문제점을 해결하기 위해 본 발명에서는 자가 제균 능력 및 인체에는 대부분 독성을 지니지 않는 것으로 알려져 있는 구리를 이산화티타늄에 도핑하여 실내 빛과 같이 약한 빛뿐만 아니라 빛이 도달하지 않는 곳에서도 제균력을 가지는 TCSPC 활성탄을 제조하였다. 또한 전자와 정공의 재결합을 막는 전하 분리(電荷分離) 역할도 함으로써, 효율성이 증대된 광 촉매 반응을 진행시키는 것이 가능하다. 다시 말해, 이산화티타늄 및 구리 나노 입자를 활성탄에 합성하여 광 분해, 흡착 및 제균 기능이 강화된 새로운 형태의 하이브리드 활성탄을 생산함으로써 경제적, 환경적 그리고 효율적 측면에서의 종래 기술의 단점을 해결하는 것이 기술적 과제이다.In order to solve the conventional problems, in the present invention, doping copper, which is known to have no self-sterilization ability and most toxic to the human body, is doped with titanium dioxide to have germicidal power even where light does not reach as well as weak light such as indoor light. TCSPC activated carbon was prepared. In addition, by acting as a charge separation that prevents recombination of electrons and holes, it is possible to advance the photocatalytic reaction with increased efficiency. In other words, by synthesizing titanium dioxide and copper nanoparticles into activated carbon to produce a new type of hybrid activated carbon with enhanced photodegradation, adsorption and bactericidal functions, it is possible to solve the shortcomings of the prior art in terms of economy, environment and efficiency. It is a task.
본 발명은 상기한 바와 같은 종래의 문제점을 해결하기 위한 것으로, 자가 제균 능력 및 인체에는 대부분 독성을 지니지 않는 것으로 알려져 있는 구리가 도핑된 이산화티타늄 나노입자를 야자 열매 각질 분말에 합성한 후, 성형, 탄화, 활성화 단계를 거쳐 실내 빛과 같이 약한 빛뿐만 아니라 빛이 도달하지 않는 곳에서도 충분한 제균력을 가지며, 높은 광 촉매 반응 효율을 가지는 구리가 합성된 구형 활성탄의 제조 방법을 제공함에 그 목적이 있다.The present invention is to solve the conventional problems as described above, after synthesizing copper-doped titanium dioxide nanoparticles known to be non-toxic to human self-sterilization and human body to palm keratin powder, molding, The purpose of the present invention is to provide a method for producing spherical activated carbon synthesized with copper, which has sufficient decontamination power and high photocatalytic reaction efficiency even when light is not reached, such as indoor light, through carbonization and activation steps. .
상기 목적을 달성하기 위하여, 본 발명에 따른 구형 활성탄의 제조 방법은 (i) 이산화티타늄 용출 재료를 제1 용매에 혼합하여 제1 졸을 생성하는 단계; (ii) 염화구리를 제2 용매에 도핑하여 제2 졸을 생성한 후 상기 제1 졸과 상기 제2 졸을 혼합 교반하고 활성화하여 염화구리가 도핑된 이산화티타늄 활성화 졸 화합물을 생성하는 단계; (iii) 상기 염화구리가 도핑된 이산화티타늄 활성화 졸 혼합물에 야자 열매 각질 분말 및 증류수를 주입하면서 교반시키는 동시에 침전물을 가수분해시켜 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 생성하는 단계; (iv) 상기 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 농축하여 남은 공기, 용매, 및 증류수를 제거하는 단계; (v) 상기 농축된 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 풀과 혼합하고 구형의 성형물로 성형한 후 건조시키는 단계; 및 (vi) 상기 건조된 구형 성형물을 탄화 및 활성화하는 단계를 포함하는 것을 특징으로 한다.In order to achieve the above object, the method for producing spherical activated carbon according to the present invention comprises the steps of (i) mixing a titanium dioxide eluting material into a first solvent to produce a first sol; (ii) doping copper chloride in a second solvent to form a second sol, followed by mixing, stirring, and activating the first sol and the second sol to produce a titanium dioxide activated sol compound doped with copper chloride; (iii) injecting palm fruit keratin powder and distilled water into the copper chloride doped titanium dioxide activated sol mixture while stirring and hydrolyzing the precipitate to produce palm fruit keratin powder synthesized with copper and titanium dioxide photocatalyst; (iv) concentrating the coconut fruit keratin powder synthesized with the copper and titanium dioxide photocatalyst to remove remaining air, solvent, and distilled water; (v) mixing the concentrated copper and titanium dioxide photocatalyst with the palm fruit keratin powder with the grass, forming a spherical molding and drying the powder; And (vi) carbonizing and activating the dried spherical molding.
본 발명에 의해 제조된 구리 및 이산화티타늄 광 촉매가 합성된 구형 활성탄은 기존의 분말 또는 입자형 광촉매/활성탄이 가지고 있는 재생 또는 재활용을 위한 2차 분리시설의 필요성, 낮은 광 촉매 반응 효율 그리고, 일정한 영역의 빛에너지에 의해서만 제균력이 생성되는 문제점들을 구리와 같이 인체에 무해한 금속을 이산화티타늄에 도핑함으로서 해결할 수 있다. 즉, 기존 광촉매/활성탄의 형상이나 코팅 및 제조 방법과 비교해 볼 때, 본 발명은 다음과 같은 3가지의 특성이 있다. The spherical activated carbon synthesized with the copper and titanium dioxide photocatalyst prepared by the present invention has the necessity of a secondary separation facility for regeneration or recycling of the existing powder or particulate photocatalyst / activated carbon, low photocatalytic reaction efficiency, and The problem that the germicidal force is generated only by the light energy of the region can be solved by doping titanium dioxide with a metal that is harmless to the human body, such as copper. That is, the present invention has three characteristics as compared with the shape, coating and manufacturing method of the existing photocatalyst / activated carbon.
첫째, 자동 대량 생산 라인(Automated Mass Production Line; 이하 'AMPL'이라 함)공정을 이용하여 구형의 TCSPC 활성탄을 생산함으로써, 충분한 분쇄 강도를 가진 일정한 크기(2 mm 이상), 바람직하게는 2~4 mm의 구형 TCSPC 활성탄 제조가 가능하여, 기존의 활성탄 사용시 발생하는 분리 및 제거와 같은 2차 처리 프로세스가 필요 없으므로, 프로세스 설치에 따른 시간적 경제적 이익을 얻을 수 있다.Firstly, spherical TCSPC activated carbon is produced using an automated mass production line (hereinafter referred to as 'AMPL') process, so that a certain size (more than 2 mm) with sufficient grinding strength, preferably 2 to 4 It is possible to manufacture the spherical TCSPC activated carbon of mm, eliminating the need for secondary treatment processes such as separation and removal that occur with the use of conventional activated carbon, thereby gaining the time and economic benefits of installing the process.
둘째, 자가 제균 능력을 가진 구리를 이산화티타늄에 도핑시킴으로써, 실내 빛과 같이 약한 빛뿐만 아니라 빛이 도달하지 않는 곳에서도 충분한 제균력을 가진 활성탄 제조가 가능하다. Second, by doping copper with self-sterilization ability to titanium dioxide, it is possible to produce activated carbon with sufficient germicidal power even in the absence of light as well as weak light, such as indoor light.
셋째, 구리 나노 입자를 이산화티타늄에 도핑시키므로, 강한 산화 및 환원력을 가진 전자 및 정공의 재결합을 방지하므로, 뛰어난 광 촉매 반응을 기대할 수 있다. Third, since the copper nanoparticles are doped with titanium dioxide, recombination of electrons and holes having strong oxidation and reducing power can be prevented, and thus an excellent photocatalytic reaction can be expected.
따라서, 본 발명에 의해 제조되는 구리와 이산화티타늄 광촉매가 합성된 구형 활성탄은 활성탄의 흡착 능력과 이산화티타늄의 광 분해 능력뿐만 아니라 구리에 의해 자가 제균 능력과 향상된 광분해 능력을 발휘함으로써, 대기, 수질 정화용 또는 유기물 제거 및 제균력을 필요로 하는 산업 전반에 걸쳐 광범위한 상품성, 적용성을 갖게 된다. 또한, 열대 지방 음식 쓰레기의 일종인 야자 열매 각질을 저 비용으로 구입하여 천연 소재만을 활용한 친환경적인 구형 활성탄을 생산함으로써, 참나무, 소나무 등의 국내 임업 자원을 보호할 수 있다. 그뿐만 아니라 고가의 종래 활성탄보다도 효능이 뛰어나고, 가격이 저렴한 고급 TCSPC 활성탄을 저가에 공급할 수 있는 산업적 기반을 제공하여 자원 절약과 지구 환경 보호에 기여할 수 있다.Therefore, the spherical activated carbon prepared by synthesizing the copper and titanium dioxide photocatalyst according to the present invention exhibits self-sterilization ability and improved photolysis ability by copper as well as adsorption capacity of activated carbon and photodegradation ability of titanium dioxide, thereby purifying the air and water. Or it will have a wide range of commercial and applicability across industries that require organic material removal and bactericidal power. In addition, palm fruit keratin, a kind of tropical food waste, can be purchased at low cost to produce eco-friendly spherical activated carbon using only natural materials, thereby protecting domestic forest resources such as oak and pine. In addition, by providing an industrial base that can supply high-quality TCSPC activated carbon, which is more effective and inexpensive than conventional, activated carbon at low cost, it can contribute to resource conservation and global environmental protection.
도 1은 본 발명인 구리를 도핑한 이산화티타늄이 합성된 TCSPC 활성탄을 제조하는 방법을 설명하는 도면이다.
도 2는 종래의 이산화티타늄 광 촉매가 합성된 활성탄의 결정상을 분석하기 위해 XRD를 이용하여 나타낸 그래프이다.
도 3은 도 1의 제조방법에 의해 제조된 TCSPC 활성탄의 결정상을 분석하기 위해 XRD를 이용하여 나타낸 그래프이다.
도 4는 종래의 이산화티타늄 광 촉매가 합성된 활성탄의 구조상 형상을 분석하기 위해 분말 형태의 야자 각탄을 SEM을 이용해 찍은 사진의 사시도이다
도 5는 도 1의 제조 방법에 의해 제조된 TCSPC 활성탄의 구조상 형상을 분석하기 위해 분말 형태의 야자 각탄을 SEM을 이용해 찍은 사진의 사시도이다.
도 6은 자외선 조사 하에서의 일반 광 촉매/활성탄 및 TCSPC 활성탄의 E.coli 제균 실험의 결과를 나타낸 그래프이다.
도 7은 빛이 조사되지 않는 상태에서 일반 광 촉매/활성탄 및 TCSPC 활성탄의 E.coli 제균 실험의 결과를 나타낸 그래프이다.BRIEF DESCRIPTION OF THE DRAWINGS It is a figure explaining the method of manufacturing TCSPC activated carbon which synthesize | combined the copper doped titanium dioxide of this invention.
2 is a graph showing the use of XRD to analyze the crystal phase of the activated carbon synthesized with a conventional titanium dioxide photocatalyst.
3 is a graph showing the use of XRD to analyze the crystal phase of the TCSPC activated carbon prepared by the manufacturing method of FIG.
Figure 4 is a perspective view of a photograph taken by using the SEM in the form of a powdery palm coal to analyze the structural shape of the activated carbon synthesized with a conventional titanium dioxide photocatalyst
FIG. 5 is a perspective view of a photograph taken by using a SEM of coal petroleum powder in the form of powder to analyze the structural shape of the TCSPC activated carbon prepared by the method of FIG. 1.
FIG. 6 is a graph showing the results of E. coli disinfection experiment of general photocatalyst / activated carbon and TCSPC activated carbon under ultraviolet irradiation.
FIG. 7 is a graph showing the results of E. coli sterilization experiments of ordinary photocatalyst / activated carbon and TCSPC activated carbon in the absence of light irradiation.
이하, 첨부된 예시 도면에 의거하여 본 발명의 실시예에 따른 구형 활성탄을 제조하는 방법을 상세히 설명한다. Hereinafter, a method of manufacturing spherical activated carbon according to an embodiment of the present invention will be described in detail with reference to the accompanying example drawings.
도 1은 본 발명의 실시예에 따른 구리를 도핑한 이산화티타늄이 합성된 활성탄의 제조 방법을 설명하는 도면이다. 1 is a view for explaining a method for producing activated carbon synthesized with copper doped titanium dioxide according to an embodiment of the present invention.
본 발명은 이산화티타늄 광 촉매와 기존의 분말 또는 입자 형태의 활성탄을 합성하여 광촉매/활성탄 복합물을 제조하여 사용할 시 나타나는 문제점을 이산화티타늄 입자에 구리를 도핑함으로써 문제점을 해결하였다. 이산화티타늄에 구리를 도핑하여 제조된 TCSPC 활성탄은 실내 빛과 같이 약한 빛뿐만 아니라 빛이 도달하지 않는 곳에서도 충분한 제균력을 가지며, 전하 분리에 의한 높은 광 촉매 반응 효율을 가지게 되는 것을 발견하고, 종래 광촉매/활성탄 복합물의 효율적, 환경적, 경제적 문제점을 해결한 과학적이고 친환경적이며 경제적인 효과를 창출할 수 있는 구리를 도핑한 이산화티타늄이 합성된 구형 활성탄의 제조 방법에 관한 것이다. The present invention solves the problem of doping copper in titanium dioxide particles by synthesizing a titanium dioxide photocatalyst and activated carbon in the form of powder or particles to produce a photocatalyst / activated carbon composite. TCSPC activated carbon prepared by doping copper with titanium dioxide has a sufficient decontamination power even in the absence of light as well as weak light, such as room light, and found to have a high photocatalytic reaction efficiency by charge separation. The present invention relates to a method for producing spherical activated carbon synthesized with copper-doped titanium dioxide, which can create a scientific, environmentally-friendly and economical effect that solves the efficient, environmental and economic problems of the photocatalyst / activated carbon composite.
상기한 기술적 과제를 해결하기 위하여, 구리를 이산화티타늄에 도핑하여, 개량된 성상과 기능을 갖는 구형 TCSPC 활성탄을 경제적, 효율적으로 제조할 수 있는 방법 검토: In order to solve the above technical problem, a method of economically and efficiently producing spherical TCSPC activated carbon having improved properties and functions by doping copper with titanium dioxide is examined:
원 재료의Raw materials 선정 조건 Selection condition
(1) 출발 물질로서는 액체 상태인 티타늄 테트라이소프로폭사이드 (Titanium tetraisopropoxide; 이하 'TTIP'라 함) 또는 티타늄-엔-부톡사이드 (Titanium-n-butoxide)와 같은 가수분해 후 이산화티타늄 용출이 가능한 재료(1) As starting material, it is possible to elute titanium dioxide after hydrolysis such as titanium tetraisopropoxide (hereinafter referred to as 'TTIP') or titanium-n-butoxide in liquid state. material
(2) 출발 물질에 도핑되는 도펀트(dopant)는 염화구리(Ⅱ)와 같은 자가 제균 능력을 보유하고, 출발 물질에 도핑이 되기 쉬운 재료(2) Dopants doped in the starting material possess a self-sterilizing ability such as copper (II) chloride and are likely to be doped in the starting material.
(3) 흡착재의 재료로서는 미세 분말로 분쇄할 수 있도록 자연 상태에서 충분히 건조되고 분쇄에 적합한 경도(강도)를 갖는 재활용 재료,(3) As the material of the adsorbent, a recycled material having sufficient hardness (strength) suitable for pulverization in a natural state so as to be pulverized into fine powder,
(4) 흡착재의 재료로서는 저 비용으로 충분한 양을 수시로 공급받을 수 있는 재료
(4) As the material of the adsorbent, a material that can be supplied in sufficient quantity at low cost from time to time.
구리를 이산화티타늄에 Copper to titanium dioxide 도핑한Doped 후 야자 열매 각질 분말에 합성시키는 조건 Conditions synthesized after coconut fruit keratin powder
(1) 염화구리(Ⅱ)를 용매인 이소프로판올(isopropanol)에 용해하여 이산화티타늄 졸에 도핑한 후 교반을 통해 활성화 (1) Copper (II) chloride was dissolved in isopropanol as a solvent, doped into a titanium dioxide sol, and activated by stirring
(2) 활성화된 졸과 야자 열매 각질 분말을 초음파 교반기를 이용하여 합성 (2) Synthesis of Activated Sol and Coconut Kernel Powder by Ultrasonic Stirrer
(3) 합성된 혼합물을 순환 진공 농축기에 넣어서 농축하여 야자 열매 각질 분말의 내, 외부에 (1)에서 활성화시킨 졸을 균등하고 견고하게 주입(3) The synthesized mixture was concentrated in a circulating vacuum concentrator, and the sol activated in (1) was evenly and firmly injected into and out of the coconut keratin powder.
(4) 구리를 도핑한 이산화티타늄과 합성된 야자 열매 각질 분말을 AMPL 공정에 투입(4) Copper-doped titanium dioxide and palm fruit keratin powder were put into AMPL process
TCSPCTCSPC 구형 성형물을 탄화 및 활성에 의해 활성탄을 제조하는 조건 Conditions for producing activated carbon by carbonizing and activating spherical moldings
(1) AMPL 공정에 의해 생산된 TCSPC 구형 성형물을 40~50°C의 건조 온도에서 4시간 이상 건조(1) TCSPC spherical moldings produced by the AMPL process are dried for at least 4 hours at a drying temperature of 40-50 ° C.
(2) 건조된 TCSPC 구형 성형물을 사용자에 의해 요구되는 탄화 온도(약 300~800°C)에 의해 탄화(2) Carbonize the dried TCSPC spherical moldings at the carbonization temperature (about 300 ~ 800 ° C) required by the user
(3) 탄화된 TCSPC 구형 성형물을 700 ~ 900°C의 활성 온도에서 사용자에 의해 요구되는 활성 시간(약 15 ~ 60분)에 의해 활성(3) Activate the carbonized TCSPC spherical moldings by the activation time (about 15 to 60 minutes) required by the user at an activation temperature of 700 to 900 ° C.
이하에, 상기 검토 내용을 기초로 하고 도 2를 참조하여 구리를 도핑한 이산화티타늄 광 촉매가 합성된 활성탄을 제조하는 방법을 설명한다. In the following, a method of producing activated carbon in which a titanium dioxide photocatalyst doped with copper is synthesized will be described based on the above-described details and with reference to FIG. 2.
먼저, 이산화티타늄 용출 재료로서 초 순도의 TTIP(97%, Aldrich) 15 ㎖을 제1 용매로서 제1 아이소프로판올(i-PrOH, 99.9%, Aldrich) 100 ㎖에 혼합하여 제1 졸을 생성한다(단계 102). 이 경우, 상기 용매인 아이소프로판올은 상기 이산화티타늄 용출 재료인 상기 TTIP 또는 상기 티타늄-엔-부톡사이드와의 몰 혼합비가 (40~80):1 범위인 것이 바람직하다.First, 15 ml of ultrapure TTIP (97%, Aldrich) as a titanium dioxide eluting material was mixed with 100 ml of first isopropanol (i-PrOH, 99.9%, Aldrich) as a first solvent to form a first sol ( Step 102). In this case, the solvent isopropanol preferably has a molar mixing ratio of (40 to 80): 1 with the TTIP or the titanium-ene-butoxide, which is the titanium dioxide eluting material.
그 후, 0.034g의 염화구리(Ⅱ) (CuCl2, Fisher Scientific)를 제2 용매로서 제2 아이소프로판올(i-PrOH, 99.9%, Aldrich) 75 ㎖에 도핑하여 제2 졸을 생성한다(단계 104). 이 경우, 상기 염화구리(Ⅱ)의 도핑양은 상기 TTIP 또는 상기 티타늄-엔-부톡사이드의 주입량의 1~10M%인 것이 바람직하다.Thereafter, 0.034 g of copper (II) chloride (CuCl 2 , Fisher Scientific) is doped into 75 ml of a second isopropanol (i-PrOH, 99.9%, Aldrich) as a second solvent to generate a second sol (step 104). In this case, the doping amount of the copper (II) chloride is preferably 1 ~ 10M% of the injection amount of the TTIP or the titanium-ene-butoxide.
상기 제1 졸과 상기 제2 졸을 혼합하여 졸 혼합물을 생성하고 상기 졸 혼합물을 상온에서 1 시간 동안 교반하고 활성화하여 염화구리가 도핑된 이산화티타늄 활성화 졸 혼합물을 생성한다(단계 106). The first sol and the second sol are mixed to form a sol mixture, and the sol mixture is stirred and activated at room temperature for 1 hour to produce a titanium dioxide activated sol mixture doped with copper chloride (step 106).
그 후 상기 염화구리가 도핑된 이산화티타늄 활성화 졸 혼합물에 일정한 양, 예를 들면10 ~ 80g의 야자 열매 각질 분말 및 15 ㎖의 증류수를 주입하면서(단계 108), 초음파 교반기를 이용하여 60분 동안 교반시키는 동시에 침전물을 가수분해하여 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 생성한다(단계 110). 본 발명의 실시예에서는 자가 제균 능력을 갖는 구리를 이용하지만, 본 발명은 이에 한정되지 않는다. 즉, 백금, 금, 은, 텅스텐, 아연 등의 금속도 적용 가능하다.The copper chloride-doped titanium dioxide activated sol mixture was then stirred for 60 minutes using an ultrasonic stirrer, while injecting a constant amount, e.g. 10-80 g of coconut keratin powder and 15 ml of distilled water (step 108). At the same time, the precipitates are hydrolyzed to produce palm fruit keratin powders in which copper and titanium dioxide photocatalysts are synthesized (step 110). Although the embodiment of the present invention uses copper having self-sterilization ability, the present invention is not limited thereto. That is, metals, such as platinum, gold, silver, tungsten, and zinc, are also applicable.
그 후, 순환 진공 농축기를 이용하여 상기 교반된 염화구리(Ⅱ) (CuCl2)가 도핑된 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 농축시킴으로써, 균등하고 견고하게 코팅이 되고 남아있는 공기, 용매, 및 증류수를 완전히 제거한다(단계 112).Thereafter, by using a circulating vacuum concentrator to concentrate the coconut fruit keratin powder synthesized with the titanium dioxide photocatalyst doped with the stirred copper chloride (II) (CuCl 2 ), uniformly and firmly coated and remaining air, The solvent and distilled water are removed completely (step 112).
상기 농축된 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 일정량의 풀을 점결재로 혼합한 후(단계 114), AMPL 공정을 통하여 구형의 성형물로 성형한다(단계 116). 단계 114에서 상기 야자 열매 각질 분말과 상기 풀의 혼합 비율은 1:(0.75~0.95)이고, 상기 풀은 물과 밀가루의 혼합비가 (8~11):1 범위인 것이 바람직하다. 상기 AMPL 공정은 TCSPC 혼합물의 점결력을 증대시키는 반죽 및 압밀하는 반죽기와 압밀기 그리고, 환의 형태로 생산하기 위한 환 제조기, 마지막으로 제조된 환의 분쇄 강도를 증대시키기 위해 회전시키는 회전 롤러로 구성되어 있다.Coconut keratin powder synthesized with the concentrated copper and titanium dioxide photocatalyst is mixed with a predetermined amount of grass as a caking additive (step 114), and then molded into a spherical molding through an AMPL process (step 116). In step 114, the mixing ratio of the coconut fruit keratin powder and the grass is 1: (0.75-0.95), and the mixing ratio of water and wheat flour is preferably in the range of (8-11): 1. The AMPL process consists of a dough to increase the cohesive force of the TCSPC mixture, a compacting kneader and a compactor, a ring making machine for producing in the form of a ring, and a rotating roller rotating to increase the breaking strength of the finally produced ring. .
상기 AMPL 공정을 통해 제조된 구형의 성형물을 40 ~ 50°C의 건조 온도에서 4 시간 이상, 바람직하게는 4 ~ 10 시간 동안 건조한다(단계 118).The spherical moldings produced through the AMPL process are dried at a drying temperature of 40-50 ° C. for at least 4 hours, preferably 4-10 hours (step 118).
그 후, 상기 건조된 구형 성형물을 300 ~ 800°C의 탄화온도에서 30 ~ 120분, 바람직하게는 60분 동안 탄화하여 탄화물을 생성한다(단계 120). 상기 탄화 공정을 통해 제조된 탄화물을 700 ~ 900°C의 활성 온도에서 15 ~ 60분 동안 활성화하여 구형 활성탄을 제조한다(단계 122).The dried spherical molding is then carbonized at a carbonization temperature of 300-800 ° C. for 30-120 minutes, preferably 60 minutes, to produce carbide (step 120). The carbide produced through the carbonization process is activated for 15 to 60 minutes at an activation temperature of 700 to 900 ° C to produce spherical activated carbon (step 122).
상기 구리 및 이산화티타늄이 합성된 TCSPC 활성탄은 여러 번의 실험을 통해 출발 물질, 도펀트, 용매 그리고, 증류수의 주입량을 결정하였다. 또한 순환 진공 농축 및 AMPL 공정에 의해 구리/이산화티타늄 나노 입자는 야자 열매 각질 가루 표면에 더욱 균등하고 견고하게 합성되고, 자동화 공정에 따른 대량생산 및 분쇄강도가 증대되어, 성능 및 형상이 우수한 구형 TCSPC 활성탄을 완성한다.The TCSPC activated carbon obtained by synthesizing copper and titanium dioxide was determined through a number of experiments to determine the amount of starting material, dopant, solvent, and distilled water. In addition, copper / titanium dioxide nanoparticles are more uniformly and firmly synthesized on the surface of coconut fruit keratin by circulating vacuum concentration and AMPL process. Complete activated carbon.
다음의 실시예에 의하여 본 발명을 더욱 명확하고 구체적으로 이해할 수 있을 것이다. 그러나 다음 실시예에는 본 발명의 범위를 한정하거나 제한하지 않음을 밝혀 둔다. The following examples will more clearly and specifically understand the present invention. However, the following examples are not intended to limit or limit the scope of the present invention.
실시예Example 1 One
기존의 이산화티타늄이 합성된 활성탄과 본 발명에 의해 제조된 TCSPC 활성탄의 XRD 패턴 비교 실험 결과가 도 2 및 도 3에 설명되어 있다. 도 2는 종래의 이산화티타늄 광 촉매가 합성된 활성탄의 결정상을 분석하기 위해 XRD를 이용하여 나타낸 그래프이다. 도 3은 도 1의 제조방법에 의해 제조된 TCSPC 구형 활성탄의 결정상을 분석하기 위해 XRD를 이용하여 나타낸 그래프이다.The XRD pattern comparison test results of the activated carbon synthesized with the conventional titanium dioxide and the TCSPC activated carbon prepared by the present invention are illustrated in FIGS. 2 and 3. 2 is a graph showing the use of XRD to analyze the crystal phase of the activated carbon synthesized with a conventional titanium dioxide photocatalyst. 3 is a graph using XRD to analyze the crystal phase of the TCSPC spherical activated carbon prepared by the manufacturing method of FIG.
실시예Example 2 2
기존의 이산화티타늄이 합성된 활성탄과 본 발명에 의해 제조된 TCSPC 활성탄의 SEM 영상 비교 실험 결과가 도 4 및 도 5에 설명되어 있다. 도 4는 종래의 이산화티타늄 광 촉매가 합성된 활성탄의 구조상 형상을 분석하기 위해 분말 형태의 야자 각탄을 SEM을 이용해 찍은 사진의 사시도이다. 도 5는 도 1의 제조 방법에 의해 제조된 TCSPC 활성탄의 구조상 형상을 분석하기 위해 분말 형태의 야자 각탄을 SEM을 이용해 찍은 사진의 사시도이다.The SEM image comparison experiment results of the activated carbon synthesized with the conventional titanium dioxide and the TCSPC activated carbon prepared according to the present invention are illustrated in FIGS. 4 and 5. Figure 4 is a perspective view of the photograph taken by using the SEM in the form of palm pentagonal powder in order to analyze the structural shape of the activated carbon synthesized with a conventional titanium dioxide photocatalyst. FIG. 5 is a perspective view of a photograph taken by using a SEM of coal petroleum powder in the form of powder to analyze the structural shape of the TCSPC activated carbon prepared by the method of FIG. 1.
실시예Example 3 3
자외선 조사 하에서의 기존의 광 촉매/활성탄 및 TCSPC 활성탄의 Escherichia coli (pathogenic microorganisms, 이하 E. coli) 제균 실험 결과가 도 6에 설명되어 있다. 도 6은 자외선 조사 하에서의 일반 광촉매/활성탄 및 TCSPC 활성탄의 E.coli 제균 실험의 결과를 나타낸 그래프이다.Experimental results of Escherichia coli (E. coli) disinfection of conventional photocatalyst / activated carbon and TCSPC activated carbon under ultraviolet irradiation are described in FIG. 6. 6 is a graph showing the results of the E. coli bactericidal experiment of ordinary photocatalyst / activated carbon and TCSPC activated carbon under ultraviolet irradiation.
E. coli는 배설물 대장균의 일종으로써, 하수나 축산폐수에 흔히 존재하는 물질이다. 따라서, 본 발명에 의해 제조된 TCSPC 활성탄을 이용하여 수중에 존재하는 E. coli의 제거율을 평가하기 위해 자외선이 조사되는 조건 하에서 비교 실험을 하였다. (E. coli의 초기농도= ~108CFU/㎖, pH=6.5, T=25°C, UVC=11W) E. coli is a species of fecal coliform that is common in sewage and livestock wastewater. Therefore, in order to evaluate the removal rate of E. coli present in water using the TCSPC activated carbon prepared according to the present invention, a comparative experiment was conducted under the condition of ultraviolet irradiation. (E. coli initial concentration = ~ 10 8 CFU / ㎖, pH = 6.5, T = 25 ° C, UVC = 11W)
실시예Example 4 4
빛이 조사되지 않는 상태에서 일반 광 촉매, 활성탄 및 광 촉매가 합성된 활성탄 그리고 TCSPC 활성탄의 E. coli 제균 실험 결과가 도 7에 설명되어 있다. 도 7은 빛이 조사되지 않는 상태에서 일반 광 촉매/활성탄 및 TCSPC 활성탄의 E.coli 제균 실험의 결과를 나타낸 그래프이다. 도 7을 참조하면, 빛이 조사되는 않는 상태에서 수중에 존재하는 E. coli의 제거율을 평가하기 위해 다양한 광촉매 및 흡착제와 비교 실험을 하였다. (E. coli의 초기농도= ~108 CFU/㎖, pH=6.5, T=25°C).E. coli bactericidal test results of the general photocatalyst, activated carbon and activated carbon synthesized photocatalyst, and TCSPC activated carbon without light irradiation are described in FIG. 7. FIG. 7 is a graph showing the results of E. coli sterilization experiments of ordinary photocatalyst / activated carbon and TCSPC activated carbon in the absence of light irradiation. Referring to FIG. 7, comparative experiments were performed with various photocatalysts and adsorbents in order to evaluate the removal rate of E. coli present in water in the absence of light irradiation. (Initial concentration of E. coli = -10 8 CFU / mL, pH = 6.5, T = 25 ° C.).
이상에서는 본 발명을 특정의 바람직한 실시예로서 설명하였으나, 본 발명은 상기한 실시예에 한정되지 아니하며, 특허 청구의 범위에서 청구하는 본 발명의 요지를 벗어남이 없이 당해 발명이 속하는 분야에서 통상의 지식을 가진 자라면 누구든지 다양한 변형이 가능할 것이다.Although the present invention has been described as a specific preferred embodiment, the present invention is not limited to the above-described embodiments, and the present invention is not limited to the above-described embodiments without departing from the gist of the present invention as claimed in the claims. Anyone with a variety of variations will be possible.
본 발명에 따라 제조된 TCSPC 활성탄은 구리를 이산화티타늄에 도핑함으로써, 약한 빛뿐만 아니라 빛이 도달하지 않는 어두운 곳에서도 제균 작용이 일어나므로, 에너지 소비량을 감소시키고, 전하 분리의 역할에 의한 광분해 활성도를 크게 향상시키며, 다양한 형태로 제조하여 수질 정화, 대기 오염 정화, 방습제, 방오제 및 제균제 등 광범위한 산업분야에 적용이 가능하다. 이러한 본 발명은 정부가 국책 과제로 육성하고 있는 신성장 동력 분야 중 (1) 탄소 저감 에너지 분야의 연소 배가스, CO2 포집 소재 기술, CO2 흡수 분리 소재 기술, 저가 산소 대량 생산 기술, (2) 고도 물처리 분야의 미량 유해 물질의 선택적 제거 및 수질 조정 기술, 미생물 재성장 및 소독 부산물 관리 기술, 하수 재 이용 공정 농축수 처리 기술, 하수 내 유해 물질 제거 및 수질 안정성 확보 기술, 생태 하천 복원 용수 확보 기술, 탁수 저감 및 확산 방지 기술, 부 영양화 제어 기술 분야 등 대기, 수질 분야에서 광범위하게 경제적으로 응용될 수 있는 중요한 소재이며 방습재, 방오재, 제균재 등 산업 전반에 걸쳐 적용성이 풍부하고 수입 대체 효과가 매우 크며 해외 수출이 가능한 주요 기술이다.The TCSPC activated carbon prepared according to the present invention has a decontamination effect not only in weak light but also in dark places where light does not reach by doping copper with titanium dioxide, thereby reducing energy consumption and improving photolysis activity by the role of charge separation. It is greatly improved and manufactured in various forms, and can be applied to a wide range of industrial fields such as water purification, air pollution purification, desiccant, antifouling agent and bactericide. The present invention is a new growth engine field that the government is developing as a national project (1) combustion flue gas, CO 2 capture material technology, CO 2 in the field of carbon reduction energy Absorption separation material technology, low-cost oxygen mass production technology, (2) selective removal and removal of trace harmful substances in advanced water treatment, microbial regrowth and disinfection by-product management technology, sewage recycling process concentrated water treatment technology, hazardous waste in sewage It is an important material that can be widely applied economically in the air and water quality fields, such as material removal and water quality securing technology, ecological river restoration water securing technology, turbidity reduction and diffusion prevention technology, and nutrient control technology. It is a key technology that can be exported abroad, with abundant applicability, a great effect of import substitution, and a wide range of industries including fungicides.
Claims (5)
(ii) 염화구리를 제2 아이소프로판올에 도핑하여 제2 졸을 생성한 후 상기 제1 졸과 상기 제2 졸을 교반하고 활성화하여 염화구리가 도핑된 이산화티타늄 활성화 졸 혼합물을 생성하는 단계;
(iii) 상기 염화구리가 도핑된 이산화티타늄 활성화 졸 혼합물에 야자 열매 각질 분말 및 증류수를 주입하면서 교반시키는 동시에 침전물을 가수분해하여 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 생성하는 단계;
(iv) 상기 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 농축시켜 남아 있는 공기, 용매, 및 증류수를 제거하는 단계;
(v) 상기 농축된 구리 및 이산화티타늄 광 촉매가 합성된 야자 열매 각질 분말을 풀과 혼합하고 구형의 성형물로 성형한 후 건조시키는 단계; 및
(vi) 상기 건조된 구형 성형물을 탄화 및 활성화하는 단계를 포함하며,
단계 (i)에서 상기 아이소프로판올과 상기 티타늄 테트라이소프로폭사이드 또는 상기 티타늄-엔-부톡사이드의 몰 혼합비가 (40~80):1 범위이고, 단계 (ii)에서 상기 염화구리의 도핑량은 상기 티타늄 테트라이소프로폭사이드 또는 상기 티타늄-엔-부톡사이드의 주입량의 1 ~ 10 M%이고, 단계 (v)에서 상기 야자 열매 각질 분말과 상기 풀의 혼합 비율은 1:(0.75~0.95)이고, 상기 풀은 물과 밀가루의 혼합비가 (8~11):1 범위이며, 상기 구형의 성형물로 성형하는 과정은 반죽, 압밀, 환 제조, 회전, 및 건조 공정을 순차적으로 수행하는 자동 대량 생산 라인을 통하여 이루어지며, 상기 구형의 성형물을 40 ~ 50°C의 건조 온도에서 4 ~ 10시간 동안 건조하는 구형 활성탄의 제조 방법.(i) mixing titanium tetraisopropoxide or titanium-ene-butoxide with the first isopropanol to produce a first sol;
(ii) doping copper chloride to the second isopropanol to form a second sol, followed by stirring and activating the first sol and the second sol to produce a copper chloride doped titanium dioxide activated sol mixture;
(iii) injecting palm fruit keratin powder and distilled water into the copper chloride doped titanium dioxide activated sol mixture while stirring and hydrolyzing the precipitate to produce palm fruit keratin powder synthesized with copper and titanium dioxide photocatalyst;
(iv) concentrating the palm fruit keratin powder synthesized with the copper and titanium dioxide photocatalyst to remove remaining air, solvent, and distilled water;
(v) mixing the concentrated copper and titanium dioxide photocatalyst with the palm fruit keratin powder with the grass, forming a spherical molding and drying the powder; And
(vi) carbonizing and activating the dried spherical molding,
The molar mixing ratio of the isopropanol and the titanium tetraisopropoxide or the titanium-ene-butoxide in step (i) is in the range of (40 to 80): 1, and the doping amount of the copper chloride in step (ii) is 1-10 M% of the injection amount of the titanium tetraisopropoxide or the titanium-ene-butoxide, and the mixing ratio of the palm kernel keratin powder and the grass in step (v) is 1: (0.75-0.95) , The pool is a mixture of water and wheat flour (8 ~ 11): 1, the molding process of the spherical molding is an automatic mass production line to sequentially perform the kneading, consolidation, ring manufacturing, rotation, and drying process Made through, the spherical molded product is a method for producing spherical activated carbon is dried for 4 to 10 hours at a drying temperature of 40 to 50 ° C.
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| CN112516979A (en) * | 2020-11-24 | 2021-03-19 | 中国人民解放军92609部队 | Coconut shell carbon loaded titanium dioxide and preparation method thereof |
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| KR20000030368A (en) * | 2000-02-25 | 2000-06-05 | 김영규 | Manufactural method of activated carbon as a bactericidal photo-catalyst. |
| JP2000317271A (en) * | 1999-05-06 | 2000-11-21 | Nissan Motor Co Ltd | Adsorbent |
| KR100292140B1 (en) | 1999-04-08 | 2001-06-01 | 임창혁 | Metal deposited active carbon having selective absorption capability for polar contaminants and preparation method thereof |
| US6673738B2 (en) * | 2001-11-28 | 2004-01-06 | K.K. Ueda Shikimono Kojyo | Photocatalytic active carbon, colored photocatalytic active carbon, coloring active carbon, and deodorant and adsorption product using them |
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| KR100292140B1 (en) | 1999-04-08 | 2001-06-01 | 임창혁 | Metal deposited active carbon having selective absorption capability for polar contaminants and preparation method thereof |
| JP2000317271A (en) * | 1999-05-06 | 2000-11-21 | Nissan Motor Co Ltd | Adsorbent |
| KR20000030368A (en) * | 2000-02-25 | 2000-06-05 | 김영규 | Manufactural method of activated carbon as a bactericidal photo-catalyst. |
| US6673738B2 (en) * | 2001-11-28 | 2004-01-06 | K.K. Ueda Shikimono Kojyo | Photocatalytic active carbon, colored photocatalytic active carbon, coloring active carbon, and deodorant and adsorption product using them |
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| CN112516979A (en) * | 2020-11-24 | 2021-03-19 | 中国人民解放军92609部队 | Coconut shell carbon loaded titanium dioxide and preparation method thereof |
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