KR102607954B1 - Manufacturing method of porous carbon composites for sterilization and antimicrobial including transition metals - Google Patents
Manufacturing method of porous carbon composites for sterilization and antimicrobial including transition metals Download PDFInfo
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- KR102607954B1 KR102607954B1 KR1020210026147A KR20210026147A KR102607954B1 KR 102607954 B1 KR102607954 B1 KR 102607954B1 KR 1020210026147 A KR1020210026147 A KR 1020210026147A KR 20210026147 A KR20210026147 A KR 20210026147A KR 102607954 B1 KR102607954 B1 KR 102607954B1
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- porous carbon
- transition metal
- sterilization
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- 230000001954 sterilising effect Effects 0.000 title claims abstract description 25
- 238000004659 sterilization and disinfection Methods 0.000 title claims abstract description 21
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 21
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 150000001721 carbon Chemical class 0.000 title claims abstract description 5
- 230000000845 anti-microbial effect Effects 0.000 title 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 101710134784 Agnoprotein Proteins 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 229910021524 transition metal nanoparticle Inorganic materials 0.000 abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052802 copper Inorganic materials 0.000 abstract description 6
- 239000004332 silver Substances 0.000 abstract description 6
- 229910052725 zinc Inorganic materials 0.000 abstract description 6
- 239000011701 zinc Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000004887 air purification Methods 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract 1
- 241000894006 Bacteria Species 0.000 description 5
- 239000000428 dust Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000010169 landfilling Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000008786 sensory perception of smell Effects 0.000 description 1
- 229910001958 silver carbonate Inorganic materials 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
-
- 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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
본 발명은 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법에 관한 것으로, 더욱 상세하게는 다공성탄소에 구리, 은, 아연 등을 포함하는 전이금속 나노입자를 담지하여 살균 및 항균용 다공성 탄소복합체를 제조하는 방법에 관한 것이다.
본 발명에 따르면, 살균 및 항균성능이 최적화된 전이금속 나노입자가 담지된 다공성 탄소복합체를 제공함에 따라, 공기정화 및 유해오염물 제거를 위한 필터여재소재 및 흡착탑 충진제 등의 소재로 이용될 수 있다.The present invention relates to a method of manufacturing a porous carbon composite for sterilization and antibacterial purposes loaded with a transition metal. More specifically, the present invention relates to a method of manufacturing a porous carbon composite for sterilization and antibacterial purposes by loading transition metal nanoparticles containing copper, silver, zinc, etc. on porous carbon. It relates to a method of manufacturing carbon composites.
According to the present invention, a porous carbon composite containing transition metal nanoparticles with optimized sterilization and antibacterial performance is provided, and thus can be used as a material for filter media and adsorption tower filler for air purification and removal of harmful contaminants.
Description
본 발명은 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법에 관한 것으로, 더욱 상세하게는 다공성탄소에 구리, 은, 아연 등을 포함하는 전이금속 나노입자를 담지하여 살균 및 항균용 다공성 탄소복합체를 제조하는 방법에 관한 것이다.The present invention relates to a method of manufacturing a porous carbon composite for sterilization and antibacterial purposes loaded with a transition metal. More specifically, the present invention relates to a method of manufacturing a porous carbon composite for sterilization and antibacterial purposes by loading transition metal nanoparticles containing copper, silver, zinc, etc. on porous carbon. It relates to a method of manufacturing carbon composites.
현대인의 일상생활 중 약 85% 이상이 실내생활시간으로 보고되고 있으며, 이러한 실내활동시간이 더욱 높아짐에 따라 실내공기질 향상에 대한 요구가 증가하고 있다. 실내공기에는 물리적, 화학적, 생물학적 오염물질이 존재하며, 이에 따라 사람의 후각을 자극하여 불쾌감이나 혐오감을 주는 악취물질, 공기 중 분진이나 세균 등을 제거하기 위한 공기청정소재 개발에 대한 요구가 증가하고 있다. 그러나 공기청정용 필터의 장시간 사용에 있어 필터에 걸러진 미생물은 분진 및 이물질을 영양분으로 증식하고, 증식된 미생물은 공기의 흐름에 따라 유출부로 이동하여 세균의 2차오염이라는 심각한 문제를 초래할 수 있다. 따라서 생물학적 오염물질을 사멸시키는 소재는 병원, 공공시설 등 업무용 공기정화시스템과 식품, 의약품, 생활용품, 농축산업, 어업, 첨단바이오 산업에 이르기 까지 광범위한 활용가치를 가진다. 현재 활용되고 있는 공기청정기술은 활성탄이나 유리섬유 또는 세라믹 필터를 사용하는 여과, 흡착, 전기집진 및 음이온발생기술 등이 있다. 그러나 기존의 다공성 여재를 사용한 여과, 흡착기술은 오염물질을 기체상에서 고체상으로 이동시키는 것으로 재사용을 위한 매립 또는 소각시 2차오염을 유발시킨다는 단점이 있다.It is reported that more than 85% of modern people's daily lives are spent indoors, and as the indoor activity time increases, the demand for improving indoor air quality is increasing. Physical, chemical, and biological contaminants exist in indoor air, and as a result, there is an increasing demand for the development of air cleaning materials to remove odorous substances and airborne dust or bacteria that stimulate a person's sense of smell and cause discomfort or disgust. there is. However, when an air purifying filter is used for a long time, the microorganisms caught in the filter proliferate using dust and foreign substances as nutrients, and the proliferated microorganisms move to the outlet according to the air flow, which can cause a serious problem of secondary bacterial contamination. Therefore, materials that kill biological pollutants have a wide range of applications, ranging from business air purification systems such as hospitals and public facilities to food, medicine, household goods, agricultural and livestock industries, fisheries, and high-tech bio industries. Air purification technologies currently in use include filtration, adsorption, electrostatic dust collection, and negative ion generation technologies using activated carbon, glass fiber, or ceramic filters. However, filtration and adsorption technology using existing porous filter media has the disadvantage of causing secondary pollution when landfilling or incineration for reuse as it moves pollutants from the gas phase to the solid phase.
이에 본 발명자는 다공성탄소에 구리, 은, 아연 등을 포함하는 전이금속 나노입자를 담지하여 살균 및 항균성능이 극대화된 다공성 탄소복합체를 제공함에 따라, 생물학적 대기유해인자인 세균의 살균 및 항균을 위한 소재 및 이의 제조방법을 제공하고자 한다.Accordingly, the present inventor has provided a porous carbon composite with maximized sterilization and antibacterial performance by carrying transition metal nanoparticles containing copper, silver, zinc, etc. on porous carbon, thereby providing a porous carbon composite for sterilization and antibacterial purposes of bacteria, which are biological harmful factors in the atmosphere. The purpose is to provide materials and manufacturing methods.
본 발명의 목적은, 다공성탄소에 구리, 은, 아연 등을 포함하는 전이금속 나노입자를 담지하여 살균 및 항균성능이 극대화된 다공성 탄소복합체를 제공함에 따라, 생물학적 대기유해인자인 세균의 살균 및 항균을 위한 소재 및 이의 제조방법을 제공하는 것이다.The purpose of the present invention is to provide a porous carbon composite with maximized sterilization and antibacterial performance by carrying transition metal nanoparticles containing copper, silver, zinc, etc. on porous carbon, thereby providing sterilization and antibacterial properties for bacteria, which are biological harmful factors in the atmosphere. To provide materials and methods for manufacturing the same.
상기 목적을 달성하기 위하여, 본 발명은 다공성탄소에 구리, 은, 아연 등을 포함하는 전이금속 나노입자를 담지하여 살균 및 항균성이 극대화된 다공성 탄소복합체를 제조하는 방법으로, 1) 다공성탄소에 전이금속 전구체를 용매를 사용하여 혼합하는 단계; 2) 상기 1)단계에서 얻어진 혼합물을 열처리 및 건조하는 단계; 3) 상기 2)단계에서 합성된 전이금속 탄소복합체를 열환원하는 단계; 4) 상기 3)단계 이후 세척 및 건조하는 단계;를 포함할 수 있다.In order to achieve the above object, the present invention is a method of producing a porous carbon composite with maximized sterilization and antibacterial properties by supporting transition metal nanoparticles containing copper, silver, zinc, etc. on porous carbon, which includes: 1) transfer to porous carbon mixing metal precursors using a solvent; 2) heat treating and drying the mixture obtained in step 1); 3) thermally reducing the transition metal carbon composite synthesized in step 2); 4) washing and drying after step 3).
바람직하게, 상기 1)단계에서 전이금속 전구체로써 질산구리(Cu(NO3)2), 질산은(AgNO3), 질산아연(Zn(NO3)2), 탄산구리(CuCO3), 탄산은(Ag2CO3), 탄산아연(ZnCO3), 염화구리(CuCl2), 염화은(AgCl), 염화아연(ZnCl2)으로 이루어진 군에서 선택된 하나를 사용하는 것을 포함할 수 있다.Preferably, in step 1), copper nitrate (Cu(NO 3 ) 2 ), silver nitrate (AgNO 3 ), zinc nitrate (Zn(NO 3 ) 2 ), copper carbonate (CuCO 3 ), and silver carbonate ( It may include using one selected from the group consisting of Ag 2 CO 3 ), zinc carbonate (ZnCO 3 ), copper chloride (CuCl 2 ), silver chloride (AgCl), and zinc chloride (ZnCl 2 ).
바람직하게, 상기 1)단계에서 혼합은, 다공성탄소와 전이금속 전구체를 1:0.01 내지 1:10 무게비로 사용하여 혼합하는 것을 포함할 수 있다.Preferably, mixing in step 1) may include mixing porous carbon and transition metal precursor at a weight ratio of 1:0.01 to 1:10.
바람직하게, 상기 1)단계에서 상기 용매는, 증류수, 에탄올, 아세톤 중에서 선택된 하나인 것을 포함할 수 있다.Preferably, in step 1), the solvent may include one selected from distilled water, ethanol, and acetone.
바람직하게, 상기 2)단계의 열처리는, 20 내지 200℃의 온도범위에서 30분 내지 48시간 동안 수행하는 것을 포함할 수 있다.Preferably, the heat treatment in step 2) may include being performed for 30 minutes to 48 hours at a temperature range of 20 to 200°C.
바람직하게, 상기 3)단계의 열환원은, 수소, 아르곤 등을 포함하는 혼합 환원기체 분위기에서 100 내지 1000℃의 온도범위에서 10분 내지 5시간 동안 수행하는 것을 포함할 수 있다.Preferably, the thermal reduction in step 3) may include being performed for 10 minutes to 5 hours at a temperature range of 100 to 1000° C. in a mixed reducing gas atmosphere containing hydrogen, argon, etc.
바람직하게, 상기 4)단계의 세척은, 1 내지 48시간 동안 세척하는 것이고, 상기 건조는, 6 내지 48시간 동안 건조하는 것을 포함할 수 있다.Preferably, the washing in step 4) includes washing for 1 to 48 hours, and the drying may include drying for 6 to 48 hours.
상기와 같은 본 발명에 따르면, 다공성탄소에 구리, 은, 아연 등을 포함하는 전이금속 나노입자를 담지하여 살균 및 항균성능이 극대화된 다공성 탄소복합체를 제공함에 따라, 생물학적 대기유해인자인 세균의 살균 및 항균을 위한 소재로의 응용 및 관련 분야로서의 다양한 활용이 가능하여 고부가가치를 창출할 수 있는 효과가 있다.According to the present invention as described above, transition metal nanoparticles containing copper, silver, zinc, etc. are supported on porous carbon to provide a porous carbon composite with maximized sterilizing and antibacterial performance, thereby sterilizing bacteria, which are biological harmful factors in the atmosphere. It can be used as an antibacterial material and in various related fields, creating high added value.
도 1은 본 발명에서 얻어진 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 주사전자현미경(scanning electron microscope, SEM) 사진이다.
도 2는 본 발명에서 얻어진 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체를 활용한 살균 및 항균평가 광학이미지이다.Figure 1 is a scanning electron microscope (SEM) photograph of a porous carbon composite for sterilization and antibacterial use carrying a transition metal obtained in the present invention.
Figure 2 is an optical image of sterilization and antibacterial evaluation using the transition metal-supported porous carbon composite for sterilization and antibacterial use obtained in the present invention.
이하, 실시 예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실시 예는 오로지 본 발명을 예시하기 위한 것으로서, 본 발명의 범위가 이들 실시 예에 의해 제한되는 것으로 해석되지는 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail through examples. These examples are only for illustrating the present invention, and it will be obvious to those skilled in the art that the scope of the present invention is not to be construed as limited by these examples.
실시예 1. Example 1 .
다공성탄소 2g과 전이금속 전구체로 질산염(AgNO3) 2g을 혼합한 뒤 에탄올 용액이 담긴 비커에 넣고 교반하며 80℃의 온도조건에서 24시간 동안 열처리이후 건조하였다. 상기 전이금속이 담지된 탄소복합체를 튜브형 퍼니스에 넣고 수소/아르곤(H2/Ar) 혼합환원기체 분위기 하에서 200℃의 온도까지 승온시켜 120분간 유지하여 열환원 한 후, 실온까지 냉각시켰다. 이후 환원된 전이금속/탄소복합체를 증류수를 이용하여 8시간 동안 세척하고, 80℃에서 24시간 동안 건조하였다.After mixing 2 g of porous carbon and 2 g of nitrate (AgNO 3 ) as a transition metal precursor, the mixture was placed in a beaker containing an ethanol solution, stirred, and heat treated at 80°C for 24 hours before drying. The carbon composite carrying the transition metal was placed in a tubular furnace, heated to 200°C under a hydrogen/argon (H 2 /Ar) mixed reduction gas atmosphere, maintained for 120 minutes, thermally reduced, and then cooled to room temperature. Afterwards, the reduced transition metal/carbon composite was washed with distilled water for 8 hours and dried at 80°C for 24 hours.
실시예 2.Example 2.
상기 실시예 1과 동일하게 과정을 실시하되, 열처리단계에서 온도를 200℃로 하여 열처리시켰다.The same process as Example 1 was performed, but heat treatment was performed at a temperature of 200°C in the heat treatment step.
실시예 3.Example 3.
상기 실시예 1과 동일하게 과정을 실시하되, 열처리단계에서 온도를 20℃로 하여 열처리시켰다.The same process as Example 1 was performed, but heat treatment was performed at a temperature of 20°C in the heat treatment step.
실시예 4.Example 4.
상기 실시예 1과 동일하게 과정을 실시하되, 열처리단계에서 열처리시간을 30분으로 하여 열처리시켰다.The same process as Example 1 was performed, but the heat treatment time was set to 30 minutes in the heat treatment step.
실시예 5.Example 5.
상기 실시예 1과 동일하게 과정을 실시하되, 열처리단계에서 열처리시간을 48시간으로 하여 열처리시켰다.The same process as Example 1 was performed, but the heat treatment time was set to 48 hours in the heat treatment step.
실시예 6.Example 6.
상기 실시예 1과 동일하게 과정을 실시하되, 혼합단계에서 전이금속 전구체를 0.2g으로 하여 혼합하였다.The same process as Example 1 was performed, except that 0.2 g of transition metal precursor was mixed in the mixing step.
실시예 7.Example 7.
상기 실시예 1과 동일하게 과정을 실시하되, 혼합단계에서 전이금속 전구체를 20g으로 하여 혼합하였다.The same process as Example 1 was performed, except that 20 g of transition metal precursor was mixed in the mixing step.
실시예 8.Example 8.
상기 실시예 1과 동일하게 과정을 실시하되, 열환원단계에서 온도를 100℃로 하여 열처리시켰다.The same process as Example 1 was performed, but heat treatment was performed at a temperature of 100°C in the heat reduction step.
실시예 9.Example 9.
상기 실시예 1과 동일하게 과정을 실시하되, 열환원단계에서 온도를 1000℃로 하여 열처리시켰다.The same process as Example 1 was performed, but heat treatment was performed at a temperature of 1000°C in the heat reduction step.
실시예 10.Example 10.
상기 실시예 1과 동일하게 과정을 실시하되, 열환원단계에서 시간을 10분으로 하여 열처리시켰다.The same process as Example 1 was performed, but heat treatment was performed for 10 minutes in the heat reduction step.
실시예 11.Example 11.
상기 실시예 1과 동일하게 과정을 실시하되, 열환원단계에서 시간을 5시간으로 하여 열처리시켰다.The same process as Example 1 was performed, but heat treatment was performed for 5 hours in the heat reduction step.
실시예 12.Example 12.
상기 실시예 1과 동일하게 과정을 실시하되, 세척단계에서 세척시간을 1시간으로 하여 세척시켰다.The same process as Example 1 was performed, but the washing time was set to 1 hour in the washing step.
실시예 13.Example 13.
상기 실시예 1과 동일하게 과정을 실시하되, 세척단계에서 세척시간을 48시간으로 하여 세척시켰다.The same process as Example 1 was performed, but the washing time was set to 48 hours in the washing step.
실시예 14.Example 14.
상기 실시예 1과 동일하게 과정을 실시하되, 건조단계에서 건조시간을 6시간으로 하여 건조시켰다.The same process as Example 1 was performed, but the drying time was set to 6 hours in the drying step.
실시예 15.Example 15.
상기 실시예 1과 동일하게 과정을 실시하되, 건조단계에서 건조시간을 48시간으로 하여 건조시켰다.The same process as Example 1 was performed, but the drying time was set to 48 hours in the drying step.
비교예 1.Comparative Example 1.
상기 실시예 1과 동일하게 과정을 실시하되, 금속담지 및 열환원 단계를 시행하지 않았다.The same process as Example 1 was performed, but the metal loading and heat reduction steps were not performed.
측정예 1. 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 형태 및 구조 관찰Measurement Example 1. Observation of the shape and structure of a porous carbon composite containing transition metals for sterilization and antibacterial purposes.
Scanning Electron Microscopy(SEM, SU8010, Hitach Co., Ltd.)를 통해 본 발명에서 제조한 탄소복합체의 형태, 표면구조 및 내부 형상을 관찰하였다.The shape, surface structure, and internal shape of the carbon composite prepared in the present invention were observed through Scanning Electron Microscopy (SEM, SU8010, Hitach Co., Ltd.).
측정예 2. 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 항균 및 살균성능측정Measurement Example 2. Measurement of antibacterial and sterilizing performance of porous carbon composite for sterilization and antibacterial use carrying transition metals
본 발명에 따른 탄소복합체의 항균 및 살균성능을 평가하기 위하여, 37℃에서 배양된 1.6*105 (CFU/ml) S. aureus 균이 포함된 LB(Luria-Bertani) 배지를 이용하여 제조된 탄소복합체 2g을 세균배양 배지에 배치한 후 12시간 동안 37℃조건에서 배양하였다.In order to evaluate the antibacterial and sterilizing performance of the carbon composite according to the present invention, carbon prepared using LB (Luria-Bertani) medium containing 1.6*10 5 (CFU/ml) S. aureus bacteria cultured at 37°C 2 g of the complex was placed in a bacterial culture medium and cultured at 37°C for 12 hours.
아래 표 1에는 본 발명에 따른 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조조건을 나타내고, 아래 표 2에는 본 발명에 따른 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 살균 및 항균특성을 나타낸다.Table 1 below shows the manufacturing conditions for the porous carbon composite for sterilization and antibacterial use carrying a transition metal according to the present invention, and Table 2 below shows the sterilization and antibacterial conditions of the porous carbon composite for sterilization and antibacterial use carrying a transition metal according to the present invention. It represents the characteristics.
이상, 본 발명내용의 특정한 부분을 상세히 기술하였는바, 당업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적인 기술은 단지 바람직한 실시양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점은 명백할 것이다. 따라서 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의해 정의된다고 할 것이다. As above, specific parts of the present invention have been described in detail, and it is clear to those skilled in the art that these specific techniques are merely preferred embodiments and do not limit the scope of the present invention. something to do. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (7)
상기 1)단계에서 전이금속 전구체로써 질산은(AgNO3)을 사용하고, 상기 1)단계에서 혼합은, 다공성 탄소와 전이금속 전구체를 1:0.01 내지 1:10 무게비로 사용하여 혼합하는 것을 특징으로 하는 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법.1) mixing a transition metal precursor with porous carbon using a solvent; 2) heat treating and drying the mixture obtained in step 1); 3) thermally reducing the transition metal carbon composite synthesized in step 2); 4) washing and drying after step 3);
In step 1), silver nitrate (AgNO 3 ) is used as a transition metal precursor, and in step 1), the mixing is characterized by mixing porous carbon and the transition metal precursor at a weight ratio of 1:0.01 to 1:10. Method for manufacturing porous carbon composites containing transition metals for sterilization and antibacterial purposes.
상기 1)단계에서 상기 용매는, 증류수, 에탄올, 아세톤 중에서 선택된 하나인 것을 특징으로 하는 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법. According to clause 1,
In step 1), the solvent is one selected from distilled water, ethanol, and acetone.
상기 2)단계의 열처리는, 20 내지 200℃의 온도범위에서 30분 내지 48시간 동안 수행하는 것을 특징으로 하는 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법.According to clause 1,
The heat treatment in step 2) is a method of producing a porous carbon composite for sterilization and antibacterial use carrying a transition metal, characterized in that it is performed for 30 minutes to 48 hours at a temperature range of 20 to 200 ° C.
상기 3)단계의 열환원은, 수소 및 아르곤을 포함하는 혼합 환원기체 분위기에서 100 내지 1000℃의 온도범위에서 10분 내지 5시간 동안 수행하는 것을 특징으로 하는 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법. According to clause 1,
The thermal reduction in step 3) is performed in a mixed reducing gas atmosphere containing hydrogen and argon at a temperature range of 100 to 1000°C for 10 minutes to 5 hours. Method for manufacturing carbon composites.
상기 4)단계의 세척은, 1 내지 48시간 동안 세척하는 것이고, 상기 건조는, 6 내지 48시간 동안 건조하는 것을 특징으로 하는 전이금속이 담지된 살균 및 항균용 다공성 탄소복합체의 제조방법.According to clause 1,
The washing in step 4) involves washing for 1 to 48 hours, and the drying includes drying for 6 to 48 hours.
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