KR102438589B1 - Adsorptive-catalytic for removing formaldehyde, a metod of manufacturing the same, adsorbent and non-woven filter using the same - Google Patents
Adsorptive-catalytic for removing formaldehyde, a metod of manufacturing the same, adsorbent and non-woven filter using the same Download PDFInfo
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/32—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of manganese, technetium or rhenium
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- B01D39/14—Other self-supporting filtering material ; Other filtering material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
본 발명은 폴리에틸렌글리콜이 결합된 이산화망간을 포함하는 흡착 촉매에 관한 것으로서, 소량의 흡착 촉매로 높은 포름알데히드의 제거율을 보이며 제조 비용이 저렴한 포름알데히드 제거용 흡착 촉매, 이의 제조방법, 이를 포함하는 포름알데히드 흡착제 및 부직포 필터에 관한 것이다.The present invention relates to an adsorption catalyst comprising manganese dioxide bound to polyethylene glycol, which shows a high removal rate of formaldehyde with a small amount of adsorption catalyst and is inexpensive to manufacture, an adsorption catalyst for removing formaldehyde, a method for preparing the same, and formaldehyde comprising the same It relates to adsorbents and non-woven filters.
Description
본 발명은 포름알데히드 제거용 흡착 촉매, 이의 제조방법, 이를 포함하는 포름알데히드 제거용 흡착제 및 부직포 필터에 관한 것이다.The present invention relates to an adsorption catalyst for removing formaldehyde, a method for preparing the same, an adsorbent for removing formaldehyde and a nonwoven filter comprising the same.
최근 고농도 미세먼지 발생으로 인해 실내의 공기 정화가 주목받고 있다. 이에 따라, 실내에서 자체적으로 공기를 정화할 수 있는 공기청정장치가 개발되었고, 제거율을 높이기 위한 연구가 진행되고 있다. 종래의 개발된 공기청정장치는 미세먼지와 같은 입자상 오염물질의 제거에는 효율적이나, 포름알데히드 및 휘발성 유기화합물(VOCs)와 같은 가스상 오염물질의 제거 효율은 낮아 이에 대한 연구가 필요한 실정이다.Recently, due to the high concentration of fine dust, indoor air purification is attracting attention. Accordingly, an air purifier capable of purifying air indoors has been developed, and research is being conducted to increase the removal rate. The conventionally developed air purifier is efficient in removing particulate pollutants such as fine dust, but the removal efficiency of gaseous pollutants such as formaldehyde and volatile organic compounds (VOCs) is low, so research on this is required.
상기의 가스상 오염물질 중 포름알데히드는 실내 공기질에서 호흡기 질환 및 발암 물질로 알려져 있으며, 새집증후군의 원인 물질로 알려져 있다. 이를 제거하기 위해 다양한 합성 흡착 촉매들이 개발되고 있는데, 합성 흡착 촉매란 두 가지 이상의 다공성 구조를 결합시켜 제조된 중합체 또는 구체 입자들을 의미한다. 합성 흡착 촉매는 화합물을 쉽게 제거할 수 있고 활성탄보다 오래 사용할 수 있는 장점이 있으나 비용이 많이 드는 단점이 있어, 경제성과 효율성을 모두 만족하는 흡착 촉매의 개발이 요구되고 있다. 일례로 일본 공개특허 WO2009/084632에 의하면, 알루미늄 규산염복합체를 제조하여 흡착 촉매로도 이용하였는데 비용이 상대적으로 많이 발생하는 문제가 있었다.Among the gaseous pollutants, formaldehyde is known as a respiratory disease and carcinogen in indoor air quality, and is known as a causative agent of sick house syndrome. To remove this, various synthetic adsorption catalysts have been developed. The synthetic adsorption catalyst refers to polymers or spherical particles prepared by combining two or more porous structures. Synthetic adsorption catalysts have advantages in that compounds can be easily removed and can be used for a longer time than activated carbon, but have a disadvantage in that they are expensive. For example, according to Japanese Patent Application Laid-Open No. WO2009/084632, an aluminum silicate composite was prepared and used as an adsorption catalyst, but there was a problem in that the cost was relatively high.
한편, 이산화망간(MnO2)과 같은 금속산화물은 대기 중의 산소와 접촉시 잔류물이 탈착되어 재생되는 것을 보고되고 있어 합성 흡착 촉매의 재료로 적합하다.On the other hand, it has been reported that metal oxides such as manganese dioxide (MnO 2 ) are regenerated by desorption of residues when they come into contact with oxygen in the atmosphere, so they are suitable as a material for a synthetic adsorption catalyst.
본 발명은 상기한 바와 같은 문제점을 해결하기 위하여 제안된 것으로, 가스상 오염물질을 제거하는 데 아주 높은 제거율을 보일 뿐만 아니라, 제조단가가 저렴하여 경제성 또한 우수한 포름알데히드 제거용 흡착 촉매 및 이의 제조방법을 제공하고, 이를 적용한 포름알데히드 제거용 흡착제 및 부직포 필터를 제조하는 데 목적이 있다.The present invention has been proposed to solve the above-described problems, and provides an adsorption catalyst for removing formaldehyde and a method for manufacturing the same, which not only shows a very high removal rate for removing gaseous pollutants, but also has excellent economic feasibility due to low manufacturing cost. It aims to provide an adsorbent for removing formaldehyde and a non-woven filter to which it is applied.
상기한 과제를 해결하기 위한 본 발명의 포름알데히드 제거용 흡착 촉매의 제조방법은 폴리에틸렌글리콜(Polyethylene glycol), 이산화망간 전구체 및 물을 포함한 용액을 준비하는 1단계; 상기 용액을 반응시켜 폴리에틸렌글리콜이 결합된 이산화망간(MnO2) 복합체를 합성하는 2단계; 상기 복합체를 포함하는 용액을 여과하여 여과물을 수득한 뒤 세척하는 3단계; 및 세척한 여과물을 건조시켜 흡착 촉매를 수득하는 4단계;를 포함할 수 있다.The method for preparing an adsorption catalyst for removal of formaldehyde of the present invention for solving the above-described problems includes the first step of preparing a solution containing polyethylene glycol, a manganese dioxide precursor, and water; A second step of reacting the solution to synthesize a polyethylene glycol-coupled manganese dioxide (MnO 2 ) complex; Step 3 of filtering the solution containing the complex to obtain a filtrate and then washing; and drying the washed filtrate to obtain an adsorption catalyst.
본 발명의 일실시예로써, 상기 1단계에 있어서, 상기 용액은 상기 폴리에틸렌글리콜 및 이산화망간 전구체를 1 : 5.0 ~ 1 : 8.0 중량비로 포함할 수 있다.As an embodiment of the present invention, in the first step, the solution may contain the polyethylene glycol and the manganese dioxide precursor in a weight ratio of 1:5.0 to 1:8.0.
본 발명의 일실시예로써, 상기 이산화망간 전구체는 과망간산칼륨(KMnO4), 망간아세테이트(Mn(CH3CO2)2), 과망간산나트륨(NaMnO4) 및 황산망간(MnSO4) 중에서 선택된 1종 이상을 포함할 수 있다.As an embodiment of the present invention, the manganese dioxide precursor is potassium permanganate (KMnO 4 ), manganese acetate (Mn(CH 3 CO 2 ) 2 ), sodium permanganate (NaMnO 4 ) and manganese sulfate (MnSO 4 ) At least one selected from the group consisting of may include
본 발명의 일실시예로써, 2단계의 반응은 60 ~ 100℃ 하에서 5 ~ 25분 동안 중탕 및 교반하여 수행할 수 있다.As an embodiment of the present invention, the reaction in step 2 may be performed by bathing and stirring for 5 to 25 minutes at 60 to 100°C.
본 발명의 일실시예로써, 4단계의 건조는 80 ~ 130℃ 하에서 10 ~ 14시간 동안 수행할 수 있다.As an embodiment of the present invention, the fourth step of drying may be performed under 80 to 130° C. for 10 to 14 hours.
본 발명의 다른 목적으로, 포름알데히드 제거용 흡착 촉매는 이산화망간(MnO2); 및 상기 이산화망간과 결합된 폴리에틸렌글리콜(Polyethylene glycol);을 포함할 수 있다.For another object of the present invention, the adsorption catalyst for removing formaldehyde is manganese dioxide (MnO 2 ); and polyethylene glycol combined with the manganese dioxide.
본 발명의 일실시예로써, 상기 폴리에틸렌글리콜은 중량평균분자량(Mw)이 15,000 ~ 25,000인 것을 포함할 수 있다.As an embodiment of the present invention, the polyethylene glycol may include a weight average molecular weight (Mw) of 15,000 to 25,000.
본 발명의 다른 목적으로, 포름알데히드 흡착제는 폴리에틸렌글리콜이 결합된 이산화망간(MnO2)을 포함하는 흡착 촉매; 바인더; 및 에탄올;을 포함할 수 있다.For another object of the present invention, the formaldehyde adsorbent is an adsorption catalyst comprising polyethylene glycol bound manganese dioxide (MnO 2 ); bookbinder; and ethanol;
본 발명의 일실시예로써, 상기 에탄올 및 흡착 촉매를 1 : 0.08 ~ 1 : 0.11의 중량비로 포함할 수 있다.As an embodiment of the present invention, the ethanol and the adsorption catalyst may be included in a weight ratio of 1: 0.08 to 1: 0.11.
본 발명의 일실시예로써, 상기 바인더는 에틸 셀룰로오스(ethyl cellulose), 메틸 셀룰로오스(methyl cellulose), 니트로셀룰로오스(nitrocellulose), 메타크릴산 에스테르(methacrylic acid ester), 아크릴산 에스테르(acrylic acid ester), 폴리비닐알콜(polyvinyl alcohol) 및 폴리비닐부티랄(polyvinyl butyral) 중에서 선택된 1종 이상을 포함할 수 있다.In one embodiment of the present invention, the binder is ethyl cellulose, methyl cellulose, nitrocellulose, methacrylic acid ester, acrylic acid ester, poly It may include one or more selected from vinyl alcohol (polyvinyl alcohol) and polyvinyl butyral (polyvinyl butyral).
본 발명의 일실시예로써, 상기 바인더를 상기 흡착 촉매 100 중량부에 대하여 0.10 ~ 0.30 중량부로 포함할 수 있다.As an embodiment of the present invention, the binder may be included in an amount of 0.10 to 0.30 parts by weight based on 100 parts by weight of the adsorption catalyst.
본 발명의 다른 목적으로, 포름알데히드 제거용 부직포 필터는 상기 흡착제를 포함할 수 있다. For another object of the present invention, a non-woven filter for removing formaldehyde may include the adsorbent.
본 발명을 통해 포름알데히드 등 가스상 오염물질 제거에 효율적일 뿐만 아니라, 제조 단가가 상대적으로 낮아 경제적인 포름알데히드 제거용 흡착 촉매를 제조할 수 있고, 이를 포함하는 포름알데히드 흡착제 및 부직포 필터를 제조할 수 있다.Through the present invention, it is possible to prepare an economical adsorption catalyst for formaldehyde removal, which is not only efficient in removing gaseous pollutants such as formaldehyde, but also has a relatively low manufacturing cost, and a formaldehyde adsorbent and a nonwoven filter including the same can be manufactured. .
도 1은 본 발명의 일 실시예에 따른 포름알데히드 제거용 흡착 촉매를 관찰한 주사전자현미경(Scanning electron microscopy, SEM) 이미지이다.
도 2는 부직포 필터 성능 평가에 이용되는 챔버를 촬영한 사진으로, 챔버의 내부에는 환풍구(실험 종료 후 후드로 연결시켜 챔버 내부를 환기시키는 용도임.), 가열기(포름알데히드를 기화시키는 용도임.), 순환용 선풍기(기화된 포름알데히드가 챔버 내 골고루 퍼지게 하기 위한 용도임), 공기청정기가 있다.1 is a scanning electron microscopy (SEM) image of an adsorption catalyst for removing formaldehyde according to an embodiment of the present invention.
2 is a photograph of a chamber used for evaluating the performance of a non-woven fabric filter, and the inside of the chamber has a vent (used to ventilate the inside of the chamber by connecting it to a hood after the end of the experiment.), a heater (for vaporizing formaldehyde). ), a circulation fan (used to spread the vaporized formaldehyde evenly in the chamber), and an air purifier.
이하, 본 발명의 포름알데히드 제거용 흡착 촉매의 제조방법을 통해 본 발명에 대해 더 구체적으로 설명한다. Hereinafter, the present invention will be described in more detail through the method for preparing the adsorption catalyst for removal of formaldehyde of the present invention.
포름알데히드 제거용 흡착 촉매의 제조 방법은 폴리에틸렌글리콜(Polyethylene glycol), 이산화망간 전구체 및 물을 포함한 용액을 준비하는 1단계; 상기 용액을 반응시켜 폴리에틸렌글리콜이 결합된 이산화망간(MnO2) 복합체를 합성하는 2단계; 상기 복합체를 포함하는 용액을 여과하여 여과물을 수득한 뒤 세척하는 3단계; 및 세척한 여과물을 건조시켜 흡착 촉매를 수득하는 4단계;를 포함할 수 있다.A method for preparing an adsorption catalyst for removing formaldehyde includes a first step of preparing a solution containing polyethylene glycol, a manganese dioxide precursor, and water; A second step of reacting the solution to synthesize a polyethylene glycol-coupled manganese dioxide (MnO 2 ) complex; Step 3 of filtering the solution containing the complex to obtain a filtrate and then washing; and drying the washed filtrate to obtain an adsorption catalyst.
상세하게는, 1단계의 용액은 상기 폴리에틸렌글리콜 및 이산화망간 전구체를 1 : 5.0 ~ 1 : 8.0의 중량비로 포함할 수 있고, 바람직하게는 1 : 5.5 ~ 1 : 7.5의 중량비로 포함할 수 있으며, 더욱 바람직하게는 1 : 6.0 ~ 1 : 7.0의 중량비로 포함할 수 있다. 만일 상기 이산화망간 전구체를 5.0 중량비 미만으로 포함하는 경우 포름알데히드 제거율이 저하되는 문제가 발생할 수 있고, 이산화망간 전구체를 8.0 중량비를 초과하여 포함하는 경우 이산화망간의 반응성이 떨어지는 문제가 발생할 수 있다.Specifically, the solution of step 1 may include the polyethylene glycol and the manganese dioxide precursor in a weight ratio of 1: 5.0 to 1: 8.0, preferably 1: 5.5 to 1: 7.5, and more Preferably, it may be included in a weight ratio of 1: 6.0 to 1: 7.0. If the manganese dioxide precursor is included in a weight ratio of less than 5.0, the formaldehyde removal rate may be lowered, and if the manganese dioxide precursor is included in an amount exceeding 8.0 weight ratio, the reactivity of manganese dioxide may decrease.
이때, 상기 이산화망간 전구체는 과망간산칼륨(KMnO4), 망간아세테이트(Mn(CH3CO2)2), 과망간산나트륨(NaMnO4) 및 황산망간(MnSO4) 중에서 선택된 1종 이상을 포함할 수 있고, 바람직하게는 과망간산칼륨(KMnO4)을 포함할 수 있다.In this case, the manganese dioxide precursor may include at least one selected from potassium permanganate (KMnO 4 ), manganese acetate (Mn(CH 3 CO 2 ) 2 ), sodium permanganate (NaMnO 4 ) and manganese sulfate (MnSO 4 ), Preferably, potassium permanganate (KMnO 4 ) may be included.
또한, 상기 이산화망간 전구체는 평균 입경이 0.5mm ~ 5mm일 수 있고, 바람직하게는 1.0mm ~ 3mm일 수 있다.In addition, the manganese dioxide precursor may have an average particle diameter of 0.5 mm to 5 mm, preferably 1.0 mm to 3 mm.
한편, 상기 폴리에틸렌글리콜은 중량평균분자량(Mw)이 15,000 ~ 25,000일 수 있고, 바람직하게는 17,000 ~ 22,000일 수 있다. 만일 상기 중량평균분자량이 15,000 미만일 경우 촉매의 안정성이 떨어지는 문제가 발생할 수 있고, 25,000를 초과하는 경우 이산화망간 전구체와의 블랜딩이 균일하게 이루어지지 않는 문제가 있었다.Meanwhile, the polyethylene glycol may have a weight average molecular weight (Mw) of 15,000 to 25,000, preferably 17,000 to 22,000. If the weight average molecular weight is less than 15,000, the stability of the catalyst may be deteriorated, and if it exceeds 25,000, there is a problem in that blending with the manganese dioxide precursor is not uniformly made.
다음으로, 2단계의 반응은 60 ~ 100℃ 하에서 5 ~ 25분 동안 중탕 및 교반하여 수행할 수 있고, 바람직하게는 70 ~ 90℃ 하에서 10 ~ 20분 동안 수행할 수 있다.Next, the reaction of step 2 may be carried out by bathing and stirring for 5 to 25 minutes at 60 to 100° C., preferably, it may be performed for 10 to 20 minutes at 70 to 90° C.
다음으로, 3단계의 여과 및 세척에서 상기 세척은 여러 번 반복되어 수행할 수 있고, 바림직하게는 증류수로 여러 번 반복하여 수행할 수 있다.Next, in the three-step filtration and washing, the washing may be repeated several times, and preferably, it may be repeated several times with distilled water.
다음으로, 4단계의 건조는 80 ~ 130℃ 하에서 10 ~ 14시간 동안 수행할 수 있으며, 바람직하게는 90 ~ 120℃ 하에서 11 ~ 13시간 동안 수행할 수 있다.Next, the drying in step 4 may be performed for 10 to 14 hours under 80 to 130° C., preferably for 11 to 13 hours under 90 to 120° C.
한편, 상기의 제조방법을 통해 제조된 흡착 촉매를 소성시키는 단계를 더 포함하여 산소 공백(Oxygen vacancy) 흡착 촉매를 제조할 수 있다.On the other hand, it is possible to prepare an oxygen vacancy (Oxygen vacancy) adsorption catalyst further comprising the step of calcining the adsorption catalyst prepared through the above preparation method.
이때, 상기 소성은 불활성 기체 하에서 이루어지며, 200 ~ 280℃ 하에서 수행할 수 있고, 바람직하게는 210 ~ 270℃ 하에서 수행할 수 있으며, 200 ~ 280℃ 하에서 20 ~ 60분 동안 수행할 수 있고, 바람직하게는 25 ~ 55분 동안 수행할 수 있다. 만일 상기 소성 온도가 200℃ 미만인 경우 입자의 구조가 변형되지 않는 문제가 있을 수 있고, 280℃를 초과하는 경우 산소 공공 구조가 형성되지 않는 문제가 있을 수 있다. 또한, 상기 소성 시간이 20분 미만이면 입자의 구조가 변형되지 않는 문제가 있을 수 있고, 60분을 초과하면 산소 공공 구조가 형성되지 문제가 있을 수 있다.At this time, the calcination is made under an inert gas, may be carried out under 200 ~ 280 ℃, preferably may be carried out under 210 ~ 270 ℃, may be carried out under 200 ~ 280 ℃ for 20 ~ 60 minutes, preferably It can be carried out for 25 to 55 minutes. If the firing temperature is less than 200 ℃ there may be a problem that the structure of the particles is not deformed, if it exceeds 280 ℃ there may be a problem that oxygen vacancy structure is not formed. In addition, if the firing time is less than 20 minutes, there may be a problem in that the structure of the particles is not deformed, and if it exceeds 60 minutes, there may be a problem in that an oxygen vacancy structure is not formed.
상술한 방법으로 제조한 포름알데히드 제거용 흡착 촉매는 이산화망간(MnO2); 및 상기 이산화망간과 결합된 폴리에틸렌글리콜(Polyethylene glycol);을 포함할 수 있다.The adsorption catalyst for the removal of formaldehyde prepared by the above method is manganese dioxide (MnO 2 ); and polyethylene glycol combined with the manganese dioxide.
또한, 상기 흡착 촉매는 평균 입경이 0.05 ~ 0.5mm일 수 있고, 바람직하게는 0.1mm ~ 0.4mm일 수 있으며, 더욱 바람직하게는 0.15 ~ 0.3mm일 수 있다.In addition, the adsorption catalyst may have an average particle diameter of 0.05 to 0.5 mm, preferably 0.1 mm to 0.4 mm, and more preferably 0.15 to 0.3 mm.
본 발명의 다른 목적으로, 폴리에틸렌글리콜이 결합된 이산화망간(MnO2)을 포함하는 흡착 촉매; 바인더; 및 에탄올;을 포함하는 포름알데히드 흡착제를 제조할 수 있다.For another object of the present invention, polyethylene glycol-bonded manganese dioxide (MnO 2 ) Adsorption catalyst comprising; bookbinder; And ethanol; it can be prepared a formaldehyde adsorbent containing.
이때, 상기 에탄올 및 흡착 촉매를 1 : 0.08 ~ 1 : 0.11의 중량비로 포함할 수 있고, 바람직하게는 1 : 0.075 ~ 1 : 0.10의 중량비로 포함할 수 있으며, 더욱 바람직하게는 1 : 0.070 ~ 1 : 0.095의 중량비로 포함할 수 있다. 만일, 상기 흡착 촉매가 0.08 중량비 미만으로 포함되는 경우 포름알데히드 제거율이 불량해지는 문제가 발생할 수 있고, 0.11 중량비를 초과하는 경우 흡착 촉매의 함량이 증가함에 따라 점도가 높아지고, 부직포에 고르게 도포 시키는데 어려움이 있다는 문제가 발생할 수 있다.In this case, the ethanol and the adsorption catalyst may be included in a weight ratio of 1: 0.08 to 1: 0.11, preferably in a weight ratio of 1: 0.075 to 1: 0.10, more preferably 1: 0.070 to 1 : It may be included in a weight ratio of 0.095. If the adsorption catalyst is included in an amount of less than 0.08 weight ratio, a problem of poor formaldehyde removal rate may occur. There may be a problem that
한편, 상기 바인더는 상기 흡착 촉매 100 중량부에 대하여 0.10 ~ 0.30 중량부로 포함할 수 있고, 바람직하게는 0.15 ~ 0.25 중량부로 포함할 수 있다. 만일 상기 바인더를 0.10 중량부 미만으로 포함하는 경우 부직포에 도포되는 촉매의 양이 줄어드는 문제가 발생 할 수 있고, 0.30 중량부를 초과하여 포함하는 경우 점도가 과도하게 높아 부직포에 고르게 도포되지 않을 뿐만 아니라 기공이 폐색되어 포름알데히드 제거율이 저하되는 문제가 발생할 수 있다.Meanwhile, the binder may be included in an amount of 0.10 to 0.30 parts by weight, preferably 0.15 to 0.25 parts by weight, based on 100 parts by weight of the adsorption catalyst. If the binder is included in an amount of less than 0.10 parts by weight, there may be a problem in that the amount of catalyst applied to the nonwoven fabric is reduced. This occlusion may cause a problem in that the formaldehyde removal rate is lowered.
이때, 상기 바인더는 에틸 셀룰로오스(ethyl cellulose), 메틸 셀룰로오스(methyl cellulose), 니트로셀룰로오스(nitrocellulose), 메타크릴산 에스테르(methacrylic acid ester), 아크릴산 에스테르(acrylic acid ester), 폴리비닐알콜(polyvinyl alcohol) 및 폴리비닐부티랄(polyvinyl butyral) 중에서 선택된 1종 이상을 포함할 수 있다.At this time, the binder is ethyl cellulose (ethyl cellulose), methyl cellulose (methyl cellulose), nitrocellulose (nitrocellulose), methacrylic acid ester (methacrylic acid ester), acrylic acid ester (acrylic acid ester), polyvinyl alcohol (polyvinyl alcohol) And it may include one or more selected from polyvinyl butyral (polyvinyl butyral).
본 발명의 또 다른 목적으로, 상기 포름알데히드 흡착제를 부직포에 도포하여 포름알데히드 제거용 부직포 필터를 제조할 수 있다.As another object of the present invention, the formaldehyde adsorbent may be applied to the nonwoven fabric to manufacture a nonwoven fabric filter for removing formaldehyde.
이때, 상기 포름알데히드 제거용 부직포 필터는 30분 후 포름알데히드 제거율이 80% 이상일 수 있고, 바람직하게는 80 ~ 99%일 수 있으며, 더욱 바람직하게는 80 ~ 95%일 수 있다.In this case, the non-woven fabric filter for removing formaldehyde may have a formaldehyde removal rate of 80% or more after 30 minutes, preferably 80 to 99%, and more preferably 80 to 95%.
상기의 포름알데히드 제거용 부직포 필터는 공기청정기, 에어컨 등에 적용할 수 있으나, 이에 한정하는 것은 아니다.The non-woven fabric filter for removing formaldehyde may be applied to an air purifier, an air conditioner, and the like, but is not limited thereto.
하기의 실시예를 통하여 본 발명을 더욱 구체적으로 설명하기로 하지만, 하기 실시예가 본 발명의 범위를 제한하는 것은 아니며, 이는 본 발명의 이해를 돕기 위한 것으로 해석되어야 할 것이다.The present invention will be described in more detail through the following examples, but the following examples are not intended to limit the scope of the present invention, which should be construed to aid understanding of the present invention.
[실시예][Example]
실시예 1: 포름알데히드 제거용 흡착 촉매(PEG/MnOExample 1: Adsorption Catalyst for Formaldehyde Removal (PEG/MnO 22 )의 제조) manufacturing
이산화망간 전구체로 과망간산칼륨(KMnO4) 및 폴리에틸렌글리콜(Polyethylene glycol, PEG)을 증류수 260mL에 투입하여 용액을 제조했다.As a manganese dioxide precursor, potassium permanganate (KMnO 4 ) and polyethylene glycol (PEG) were added to 260 mL of distilled water to prepare a solution.
이때, 상기 폴리에틸렌글리콜 및 상기 과망간산칼륨은 1 : 6.67의 중량비로 투입되었다.At this time, the polyethylene glycol and the potassium permanganate were added in a weight ratio of 1:6.67.
또한, 상기 폴리에틸렌글리콜의 중량평균분자량(Mw)은 20,000인 것을 사용하였다.In addition, the polyethylene glycol had a weight average molecular weight (Mw) of 20,000.
그리고, 상기 용액을 반응시켜 반응생성물로 폴리에틸렌글리콜이 결합된 이산화망간(MnO2)을 합성하였다.Then, the solution was reacted to synthesize manganese dioxide (MnO 2 ) to which polyethylene glycol was bound as a reaction product.
이때, 상기 반응은 상기 용액을 수조에 옮긴 뒤, 80℃ 하에서 15분 동안 중탕 및 교반하여 수행되었다. At this time, the reaction was carried out by transferring the solution to a water bath, bathing and stirring at 80° C. for 15 minutes.
그리고, 상기 반응생성물을 포함하는 용액을 여과하여 여과물을 수득한 뒤, 증류수로 세척하였다.Then, the solution containing the reaction product was filtered to obtain a filtrate, which was washed with distilled water.
그리고, 상기 세척된 여과물을 105℃하에서 12시간 동안 건조시켜 포름알데히드 제거용 흡착 촉매(PEG/MnO2)를 수득하였다.Then, the washed filtrate was dried at 105° C. for 12 hours to obtain an adsorption catalyst for removing formaldehyde (PEG/MnO 2 ).
실시예 2 ~ 실시예 3: 포름알데히드 제거용 흡착 촉매의 제조Examples 2 to 3: Preparation of adsorption catalyst for formaldehyde removal
실시예 1과 동일한 방법으로 흡착 촉매를 제조하되, 폴리에틸렌글리콜 및 이산화망간 전구체의 중량비를 하기 표 1과 같이 하여 실시예 2 ~ 실시예 3을 실시하였다.An adsorption catalyst was prepared in the same manner as in Example 1, but Examples 2 to 3 were carried out with the weight ratios of polyethylene glycol and manganese dioxide precursor as shown in Table 1 below.
실시예 4: 산소 공백(Oxygen vacancy) 흡착 촉매의 제조Example 4: Preparation of Oxygen vacancy Adsorption Catalyst
실시예 1 동일한 방법으로 포름알데히드 제거용 흡착 촉매(PEG/MnO2)를 제조하고,Example 1 Adsorption catalyst for removal of formaldehyde (PEG/MnO 2 ) was prepared in the same manner,
상기 포름알데히드 제거용 흡착 촉매(PEG/MnO2)를 아르곤(Ar) 기체 하에서 240℃의 온도로 40분 동안 소성시켜 산소 공백(Oxygen vacancy) 흡착 촉매를 제조하였다.The adsorption catalyst for removal of formaldehyde (PEG/MnO 2 ) was calcined at a temperature of 240° C. under argon (Ar) gas for 40 minutes to prepare an oxygen vacancy adsorption catalyst.
비교예 1: 이산화망간(MnOComparative Example 1: Manganese dioxide (MnO 22 ) 흡착 촉매의 제조) Preparation of Adsorption Catalyst
이산화망간 전구체로 KMnO4 20g, (NH4)2C2O4·H2O 8g을 증류수 260mL에 투입하여 용액을 제조했다.As a manganese dioxide precursor, 20 g of KMnO 4 and (NH 4 ) 2 C 2 O 4 ·H 2 O 8g were added to 260 mL of distilled water to prepare a solution.
그리고, 상기 용액을 가열교반기를 사용하여 90℃의 가열온도에서 150rpm의 회전 속도로 교반했다.Then, the solution was stirred at a heating temperature of 90° C. at a rotation speed of 150 rpm using a heating stirrer.
그리고, 상기 단계에서 교반된 용액을 여과시켜 여과물을 수득했다.Then, the solution stirred in the above step was filtered to obtain a filtrate.
그리고, 상기 여과물을 30℃의 온도에서 10시간 건조하여 고체 타입의 여과물을 수득하였다.Then, the filtrate was dried at a temperature of 30° C. for 10 hours to obtain a solid-type filtrate.
그리고, 상기 고체 타입의 여과물을 500℃의 소성온도에서 3시간 동안 소성하여 이산화망간(MnO2) 흡착 촉매를 수득하였다.Then, the solid-type filtrate was calcined at a calcination temperature of 500° C. for 3 hours to obtain a manganese dioxide (MnO 2 ) adsorption catalyst.
비교예 2: 이산화망간(MnOComparative Example 2: Manganese dioxide (MnO 22 ) + CeO) + CeO 22 흡착 촉매의 제조 Preparation of Adsorption Catalyst
Sigma Aldrich 사에서 구입한 CeO2 분말(<5μm, 99.9% trace metals)과 비교예 1의 이산화망간(MnO2)을 1 : 1 비율로 투입하고, 이를 5분 동안 혼합하여 흡착 촉매(이산화망간(MnO2) + CeO2)를 제조하였다.CeO 2 powder purchased from Sigma Aldrich (<5 μm, 99.9% trace metals) and manganese dioxide (MnO 2 ) of Comparative Example 1 were added in a 1:1 ratio, and the adsorption catalyst (manganese dioxide (MnO 2 ) was mixed for 5 minutes. ) + CeO 2 ) was prepared.
비교예 3: 이산화망간(MnOComparative Example 3: Manganese dioxide (MnO 22 ) + FeSiO) + FeSiO 22 흡착 촉매 제조 Adsorption catalyst preparation
사이클로헥산(Cyclohexane) 100mL에 폴리에틸렌글리콜(Polyethylene glycol, PEG 400) 20.35g을 투입한 용액을 50℃에서 10분 동안 가열 및 교반시켰다.A solution of 20.35 g of polyethylene glycol (PEG 400) in 100 mL of cyclohexane was heated and stirred at 50° C. for 10 minutes.
그리고, 상기 단계를 수행한 용액에 FeCl3 수용액 20mL 및 NH3 수용액 3.20g을 첨가한 후, 3시간동안 숙성시킨다.Then, 20 mL of an aqueous solution of FeCl 3 and 3.20 g of an aqueous solution of NH 3 were added to the solution in which the above steps were performed, and then aged for 3 hours.
그리고, 상기 단계를 수행한 용액에 에틸 실리케이트(Tetraethyl orthosilicate) 5.4g을 첨가하였다.Then, 5.4 g of ethyl silicate (Tetraethyl orthosilicate) was added to the solution in which the above steps were performed.
그리고, 상기 단계를 수행한 용액에 이소프로판올(Isopropanol) 30mL을 첨가한 뒤, 원심 분리하여 침전물을 얻었다.Then, 30 mL of isopropanol was added to the solution in which the above step was performed, and then centrifuged to obtain a precipitate.
그리고, 상기 침전물을 60℃에서 24시간 동안 건조하여 FeSiO2를 수득하였다.Then, the precipitate was dried at 60° C. for 24 hours to obtain FeSiO 2 .
그리고, 상기 FeSiO2 및 비교예 1의 이산화망간(MnO2)을 1 : 1 비율로 투입하고, 이를 5분 동안 혼합하여 흡착 촉매(이산화망간(MnO2) + FeSiO2)를 수득하였다.And, the FeSiO 2 and the manganese dioxide (MnO 2 ) of Comparative Example 1 were added in a 1:1 ratio, and the mixture was mixed for 5 minutes to obtain an adsorption catalyst (manganese dioxide (MnO 2 ) + FeSiO 2 ).
비교예 4: 활성탄 흡착 촉매Comparative Example 4: Activated Carbon Adsorption Catalyst
CGC(태국)사의 활성탄 흡착 촉매를 사용하였다.An activated carbon adsorption catalyst manufactured by CGC (Thailand) was used.
비교예 5 ~ 비교예 6: 포름알데히드 제거용 흡착 촉매의 제조Comparative Example 5 to Comparative Example 6: Preparation of adsorption catalyst for formaldehyde removal
실시예 1과 동일한 방법으로 흡착 촉매를 제조하되, 폴리에틸렌글리콜 및 이산화망간 전구체의 중량비를 하기 표 1과 같이 하여 비교예 5 ~ 비교예 6을 실시하였다.An adsorption catalyst was prepared in the same manner as in Example 1, but Comparative Examples 5 to 6 were carried out with the weight ratios of polyethylene glycol and manganese dioxide precursor as shown in Table 1 below.
실험예 1: 포름알데히드 제거용 흡착 촉매의 관찰Experimental Example 1: Observation of an adsorption catalyst for removal of formaldehyde
실시예 1에서 제조된 흡착 촉매를 주사전자현미경(Scanning electron microscopy, SEM)을 통해 관찰한 이미지를 도 1에 나타내었다.An image of the adsorption catalyst prepared in Example 1 observed through a scanning electron microscope (SEM) is shown in FIG. 1 .
이를 통해, 폴리에틸렌글리콜과 이산화망간이 결합된 형태임을 확인할 수 있었다.Through this, it was confirmed that polyethylene glycol and manganese dioxide were combined.
제조예 1: 포름알데히드 제거용 부직포 필터 제조Preparation Example 1: Preparation of non-woven filter for formaldehyde removal
먼저, 하기와 같은 방법으로 포름알데히드 흡착제를 제조하였다.First, a formaldehyde adsorbent was prepared as follows.
(1)에탄올(EtOH) 및 실시예 1에서 제조된 흡착 촉매를 1 : 0.095의 중량비로 투입하고, 60℃ 하에서 15분 동안 교반한 용액을 제조하였다.(1) Ethanol (EtOH) and the adsorption catalyst prepared in Example 1 were added in a weight ratio of 1:0.095, and a solution was prepared by stirring at 60° C. for 15 minutes.
(2)상기 용액에 에틸 셀룰로오스(Ethyl cellulose, 바인더)를 첨가하였다.(2) Ethyl cellulose (binder) was added to the solution.
이때, 상기 에틸 셀룰로오스는 상기 흡착 촉매 100 중량부에 대하여 0.20 중량부가 되도록 첨가하였다.At this time, the ethyl cellulose was added so as to be 0.20 parts by weight based on 100 parts by weight of the adsorption catalyst.
(3)상기 단계를 수행한 용액의 부피가 100mL가 될 때까지 120℃ 하에서 교반하여 포름알데히드 흡착제를 제조하였다.(3) A formaldehyde adsorbent was prepared by stirring under 120° C. until the volume of the solution in the above step was 100 mL.
이와는 별개로, 폴리에스테르계 부직포를 공기청정기 내부에 들어갈 크기(300mm×400mm)로 잘라서 준비했다.Separately, a polyester-based nonwoven fabric was prepared by cutting it into a size (300mm×400mm) to fit inside the air purifier.
그리고, 상기 포름알데히드 흡착제에 부직포 필터를 담지하여 부직포 필터를 제조하였다.Then, a nonwoven filter was prepared by supporting the nonwoven filter on the formaldehyde adsorbent.
제조예 2 ~ 제조예 3: 포름알데히드 제거용 부직포 필터 제조Preparation Example 2 ~ Preparation Example 3: Preparation of non-woven filter for formaldehyde removal
제조예 1과 동일한 방법으로 부직포 필터를 제조하되, 실시예 2 ~ 실시예 3에서 제조한 흡착 촉매를 사용하여 제조예 2 ~ 제조예 3을 실시하였다.A nonwoven filter was prepared in the same manner as in Preparation Example 1, but Preparation Examples 2 to 3 were carried out using the adsorption catalysts prepared in Examples 2 to 3.
제조예 4 ~ 제조예 5: 포름알데히드 제거용 부직포 필터 제조Preparation Example 4 ~ Preparation Example 5: Preparation of non-woven filter for formaldehyde removal
제조예 1과 동일한 방법으로 부직포 필터를 제조하되, 에탄올 및 흡착 촉매의 중량비를 하기 표 2와 같이 하여 제조예 4 ~ 제조예 5를 실시하였다.A nonwoven filter was prepared in the same manner as in Preparation Example 1, but Preparation Examples 4 to 5 were carried out with the weight ratios of ethanol and adsorption catalyst as shown in Table 2 below.
제조예 6: 포름알데히드 제거용 부직포 필터 제조Preparation Example 6: Preparation of non-woven filter for formaldehyde removal
제조예 1과 동일한 방법으로 부직포 필터를 제조하되, 실시예 4에서 제조한 흡착 촉매를 사용하여 제조예 6을 실시하였다.A nonwoven filter was prepared in the same manner as in Preparation Example 1, but Preparation Example 6 was performed using the adsorption catalyst prepared in Example 4.
비교제조예 1 ~ 비교제조예 6: 포름알데히드 제거용 부직포 필터 제조Comparative Preparation Example 1 ~ Comparative Preparation Example 6: Preparation of non-woven filter for formaldehyde removal
제조예 1과 동일한 방법으로 부직포 필터를 제조하되, 비교예 1 ~ 비교예 6에서 제조한 흡착 촉매를 사용하여 비교제조예 1 ~ 비교제조예 6을 실시하였다.A nonwoven filter was prepared in the same manner as in Preparation Example 1, but Comparative Preparation Examples 1 to 6 were carried out using the adsorption catalysts prepared in Comparative Examples 1 to 6.
비교제조예 7 ~ 비교제조예 8: 포름알데히드 제거용 부직포 필터 제조Comparative Preparation Example 7 ~ Comparative Preparation Example 8: Preparation of non-woven filter for formaldehyde removal
제조예 1과 동일한 방법으로 부직포 필터를 제조하되, 에탄올 및 흡착 촉매의 중량비를 하기 표 4와 같이 하여 비교제조예 7 ~ 비교제조예 8을 실시하였다.A nonwoven filter was prepared in the same manner as in Preparation Example 1, but Comparative Preparation Examples 7 to 8 were carried out with the weight ratios of ethanol and adsorption catalyst as shown in Table 4 below.
실험예 2: 포름알데히드 제거용 부직포 필터의 성능 평가Experimental Example 2: Performance evaluation of non-woven filter for removing formaldehyde
제조예 1 ~ 제조예 6 및 비교제조예 1 ~ 비교제조예 8에서 제조된 부직포 필터의 포름알데히드 제거 성능을 다음과 같은 방법으로 평가하여 하기 표 1 ~ 표 4에 나타냈다. The formaldehyde removal performance of the nonwoven fabric filters prepared in Preparation Examples 1 to 6 and Comparative Preparation Examples 1 to 8 were evaluated in the following manner and shown in Tables 1 to 4 below.
(1)포름알데히드 제거율 측정(1) Formaldehyde removal rate measurement
1)챔버에 이상이 있는지 확인한 후 누출 실험(leak test)를 진행하였다.1) After checking if there is an abnormality in the chamber, a leak test was performed.
2)부직포 필터를 공기청정장치(웅진코웨이, AP-1009JH)에 장착하였다. 2) A non-woven filter was installed in an air purifier (Woongjin Coway, AP-1009JH).
3)포름알데히드 용액 0.3mL를 챔버 내에 넣었다.3) 0.3mL of formaldehyde solution was put into the chamber.
4)상기 포름알데히드 용액을 가열기를 사용하여 65℃의 온도에서 기화시켰다.4) The formaldehyde solution was vaporized at a temperature of 65° C. using a heater.
5)기화 후 가열기를 껐다.5) Turn off the heater after vaporization.
6)디니트로페닐하이드라진(dinitrophenylhydrazine, DNPH) 카트리지를 이용하여 초기 포름알데히드 가스 농도를 측정하였다.6) The initial formaldehyde gas concentration was measured using a dinitrophenylhydrazine (DNPH) cartridge.
7)상기 공기청정장치를 30분 동안 가동시키고, 포름알데히드의 가스 농도를 측정하였다.7) The air purifier was operated for 30 minutes, and the gas concentration of formaldehyde was measured.
이때, 상기 챔버의 구조는 도 2와 같다.At this time, the structure of the chamber is as shown in FIG. 2 .
(2)외관 평가(2) Appearance evaluation
부직포 필터의 외관을 '○', '△', '×'으로 평가하였다.The appearance of the nonwoven filter was evaluated as '○', 'Δ', and '×'.
이때, 상기 외관 평가기준은, 균일한 도포 여부, 적절한 색깔 등으로 하여 평가하였다.In this case, the appearance evaluation criteria were evaluated based on whether the application was uniformly applied, an appropriate color, and the like.
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Claims (10)
상기 용액을 70 ~ 90℃ 하에서 5 ~ 25분 동안 중탕 및 교반시켜서, 폴리에틸렌글리콜이 결합된 이산화망간(MnO2) 복합체를 합성하는 2단계;
상기 복합체를 포함하는 용액을 여과하여 여과물을 수득한 뒤 세척하는 3단계; 및
세척한 여과물을 80 ~ 130℃하에서 10 ~ 14시간 동안 건조시켜서, 흡착 촉매를 수득하는 4단계;를 포함하는 공정을 수행하며,
1단계의 용액은 폴리에틸렌글리콜 및 이산화망간 전구체를 1 : 5.0 ~ 1 : 8.0 중량비로 포함하고,
상기 이산화망간 전구체는 과망간산칼륨(KMnO4), 망간아세테이트(Mn(CH3CO2)2), 과망간산나트륨(NaMnO4) 및 황산망간(MnSO4) 중에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 포름알데히드 제거용 흡착 촉매의 제조방법.
Step 1 of preparing a solution containing polyethylene glycol having a weight average molecular weight of 15,000 to 25,000, a manganese dioxide precursor, and water;
The second step of synthesizing a polyethylene glycol-coupled manganese dioxide (MnO2) complex by boiling and stirring the solution for 5 to 25 minutes at 70 to 90° C.;
Step 3 of filtering the solution containing the complex to obtain a filtrate and then washing; and
The washed filtrate is dried at 80 to 130° C. for 10 to 14 hours, and 4 steps to obtain an adsorption catalyst; performing a process comprising;
The solution of step 1 contains polyethylene glycol and manganese dioxide precursor in a weight ratio of 1: 5.0 to 1: 8.0,
The manganese dioxide precursor is potassium permanganate (KMnO 4 ), manganese acetate (Mn(CH 3 CO 2 ) 2 ), sodium permanganate (NaMnO 4 ), and manganese sulfate (MnSO 4 ) Form comprising at least one selected from A method for preparing an adsorption catalyst for aldehyde removal.
manganese dioxide (MnO 2 ); and an adsorption catalyst prepared by the method of claim 1;
상기 에탄올 및 흡착 촉매를 1 : 0.08 ~ 1 : 0.11의 중량비로 포함하며,
상기 바인더는 에틸 셀룰로오스(ethyl cellulose), 메틸 셀룰로오스(methyl cellulose), 니트로셀룰로오스(nitrocellulose), 메타크릴산 에스테르(methacrylic acid ester), 아크릴산 에스테르(acrylic acid ester), 폴리비닐알콜(polyvinyl alcohol) 및 폴리비닐부티랄(polyvinyl butyral) 중에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 포름알데히드 흡착제.
The adsorption catalyst prepared by the method of claim 1; a binder and ethanol;
The ethanol and the adsorption catalyst are included in a weight ratio of 1: 0.08 to 1: 0.11,
The binder is ethyl cellulose, methyl cellulose, nitrocellulose, methacrylic acid ester, acrylic acid ester, polyvinyl alcohol, and poly Formaldehyde adsorbent comprising at least one selected from among vinyl butyral (polyvinyl butyral).
The formaldehyde adsorbent according to claim 7, wherein the binder is included in an amount of 0.10 to 0.30 parts by weight based on 100 parts by weight of the adsorption catalyst.
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