KR100928971B1 - How to remove PFOS or PFAO from soil - Google Patents
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Abstract
토양에서 PFOS 또는 PFOA를 제거하는 방법이 제공된다. 상기 토양에서 PFOS 또는 PFOA를 제거하는 방법은 PFOS(Perfluorooctane sulfonate) 또는 PFOA(Perfluorooctanoic acid)로 오염된 토양을 준비하는 단계, 및 산화철 및 수소화 붕소나트륨(NaBH4)을 분해제로 사용하여 오염된 토양을 정화하는 단계를 포함한다.A method is provided for removing PFOS or PFOA from soil. The method for removing PFOS or PFOA from the soil may include preparing soil contaminated with Perfluorooctane sulfonate (PFOS) or Perfluorooctanoic acid (PFOA), and using contaminated soil using iron oxide and sodium borohydride (NaBH 4 ) as disintegrators. Purifying.
오염된 토양, PFOS, PFOA, 산화철, 수소화 붕소나트륨 Contaminated soil, PFOS, PFOA, iron oxide, sodium borohydride
Description
본 발명은 PFOS 또는 PFOA를 제거하는 방법에 관한 것으로서, 보다 상세하게는 토양에서 PFOS 또는 PFOA를 제거하는 방법에 관한 것이다.The present invention relates to a method for removing PFOS or PFOA, and more particularly, to a method for removing PFOS or PFOA from soil.
PFOS 또는 PFOA는 계면활성제, 윤활유, 테프론 수지 등에 함유된 물질로서 인체에 대하여 발암성이 있는 것으로 보고되고 있다. 현재 UNEP(유엔 환경조사위원회)에서 이들에 대한 구체적인 위해성에 대하여 조사하고 있으며, 잔류성 유기오염물질(POPs, Persistent Organic Pollutants)로 분류될 가능성이 매우 높은 물질이다. PFOS 또는 PFOA는 불소 및 탄소 원자의 수에 따라 다양한 종류가 존재하나, 아래에 표시한 2종이 주로 많이 환경 중, 특히 수계에 존재하며, 그 화학적 구조는 아래와 같다.PFOS or PFOA has been reported to be carcinogenic to humans as a substance contained in surfactants, lubricants, Teflon resins and the like. UNEP is currently investigating the specific risks of these substances and is very likely to be classified as Persistent Organic Pollutants (POPs). There are various types of PFOS or PFOA depending on the number of fluorine and carbon atoms, but the two types shown below are mainly present in the environment, especially in water, and the chemical structure thereof is as follows.
본 발명의 목적은 친환경적인 토양에서 PFOS 또는 PFOA를 제거하는 방법을 제공하는 것이다.It is an object of the present invention to provide a method for removing PFOS or PFOA from environmentally friendly soils.
상기 토양에서 PFOS 또는 PFOA를 제거하는 방법은 PFOS(Perfluoroctane sulfonate) 또는 PFOA(Perfluoroctanoic acid)로 오염된 토양을 준비하는 단계, 및 산화철 및 수소화 붕소나트륨(NaBH4)을 분해제로 사용하여 상기 오염된 토양을 정화하는 단계를 포함한다.The method for removing PFOS or PFOA from the soil includes preparing a soil contaminated with Perfluoroctane sulfonate (PFOS) or Perfluoroctanoic acid (PFOA), and using the iron oxide and sodium borohydride (NaBH 4 ) as a disintegrating agent. Purifying.
상기 산화철(Fe2O3 및 FeO)은 제철공정의 산세과정의 부산물이다. 상기 산화철은 0.2~50㎛의 평균입경을 가지는 분말 형태일 수 있다.The iron oxides (Fe 2 O 3 and FeO) are by-products of the pickling process of the steelmaking process. The iron oxide may be in the form of a powder having an average particle diameter of 0.2 ~ 50㎛.
상기 오염된 토양의 100 중량부에 대하여 상기 분해제는 1~10 중량부를 첨가할 수 있다. 상기 오염된 토양을 정화하는 단계는 상기 분해제가 첨가된 상기 토양을 5일 이상 방치하는 것을 포함할 수 있다.The disintegrant may be added 1 to 10 parts by weight based on 100 parts by weight of the contaminated soil. Purifying the contaminated soil may include leaving the soil to which the disintegrant is added for at least five days.
본 발명의 실시예에 따르면, 제철공정의 산세과정의 부산물이 산화철을 이용하여 토양 중에 오염된 PFOS 또는 PFOA가 제거된다. 본 발명의 방법으로 토양 중에 함유되어 있던 PFOS 또는 PFOA이 효과적으로 제거됨과 아울러, 농작물의 생육에 적합한 중성 pH가 유지될 수 있다. 따라서, 처리 후의 토양 특히 논 토양이나 밭 토 양은 추가적인 처리를 실시하지 않더라도, 농작물의 배양용 토양으로서 그대로 사용할 수 있다. 또한 이 처리방법에서 사용되는 물질은 농작물이나 주변 환경에 악영향을 줄 가능성이 적으므로, 처리 후의 토양은 농작물이나 주변 환경에 안전하다.According to an embodiment of the present invention, byproducts of the pickling process of the steelmaking process are removed PFOS or PFOA contaminated in the soil using iron oxide. In addition to the effective removal of PFOS or PFOA contained in the soil by the method of the present invention, a neutral pH suitable for growing crops can be maintained. Therefore, the treated soil, especially paddy soil or field soil, can be used as it is as soil for cultivation of crops even without further treatment. In addition, since the material used in this treatment method is less likely to adversely affect the crops or the surrounding environment, the treated soil is safe for the crops or the surrounding environment.
이하에서는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 본 발명의 기술적 사상을 용이하게 실시할 수 있도록 본 발명의 실시예를 첨부된 도면을 참조하여 설명하기로 한다. 그러나, 본 발명은 여기서 설명되어지는 실시예들에 한정되지 않고 다른 형태로 구체화될 수도 있다. 오히려, 여기서 소개되는 실시예는 개시된 내용이 철저하고 완전해질 수 있도록 그리고 당업자에게 본 발명의 기술적 사상이 충분히 전달될 수 있도록 제공되는 것이다.DETAILED DESCRIPTION Hereinafter, exemplary embodiments of the present invention will be described with reference to the accompanying drawings so that those skilled in the art may easily implement the technical idea of the present invention. However, the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided so that the disclosed contents may be thorough and complete, and the technical spirit of the present invention may be sufficiently delivered to those skilled in the art.
도 1은 본 발명의 실시예에 따른 토양에서 PFOS 또는 PFOA를 제거하는 방법을 설명하기 위한 순서도이다.1 is a flowchart illustrating a method for removing PFOS or PFOA from soil according to an embodiment of the present invention.
도 1을 참조하면, 토양에서 PFOS 또는 PFOA를 제거하는 방법은 PFOS(Perfluorooctane sulfonate) 또는 PFOA(Perfluorooctanoic acid)로 오염된 토양을 준비하는 단계(S1), 산화철 및 수소화 붕소나트륨(NaBH4)을 분해제를 첨가하는 단계(S2) 및 분해제가 첨가된 토양을 방치하는 단계(S3)를 포함한다.Referring to FIG. 1, the method for removing PFOS or PFOA from the soil may include preparing soil contaminated with Perfluorooctane sulfonate (PFOS) or Perfluorooctanoic acid (PFOA), powdering iron oxide and sodium borohydride (NaBH 4 ). Adding the release (S2) and leaving the soil to which the degradation agent is added (S3).
본 발명의 목적은 토양에 함유된 PFOS 또는 PFOA를 효과적으로 분해하는 것에 있다. 본 발명의 방법은 산화철(예, Fe2O3 및 FeO) 및 수소화붕소(NaBH4)를 사용 하여 PFOS 또는 PFOA으로 오염된 토양을 정화하는 방법을 제공하는 것이다.An object of the present invention is to effectively decompose PFOS or PFOA contained in soil. The method of the present invention provides a method of purifying soil contaminated with PFOS or PFOA using iron oxides (eg Fe 2 O 3 and FeO) and boron hydride (NaBH 4).
본 발명에서 사용하는 분해제의 조제방법은 산화철(예, Fe2O3 및 FeO)대비 중량으로 10 % 미만으로 수소화붕소(NaBH4)를 혼합하고 충분히 교반하여 혼합한다. 이때 사용하는 산화철은 제철소 산세공정에서 부산물로 회수되는 것을 이용할 수 있다. 예를 들면, 제철소의 냉연강판 제조과정의 산세공정에서 얻어지는 철 함유 염산으로부터 회수되는 산화철을 사용할 수 있다. 이렇게 얻어진 산화철은 분말형태의 것이 바람직하며, 구체적으로는 평균입경이 0.2 ∼ 50㎛인 분말형태가 보다 바람직하다. 또한, 수소를 이온 상태로 방출할 수 있는 물질은 수소화 붕소나트륨(NaBH4)을 들 수 있다. 본 발명의 처리대상이 되는 토양은 논 토양, 밭 토양 등이다.In the preparation method of the disintegrating agent used in the present invention, boron hydride (NaBH 4) is mixed with less than 10% by weight relative to iron oxide (eg, Fe 2 O 3 and FeO), followed by mixing with sufficient stirring. At this time, the iron oxide used may be recovered as a by-product from the iron pickling process. For example, iron oxide recovered from iron-containing hydrochloric acid obtained in the pickling process of the cold rolled steel sheet manufacturing process of the steel mill can be used. The iron oxide thus obtained is preferably in the form of a powder, and more preferably in the form of a powder having an average particle diameter of 0.2 to 50 µm. Further, the substance capable of releasing hydrogen in ionic state may be mentioned sodium borohydride (NaBH 4). The soil to be treated in the present invention is paddy soil, field soil and the like.
본 발명의 실시예에 따른 PFOS 또는 PFOA로 오염된 토양을 처리하는 방법은 다음과 같다.Method for treating soil contaminated with PFOS or PFOA according to an embodiment of the present invention is as follows.
먼저 처리대상이 되는 토양에 상술한 바와 같이 조제한 분해제를 첨가하여 혼합한다. 이때, 분해제의 혼합비율은 토양 100 g에 대해1 ∼ 10 g으로 설정하는 것이 바람직하고, 5 ∼ 10 g으로 설정하는 것이 보다 바람직하다. 분해제의 비율이 1% 미만인 경우에는 토양 중에 함유된 PFOS 또는 PFOA을 효과적으로 제거하는 것이 곤란해질 가능성이 있다. 역으로, 10 %를 초과할 경우에는 처리후의 토양 중에 산화철이 과잉으로 존재할 가능성이 있기 때문에 해당 토양을 농경지용 토양으로서 이용할 경우, 농작물 등의 식물 등에 악영향을 줄 가능성이 있다. 또한 토양과 분 해제와의 혼합물 중 수분량은 전체 고형분의 50∼100중량 %로 설정하는 것이 바람직하다. 이 수분량이 50중량 % 미만인 경우에는 토양중의 PFOS 또는 PFOA이 제거되기 어려워질 우려가 있다. 역으로, 200중량 %를 초과할 경우에는 토양입자가 수중에서 침강하기 쉬워지므로, 토양입자와 물과의 접촉율이 저하되어 토양중의 PFOS 또는 PFOA이 제거될 때까지 장기간을 요할 가능성이 있다. 이렇게 분해제가 혼합된 토양을 7일 이상 방치한다. 방치기간은 통상 5일 이상 바람직하게는 7일 이상으로 설정하는 것이 좋다. 방치기간이 5일 미만인 경우에는 토양 중에 함유된 PFOS 또는 PFOA을 해당 토양으로부터 충분히 제거할 수 없는 경우가 있다.First, a decomposition agent prepared as described above is added to the soil to be treated and mixed. At this time, the mixing ratio of the disintegrating agent is preferably set to 1 to 10 g, more preferably 5 to 10 g with respect to 100 g of the soil. If the ratio of the disintegrant is less than 1%, it may be difficult to effectively remove PFOS or PFOA contained in the soil. On the contrary, if it exceeds 10%, there may be an excessive amount of iron oxide in the treated soil, so that if the soil is used as cropland soil, it may adversely affect plants such as crops. In addition, it is preferable to set the water content in the mixture of soil and powder release to 50 to 100% by weight of the total solids. If the moisture content is less than 50% by weight, there is a fear that PFOS or PFOA in the soil will be difficult to remove. On the contrary, if it exceeds 200% by weight, the soil particles are likely to settle in water, so the contact rate between the soil particles and water is lowered, which may require a long time until the PFOS or PFOA in the soil is removed. Soil mixed with disintegrant is left for 7 days or more. The leaving period is usually set to 5 days or more, preferably 7 days or more. If it is less than 5 days, PFOS or PFOA contained in the soil may not be sufficiently removed from the soil.
제철공정의 부산물로 얻어지는 산화철(순도 90 %이상) 분말 50 g과 수소화 붕소 나트륨(시약급) 분말 5 g을 충분히 혼합하였다. 이어서, PFOS 또는 PFOA로 오염된 토양 300 g에 상기 혼합 분해제 15 g을 혼합하고 또 물 300 ml를 추가로 첨가하였다. 이와 같이 하여 처리한 토양을 그대로 방치하고 1일 후, 5일 후 및 10일 후의 PFOS 또는 PFOA 함유량 및 pH를 조사하였다. PFOS 또는 PFOA의 분석은 다음과 같이 하였다. 분해제로 처리 전 및 처리 후의 토양을 메탄올 용매에서 속실렛 장치(Soxhlet apparatus)에서 24시간 동안 PFOS/PFOA성분이 포함된 유기물질들을 추출하였다. 추출된 용매는 회전 증발기로 1 ml로 농축시킨 뒤, SPE(solid phase extraction)-C18 카트리지에 주입하고 20 ml의 40 % 메탄올이 함유된 HPLC용 증류수로 흘리고 난 뒤에 최종적으로 30 ml의 메탄올에 용리된 분획을 폴리프로필렌(Polypropylene) 튜브에 모은다. 다시 메탄올 용액은 질소 가스를 사용하여 0.2 ml로 농축시켰다. 농축된 것을 최종적으로 액체 크로마토그래피/질량분 석기(HPLC-MS/MS)로 정량하였다. 또한 pH는 pH계를 사용하여 측정하였다. 그 결과를 아래 표에 나타내었다.50 g of iron oxide (purity 90% or more) powder and 5 g of sodium borohydride (reagent grade) powder obtained as a by-product of the steelmaking process were sufficiently mixed. Subsequently, 15 g of the mixed disintegrant was mixed with 300 g of soil contaminated with PFOS or PFOA and further 300 ml of water were added. The soil treated in this way was left as it was and the PFOS or PFOA content and pH after 1 day, 5 days and 10 days were examined. Analysis of PFOS or PFOA was as follows. Soil before and after the treatment with the disintegrant was extracted organic solvents containing PFOS / PFOA component for 24 hours in a Soxhlet apparatus in methanol solvent. The extracted solvent was concentrated to 1 ml on a rotary evaporator, injected into a solid phase extraction (SPE) -C18 cartridge, flowed into distilled water for HPLC containing 20 ml of 40% methanol, and finally eluted with 30 ml of methanol. Collected fractions are collected in a polypropylene tube. The methanol solution was again concentrated to 0.2 ml using nitrogen gas. The concentrated one was finally quantified by liquid chromatography / mass spectrometry (HPLC-MS / MS). In addition, pH was measured using the pH meter. The results are shown in the table below.
본 발명의 방법으로 토양 중에 함유되어 있던 PFOS 또는 PFOA이 효과적으로 제거됨과 아울러, 농작물의 생육에 적합한 중성으로 pH가 유지될 수 있다. 따라서, 처리 후의 토양 특히 논 토양이나 밭 토양은 추가적인 처리를 실시하지 않더라도, 농작물의 배양용 토양으로서 그대로 사용할 수 있다. 또한 이 처리방법에서 사용되는 물질은 농작물이나 주변 환경에 악영향을 줄 가능성이 적으므로, 처리후의 토양은 농작물이나 주변 환경에 안전하다.In addition to the effective removal of PFOS or PFOA contained in the soil by the method of the present invention, pH can be maintained at a neutral level suitable for growing crops. Therefore, the treated soil, in particular, paddy or field soil, can be used as it is as a soil for cultivating crops without additional treatment. In addition, since the material used in this treatment method is less likely to adversely affect the crops or the surrounding environment, the treated soil is safe for the crops or the surrounding environment.
도 1은 본 발명의 실시예에 따른 토양에서 PFOS 또는 PFOA를 제거하는 방법을 설명하기 위한 순서도이다.1 is a flowchart illustrating a method for removing PFOS or PFOA from soil according to an embodiment of the present invention.
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| US11697043B2 (en) | 2019-04-29 | 2023-07-11 | HMR Solutions, Inc. | Method and reagents for treating materials contaminated with mercury, PFAS, or other contaminants |
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| JP2005230643A (en) * | 2004-02-18 | 2005-09-02 | Sumitomo Metal Ind Ltd | Cleaning method for polluted soil |
| KR20060071565A (en) * | 2004-12-22 | 2006-06-27 | 재단법인 포항산업과학연구원 | Degradation of method of pcbs contained soil by steel-byproduct |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005230643A (en) * | 2004-02-18 | 2005-09-02 | Sumitomo Metal Ind Ltd | Cleaning method for polluted soil |
| KR20060071565A (en) * | 2004-12-22 | 2006-06-27 | 재단법인 포항산업과학연구원 | Degradation of method of pcbs contained soil by steel-byproduct |
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| CN110869140A (en) * | 2017-05-30 | 2020-03-06 | 雪佛龙美国公司 | System and method for destroying unwanted materials by smoldering combustion heat |
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