KR100644518B1 - The extraction method for halogenated organic compounds in waste water - Google Patents

The extraction method for halogenated organic compounds in waste water Download PDF

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KR100644518B1
KR100644518B1 KR1020050103913A KR20050103913A KR100644518B1 KR 100644518 B1 KR100644518 B1 KR 100644518B1 KR 1020050103913 A KR1020050103913 A KR 1020050103913A KR 20050103913 A KR20050103913 A KR 20050103913A KR 100644518 B1 KR100644518 B1 KR 100644518B1
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water
chlorine
based organic
soluble
organic compound
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김병억
김민균
사영삼
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재단법인 포항산업과학연구원
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D37/00—Processes of filtration
    • B01D37/03—Processes of filtration using flocculating agents

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Abstract

A method for extracting chlorine organic compound contained in the water is provided to carry out the extraction in a short time with improved extraction efficiency by using a water-soluble adsorption agent. A method for extracting chlorine organic compound contained in the water includes the steps of oxidizing cokes powder by adding oxygenated water to the cokes powder and filtering to recover the cokes powder. An NaOH solution is added to the cokes powder for alkaline treatment. The result is filtered and recovered to form a water-soluble adsorption agent. 0.0001-0,001we% of the water-soluble adsorption agent is added to a subject water and the mixture is stirred. A cationic organic cohesive agent is added to the subject water and stirred, a weight of the cationic organic cohesive agent is 25-30 times of the weight of the water-soluble adsorption agent. A sample adsorbing chlorine organic compound is cohered. The subject water is filtered to recover the sample.

Description

수중에 함유된 염소계 유기화합물 추출 방법{The extraction method for halogenated organic compounds in waste water}The extraction method for halogenated organic compounds in waste water}

본 발명은 코크스 분말에 과산화수소수를 가하여 산화 처리하고 여과하여 회수하는 단계와, 상기 코크스 분말에 수산화나트륨(NaOH) 용액을 가하여 알칼리 처리하고 여과 회수하고 건조하여 수용성 흡착제를 형성하는 단계와, 피실험수에 상기 수용성 흡착제 0.0001 ~ 0.001 중량%를 첨가하여 교반하는 단계와, 상기 피실험수에 수용성 흡착제의 25 ~ 30 배 중량인 양이온계 유기 응집제를 첨가 교반하여 염소계 유기화합물이 흡착된 시료를 응집시키는 단계와, 상기 피실험수를 여과하여 시료를 회수하는 단계로 구성되어 수중에 함유된 염소계 유기화합물을 용이하게 추출하고 그 추출 효율을 크게 향상시킬 수 있는 염소계 유기화합물의 추출 방법에 관한 것이다.The present invention comprises the steps of adding hydrogen peroxide water to the coke powder to oxidize and recover by filtration, the addition of sodium hydroxide (NaOH) solution to the coke powder, alkali treatment, filtration recovery and drying to form a water-soluble adsorbent, and the test Stirring and adding 0.0001 to 0.001% by weight of the water-soluble adsorbent to water and agitating the sample to which the chlorine-based organic compound is adsorbed by adding and stirring the cationic organic flocculant, which is 25 to 30 times the weight of the water-soluble adsorbent, to the test water. And extracting the sample by filtration of the test water. The present invention relates to a method for extracting chlorine-based organic compounds which can easily extract chlorine-based organic compounds contained in water and greatly improve its extraction efficiency.

생활폐수 및 공장폐수 등의 오폐수 뿐만 아니라 하천수, 호수, 해양수, 지하수가 다이옥신(dioxins), 폴리염화비페닐(PCBs)과 같은 염소계 유기화합물에 의하여 오염되어 있을 가능성이 상존한다. 다이옥신류는 폴리염화디벤조-파라-디옥신(PCDDs)이나 폴리염화디벤조푸란(PCDFs) 등의 총칭이며, 매우 독성이 강한 환경오염 물질인데, 그 중에서도 2,3,7,8-사염화디벤조-파라-디옥신(T4CDDs)은 최강의 독성물질로 알려져 있다. 한편, 클로로페놀이나 클로로벤젠 등의 유기화합물은 다이옥신류에 비하여 독성은 약하지만, 상대적으로 물에 대한 용해도가 크기 때문에 수중에 고농도로 함유되어 있을 가능성이 높다. 따라서, 수중에 함유되어 있는 염소계 유기화합물을 정확하게 분석하는 것이 매우 중요하다. River water, lakes, ocean water and groundwater, as well as wastewater such as domestic wastewater and factory wastewater, are likely to be contaminated by chlorine-based organic compounds such as dioxins and polychlorinated biphenyls (PCBs). Dioxins are generic terms such as dibenzo-para-dioxin (PCDDs) and dibenzofuran (PCDFs), and are highly toxic environmental pollutants, among which 2,3,7,8-tetrachloride Benzo-para-dioxin (T 4 CDDs) is known to be the strongest toxicant. On the other hand, organic compounds such as chlorophenol and chlorobenzene are less toxic than dioxins, but are more likely to be contained in water due to their relatively high solubility in water. Therefore, it is very important to accurately analyze chlorine-based organic compounds contained in water.

수중에 함유된 염소계 유기화합물을 분석하기 위해서는, 우선 분석대상인 물에서 정밀하고 정확하게 시료를 추출하여야 한다. 특히, 다이옥신류는 수중에 입자 상태나 용해된 상태 등으로 매우 미량 함유되어 있기 때문에 고추출 효율로 추출하지 않으면 신뢰성 높은 분석결과를 기대할 수 없다. In order to analyze chlorine-based organic compounds in water, samples must be accurately and accurately extracted from the water to be analyzed. In particular, since dioxins are contained in a very small amount in the particulate state or dissolved state in water, reliable analysis results cannot be expected unless they are extracted with red pepper efficiency.

종래의 염소계 유기화합물의 추출 방법은 분석 대상인 물을 유리섬유 여과지에 의해 여과하는 단계와, 상기 여과된 물을 고체 상태의 디스크(disk)에 흡착하는 단계로 구성되며, 상기와 같이 유리섬유 여과지와 디스크에 흡착된 다이옥신류는 속실렛(soxhlet) 추출 장치에서 유기용매에 의해 추출된다. 이러한 종래의 방법은 물의 여과 속도가 빠르면 염소계 유기화합물의 흡착 효율이 저하되므로 흡착 효율을 유지하기 위하여 물을 여과하는 작업에 매우 장시간이 소요되며, 수중에 함유된 염소계 유기화합물이 유리섬유 여과지와 디스크에 제대로 흡착되지 않기 때문에 염소계 유기화합물의 추출 효율이 10 ~ 40 %에 불과하다는 문제점이 있다.Conventional chlorine-based organic compound extraction method comprises the step of filtering the water to be analyzed by a glass fiber filter paper, and the step of adsorbing the filtered water to a disk (solid) of the solid state, and the glass fiber filter paper as described above Dioxins adsorbed on the disk are extracted by an organic solvent in a soxhlet extraction apparatus. In this conventional method, since the adsorption efficiency of chlorine-based organic compounds decreases when the filtration rate of water is high, it takes a very long time to filter the water in order to maintain the adsorption efficiency. There is a problem that the extraction efficiency of the chlorine-based organic compound is only 10 to 40% because it is not properly adsorbed on.

상기와 같은 문제점을 해결하기 위하여, 본 발명의 목적은 코크스 분말을 과 산화수소수로 산화 처리하고 수산화나트륨 용액으로 알칼리 처리하여 수용성 흡착제를 형성하고, 피실험수에 상기 수용성 흡착제를 첨가 교반하여 염소계 유기화합물을 흡착시키고, 상기 피실험수에 양이온계 유기 응집제를 첨가 교반하여 시료를 응집시키고 여과 회수하므로서 수중에 함유된 염소계 유기화합물의 추출 효율을 크게 향상시킬 수 있는 염소계 유기화합물의 추출 방법을 제공하는데 있다.In order to solve the above problems, an object of the present invention is to oxidize the coke powder with hydrogen peroxide water and alkali treatment with sodium hydroxide solution to form a water-soluble adsorbent, by adding and stirring the water-soluble adsorbent to the test water to chlorine-based organic The present invention provides a method for extracting a chlorine-based organic compound that can greatly improve the extraction efficiency of chlorine-based organic compounds contained in water by adsorbing a compound and adding and stirring a cationic organic flocculant to the test water. have.

본 발명의 수중에 함유된 염소계 유기화합물 추출 방법은 코크스 분말에 과산화수소수를 가하여 산화 처리하고 여과하여 회수하는 단계와, 상기 코크스 분말에 수산화나트륨(NaOH) 용액을 가하여 알칼리 처리하고 여과 회수하고 건조하여 수용성 흡착제를 형성하는 단계와, 피실험수에 상기 수용성 흡착제 0.0001 ~ 0.001 중량%를 첨가하여 교반하는 단계와, 상기 피실험수에 수용성 흡착제의 25 ~ 30 배 중량인 양이온계 유기 응집제를 첨가 교반하여 염소계 유기화합물이 흡착된 시료를 응집시키는 단계와, 상기 피실험수를 여과하여 시료를 회수하는 단계로 구성되는 특징이 있다.The chlorine-based organic compound extraction method contained in the water of the present invention comprises the steps of oxidizing the coke powder by adding hydrogen peroxide water, filtration and recovery, and by adding sodium hydroxide (NaOH) solution to the coke powder, alkali treatment, filtration recovery and drying Forming a water-soluble adsorbent, adding and stirring 0.0001 to 0.001% by weight of the water-soluble adsorbent to the test water, and adding and stirring a cationic organic flocculant which is 25 to 30 times the weight of the water-soluble adsorbent to the test water. Agglomeration of the sample to which the chlorine-based organic compound is adsorbed, and collecting the sample by filtering the test water.

또한, 상기 양이온계 유기 응집제는 염화알루미늄, 황산제이철로 이루어진 군으로부터 선택된다.In addition, the cationic organic flocculant is selected from the group consisting of aluminum chloride and ferric sulfate.

다음에서 본 발명을 상세하게 설명한다.The present invention is described in detail below.

탄소 성분이 주성분이 코크스 분말에 과량의 과산화수소수를 가하여 산화 처리를 실시하고, 상기 혼합물을 여과하여 표면이 산화 처리된 코크스 분말을 회수한다. The carbon component is subjected to oxidation treatment by adding an excess of hydrogen peroxide to the coke powder as a main component, and the mixture is filtered to recover the coke powder whose surface is oxidized.

상기 코크스 분말에 과량의 수산화나트륨(NaOH) 용액을 가하여 알칼리 처리를 실시하고, 상기 혼합물을 여과하여 표면이 알칼리 처리된 코크스 분말을 회수하고, 회수된 코크스 분말을 상온에서 완전히 건조하여 수용성 흡착제를 구성한다. 상기와 같이 구성된 수용성 흡착제는 염소계 유기화합물을 흡착할 수 있으며 수중에서 콜로이드 상태로 분산 용해된다.An excess of sodium hydroxide (NaOH) solution was added to the coke powder for alkali treatment, the mixture was filtered to recover the coke powder whose surface was alkali treated, and the recovered coke powder was completely dried at room temperature to form a water-soluble adsorbent. do. The water-soluble adsorbent configured as described above can adsorb chlorine-based organic compounds and disperse and dissolve in colloidal state in water.

상기와 같이 구성된 수용성 흡착제를 분석대상인 피실험수에 첨가하되, 상기 피실험수를 기준으로 수용성 흡착제 0.0001 ~ 0.001 중량%를 첨가하며, 피실험수에 수용성 흡착제가 신속하게 분산 용해되도록 상기 피실험수를 교반하여 상기 수용성 흡착제에 염소계 유기화합물을 흡착시킨다.The water-soluble adsorbent configured as described above is added to the test water to be analyzed, and 0.0001 to 0.001% by weight of the water-soluble adsorbent is added based on the test water, and the water to be rapidly dispersed and dissolved in the test water is dissolved. By stirring, the chlorine-based organic compound is adsorbed to the water-soluble adsorbent.

상기 피실험수에 수용성 흡착제를 응집하는 양이온계 유기 응집제를 첨가하되, 상기 양이온계 유기 응집제는 수용성 흡착제의 25 ~ 30 배 중량으로 첨가하며, 상기 양이온계 유기 응집제가 수용성 흡착제를 효과적으로 응집하도록 상기 피실험수를 교반하여 염소계 유기화합물이 흡착된 시료를 응집시킨다. 양이온계 유기 응집제가 수용성 흡착제의 25 배 미만의 중량으로 첨가되면 양이온계 유기 응집제가 수용성 흡착제를 충분히 응집시키지 못하며, 양이온계 유기 응집제가 수용성 흡착제의 30 배를 초과하는 중량으로 첨가되면 첨가되는 양이온계 유기 응집제에 비해 수용성 흡착제를 응집하는 효율이 더이상 증가되지 않는다.A cationic organic coagulant is added to the test water, and the cationic organic coagulant is added at 25 to 30 times the weight of the water soluble adsorbent, and the cationic organic coagulant is effectively coagulated with the water soluble adsorbent. The test water is stirred to agglomerate the sample to which the chlorine-based organic compound is adsorbed. If the cationic organic flocculant is added at less than 25 times the weight of the water-soluble adsorbent, the cationic organic flocculant does not sufficiently aggregate the water-soluble adsorbent. If the cationic organic flocculant is added at the weight of more than 30 times the water-soluble adsorbent, the cationic system is added. The efficiency of flocculating water soluble adsorbents no longer increases compared to organic flocculants.

양이온계 유기 응집제는 염화알루미늄, 황산제이철로 이루어진 군으로부터 선택되며, 상기 양이온계 유기 응집제에 의해 응집된 시료는 침강하게 된다.The cationic organic flocculant is selected from the group consisting of aluminum chloride and ferric sulfate, and the sample aggregated by the cationic organic flocculant is settled.

상기 피실험수를 여과하여 시료를 회수한다. 회수된 시료를 통상적인 염소화 유기화합물의 분석 방법에 의거하여 분석한다.The test water is filtered to recover a sample. The recovered sample is analyzed according to the conventional method for analyzing chlorinated organic compounds.

실시예를 참조하여 본 발명을 구체적으로 설명한다.The present invention will be described in detail with reference to Examples.

[실시예 1]Example 1

독성을 가지고 있으며 통칭 다이옥신이라 불리우는 염소계 유기화합물 7 종과 퓨란 표준물질 10 종을 아세톤 용매에 용해하여 조제하고, 상기 조제물을 증류수에 혼합 교반하여 피실험수를 제조하였다.Seven chlorine-based organic compounds called dioxin and ten kinds of furan standards were dissolved and prepared in acetone solvent, and the test mixture was prepared by mixing and stirring the preparation in distilled water.

코크스 분말 10 g에 30 % 과산화수소 10 ml를 가하여 산화 처리를 실시하고, 상기 혼합물을 여과하여 코크스 분말을 회수하였다.10 g of 30% hydrogen peroxide was added to 10 g of coke powder for oxidation treatment, and the mixture was filtered to recover coke powder.

상기 코크스 분말에 과량의 수산화나트륨(NaOH) 용액을 가하여 알칼리 처리를 실시하고, 상기 혼합물을 여과하여 코크스 분말을 회수하고, 회수된 코크스 분말을 상온에서 완전히 건조하여 수용성 흡착제를 구성하였다.An excess of sodium hydroxide (NaOH) solution was added to the coke powder for alkali treatment, the mixture was filtered to recover the coke powder, and the recovered coke powder was completely dried at room temperature to form a water-soluble adsorbent.

상기 피실험수 1 리터에 상기 수용성 흡착제 5 ㎎을 첨가하고 교반하여 상기 수용성 흡착제에 염소계 유기화합물을 흡착시켰다.5 mg of the water-soluble adsorbent was added to 1 liter of the test water and stirred to adsorb the chlorine-based organic compound to the water-soluble adsorbent.

상기 피실험수에 양이온계 유기 응집제인 황산제이철 150 ㎎을 첨가하고 교반하여 염소계 유기화합물이 흡착된 시료를 응집시켰다.150 mg of ferric sulfate, a cationic organic flocculant, was added to the test water and stirred to agglomerate the sample to which the chlorine-based organic compound was adsorbed.

상기 피실험수를 5 ㎛의 유리섬유 여과지에 의해 여과하고, 상기 유리섬유 여과지에 잔류된 시료를 회수하였다. The test water was filtered with a 5 μm glass fiber filter paper, and a sample remaining on the glass fiber filter paper was collected.

회수된 시료를 속실렛 장치(soxhlet apparatus)에서 16 시간동안 톨루엔으로 추출하였다. 상기 추출물을 미국 EPA 1613인 다이옥신류의 정제 방법에 의거하여 정제하고 고성능 가스크로마토그래피/질량분석기로 분석하였다.The recovered sample was extracted with toluene for 16 hours in a soxhlet apparatus. The extract was purified according to the purification method of dioxins of US EPA 1613 and analyzed by high performance gas chromatography / mass spectrometry.

상기 실시예 1에 의거한 테스트를 여러회 반복 실시하고 분석한 결과 다이옥신류의 추출 효율이 85 ~ 95 %인 것으로 나타났다.The test according to Example 1 was repeated several times and analyzed, and the extraction efficiency of dioxins was 85-95%.

[실시예 2]Example 2

피실험수 1 리터에 상기 수용성 흡착제 1 ㎎을 첨가하고 교반하는 것과, 상기 피실험수에 양이온계 유기 응집제인 염화알루미늄 25 ㎎을 첨가하고 교반하는 것 이외에는 실시예 1과 동일하다.It is the same as Example 1 except adding and stirring 1 mg of said water-soluble adsorbents to 1 liter of test water, and stirring and adding 25 mg of aluminum chloride which is a cationic organic flocculant to the test water.

상기 실시예 2에 의거한 테스트를 여러회 반복 실시하고 분석한 결과 다이옥신류의 추출 효율이 80 ~ 90 %인 것으로 나타났다.The test according to Example 2 was repeatedly performed and analyzed, and the extraction efficiency of dioxins was 80-90%.

상기한 바와 같이 실시예 1 및 2에 의거하여 추출된 시료를 분석한 결과, 다이옥신류의 추출 효율이 80 ~ 95 %로서, 종래 기술에 의한 다이옥신류의 추출 효율 10 ~ 40 %에 비해 다이옥신류의 추출 효율이 훨씬 탁월한 것으로 나타났다.As a result of analyzing the samples extracted according to Examples 1 and 2, the extraction efficiency of dioxins was 80 to 95%, which was higher than that of dioxins according to the prior art. The extraction efficiency was found to be much superior.

본 발명에 의한 염소계 유기화합물 추출 방법은 수중에 함유된 염소계 유기화합물의 추출 작업을 단시간에 용이하게 실시할 수 있게 하며, 다이옥신을 비롯한 염소계 유기화합물의 추출 효율을 크게 향상시킬 수 있게 하는 효과가 있다.The chlorine-based organic compound extraction method according to the present invention makes it possible to easily perform the extraction operation of the chlorine-based organic compound contained in water in a short time, and has the effect of greatly improving the extraction efficiency of chlorine-based organic compounds, including dioxins. .

상기와 같이 본 발명은 기재된 실시예를 중심으로 상세하게 설명하였지만, 본 발명의 범주 및 기술사상 범위 내에서 다양한 변형 및 수정이 가능하다는 것은 당업자에 있어서 명백한 것이며, 이러한 변형 및 수정이 첨부된 특허청구범위에 속하는 것도 당연한 것이다.As described above, the present invention has been described in detail with reference to the described embodiments, but it will be apparent to those skilled in the art that various changes and modifications can be made within the scope and spirit of the present invention. It is also natural to fall within the scope.

Claims (2)

코크스 분말에 과산화수소수를 가하여 산화 처리하고 여과하여 회수하는 단계;Adding hydrogen peroxide solution to the coke powder for oxidation, filtration and recovery; 상기 코크스 분말에 수산화나트륨(NaOH) 용액을 가하여 알칼리 처리하고 여과 회수하고 건조하여 수용성 흡착제를 제조하는 단계;Adding an aqueous sodium hydroxide (NaOH) solution to the coke powder for alkali treatment, filtration, and drying to prepare a water-soluble adsorbent; 염소계 유기화합물이 함유된 물에 상기 수용성 흡착제 0.0001 ~ 0.001 중량%를 첨가하여 교반하는 단계;Stirring by adding 0.0001 to 0.001% by weight of the water-soluble adsorbent to water containing a chlorine-based organic compound; 상기 물에 수용성 흡착제의 25 ~ 30 배 중량인 양이온계 유기 응집제를 첨가 교반하여 염소계 유기화합물이 흡착된 시료를 응집시키는 단계;Aggregating a sample having a chlorine-based organic compound adsorbed by adding and stirring a cationic organic coagulant having 25 to 30 times the weight of the water-soluble adsorbent to the water; 상기 물을 여과하여 시료를 회수하는 단계;로 Recovering a sample by filtering the water; 구성되는 것을 특징으로 하는 수중에 함유된 염소계 유기화합물 추출 방법.Method for extracting chlorine-based organic compounds contained in water, characterized in that the configuration. 제 1 항에 있어서, 상기 양이온계 유기 응집제는 염화알루미늄, 황산제이철로 이루어진 군으로부터 선택되는 것을 특징으로 하는 수중에 함유된 염소계 유기화합물 추출 방법.The method of extracting chlorine-based organic compounds contained in water according to claim 1, wherein the cationic organic flocculant is selected from the group consisting of aluminum chloride and ferric sulfate.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR0151988B1 (en) * 1995-06-19 1998-10-01 김종진 Method for treating waste water from cokes manufacturing process
JP3269901B2 (en) 1993-12-14 2002-04-02 株式会社荏原製作所 Treatment of organic chlorine compounds
JP2002153703A (en) 2000-11-16 2002-05-28 Miura Co Ltd Flocculant for collecting organochlorine compound
KR100391561B1 (en) 2000-08-25 2003-07-12 재단법인 포항산업과학연구원 Preparation of dioxin removal adsorbent from coke breeze

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3269901B2 (en) 1993-12-14 2002-04-02 株式会社荏原製作所 Treatment of organic chlorine compounds
KR0151988B1 (en) * 1995-06-19 1998-10-01 김종진 Method for treating waste water from cokes manufacturing process
KR100391561B1 (en) 2000-08-25 2003-07-12 재단법인 포항산업과학연구원 Preparation of dioxin removal adsorbent from coke breeze
JP2002153703A (en) 2000-11-16 2002-05-28 Miura Co Ltd Flocculant for collecting organochlorine compound

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