KR100545687B1 - Desalination of polyphenyl phenyl using acid solution - Google Patents
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- KR100545687B1 KR100545687B1 KR20030095874A KR20030095874A KR100545687B1 KR 100545687 B1 KR100545687 B1 KR 100545687B1 KR 20030095874 A KR20030095874 A KR 20030095874A KR 20030095874 A KR20030095874 A KR 20030095874A KR 100545687 B1 KR100545687 B1 KR 100545687B1
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Abstract
본 발명은 저렴하고 간단한 방법에 의해 폴리염화비페닐(PCBs)을 분해할 수 있는 PCBs 무해화 방법을 제공함을 목적으로 한다.It is an object of the present invention to provide a PCBs detoxification method that can decompose polychlorinated biphenyls (PCBs) by a low cost and simple method.
이를 위하여 본 발명은, 100℃ 미만의 온도에서 PCBs를 함유한 물질을 금속이온이 용해된 염산산성 수용액에 접촉시켜 PCBs를 분해하는 PCBs 무해화 방법을 제공하며, 염산산성 수용액과 PCBs와의 접촉을 촉진하기 위하여 접촉 촉진제가 첨가된다.To this end, the present invention provides a PCBs detoxification method for decomposing PCBs by contacting a material containing PCBs at a temperature of less than 100 ° C. with an aqueous hydrochloric acid solution in which metal ions are dissolved, and promoting contact between the hydrochloric acid aqueous solution and the PCBs. In order to do this, a contact promoter is added.
폴리염화비페닐(PCBs), 유기염소계 화합물, 다이옥신, 무해화Polychlorinated biphenyls (PCBs), organochlorine compounds, dioxins, harmless
Description
본 발명은 산성용액을 이용한 폴리염화비페닐(PCBs)의 무해화 처리방법에 관한 것으로, 특히 비산재(Flying Ash) 중에 포함되어 있는 PCBs를 반응촉매와 염소이온이 함유된 산성용액과 반응시켜 100℃ 보다 낮은 온도에서 무해화하는 방법에 관한 것이다.The present invention relates to a method for the detoxification of polychlorinated biphenyls (PCBs) using an acidic solution. In particular, the PCBs contained in fly ash are reacted with an acidic solution containing a reaction catalyst and chlorine ion at 100 ° C. A method of detoxifying at lower temperatures.
폴리염화비페닐(Polychlorinated Biphenyls)은 절연특성을 가지고 있어 산업계에서 수십 년 동안 사용되어온 유기염소계 화합물로서, 1960년대와 1970년대에 와서는 PCBs의 독성문제에 대한 자각이 높아짐에 따라 지금은 대부분의 국가에서 사용이 금지되었음에도 불구하고 생태계에 광범위하게 퍼져있다. 이 물질은 동물의 지방조직에 분포하며 쉽게 분해되지 않는 잔류성 유기오염물질(POPs, Persistent Organic Pollutants)로 분류되며, 환경호르몬 의심물질로서 스톡홀름 협약이 2004년 상반기에 발효되면 이 물질이 함유된 모든 제품 및 부산물에 대하여 의무적으로 무해화를 위한 조치가 취해져야 한다.Polychlorinated Biphenyls are organic chlorine compounds that have been used for decades in the industry because of their insulating properties.In the 1960s and 1970s, polychlorinated Biphenyls have become more aware of the toxicity of PCBs. Although it is banned from use, it is widespread in the ecosystem. This substance is classified as Persistent Organic Pollutants (POPs), which are distributed in animal adipose tissue and are not easily degraded.As a suspected environmental hormone, all products containing this substance when the Stockholm Convention enters into force in the first half of 2004. And mandatory measures should be taken for harmless by-products.
이러한 PCBs를 무해화하기 위한 방법으로 미생물의 탈염소 분해능력을 이용 한 PCBs 독성제거 가능성이 제시되고 있으며, 다이옥신이 발생하지 않을 정도의 고온(2000℃ 이상)으로 연소시키는 방법 등이 제시되고 있으나 아직 상용화되기에는 오랜 연구가 필요하거나 경제성이 떨어지는 문제점이 있다. 따라서 PCBs의 무해화는 다이옥신을 무해화 시키는 방법이 그대로 적용함을 통해 이루어지고 있는 실정이다.As a method to detoxify these PCBs, the possibility of eliminating PCBs toxicity by using the dechlorination ability of microorganisms has been suggested, and a method of burning them at a high temperature (more than 2000 ° C.) that dioxin does not occur has been proposed. To be commercialized, there is a problem that requires long research or poor economics. Therefore, the harmlessness of PCBs is made by applying the method of harmless to dioxin.
다이옥신 무해화 방법에는 소각법, 용융법, 열분해법, 광분해법, 오존분해법, 과산화수소에 의한 산화분해법, 수열분해법 및 알칼리분해법 등을 들 수 있으며, 그 일례로서 일본 공개특허공보 평10-146574 호에는 다이옥신류를 함유하는 비산재에 황산 등의 산을 첨가하여 슬러리상을 만들고, 이 슬러리를 100 ℃ 이상의 온도로 가열하여 다이옥신을 분해하는 방법이 제안되어 있다. Dioxin detoxification methods include incineration, melting, thermal decomposition, photolysis, ozone decomposition, oxidative decomposition with hydrogen peroxide, hydrothermal decomposition and alkali decomposition, and examples thereof include JP 10-146574 A. A method of adding a acid such as sulfuric acid to a fly ash containing dioxins to form a slurry phase, and heating the slurry to a temperature of 100 ° C or higher has been proposed to decompose dioxins.
그러나 이 방법은 비교적 효율적으로 다이옥신류를 무해화할 수 있지만, 그 처리온도가 물의 비점 이상의 온도인 100 ℃ 이상, 바람직하게는 200 ℃ 이상이며, 또한 물을 증발시키면서 처리를 실시하기 때문에 에너지의 소비비율이 크고 장치비용이 많이 든다는 문제점이 있다. PCBs에 맞는 보다 효율적인 무해화 처리방법의 개발이 요구된다.However, this method can detoxify dioxin relatively efficiently, but since the treatment temperature is at least 100 ° C, preferably at least 200 ° C, which is at a temperature above the boiling point of water, and the treatment is performed while evaporating water, the ratio of energy consumption There is a problem that this large and expensive equipment. There is a need for the development of more efficient harmless treatment methods for PCBs.
본 발명은 상술한 바와 같은 문제점을 해결하기 위하여 제안된 것으로, PCBs의 분해에 적합하며, 다이옥신 무해화 방법에 의한 PCBs 무해화 비용 보다 저렴한 비용으로 간단하게 처리할 수 있는 폴리염화비페닐 무해화 처리방법을 제공함을 목적으로 한다.The present invention has been proposed to solve the problems described above, and is suitable for decomposition of PCBs, polychlorinated biphenyl harmless treatment that can be easily processed at a lower cost than PCBs harmlessness by the dioxin harmless method The purpose is to provide a method.
상기한 바와 같은 목적을 달성하기 위한 본 발명에 따른 PCBs 무해화 방법은, 염소이온과 금속이온이 용해되고 염산산성 수용액에 PCBs를 함유한 물질을 접촉시키고, 100℃ 미만 30℃ 이상의 온도로 가열교반하여 상기 PCBs를 분해하는 것을 특징으로 한다.PCBs detoxification method according to the present invention for achieving the above object, chlorine ions and metal ions are dissolved and contacting a substance containing PCBs in an aqueous solution of hydrochloric acid, and stirred under heating at a temperature of less than 100 ℃ 30 ℃ By disassembling the PCBs.
또한, 염산산성 수용액에서의 염소이온(Cl-) 농도는 수용액 1ℓ당 50 mmol 이상, 바람직하게는 100 mmol 이상이고, 그 상한치는 2000 mmol 정도이다. 그리고 pH 는 6 이하, 바람직하게는 5 이하이며, 그 하한치는 통상 2 정도이다.In addition, the concentration of chlorine ion (Cl − ) in an aqueous solution of hydrochloric acid is 50 mmol or more, preferably 100 mmol or more, per liter of the aqueous solution, and the upper limit thereof is about 2000 mmol. And pH is 6 or less, Preferably it is 5 or less, The lower limit is about 2 normally.
또한, 염산산성 수용액에 용해된 금속이온은 구리이온 또는 철이온 중 적어도 어느 하나를 포함하는 것이 바람직하다.In addition, the metal ion dissolved in the acidic hydrochloric acid solution preferably contains at least one of copper ions and iron ions.
또한, 염산산성 수용액에는, PCBs와 염산산성 수용액의 접촉을 촉진하기 위한 접촉 촉진제로서 계면활성제 또는 알코올류 중 하나가 첨가되는 것이 바람직하다.Moreover, it is preferable to add one of surfactant or alcohol to a hydrochloric acid aqueous solution as a contact promoter for accelerating contact of PCBs and hydrochloric acid aqueous solution.
이러한 처리방법에 의하여 PCBs는 적어도 90% 이상의 분해율로 무해화된다.This treatment makes PCBs harmless with at least 90% degradation.
염산산성 수용액은 다른 무기산, 예컨대 황산을 함유할 수 있는데, 이 경우 수용액중의 염소이온과 황산이온의 몰비 [Cl]/[SO4] 는 5 이상, 바람직하게는 20 이상으로 조절하는 것이 좋다. PCBs와 수용액의 접촉방법으로서는, PCBs를 함유하는 고체를 수용액중에서 교반하는 방법, 또는 이를 함유하는 고체에 수용액을 spray시켜 접촉시키는 방법 등을 들 수 있다.The hydrochloric acid aqueous solution may contain other inorganic acids such as sulfuric acid. In this case, the molar ratio [Cl] / [SO 4 ] of chlorine ion and sulfate ion in the aqueous solution is preferably adjusted to 5 or more, preferably 20 or more. As a contact method of PCBs and aqueous solution, the method of stirring the solid containing PCBs in aqueous solution, the method of spraying aqueous solution and contacting the solid containing this, etc. are mentioned.
본 설명에서 지칭하는 염산산성 수용액(이하 '수용액')이란 염소이온을 함유 하는 산성 수용액을 의미하며, 산성을 유지하기 위한 산은 염산, 황산, 질산 등이 사용될 수 있으며, 바람직하게는 염산을 사용하거나 염산과 기타의 산을 혼합하여 사용한다.The hydrochloric acid aqueous solution (hereinafter 'aqueous solution') referred to in the present description means an acidic aqueous solution containing chlorine ions, and an acid for maintaining acidity may be hydrochloric acid, sulfuric acid, nitric acid, or the like. Use a mixture of hydrochloric acid and other acids.
본 발명에서 PCBs에 대한 반응처리제로서 사용하는 수용액에는 PCBs의 분해를 촉진시키는 반응촉매를 첨가된다. 반응촉매가 첨가되지 않는 경우에는 PCBs를 무해화하는 데 상당히 긴 시간을 요하게 되기 때문에, 반응촉매를 수용액에 함유시키는 것은 매우 중요하다. 이와 같은 반응촉매로서는 금속이온이 사용되는데, 예로서 철, 망간, 구리, 니켈, 코발트, 몰리브덴, 크롬, 바나듐, 텅스텐, 은, 주석 등이 가능하며, 바람직하게는 구리이온 또는 철이온이 사용된다. 수용액중에 함유시키는 금속이온의 양은 구리이온의 경우, 금속 환산량으로 20 ∼ 10,000 ㎎/ℓ, 바람직하게는 100 ∼ 5,000 ㎎/ℓ정도이다.In the present invention, a reaction catalyst for promoting decomposition of PCBs is added to an aqueous solution used as a reaction treatment agent for PCBs. It is very important to include the reaction catalyst in the aqueous solution because it will take a long time to harm the PCBs if no reaction catalyst is added. As the reaction catalyst, metal ions are used, for example, iron, manganese, copper, nickel, cobalt, molybdenum, chromium, vanadium, tungsten, silver, tin, and the like, and preferably copper or iron ions are used. . The amount of metal ions to be contained in the aqueous solution is 20 to 10,000 mg / L, preferably 100 to 5,000 mg / L, in terms of metal in the case of copper ions.
반응촉매는 염화물, 산화물, 탄산염, 황산염 등의 금속산화물 또는 금속염의 형태로 공급될 수 있으며, 이 경우 수용액에는 금속산화물 또는 금속염의 미용해분이 함유될 수 있다. The reaction catalyst may be supplied in the form of a metal oxide or metal salt such as chloride, oxide, carbonate, sulfate, and in this case, the aqueous solution may contain an undissolved portion of the metal oxide or metal salt.
또한 반응촉매는, 비산재(fly ash)나 바닥재(bottom ash) 등의 소각재 중에 함유되어 있는 금속성분이 이용될 수 있다. 소각재에는 상기한 바와 같은 반응촉매로서 작용하는 금속이 함유되어 있는 경우가 많다. 소각재 중에 함유되어 있는 금속성분을 반응촉매로서 이용하기 위해서는, 소각재를 수용액에 첨가하여 교반하는 것으로 족하다. 교반에 의해 소각재에 함유된 금속성분은 수용액 내에서 금속이온으로 용해되며, 이러한 금속이온을 용해상태로 함유하는 수용액은 본 발명에 있어 서의 PCBs에 대한 반응처리제로서 충분히 사용될 수 있다.As the reaction catalyst, a metal component contained in an incineration ash such as fly ash or bottom ash may be used. Incinerators often contain metals which act as reaction catalysts as described above. In order to use the metal component contained in an incineration ash as a reaction catalyst, it is sufficient to add the incineration ash to aqueous solution, and to stir. By stirring, the metal component contained in the incineration ash is dissolved into metal ions in an aqueous solution, and the aqueous solution containing such metal ions in a dissolved state can be sufficiently used as a reaction treatment agent for PCBs in the present invention.
반응처리제로서 사용하는 수용액에는 수용액과 PCBs의 접촉을 촉진시키는 물질을 함유시킬 수 있다. 이러한 물질은 계면활성제 또는 알코올류가 포함된다. 계면활성제의 종류는 특별히 제약되지 않으며, 음이온계, 양이온계, 비이온계 및 양성의 계면활성제를 사용할 수 있다. 계면활성제의 첨가량은 0.005 ∼ 1 중량%, 바람직하게는 0.01 ∼ 0.5 중량% 이다. 알코올류로서는 메탄올, 에탄올, 프로판올 등을 사용할 수 있으며, 그 첨가량은 0.5 ∼ 10 중량%, 바람직하게는 1 ∼ 10 중량% 이다.The aqueous solution used as the reaction treatment agent may contain a substance that promotes contact between the aqueous solution and the PCBs. Such materials include surfactants or alcohols. The kind of surfactant is not particularly limited, and anionic, cationic, nonionic and amphoteric surfactants can be used. The addition amount of surfactant is 0.005 to 1 weight%, Preferably it is 0.01 to 0.5 weight%. Methanol, ethanol, propanol, etc. can be used as alcohol, The addition amount is 0.5 to 10 weight%, Preferably it is 1 to 10 weight%.
이하에서는 본 발명에 따른 구체적인 실시예를 살펴본다.Hereinafter, a specific embodiment according to the present invention will be described.
실시예 1Example 1
소각로에서 분리회수된 비산재 중에 함유된 PCBs의 무해화 처리를 다음과 같이 실시한다. The detoxification of PCBs contained in fly ash separated and recovered from the incinerator is carried out as follows.
(비산재의 성상)(Appearance of fly ash)
(ⅰ) 탄소질물질의 함유량 : 0.1 중량%(Iii) Content of carbonaceous substance: 0.1 wt%
(ⅱ) 구리 함유량 : 0.35 중량%(Ii) Copper content: 0.35 wt%
(ⅲ) PCBs 함유량 : 56 ㎍/g(Iii) PCBs content: 56 ㎍ / g
상기한 바와 같은 성상을 갖는 비산재 400g 을 2ℓ의 순수중에 첨가하고, 가열교반하면서 염산을 첨가하여 65 ℃, pH 3.5 상태를 48시간 동안 유지한다. 이 때 수용액중의 염화이온 농도는 1900 mmol/ℓ, [Cl]/[SO4]는 113, 구리이온 농도는 500㎎/ℓ이다. 48 시간 교반후, 슬러리를 여과하여 비산재 중에 함유되는 PCBs를 분석 한 결과 92% 의 분해율을 얻을 수 있었다.400 g of fly ash having the above properties was added to 2 liters of pure water, and hydrochloric acid was added while heating and stirring to maintain a state of 65 DEG C and pH 3.5 for 48 hours. At this time, the chloride ion concentration in the aqueous solution is 1900 mmol / L, [Cl] / [SO 4 ] is 113, and the copper ion concentration is 500 mg / L. After stirring for 48 hours, the slurry was filtered and the PCBs contained in the fly ash were analyzed. As a result, a decomposition rate of 92% was obtained.
실시예 2Example 2
소각로에서 분리회수된 비산재 중에 함유된 PCBs의 무해화 처리를 다음과 같이 실시한다. The detoxification of PCBs contained in fly ash separated and recovered from the incinerator is carried out as follows.
(비산재의 성상)(Appearance of fly ash)
(ⅰ) 탄소질물질의 함유량 : 3.0 중량%(Iii) Content of carbonaceous substance: 3.0 wt%
(ⅱ) 구리 함유량 : 0.17 중량%(Ii) Copper content: 0.17 wt%
(ⅲ) PCBs 함유량 : 170 ㎍/g(Iii) PCBs content: 170 ㎍ / g
순수중에 메탄올이 10 wt% 첨가된 4ℓ의 용액에 상기한 바와 같은 성상을 갖는 비산재 400g 을 넣고 가열 교반하면서 염산을 혼합하여 온도 65 ℃, pH 3.5 의 상태를 48 시간 유지한다. 이때 수용액중의 염화이온 농도는 480 mmol/ℓ, [Cl]/[SO4] 몰비는 29, 구리이온 농도는 100 ㎎/ℓ이다. 400 g of fly ash having the properties as described above was added to a 4 L solution to which 10 wt% of methanol was added to the pure water, and hydrochloric acid was mixed while heating and stirred to maintain a temperature of 65 DEG C and a pH of 3.5 for 48 hours. At this time, the chloride ion concentration in the aqueous solution is 480 mmol / L, the [Cl] / [SO 4 ] molar ratio is 29, and the copper ion concentration is 100 mg / L.
48 시간 교반후, 슬러리를 여과하여 비산재 중에 함유되는 PCBs를 분석한 결과 90% 의 분해율을 얻을 수 있었다.After stirring for 48 hours, the slurry was filtered to analyze the PCBs contained in the fly ash. As a result, a decomposition rate of 90% was obtained.
상술한 바와 같은 폴리염화비페닐 무해화 방법에 의하면, 낮은 온도와 간단한 설비만으로도 PCBs 90% 이상 무해화할 수 있게 되어, PCBs 무해화 처리비용이 절감된다.According to the polychlorinated biphenyl desalination method as described above, the PCBs can be detoxified 90% or more even at low temperatures and simple facilities, thereby reducing the cost of PCBs desalination.
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