KR20010055244A - A method for decreasing sludges discharged by neutralizing pickling waste waters of stainless steels - Google Patents
A method for decreasing sludges discharged by neutralizing pickling waste waters of stainless steels Download PDFInfo
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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Abstract
Description
본 발명은 스테인레스강 산세 폐수를 중화처리시 배출되는 슬러지량을 저감하는 방법에 관한 것으로, 보다 상세하게는 스테인레스강 제조 공정중 산세 공정에서 배출되는 폐수를 제철소 폐기물로부터 추출한 액상 중화제로 중화함으로써 중화제로서 사용되는 소석회 사용량은 실질적으로 줄이고 슬러지의 배출량은 저감하는 새로운 방법에 관한 것이다.The present invention relates to a method for reducing the amount of sludge discharged during the neutralization treatment of stainless steel pickling wastewater. It relates to a new way to substantially reduce the amount of slaked lime used and to reduce sludge emissions.
기존의 스테인레스 공정에서는 열처리 과정중에 스테인레스 표면에 생성된 스케일을 제거하기 위하여 질산과 불산의 혼산으로 세척하는 산세 공정을 거친다. 이때 발생되는 산세 폐액은 질산기(NO3 -), 불산기(F-)의 산기와 철, 크롬, 니켈의 이온을 포함하며, 초기 pH도 0.76으로 매우 강산성을 띤다. 따라서 이 폐수를 pH 6∼7이 되도록 중화시킨 다음 방류하는데, 현재 대부분의 스테인레스 제조 회사에서는 일본 특허 공개 소50-6574호 및 특허 공개 평 10-202271호에서와 같이 소석회를 사용하여 이 폐액을 중화처리하고 있다.In the conventional stainless steel process, the pickling process is performed by washing with a mixture of nitric acid and hydrofluoric acid to remove scale generated on the stainless surface during heat treatment. At this time, the pickling waste liquid generated includes nitrate groups (NO 3 − ), acid groups of hydrofluoric acid (F − ), and ions of iron, chromium and nickel, and has an initial pH of 0.76, which is very acidic. Therefore, the wastewater is neutralized to pH 6-7 and then discharged. At present, most stainless steel manufacturers neutralize this waste liquor using slaked lime, as in Japanese Patent Application Laid-open No. 50-6574 and Japanese Patent Application Laid-open No. Hei 10-202271. Processing.
이때 사용되는 소석회는 물에 소석회 분말을 20∼25중량% 농도가 되도록 장입한 소석회 현탁액이다. 이 소석회 현탁액을 사용하여 중화하면 소석회 현탁액중의 Ca 이온과 산세 폐액내 NO3 -, F-및 Fe+2, Ni+2, Cr+3이 반응하여 생성된 CaNO3는 물에 용해되어 액상으로 존재하고, 잔류하는 CaF2, FeOOH, Ni(OH)2, Cr(OH)3는 침전물로서 침강된다. 또한 상기 침전물과 함께 미반응 소석회 입자가 침전되어 슬러지를 형성한다.The slaked lime used at this time is a slaked lime suspension loaded with the slaked lime powder in water at a concentration of 20 to 25% by weight. When calcium hydroxide is neutralized by using a suspension in Ca ions and the pickling waste liquid of the NO of the calcium hydroxide suspension 3 -, F -, and Fe +2, Ni +2, CaNO 3 of Cr +3 in the reaction to produce the liquid phase it is soluble in water Present and remaining CaF 2 , FeOOH, Ni (OH) 2 , Cr (OH) 3 precipitates as a precipitate. In addition, the unreacted limestone particles are precipitated together with the precipitate to form sludge.
이를 반응식으로 나타내면 다음과 같다.This is represented by the following scheme.
용액을 분리한 다음 배출되는 상기 슬러지는 현재로는 특별한 용도가 없는 실정이고, 특히 미반응 소석회 입자를 함유하므로 알칼리성 폐수를 방출하여 주변 토양을 오염시키는 문제가 있다.The sludge that is discharged after separating the solution is not currently used for a particular purpose, and particularly contains unreacted calcined lime particles, thus causing a problem of polluting the surrounding soil by releasing alkaline wastewater.
상기 공정을 보다 구체적으로 살펴보면, 폐수중의 산기는 액체중에 용해되어있는 이온 상태이고, 중화 반응할 소석회는 물에 대한 용해도가 작은 고체 상태의 분말이 대부분이므로, 상기 반응은 고체와 액체가 반응하는 고-액 반응계이다.Looking at the process in more detail, the acid in the waste water is in the ionic state dissolved in the liquid, and the slaked lime to be neutralized reaction is most of the powder in the solid state of low solubility in water, the reaction is a reaction between the solid and the liquid Solid-liquid reaction system.
일반적으로 고-액 반응은 액-액 반응보다 속도가 느린데, 특히 본 발명에서와 같이 스테인레스 산세 폐액의 경우, 고체인 소석회 분말은 용해도가 작고 용해 속도도 느리므로 대단히 느린 고-액 반응계가 된다.In general, solid-liquid reactions are slower than liquid-liquid reactions, especially in the case of stainless pickling waste liquids as in the present invention, which is a solid slaked lime powder because of its low solubility and slow dissolution rate, resulting in a very slow solid-liquid reaction system.
따라서 단시간내에 중화 반응을 종료하기 위해서 중화제로서 소석회 현탁액을 과량으로 투입하면, 미반응 소석회 현탁액 입자중 상당수가 슬러지 상태로 배출되게 된다.Therefore, when the slaked lime suspension is excessively added as a neutralizing agent in order to complete the neutralization reaction in a short time, many of the unreacted slaked lime suspension particles are discharged in the sludge state.
그러므로 이같은 고-액 반응계를 액-액 반응계로 대체하면 슬러지 발생량은 가능한한 줄이면서 소석회를 과량 사용할 필요도 없을 것이다.Therefore, replacing such a solid-liquid reaction system with a liquid-liquid reaction system will reduce sludge generation as much as possible and eliminate the need for excessive use of slaked lime.
이에 본 발명의 목적은 스테인레스강 산세 폐수를 중화하는데 사용하는 중화제를 액상 중화제로 대체함에 따라 중화제의 실질적인 사용량을 줄이는 방법을 제공하려는데 있다.Accordingly, an object of the present invention is to provide a method for reducing the substantial amount of neutralizing agent by replacing the neutralizing agent used to neutralize the stainless steel pickling wastewater with a liquid neutralizing agent.
본 발명의 다른 목적은 제철소 폐기물로부터 액상 중화제를 추출함으로써 제철소 폐기물량을 줄이면서 스테인레스강 산세 폐수로부터 배출되는 슬러지량을 저감하는 방법을 제공하려는데 있다.Another object of the present invention is to provide a method for reducing the amount of sludge discharged from stainless steel pickling wastewater while reducing the amount of steel mill waste by extracting the liquid neutralizer from steel mill waste.
본 발명에 의하면,According to the invention,
석회와 고토 성분이 함유된 제철소 폐기물을 물에 침지한 다음 최대 5분간 교반하는 단계;Immersing the steel mill waste containing lime and goto in water and stirring for up to 5 minutes;
교반후 석회와 고토 성분을 함유하고 pH가 10이상인 상등액을 추출하는 단계; 및Extracting a supernatant containing lime and goto after stirring and having a pH of 10 or more; And
상기 추출액을 사용하여 스테인레스강 산세 처리시 배출되는 Fe(NO3)2, Ni(NO3)2, Cr(NO3)3, F-, NO3 -포함 폐수를 중화시켜 CaNO3가 용해된 용액을 분리하고, 잔류하는 FeOOH, Ni(OH)2, Cr(OH)3,CaF2침전물은 슬러지로배출하는 단계;로 이루어지는 스테인레스강 산세 폐수를 중화처리시 배출되는 슬러지량을 저감하는 방법이 제공된다.Fe using the above extract liquid discharged when stainless steel pickling process (NO 3) 2, Ni ( NO 3) 2, Cr (NO 3) 3, F -, NO 3 - to neutralize the contained wastewater solution is CaNO 3 dissolved Separation, and the remaining FeOOH, Ni (OH) 2 , Cr (OH) 3, CaF 2 precipitates are discharged to the sludge; provides a method for reducing the amount of sludge discharged during the neutralization treatment of stainless steel pickling wastewater do.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명에서는 종래에 스테인레스강 산세 폐액을 중화시키는데 사용되는 소석회 현탁액을 액상 소석회로 대체함으로써 소석회의 실질적인 사용량을 줄이면서 슬러지 배출량도 저감시키게 된다.In the present invention, by replacing the slaked lime suspension conventionally used to neutralize the stainless steel pickling waste liquor with liquid slaked, it reduces the sludge emissions while substantially reducing the amount of slaked lime.
상기 액상 중화제의 제조 원료로서 본 발명에서는 제철소 폐기물을 사용한다. 제철 공장에서 발생되는 산업 부산물에는 슬래그, 폐시멘트, 폐소석회 슬러지, 해수 마그네시아 제조시 발생하는 탈탄산 슬러지등이 있다.In the present invention, steel mill waste is used as a raw material for producing the liquid neutralizer. Industrial by-products from steel mills include slag, waste cement, waste lime sludge, and decarbonate sludge from seawater magnesia.
이 중에서 알루미나 성분이 다량 포함된 경우에는 본 발명의 방법에 의해 제조한 중화제내에도 알루미늄 이온이 포함되어 슬러지내에 수산화알루미늄을 배출하므로 바람직하지 않다.In the case where a large amount of the alumina component is contained, aluminum ions are included in the neutralizing agent produced by the method of the present invention, which is not preferable because aluminum hydroxide is discharged into the sludge.
따라서 본 발명에서는 알루미늄 이온을 별도로 분리해낸 다음 상기 폐기물을 사용하는 것이 바람직하며, 특히 알루미늄 이온은 추출되지 않고 칼슘과 마그네슘만이 용출되는 전로 슬래그, 전기로 산화기 슬래그, 용사 탈인 슬래그 및 용선 탈규 슬래그를 사용하는 것이 보다 바람직하다.Therefore, in the present invention, it is preferable to separately separate aluminum ions, and then use the waste, in particular, converter slag in which only calcium and magnesium are eluted without aluminum ions are extracted, electric furnace oxidizer slag, thermal spray slag and molten iron slag. It is more preferable to use.
이때 마그네슘은 물에 용해되어 Mg(OH)2의 형태로 포함되어 중화 작용을 하므로 Ca(OH)2만 존재하는 경우에 비하여 상승 작용을 갖는다.At this time, magnesium is dissolved in water and included in the form of Mg (OH) 2 to neutralize, and thus has a synergistic effect compared to the case where only Ca (OH) 2 is present.
상기 슬래그들을 그대로 사용하여도 좋으나, 원료에 따라 추출 특성이 달라지게 되므로 용출 속도를 증대시키고 슬래그 활용율을 향상시키도록 미분시키는 것이 바람직하다. 미분시 입도 범위는 0.25mm이하인 것이 좋다.The slag may be used as it is, but since the extraction properties vary depending on the raw material, it is preferable to increase the elution rate and to fine-tune the slag utilization rate. The fine particle size range is preferably 0.25 mm or less.
이들 원료를 물에 침지시켜 액상 Ca(OH)2상태로 최대 5분간 교반시키면서 추출하여 균일한 추출액을 얻는다. 이때 5분이상을 교반하는 것은 pH가 더이상 증가하지 않으므로 바람직하지 않다. These raw materials are immersed in water and extracted with stirring for up to 5 minutes in a liquid Ca (OH) 2 state to obtain a uniform extract. At this time, stirring for 5 minutes or more is not preferable since the pH is no longer increased.
얻어지는 추출액의 pH를 추출할 때마다 측정하여 pH 10이상이 될 때의 추출액을 폐수 중화제로 사용한다. pH가 10이하인 경우에도 중화제로 사용할 수는 있으나, pH가 10이하가 되면 그 사용량이 많아지므로 바람직하지 않다. 이같이 사용량을 보다 줄이기 위해서는 pH 11.5이상인 추출액을 사용하는 것이 보다 바람직하다.Every time the pH of the obtained extract is extracted, it is measured and the extract when the pH is 10 or more is used as the wastewater neutralizer. Even if the pH is less than 10 can be used as a neutralizer, but if the pH is less than 10 it is not preferable because the amount of use increases. As such, it is more preferable to use an extract having a pH of 11.5 or more to further reduce the amount used.
이와 같이 얻어진 추출액을 사용하여 스테인레스강 산세 처리시 발생하는 Fe(NO3)2, Ni(NO3)2, Cr(NO3)3, F-, NO3 -포함 폐수를 중화시키면 CaNO3는 용해되어 용액 상태로 존재한다. 이들을 분리한 다음 잔류하는 FeOOH, Ni(OH)2, Cr(OH)3,CaF2침전물은 슬러지로 배출된다.Thus, Fe (NO 3) occurring in a stainless steel pickling treatment by using the resulting extract 2, Ni (NO 3) 2 , Cr (NO 3) 3, F -, NO 3 - When neutralizing including waste water CaNO 3 is dissolved In solution state. After separating these, the remaining FeOOH, Ni (OH) 2 , Cr (OH) 3 and CaF 2 precipitates are discharged as sludge.
또한 본 발명에서 추출된 중화제는 액상 Ca(OH)2로만 이루어지므로, 중화 반응후 남은 Ca(OH)2가 배출되더라도 이들은 슬러지로서 배출되는 것이 아니라 용액 상태로 배출되게 되므로, 종래 소석회 현탁액을 사용한 경우에 매립한 슬러지로부터 고체상 Ca(OH)2가 방출되어 주변 토양을 알칼리성으로 오염시키는 문제를 극복할수 있다.In addition, since the neutralizing agent extracted in the present invention is composed of only liquid Ca (OH) 2 , even if Ca (OH) 2 remaining after the neutralization reaction is discharged, they are not discharged as sludge but are discharged in a solution state. Solid phase Ca (OH) 2 is released from the landfill sludge to overcome the problem of alkaline pollution of surrounding soil.
이하, 실시예를 통하여 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.
실시예Example
하기 실시예는 나아가 본 발명의 다양한 견지를 예시하는 것으로, 본 발명의 범위를 이에 한정하는 것은 아니다.The following examples further illustrate various aspects of the invention and do not limit the scope thereof.
<실시예 1><Example 1>
본 실시예에서는 스테인레스강 산세 폐액에 제철소 폐기물로부터 제조된 액상 중화제의 최적량을 적용하여 중화처리한 다음 배출되는 슬러지량을 살펴본다.In this embodiment, the sludge discharged after neutralization by applying the optimum amount of the liquid neutralizer prepared from steel mill waste to the stainless steel pickling waste liquid is examined.
전로 슬래그를 입도 0.25mm로 분쇄한 다음, 이들 슬래그를 물에 잠긴 상태로5분간 교반시켜 pH가 12.3인 추출액을 얻었다.The converter slag was ground to a particle size of 0.25 mm, and the slag was stirred for 5 minutes while submerged in water to obtain an extract having a pH of 12.3.
초기 pH가 0.76인 스테인레스강 산세 폐액 100㎖를 비커에 투입한 다음, 비커를 자기 교반기위에 놓고 5분간 교반하면서 상기 추출액을 소량 투입하여 pH를 측정하고, pH 변화가 없으면 추출액을 재투입하여 최종 pH가 7.77이 될 때까지 중화시켰다. 이때 추출액의 총투입량은 1885㎖였으며, 중화하는데 걸린 시간은 93분이었다.100 ml of stainless steel pickling waste liquid with an initial pH of 0.76 was added to the beaker, and the beaker was placed on a magnetic stirrer and stirred for 5 minutes, and then the pH was measured by adding a small amount of the extract solution. Was neutralized until 7.77. At this time, the total dose of the extract was 1885 ml, and the time taken to neutralize was 93 minutes.
그 결과 배출되는 슬러지량을 측정하고, X선 회절 분석에 의해 그 조성을 조사한 결과를 하기표 1에 나타내었다.As a result, the amount of sludge discharged was measured, and the result of examining the composition by X-ray diffraction analysis is shown in Table 1 below.
또한 초기 pH가 0.76인 스테인레스강 산세 폐액 100㎖에 종래 사용하는 소석회 현탁액 35.2㎖(pH 12.6)를 투입한 다음 최종 pH가 7.77이 되도록 중화시켰다. 이때 중화하는데 걸리는 시간은 13분이었다. 배출되는 슬러지량과 그 조성을 조사하고 그 결과를 하기표 1에 함께 나타내었다.In addition, 35.2 mL (pH 12.6) of a conventionally used slaked lime suspension was added to 100 mL of a stainless steel pickling wastewater having an initial pH of 0.76, and then neutralized to a final pH of 7.77. The time to neutralize was 13 minutes. The amount of sludge discharged and its composition were investigated and the results are shown in Table 1 together.
상기 표에서 알 수 있듯이, 본 발명의 방법에 의해 전로 슬래그로부터 추출한 추출액을 사용하여 스테인레스강 산세 폐액을 중화하는 발명예에서는 종래 방법에 의해 사용되는 양에 비하여 중화제의 사용량이 상대적으로 과량인 것처럼 보이나, 발명예에서는 Ca(OH)2가 슬러지로 배출되지 않는데 반하여 비교예내에 존재하는 고체상 Ca(OH)2중 상당수는 반응되지 않고 슬러지로 배출되는 바, 슬러지 저감 효과를 직접적으로 확인할 수 있다.As can be seen from the above table, in the invention example of neutralizing stainless steel pickling waste liquid using the extract extracted from converter slag by the method of the present invention, the amount of neutralizer used seems to be relatively excessive compared to the amount used by the conventional method. In the invention example, Ca (OH) 2 is not discharged to the sludge, whereas many of the solid Ca (OH) 2 present in the comparative example are discharged to the sludge without reacting, and thus the sludge reduction effect can be directly confirmed.
<실시예 2><Example 2>
본 실시예에서는 제철소 폐기물로부터 제조한 액상 중화제를 현장에서 사용하기 위하여, 스테인레스강 산세 폐액에 과량 투입하고 중화시킨 다음 배출되는 슬러지량을 살펴본다.In this embodiment, in order to use the liquid neutralizer prepared from steel mill waste in the field, the amount of sludge discharged after the neutralization of the stainless steel pickling waste is neutralized.
전기로 산화기 슬래그를 입도 0.25mm로 분쇄한 다음 이들 슬래그를 물에 잠긴 상태로 5분간 교반시켜 pH가 12.3인 추출액을 얻었다.The oxidizer slag was pulverized to a particle size of 0.25 mm by electricity, and the slag was stirred for 5 minutes while submerged in water to obtain an extract having a pH of 12.3.
초기 pH가 0.76인 스테인레스강 산세 폐액 100㎖에 상기 추출액 2050㎖를 투입한 다음 5분간 교반하면서 pH가 7.77이 되도록 중화시켰다. 이때 중화하는데 걸리는 시간은 총 6분이었다.2050 ml of the extract was added to 100 ml of a stainless steel pickling wastewater having an initial pH of 0.76, and then neutralized to pH 7.77 while stirring for 5 minutes. The time to neutralize was a total of 6 minutes.
그 결과 배출되는 슬러지량과 그 조성을 조사하고 그 결과를 하기표 2에 나타내었다.As a result, the amount of sludge discharged and its composition were investigated and the results are shown in Table 2 below.
또한 본 발명의 방법에 의한 슬러지 배출량 및 그 조성과 비교하기 위하여, 초기 pH가 0.76인 스테인레스강 산세 폐액 100㎖에 종래 사용하는 소석회 현탁액 39㎖(pH 12.6)를 투입한 다음 최종 pH가 7.77이 되도록 중화시켰다. 이때 중화하는데 걸리는 시간은 총 5.5분이었다. 슬러지량과 그 조성을 측정하고, 그 결과를 하기표 2에 함께 나타내었다.In addition, in order to compare with the sludge discharge by the method of the present invention and its composition, 39 ml (pH 12.6) of conventional slaked lime suspension is added to 100 ml of stainless steel pickling waste liquid having an initial pH of 0.76, and then the final pH is 7.77. Neutralized. The time to neutralize was 5.5 minutes in total. The amount of sludge and its composition were measured, and the results are shown in Table 2 together.
상기 표에서 알 수 있듯이, 본 발명의 방법에 의해 전기로 산화기 슬래그로부터 추출한 추출액을 사용하여 스테인레스강 산세 폐액을 중화하는 발명예에서는 잔류하는 미반응 Ca(OH)2가 액상이므로 배출되더라도 슬러지량을 증가시키지 않으므로, 소석회 현탁액을 사용하여 중화한 비교예에 비하여 배출 슬러지량을 현저하게저감할 수 있음을 확인할 수 있다.As can be seen from the above table, in the invention example of neutralizing stainless steel pickling waste liquid using the extract liquid extracted from the oxidizer slag by the method of the present invention, the remaining unreacted Ca (OH) 2 is a liquid, so the amount of sludge is discharged. Since it does not increase, it can be seen that the amount of discharged sludge can be significantly reduced as compared with the comparative example neutralized using the lime lime suspension.
또한 비교예의 방법은 고-액 반응이므로 대형 장치를 사용하게 되면 균일한 교반이 더욱 어려울 뿐만 아니라 중화제를 보다 과량으로 첨가하는 실제 적용시에는 슬러지 발생량이 현저하게 증가할 것으로 여겨진다.In addition, since the method of the comparative example is a solid-liquid reaction, it is believed that the use of a large apparatus makes not only uniform stirring more difficult, but also a significant increase in the amount of sludge generated in the actual application of adding an excessive amount of neutralizer.
본 발명의 스테인레스강 산세 폐수를 처리하는 방법에 의하면, 제철소 폐기물을 재활용함과 동시에 중화 반응에 사용되는 실질적인 소석회량과 슬러지 배출량을 줄일 수 있다.According to the method of treating the stainless steel pickling wastewater of the present invention, it is possible to recycle the steel mill waste and at the same time reduce the actual amount of slaked lime and sludge used in the neutralization reaction.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100916087B1 (en) * | 2002-08-30 | 2009-09-08 | 주식회사 포스코 | Method for neutralization of slag leachate |
| CN102757141A (en) * | 2012-08-06 | 2012-10-31 | 浙江海拓环境技术有限公司 | Method for processing heavy metal nickel in stainless steel pickling mixed waste acid |
| CN102757142A (en) * | 2012-08-06 | 2012-10-31 | 浙江海拓环境技术有限公司 | Method for recycling and processing nickel in stainless steel pickling waste acid |
| KR20200077050A (en) * | 2018-12-20 | 2020-06-30 | 한국과학기술연구원 | A calcium ion extraction method in sludge generated during annealing and pickling process of stainless steel |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508541B (en) * | 2012-06-29 | 2015-08-19 | 中国科学院过程工程研究所 | A kind of method that heavy metal waste slag removing toxic substances, acid heavy metal wastewater resource utilization are reclaimed |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100916087B1 (en) * | 2002-08-30 | 2009-09-08 | 주식회사 포스코 | Method for neutralization of slag leachate |
| CN102757141A (en) * | 2012-08-06 | 2012-10-31 | 浙江海拓环境技术有限公司 | Method for processing heavy metal nickel in stainless steel pickling mixed waste acid |
| CN102757142A (en) * | 2012-08-06 | 2012-10-31 | 浙江海拓环境技术有限公司 | Method for recycling and processing nickel in stainless steel pickling waste acid |
| KR20200077050A (en) * | 2018-12-20 | 2020-06-30 | 한국과학기술연구원 | A calcium ion extraction method in sludge generated during annealing and pickling process of stainless steel |
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