KR100318660B1 - Sewage treatment with fluorine and methods for treating wastewater using the same - Google Patents
Sewage treatment with fluorine and methods for treating wastewater using the same Download PDFInfo
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Abstract
본 발명은 불소가 다량 함유된 하폐수를 완벽하게 정화처리하여 배출할 수 있는 하폐수 처리제 및 그를 사용한 하폐수 처리방법에 대한 것으로, 분말상의 탄산마그네슘(MgCO3)과 탄산칼슘(CaCO3)이 각각 0.5∼2,5 중량부 및 97.5∼99.5 중량부 혼합되어 제조된 15-25%농도의 복합염 수용액 90∼99.9중량 부에, 붕사(Na2B4O7· 10H2O)가 0.1∼10중량 부 첨가된 혼합물로 이루어지는 하폐수 처리제를, 하폐수 원수에 일정량 첨가하여 0.5∼5시간동안 교반 및 폭기시키는 단계, 응집제를 투입하여 10분간 더 교반하는 단계, 상기 재차 교반시킨 후 반응물을 침전시켜 상등수 및 슬러지를 분리하여 배출하는 단계로 하폐수를 처리함으로써, 기존의 하폐수 처리방식과는 달리 간단한 절차에 의해 하폐수 내 통상의 유해성분에 더하여 불소까지도 제거할 수 있어, 경제적으로 유익하게 하폐수를 처리할 수 있게 된다.The present invention relates to a wastewater treatment agent capable of completely purifying and discharging wastewater containing a large amount of fluorine, and to a wastewater treatment method using the same, wherein powdered magnesium carbonate (MgCO 3 ) and calcium carbonate (CaCO 3 ) are 0.5 to 0.5, respectively. 0.1 to 10 parts by weight of borax (Na 2 B 4 O 7 · 10H 2 O) to 90 to 99.9 parts by weight of a mixed aqueous solution of 15-25% concentration prepared by mixing 2,5 parts by weight and 97.5 to 99.5 parts by weight. Adding a certain amount of the sewage treatment agent consisting of the added mixture to the raw sewage water, stirring and aeration for 0.5 to 5 hours, adding a flocculant and stirring for 10 minutes, stirring again, and then precipitating the reactant to precipitate supernatant and sludge. By treating wastewater in the stage of separating and discharging, unlike conventional wastewater treatment method, it is possible to remove fluorine in addition to the usual harmful components in wastewater by simple procedure. It is possible to advantageously process the sewage.
Description
본 발명은 불소(Fluorine)를 함유한 하폐수 처리제 및 그를 사용한 하폐수 처리방법에 관한 것으로, 보다 상세하게 말하면 하폐수 정화처리시 그 내에 다량 함유된 불소까지도 제거하여 수질 오염 없이 하폐수를 완벽하게 정수시켜 배출할 수 있는 불소를 함유한 하폐수 처리제 및 그를 사용한 하폐수 처리방법에 대한 것이다.The present invention relates to a wastewater treatment agent containing fluorine and a wastewater treatment method using the same. More specifically, the wastewater purification process removes even a large amount of fluorine contained therein to completely purify the wastewater without water pollution. The present invention relates to a wastewater treatment agent containing fluorine and a wastewater treatment method using the same.
요즈음은 생활하수나 산업용 폐수의 정화처리가 우리생활에 미치는 영향이 중대함을 인식하여 그 처리제 및 처리방법이 다양하게 개발되어 오고 있는데, 그중최근에 가장 적절한 방법으로 실시되고 있는 방식으로는 하폐수를 집수조에서 1-24 시간동안 pH 2-3 정도에서 폭기 처리한 다음 반응조에서 중화제로서 소석회(Ca(OH)2)나 수산화나트륨(NaOH)을 대략 5,000-10,000ppm 정도 투입하여 교반하면서 pH를 10-12로 상승시켜 0.5-2시간 동안 반응시킨 후 응집조에서 액반 이나 PAC(poly aluminium chloride), 염산, 황산 또는 불산저감제를 첨가하여 pH 7로 조정한 다음 적당한 고분자 응집제를 투여하여 하폐수를 정화처리하며 또한 하폐수내불소성분도 슬러지(sludge)상태로 응집시켜 배출해 오고 있다.Nowadays, we recognize that the treatment of domestic sewage and industrial wastewater has a significant impact on our lives, and various treatments and treatment methods have been developed. Among them, wastewater is currently being used in the most appropriate way. Aeration at pH 2-3 for 1-24 hours in the sump, and then add approximately 5,000-10,000 ppm of slaked lime (Ca (OH) 2 ) or sodium hydroxide (NaOH) as a neutralizing agent in the reactor and stir the pH to 10- After rising to 12 and reacting for 0.5-2 hours, the mixture was adjusted to pH 7 by adding liquid plate or PAC (poly aluminum chloride), hydrochloric acid, sulfuric acid, or hydrofluoric acid reducing agent, and then purified wastewater by administering appropriate polymer flocculant. In addition, fluorine in sewage water has been sludged and discharged.
그러나, 이러한 처리는 불소가 소량 함유되어 있을 경우에는 권장할 만하나 불소가 많이 섞여 배출되는 전자부품공장 등에서의 폐수의 경우에는 불소저감제를 투입함에도 불구하고 불소가 완전히 제거되지 못하고 불산으로 내재하게되어 처리된 폐수의 상등수의 pH 가 방류 기준(pH 5.8-8.5)을 넘으므로 재차 처리되어야 하며 또 슬러지 내에도 불소가 잔류하게 되므로 따로 그 제거 처리를 해야 하기에 번거롭고 비용이 많이 들뿐만 아니라 이러한 별도의 처리에서 조차도 불소의 완전한 제거가 불가능하여 큰 문제점이 내재하고 있었다.However, this treatment is recommended in the case of containing a small amount of fluorine, but in the case of wastewater from an electronic parts factory where a large amount of fluorine is discharged, fluorine is not completely removed but fluorine is inherently introduced in fluoric acid. The pH of the supernatant of the treated wastewater exceeds the discharge standard (pH 5.8-8.5), so it must be treated again and fluorine remains in the sludge. Even in the treatment of fluorine, the complete removal of fluorine was inherent, causing a great problem.
본 발명자들은 이 분야에 오래 동안 종사해 오면서 불소가 다량 함유된 하폐수도 완벽하게 정화시켜 산업발달로 인한 더 이상의 환경 오염을 유발하지 않도록 하기 위하여 세심한 주의와 지속적인 연구를 기울인 바, 기존의 방식과는 달리 간단한 절차와 저렴한 비용으로도 하폐수 내에 함유된 유해물질은 물론 불소도 효율적으로 제거할 수 있어 하폐수 정화시의 상기 문제점을 근본적으로 해결할 수 있는 처리제 및 그를 사용한 처리방법을 개발하게 되었다.The present inventors have been working in this field for a long time and have paid careful attention and continuous research to completely purify fluorine-containing sewage water so as not to cause further environmental pollution due to industrial development. It is possible to efficiently remove harmful substances contained in sewage water as well as fluorine even with a simple procedure and low cost, thereby developing a treatment agent and a treatment method using the same, which can fundamentally solve the above problems in waste water purification.
즉, 본 발명은 일반폐수는 물론 불소가 고도로 내포된 산업용 폐수에도 간단한 방식으로 거의 제로 수준으로 까지 불소를 제거하여 실제로 하폐수 정화를 완벽하게 실행할 수 있는 하폐수 처리제 및 처리방법을 제공하고자 의도된 것이다.That is, the present invention is intended to provide a wastewater treatment agent and a treatment method capable of completely performing wastewater purification by removing fluorine to almost zero levels in a simple manner in general wastewater as well as industrial wastewater in which fluorine is highly contained.
본 발명에 따르면 하폐수에 함유된 불소를 제거하기 위하여 분말상의 탄산마그네슘(MgCO3)과 탄산칼슘(CaCO3)이 각각 0.5∼2.5 중량부 및 97.5∼99.5 중량부 혼합되어 제조된 15-25%농도의 복합염 수용액 90∼99.9중량 부에 붕사(Na2B4O7·10H2O)가 0.1.∼10중량 부 첨가된 혼합물로 이루어지는 불소를 함유한 하페수 처리제를 제공하게 된다.According to the present invention, in order to remove fluorine contained in sewage water, 15-25% of magnesium magnesium carbonate (MgCO 3 ) and calcium carbonate (CaCO 3 ) are mixed by 0.5 to 2.5 parts by weight and 97.5 to 99.5 parts by weight, respectively. A fluorine-containing hape water treatment agent composed of a mixture in which 0.1 to 10 parts by weight of borax (Na 2 B 4 O 7 · 10H 2 O) is added to 90 to 99.9 parts by weight of a composite salt aqueous solution of the present invention is provided.
또한, 본 발명에 따르면 하폐수 원수에 상기 불소를 제거할 수 있는 하폐수 처리제를 일정량 첨가하여 0.5∼5시간동안 교반 및 폭기시키는 단계;In addition, according to the present invention, by adding a predetermined amount of sewage treatment agent capable of removing the fluorine to the raw water sewage, stirring and aeration for 0.5 to 5 hours;
응집제를 투입하여 10분간 더 교반하는 단계;Adding a flocculant and further stirring for 10 minutes;
교반시킨 후 반응물을 침전시켜 상등수 및 슬러지를 분리하여 배출하는 단계로 이루어지는 불소를 함유한 하폐수 처리방법을 제공하게 된다.After stirring, the reactant is precipitated to provide a fluorine-containing wastewater treatment method comprising separating and discharging the supernatant and sludge.
또한, 처리되는 하폐수의 양이 다량인 경우, 상기 교반 및 폭기 단계 후 산화란탄(La2O3) 0.01∼1중량%, 붕산(boric acid) 0.5∼2.5중량%와 산화알루미늄(Al2O3) 농도가 2∼7%인 액반, 2∼5%인 폐액반 또는 2∼17%인 PAC를 나머지 양으로 하여 이루어지는 역중화제에 의한 중화처리단계를 더 거치는 것이 바람직하다.In addition, when the amount of wastewater to be treated is a large amount, after the stirring and aeration step, 0.01 to 1% by weight of lanthanum oxide (La 2 O 3 ), 0.5 to 2.5% by weight of boric acid and aluminum oxide (Al 2 O 3). ) It is preferable to further carry out the neutralization step by the anti-neutralizing agent consisting of the remaining 2 to 7% liquid plate, the 2 to 5% waste plate or the 2 to 17% PAC as the remaining amount.
따라서, 역중화제로 하폐수를 더 처리함으로써 하폐수를 중화시켜 하폐수의 pH를 낮춤과 아울러 불산이 함유된 하폐수의 응집시 전리도를 상승시켜 미세 입자까지도 응집되도록 하여 응집성을 한층 향상시켜 주므로 불소의 농도를 상당히 낮춰 주게 된다. 적용되는 역중화제의 양은 상기 본 발명에 따른 처리제가 5000ppm(4.0㎖) 사용되었을 경우 대략 0.1㎖ 정도 또는 그 보다 약간 상회하나 이는 일률적으로 한정할 수 없으며 하폐수의 성상 및 양에 따라 가감될 수 있다.Therefore, by treating the wastewater further with a neutralizing agent, it neutralizes the wastewater and lowers the pH of the wastewater, and also increases the ionization degree during the flocculation of the wastewater containing hydrofluoric acid so that even fine particles are aggregated to improve the cohesiveness. Will be lowered. The amount of anti-neutralizing agent applied is about 0.1 ml or slightly higher when the treatment agent according to the present invention is used at 5000 ppm (4.0 ml), but this can not be limited uniformly and can be added or subtracted depending on the nature and amount of the wastewater.
하폐수내 유해성분의 입자를 응집시키기 위해 상기 투입되는 응집제는 통상의 비이온성, 음이온성, 양이온성 및 양쪽이온성의 것이 하폐수의 성상에 따라 적의 선정되어 사용되며, 그 투입량은 1㎖ 정도이나 응집되는 상태에 따라 추가적으로 완전히 응집될 때까지 조금씩 투여되므로, 일률적으로 한정될 수 없으며 하폐수량에 따라 약간씩 차이가 있다.The coagulant introduced to agglomerate particles of harmful constituents in the sewage water is generally selected from nonionic, anionic, cationic and zwitterionic ones according to the characteristics of the waste water, and the amount of the coagulant is about 1 ml. In addition, depending on the additional state is administered little by little until completely coagulated, can not be uniformly limited, there is a slight difference depending on the amount of wastewater.
상기 붕사는 탄산칼슘과 물과의 엉김 현상을 막는 분산제 및 불산의 반응을 촉진시키는 촉매 역할을 한다. 그러므로, 붕사의 양이 0.1중량 부 미만일 경우에는 탄산칼슘의 물과의 반응을 억제하는 작용이 미약하여 탄산칼슘의 불소등 기타 유해성분과의 반응에 앞서 물과 먼저 반응하여 고상의 응고물을 발생시키거나 하폐수처리제의 반응을 불안정하게 하므로 부적당하며, 또 상기 상한인 10중량 부를 상회하는 경우에는 비경제적일 뿐만 아니라 오히려 반응되지 않고 붕사가 슬러지 내에 잔존하므로 상기 범위 내에서 첨가되어야 한다. 또, 본 발명의 하폐수 처리제에서의 탄산칼슘과 탄산마그네슘과의 상기 복합염이 15%농도 미만일 경우에는 불소처리능력이 떨어지며 처리비용이 상승하며 25%농도를 넘을 경우에는 오히려 희석하여 사용하여야 하므로 상기 농도로 유지되어야 한다.The borax serves as a catalyst for promoting the reaction of the dispersant and hydrofluoric acid to prevent the entanglement of calcium carbonate and water. Therefore, when the amount of borax is less than 0.1 parts by weight, the action of inhibiting the reaction of calcium carbonate with water is weak, and reacts with water prior to the reaction of calcium carbonate with other harmful components such as fluorine to produce a solidified solid. In addition, the reaction of the sewage treatment agent is unstable, and if it exceeds the upper limit of 10 parts by weight, it is not only economically effective but rather unreacted and borax remains in the sludge and should be added within the above range. In addition, when the composite salt of calcium carbonate and magnesium carbonate in the sewage treatment agent of the present invention is less than 15% concentration, the fluorine treatment capacity is lowered and the treatment cost is increased. Should be maintained at concentration.
상술한 본 발명에 따른 하폐수 처리제에 의한 하폐수 정화시의 주요 반응기구는 대략 다음과 같다.The main reactor in the wastewater purification by the wastewater treatment agent according to the present invention described above is as follows.
2HF + CaCO3→ CaF2↓ + CO2+ H2O2HF + CaCO 3 → CaF 2 ↓ + CO 2 + H 2 O
2HF + MgCO3→ MgF2↓ + CO2+ H2O2HF + MgCO 3 → MgF 2 ↓ + CO 2 + H 2 O
이하, 본 발명을 보다 명확하게 이해할 수 있도록 하기 위해 실시례들을 들어 기술하나 본 발명은 이들 실시례에 한정되지 않고 수반된 특허청구의 범위 및 본 발명의 정신과 범주 내에서 그 정정 및 변형이 가능함은 본 분야에 숙지된 자들은 용이하게 이해될 것이다. (실시례에서의 부는 중량백분율을 나타낸다.)Hereinafter, the present invention will be described with reference to examples in order to more clearly understand the present invention, but the present invention is not limited to these examples, and modifications and variations are possible within the scope of the accompanying claims and the spirit and scope of the present invention. Those skilled in the art will readily understand. (Parts in the examples represent weight percentages.)
(실시례1)Example 1
먼저 본 발명의 하폐수 처리제를 만들기 위하여 분말상의 탄산마그네슘 1.5부와 탄산칼슘 98.5부를 잘 혼합하여 20%농도의 수용액으로 만들었다. 이 수용액 95부에 붕사를 5부 첨가하여 충분히 혼합하여 본 발명에 따른 하폐수 처리제를 제조하였다.First, 1.5 parts of powdered magnesium carbonate and 98.5 parts of calcium carbonate were mixed well to prepare a wastewater treatment agent of the present invention, thereby preparing an aqueous solution having a concentration of 20%. 5 parts of borax was added to 95 parts of this aqueous solution, and the mixture was sufficiently mixed to prepare a wastewater treatment agent according to the present invention.
pH가 2.56 이고 불소가 172.5(mg/ℓ)함유된 폐수를 각기 500㎖취하여(이하, 이를 원수로 함) 8개 반응조에 투입한 다음, 상기 제조된 본 발명의 하폐수 처리제를 3000ppm(2.4㎖) 및 5000ppm(4.0㎖) 씩을 취하여 각기 4군데씩 상기 원수가 담겨 있는 각 반응조에 첨가한 후 상온에서 교반 및 폭기시간을 다음과 같이 30분, 1시간, 3시간 및 5시간씩 각기 다르게 처리 하였다.500 ml of each wastewater containing pH of 2.56 and 172.5 (mg / l) (hereinafter referred to as raw water) were added to eight reactors, and then 3000 ppm (2.4 ml) of the wastewater treatment agent of the present invention prepared as described above. And 5000ppm (4.0ml) was added to each of the four reactors each place containing the raw water and then stirred and aeration time at room temperature was treated differently for 30 minutes, 1 hour, 3 hours and 5 hours as follows.
그 다음, 이들 처리 원수를 각각 응집조로 보내 동일한 반응성의 응집제를 1 ㎖씩 각기 투입하여 일률적으로 10분간 반응시킨 후 침전조에서 4시간동안 침전시켰다. 그 후 상등수를 취하여 그내에 함유된 불소함량을 각기 조사 해 보았다.Then, each of these treated raw water was sent to a flocculation tank, and 1 ml of the same reactive flocculant was added to each of them to react for 10 minutes uniformly, and then precipitated in the precipitation tank for 4 hours. After that, the supernatant was taken and the fluorine content contained therein was examined.
그 시험 결과를 다음 표1에 나타낸다.The test results are shown in Table 1 below.
(실시례2)Example 2
산화란탄 0.08% 및 붕산 1.5%에, 산화알루미늄 농도가 5%인 액반을 전체 100% 가 되도록 일정랑 첨가하여 역중화제를 별도로 준비하였다.The anti-neutralizer was separately prepared by adding a predetermined amount of bantan oxide to 0.08% and boric acid to 1.5% so that a liquid plate having an aluminum oxide concentration of 5% was 100% in total.
그런 다음, 상기 실시례1과 동일한 성상의 원수를 4개의 반응조에 투입하고 거기에 상기 실시례1에서와 동일한 방식으로 제조된 본 발명의 하폐수처리제를 5,000ppm(4.0㎖)씩 각기 첨가하여 상기 실시례1과 동일하게 교반 및 폭기시켰다.Then, the raw water having the same properties as in Example 1 was added to four reactors, and the wastewater treatment agent of the present invention prepared in the same manner as in Example 1 was added thereto by 5,000 ppm (4.0 ml), respectively. It stirred and aerated in the same manner as in Example 1.
그 후, 이 원수에 상기 준비된 역중화제를 0.1㎖, 0.12㎖, 0.2㎖ 및 0.3㎖씩 각기 첨가하여 20분간 더 반응시킨 다음 상기 실시례1에서와 동일한 조건하에서 동일한 후속 절차에 의해 처리하였다. 그 결과, 다음 표2에 나타난 바와 같이 상등수내에 함유된 불소의 양은 상기 실시례1에서 보다 상당히 줄어들었음을 알 수 있었다.Thereafter, 0.1 mL, 0.12 mL, 0.2 mL and 0.3 mL of the prepared anti-neutralizing agent were added to the raw water, and further reacted for 20 minutes, followed by the same subsequent procedure under the same conditions as in Example 1 above. As a result, as shown in Table 2, it was found that the amount of fluorine contained in the supernatant water was significantly reduced than in Example 1.
이상과 같이 본 발명에 의한 하페수 처리제 및 처리방법에 따르면, 기존의 하폐수 처리방식과는 달리 간단한 절차에 의해 하폐수를 거의 완벽하게 정화시켜 주므로 하폐수 내 통상의 유해성분에 더하여 불소처리를 위한 재차 별도의 처리공정을 거치지 않고도 바로 방출이 가능하여 수월하게 하폐수를 처리하면서도 그 내에 함유된 불소 양을 대폭 줄일 수 있어, 경제적으로 유익하게 하폐수를 처리할 수 있게 된다.As described above, according to the wastewater treatment agent and treatment method according to the present invention, unlike the conventional wastewater treatment method, since the wastewater is almost completely purified by a simple procedure, in addition to the usual harmful components in the wastewater, it is separately separated for fluorine treatment. It can be discharged immediately without going through the treatment process, so that the wastewater can be easily treated, but the amount of fluorine contained therein can be greatly reduced, and the wastewater can be treated economically.
다시 말해, 하폐수의 COD농도를 기준치이하로 낮추며 유해성분중 중금속까지도 제거함과 동시에 불소도 완전히 제거시켜 PH를 거의 중성수준으로 낮춰 주게 된다.In other words, it lowers the COD concentration of sewage water to below the standard value, removes heavy metals among harmful components and completely removes fluorine, thereby lowering the pH to almost neutral level.
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| JPH0857486A (en) * | 1994-06-16 | 1996-03-05 | Kankyo Eng Kk | Method for treating waste water containing fluorine |
| JPH09225477A (en) * | 1996-02-20 | 1997-09-02 | Nippon Steel Corp | Treatment of fluorine-containing waste water |
| JPH10263532A (en) * | 1997-03-27 | 1998-10-06 | Nec Corp | Treatment of fluorine-containing waste water |
| KR19990038900A (en) * | 1997-11-07 | 1999-06-05 | 한필순 | Wastewater treatment method containing heavy metals using calcium and magnesium |
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| JPH0857486A (en) * | 1994-06-16 | 1996-03-05 | Kankyo Eng Kk | Method for treating waste water containing fluorine |
| JPH09225477A (en) * | 1996-02-20 | 1997-09-02 | Nippon Steel Corp | Treatment of fluorine-containing waste water |
| JPH10263532A (en) * | 1997-03-27 | 1998-10-06 | Nec Corp | Treatment of fluorine-containing waste water |
| KR19990038900A (en) * | 1997-11-07 | 1999-06-05 | 한필순 | Wastewater treatment method containing heavy metals using calcium and magnesium |
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