KR100195579B1 - Method for treating waste water containing ammonia nitrogen - Google Patents

Method for treating waste water containing ammonia nitrogen Download PDF

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KR100195579B1
KR100195579B1 KR1019970006228A KR19970006228A KR100195579B1 KR 100195579 B1 KR100195579 B1 KR 100195579B1 KR 1019970006228 A KR1019970006228 A KR 1019970006228A KR 19970006228 A KR19970006228 A KR 19970006228A KR 100195579 B1 KR100195579 B1 KR 100195579B1
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ammonia
wastewater
nitrogen
ammonia nitrogen
present
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KR1019970006228A
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KR19980069249A (en
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황주오
정영조
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이광열
유니온물산주식회사
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/586—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing ammoniacal nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation

Abstract

본 발명은 암모니아성 질소를 함유한 폐수에 가성소다를 첨가하여 반응시킨 다음, 발생된 암모니아를 회수하는 것으로 이루어진 폐수의 처리방법에 관한 것이다.The present invention relates to a method for treating wastewater, which comprises reacting by adding caustic soda to wastewater containing ammonia nitrogen and then recovering the generated ammonia.

본 발명의 폐수 처리방법은 가성소다를 사용하므로서 전질소를 완전히 제거할 수 있으며 본 발명에 따라 처리된 폐수의 처리수를 방류하여도 암모니아성 질소에 의한 유해한 영향이 없다. 또한 처리과정에서 발생된 암모니아를 회수하여 재사용할 수 있으므로 산업적 이용성이 크다.The wastewater treatment method of the present invention can completely remove all nitrogen by using caustic soda and there is no harmful effect of ammonia nitrogen even when the treated water of the wastewater treated according to the present invention is discharged. In addition, the industrial availability is great because the ammonia generated in the process can be recovered and reused.

Description

암모니아성 질소를 함유한 폐수의 처리방법Method of treating wastewater containing ammonia nitrogen

본 발명은 암모니아성 질소(NH4 +-N)를 함유한 폐수의 처리방법에 관한 것이다. 보다 구체적으로 말하자면, 본 발명은 암모니아성 질소를 함유한 폐수에 가성소다를 첨가하여 반응시킨 다음, 발생된 암모니아를 회수하는 것으로 이루어진 폐수의 처리방법에 관한 것이다.The present invention relates to a method for treating wastewater containing ammoniacal nitrogen (NH 4 + -N). More specifically, the present invention relates to a method for treating wastewater consisting of reacting by adding caustic soda to wastewater containing ammonia nitrogen and then recovering the generated ammonia.

암모니아성 질소는 주로 아닐린(Aniline) 유도체의 제조공정에서 발생되며, 이러한 암모니아성 질소를 그대로 방류하면 부영양화를 초래하는 등 환경상 문제를 야기시킨다. 따라서 폐수 중에 질소의 제거가 요망되고 있으며, 이의 처리방법도 계속 연구되고 있는 실정이다.Ammonia nitrogen is mainly generated in the production process of aniline derivatives, and if the ammonia nitrogen is discharged as it is, it causes environmental problems such as eutrophication. Therefore, the removal of nitrogen in the waste water is desired, and the treatment method thereof is still being studied.

본 발명에서는 폐수 중에 가성소다를 첨가함으로써 암모니아성 질소와 반응하여 질소를 암모니아 가스 형태로 회수할 수 있다는 사실에 착안하여 본 발명을 완성하기에 이르렀다.The present invention has been completed by focusing on the fact that by adding caustic soda to the wastewater, the nitrogen can be recovered in the form of ammonia gas by reacting with ammonia nitrogen.

따라서, 본 발명의 목적은 암모니아 질소를 함유한 폐수에 가성소다를 첨가하여 반응시킨 다음, 발생된 암모니아를 회수하는 것으로 이루어진 폐수의 처리방법을 제공하는 것이다.It is therefore an object of the present invention to provide a method for treating wastewater consisting of adding caustic soda to a wastewater containing ammonia nitrogen and then reacting it to recover the generated ammonia.

제1도는 암모니아성 질소를 함유한 폐수를 발생하는 아닐린 유도체의 제조공정도.1 is a manufacturing process diagram of an aniline derivative for generating wastewater containing ammonia nitrogen.

제2도는 본 발명에 따른 폐수의 처리방법을 도시한 폐수처리 공정 개략도.2 is a schematic view of a wastewater treatment process showing a method of treating wastewater according to the present invention.

본 발명에 따른 폐수의 처리방법에서는 가성소다를 이용하는 것을 특징으로 한다.In the wastewater treatment method of the present invention, caustic soda is used.

본 발명에서 적용될 수 있는 폐수는 일 예로 염료, 안료, 자외선 방지제 등의 유기화학 제품의 중간체로서 광범위하게 이용되고 있는 아닐린 유도체의 제조공정에서 발생되는 폐수이다. 즉, 아닐린 유도체는 상업적으로 벤젠 유도체와 암모니아를 고온·고압에서 반응시켜 제조한다.Wastewater that can be applied in the present invention is wastewater generated in the manufacturing process of aniline derivatives that are widely used as an intermediate of organic chemical products such as dyes, pigments, UV protection agents. That is, aniline derivatives are commercially produced by reacting benzene derivatives with ammonia at high temperature and high pressure.

보다 구체적으로 말하자면, 아닐린 유도체(예, 오르토 니트로 아닐린(Ortho Nitro Aniline, ONA))는 다음 반응식에서 처럼 클로로벤젠 유도체를 암모니아와 반응시켜 얻어진다(참조 제1도):More specifically, aniline derivatives (e.g., Ortho Nitro Aniline, ONA) are obtained by reacting chlorobenzene derivatives with ammonia, as shown in the following scheme (see FIG. 1):

Figure kpo00002
Figure kpo00002

이 때 분말(고체)상태로 ONA 를 회수한 후의 폐액에는 미반응 암모니아와 염화암모늄을 포함하여 전질소(T-N)가 약 114,800PPM 함유되어 있다.At this time, the waste liquid after recovering ONA in a powder (solid) state contains approximately 114,800 PPM of total nitrogen (T-N) including unreacted ammonia and ammonium chloride.

이러한 암모니아성 질소, 특히 염화암모늄은 가성소다를 이용한 본 발명의 처리방법에 다음과 같이 제거될 수 있다.Such ammonia nitrogen, especially ammonium chloride, can be removed as follows in the treatment method of the present invention using caustic soda.

Figure kpo00003
Figure kpo00003

본 발명에서 사용된 가성소다는 어느 것이나 가능하나, 공업적으로 쉽게 얻을 수 있는 50% 가성소다를 사용하는 것이 바람직하다.Any of the caustic soda used in the present invention can be used, but it is preferable to use 50% caustic soda which can be easily obtained industrially.

가성소다의 사용량은 원활한 반응진행을 위해 염화암모늄의 양보다 대략 10%정도 과량으로 사용한다.Caustic soda is used in excess of approximately 10% of the amount of ammonium chloride to facilitate the reaction.

또한, 폐수의 본래 포함된 암모니아 및 가성소다와 반응에 의해 생성된 암모니아는 140℃ 이상의 온도로 가열하면 쉽게 회수될 수 있다.In addition, the ammonia produced by the reaction with the ammonia and caustic soda originally contained in the wastewater can be easily recovered by heating to a temperature of 140 ° C or higher.

본 발명의 처리방법을 제2도와 관련하여 설명하면 다음과 같다.The treatment method of the present invention will be described with reference to FIG.

우선 탈수기로부터 폐수를 탈수폐수 저장조로 이송하고, 이송된 폐수를 3ℓ 반응기에 투입하여 1차 반응시킨다(반응시간 3시간 온도 140℃). 1차 반응에 의해 암모니아 가스가 배출되면 암모니아 회수탱크로 방출하여 암모니아 가스를 회수한다. 그후 폐수는 3ℓ 반응기로 이송시켜 가성소다를 넣고 2차 반응시킨다. 2차 반응에서 발생된 암모니아 가스가 배출되면 암모니아 회수탱크로 방출하여 암모니아 가스를 회수하고, 잔류액은 처리액 탱크로 이송한 다음 방류시킨다. 암모니아 회수탱크에서 회수된 암모니아는 원료로 재사용한다.First, the wastewater is transferred from the dehydrator to the dehydration wastewater storage tank, and the transferred wastewater is introduced into a 3L reactor for first reaction (reaction time 3 hours temperature 140 ° C.). When the ammonia gas is discharged by the first reaction, the ammonia recovery tank is discharged to recover the ammonia gas. The wastewater is then transferred to a 3L reactor, caustic soda and second reaction. When the ammonia gas generated in the secondary reaction is discharged, it is discharged to the ammonia recovery tank to recover the ammonia gas, and the residual liquid is transferred to the treatment liquid tank and discharged. The ammonia recovered from the ammonia recovery tank is reused as raw material.

이하 본 발명을 실시예로서 설명하면 다음과 같으나, 본 발명이 이들 실시예에 국한하는 것으로 의도되지 않는다.Hereinafter, the present invention will be described as examples, but the present invention is not intended to be limited to these examples.

[실험예]Experimental Example

3ℓ 오토클레이브(Autoclave)에 오르토 니트로클로로벤젠(ONCB, Ortho Nitro Chloro Benzene) 500g을 투입하고 28% NH4OH 2,100㎖를 첨가한후 밀폐한 상태에서 승온시켜 170℃에서 8시간 반응시켰다. 반응완료후, NH3(암모니아)를 회수하고 40℃로 냉각한 다음 탈수한다. 탈수때 발생하는 폐수는 1,800㎖였다.500 g of ortho nitro chlorobenzene (ONCB, Ortho Nitro Chloro Benzene) was added to a 3 L autoclave, 2,100 ml of 28% NH 4 OH was added thereto, and the temperature was raised in a closed state and reacted at 170 ° C. for 8 hours. After completion of the reaction, NH 3 (ammonia) is recovered, cooled to 40 ° C., and dehydrated. Wastewater generated during dehydration was 1,800 ml.

암모니아성 질소에 대해 재단법인 일본식품분석센타로부터 폐수를 분석한 결과를 다음 표 1에 제시한다.The results of the wastewater analysis from the Japan Food Analysis Center for ammonia nitrogen are shown in Table 1 below.

Figure kpo00004
Figure kpo00004

[실시예]EXAMPLE

상기 실험예에서 탈수기로부터 분리된 폐수(1,800㎖)를 3ℓ용 반응기에 투입하고 밀폐한 후 가온하여 140℃로 승온한 다음 3시간동안 연장반응시킨 다음 암모니아 회수탱크로 암모니아 가스만을 방출하여 흡수시켜 회수하고(NH3, 144.2g), 잔류액(1,624.8g)에 50% 가성소다 41g을 투입한 다음 다시 가열하여 150℃까지 승온시켜 2시간동안 연장반응시킨 다음, 암모니아 회수탱크로 암모니아 가스를 방출하여 흡수시켜 회수하였다(NH3, 17.2g). 반응기에 남아 있는 처리완료액과 암모니아 회수액의 전질소량을 측정하였다.In the above experimental example, wastewater (1,800 ml) separated from the dehydrator was added to a reactor for 3 l, sealed, warmed, heated to 140 ° C., extended for 3 hours, and released by absorbing only ammonia gas into the ammonia recovery tank. (NH 3 , 144.2g), 50% caustic soda 41g was added to the residual liquid (1,624.8g), and heated again, the temperature was raised to 150 ° C, extended for 2 hours, and the ammonia recovery tank released ammonia gas. Absorbed and recovered (NH 3 , 17.2 g). The total nitrogen amount of the treated liquid remaining in the reactor and the ammonia recovery liquid were measured.

Figure kpo00005
Figure kpo00005

본 발명의 폐수 처리방법은 가성소다를 사용함으로써 전질소를 완전히 제거할 수 있으며 본 발명에 따라 처리된 폐수의 처리수를 방류하여도 암모니아성 질소에 의한 유해한 영향이 없다. 또한 처리 과정에서 발생된 암모니아를 회수하여 재사용할 수 있으므로 산업적 이용성이 크다.The wastewater treatment method of the present invention can completely remove all nitrogen by using caustic soda and there is no harmful effect of ammonia nitrogen even when the treated water of the wastewater treated according to the present invention is discharged. In addition, the ammonia generated in the treatment process can be recovered and reused, so the industrial utility is large.

Claims (1)

아닐린 유도체 제조시 발생되는 암모니아성 질소를 함유한 폐수의 처리방법에 있어서, 암모니아성 질소를 함유한 폐수에 가성소다를 첨가하여 반응시키고, 반응4중에 발생되는 암모니아 가스를 회수하여 폐수중에 암모니아성 질소를 제거시키는 암모니아성 질소 함유 폐수의 처리방법.In the method for treating wastewater containing ammonia nitrogen generated in the preparation of aniline derivatives, caustic soda is added to the wastewater containing ammonia nitrogen and reacted to recover the ammonia gas generated in the reaction 4 to recover the ammonia nitrogen in the wastewater. A method for treating ammonia-containing nitrogen containing wastewater, which removes water.
KR1019970006228A 1997-02-27 1997-02-27 Method for treating waste water containing ammonia nitrogen KR100195579B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100345728B1 (en) * 1997-12-16 2003-02-19 주식회사 포스코 Method for eliminating nitrogen compounds from coke wastewater using ammonia stripping
KR101326874B1 (en) 2007-12-24 2013-11-12 재단법인 포항산업과학연구원 Removing method for ammonia nitrogen in wastewater using blast furnace slag

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100345728B1 (en) * 1997-12-16 2003-02-19 주식회사 포스코 Method for eliminating nitrogen compounds from coke wastewater using ammonia stripping
KR101326874B1 (en) 2007-12-24 2013-11-12 재단법인 포항산업과학연구원 Removing method for ammonia nitrogen in wastewater using blast furnace slag

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