KR100225671B1 - A waste water treating method from methylamine manufacturing process using organic compound separation method - Google Patents

A waste water treating method from methylamine manufacturing process using organic compound separation method Download PDF

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KR100225671B1
KR100225671B1 KR1019970031334A KR19970031334A KR100225671B1 KR 100225671 B1 KR100225671 B1 KR 100225671B1 KR 1019970031334 A KR1019970031334 A KR 1019970031334A KR 19970031334 A KR19970031334 A KR 19970031334A KR 100225671 B1 KR100225671 B1 KR 100225671B1
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wastewater
organic matter
manufacturing process
methylamine
raw material
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KR19990009069A (en
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박종현
최윤기
홍광표
박형담
김해연
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박영구
삼성정밀화학주식회사
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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
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

본 발명은 폐수중 유기물을 제거하는 공정기술에 관한 것으로써, 더욱 상세하게는 메틸아민 제조 공정에서 나오는 폐수를 증류하여, 저비점 유기물은 분리 회수하여 반응의 원료로 재사용하고, 유기물이 제거된 폐수는 생물학적 방법으로 처리함으로써, 폐수내의 유기물을 제거시켜 생물학적 처리장의 부하를 감소시키는 공정에 관한 것이다.The present invention relates to a process technology for removing organic matter from wastewater, and more particularly, distilled wastewater from methylamine manufacturing process, low-boiling organic matter is separated and recovered and reused as a raw material for the reaction, and wastewater from which organic matter is removed By treating by a biological method, the present invention relates to a process for removing organic matter in wastewater, thereby reducing the load on the biological treatment plant.

Description

유기물 분리공정을 이용한 메틸아민 제조 폐수 처리공정{A waste water treating method from methylamine manufacturing process using organic compound separation method}A waste water treating method from methylamine manufacturing process using organic compound separation method

본 발명은 폐수중 유기물을 제거하는 공정기술에 관한 것으로써, 더욱 상세하게는 메틸아민 제조 공정에서 나오는 폐수를 증류하여, 저비점 유기물은 분리 회수하여 반응의 원료로 재사용하고, 유기물이 제거된 폐수는 생물학적 방법으로 처리함으로써, 폐수내의 유기물을 제거시켜 생물학적 처리장의 부하를 감소시키는 공정에 관한 것이다.The present invention relates to a process technology for removing organic matter from wastewater, and more particularly, distilled wastewater from methylamine manufacturing process, low-boiling organic matter is separated and recovered and reused as a raw material for the reaction, and wastewater from which organic matter is removed By treating by a biological method, the present invention relates to a process for removing organic matter in wastewater, thereby reducing the load on the biological treatment plant.

메틸아민 제조공정에서 발생되는 폐수는 증류탑 2(6b) 및 증류탑 3(6c)에서 메틸아민류의 추출수로 쓰였던 물로서 조성은 메틸아민류 0.1~0.2 중량%, 메탄올 0.4∼1.0 중량%, 물이 대부분으로 98.8∼99.2 중량%인 폐수으로 저비점 유기물이 많이 포함되어 있는 폐수이다.The wastewater generated in the methylamine manufacturing process is water used for extraction of methylamines in distillation column 2 (6b) and distillation column 3 (6c). The composition is 0.1 to 0.2 wt% of methylamines, 0.4 to 1.0 wt% of methanol, and most of water It is 98.8 ~ 99.2% by weight wastewater, which contains a lot of low-boiling organic matter.

종래에는 상기 폐수를 처리하기 위해 폐수 전량을 생물학 방법으로 처리하였는데, 저비점 유기물의 함유량이 높아서 다량의 용수로 희석시켜야하고, pH를 조절해야하는 등 생물학 처리장의 부하를 가중시켰다. 또한 미반응된 원료뿐 아니라, 일부 제품까지도 추출수에 포함되어 나가는 등의 문제점이 있었다.Conventionally, in order to treat the wastewater, the whole amount of wastewater was treated by a biological method, and the content of low-boiling organic matter was high, so that it was diluted with a large amount of water and the pH of the biological treatment plant was increased. In addition, not only unreacted raw materials, but also some of the products contained in the extract water there was a problem.

이와 같은 폐수 발생공정을 첨부 도면 제1도에 도시하였으며, 그 공정을 상세히 설명하면 다음과 같다.Such wastewater generating process is shown in FIG. 1 of the accompanying drawings, and the process will be described in detail as follows.

원료인 메탄올(8)과 암모니아액(12), 리사이클된 메틸아민(14,15)이 원료예열기 1 및 2(1a,1b)와 열교환기 1 및 2(2a,2b)를 거쳐 반응기로 들어가서, 제품 제조시 모노메틸아민, 디메틸아민, 트리메틸아민의 세종류의 메틸아민이 생성된다. 이들은 여러개의 증류탑을 거치면서 각각의 제품으로 정제된다. 이때 증류탑 2(6b)에서 트리메틸아민과 디메틸아민, 모노메틸아민을 분리하기 위해 물(15)을 투입한다. 물에 대한 용해도가 비교적 낮은 트리메틸아민은 증류되어 나가고 나머지의 메틸아민은 물에 용해되어 다음단계의 증류탑으로 넘어간다. 증류탑 3(6c)에서 모노메틸아민과 디메틸아민은 증류하여 회수하고 추출수(16)는 폐수로 발생된다. 이때 폐수로 발생된 추출수는 고온이므로 원료예열기를 거치면서 원료를 승온시켜주고, 자신의 온도를 낮춘 후 배출된다. 이때 발생되는 폐수에는 완전히 증류되지 않은 유기물들이 많이 포함되어 있음에도 바로 폐수처리장으로 보내지므로 폐수처리장의 부하를 가중시키고, 처리비용 또한 높아지게 했다. 따라서 폐수처리장의 부하를 줄이고 폐기되는 원료 등의 회수를 위해 저비점 유기물의 분리 회수 공정의 기술확보가 절실히 필요하게 되었다.The raw material methanol (8), ammonia liquid (12), and recycled methylamine (14, 15) enter the reactor through raw material preheaters 1 and 2 (1a, 1b) and heat exchangers 1 and 2 (2a, 2b), Three kinds of methylamines are produced in the production of the product: monomethylamine, dimethylamine and trimethylamine. They are purified into individual products through several distillation columns. At this time, water (15) is added to separate trimethylamine, dimethylamine, and monomethylamine in distillation column 2 (6b). Trimethylamine, which has a relatively low solubility in water, is distilled off and the remaining methylamine is dissolved in water and passed to the next distillation column. In distillation column 3 (6c), monomethylamine and dimethylamine are recovered by distillation and the extract water 16 is generated as wastewater. At this time, the extracted water generated by the waste water is a high temperature, so that the raw material is heated while passing through the raw material preheater, and is discharged after lowering its temperature. The wastewater generated is sent directly to the wastewater treatment plant, even though it contains a lot of organic materials that are not completely distilled, thus increasing the load on the wastewater treatment plant and increasing the treatment cost. Therefore, in order to reduce the load of the wastewater treatment plant and recover the waste materials, there is an urgent need to secure the technology of the separate recovery process of the low-boiling organic matter.

따라서 본 발명에서는 상기의 문제점을 해결하고자 메틸아민 제조 공정에서 발생되는 폐수를 증류함으로써, 저비점 유기물은 다시 회수하여 반응의 원료로 사용하고, 유기물이 제거된 폐수는 생물학적 방법으로 쉽게 처리하도록 하는데 목적이 있다.Therefore, in the present invention, to solve the above problems, by distilling the wastewater generated in the methylamine manufacturing process, the low-boiling organic matter is recovered and used as a raw material of the reaction, and the wastewater from which the organic matter is removed is easily treated by a biological method. have.

제1도는 메틸아민 제조공정중 유기물 분리공정의 도입전 공정개략도.1 is a process schematic diagram before the introduction of the organic material separation process in the methylamine manufacturing process.

제2도는 메틸아민 제조공정중 본 발명의 유기물 분리공정의 도입후 공정개략도.2 is a process schematic diagram after the introduction of the organic material separation process of the present invention in the methylamine manufacturing process.

* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings

1a : 원료예열기 1, 1b : 원료예열기1a: raw material preheater 1, 1b: raw material preheater

1, 2b : 열교환기 1, 6b : 증류탑1, 2b: heat exchanger 1, 6b: distillation column

2, 2a : 열교환기 2, 3 : 반응기2, 2a: heat exchanger 2, 3: reactor

2, 6c : 증류탑 3, 6d : 증류탑2, 6c: distillation column 3, 6d: distillation column

4 : 가스쿨러 4, 7 : 암모니아4: gas cooler 4, 7: ammonia

5 : 가스세퍼레이트 6a : 증류탑5: gas separator 6a: distillation column

8 : 메탄올 9 : 리사이클 트리메틸아민(TMA)8: methanol 9: recycled trimethylamine (TMA)

10 : 리사이클 모노메틸아민(MMA) 11 : 합성가스10: recycled monomethylamine (MMA) 11: synthesis gas

12 : 암모니아액 13 : 합성원료12: ammonia liquid 13: synthetic raw materials

14 : 제품 디메틸아민(DMA) 15 : 물14 product dimethylamine (DMA) 15 water

16 : 추출수 17 : 배출수16: extract water 17: discharge water

18 : 스트립퍼 19 : 저비점 유기물18: stripper 19: low boiling organic matter

20 : 폐수 21 : 리사이클 탱크20: wastewater 21: recycling tank

22 : 리사이클 원료22: recycled raw materials

따라서 본 발명은 메틸아민 제조공정시 발생되는 폐수를 처리함에 있어서, 제조공정에서 생성되는 폐수(17)를 스트립퍼(18)를 통과시켜 저비점 유기물을 분리 회수하고, 분리 회수된 저비점 유기물(19)과 리사이클된 아민류가 합쳐져 원료로 투입시키고, 폐수에서 저비점 유기물이 제거된 처리액(20)을 생물학적 처리장으로 이송시켜 처리함을 특징으로 하는 폐수 처리공정에 관한 것이다. 이때 상기 스트립퍼(18)는 직접 수증기법을 사용함을 특징으로 한다.Therefore, in the present invention, in treating the wastewater generated during the methylamine manufacturing process, the wastewater 17 generated in the manufacturing process is passed through the stripper 18 to separate and recover the low boiling point organic matter, and the separated and recovered low boiling point organic matter 19 and The recycled amines are combined to be added as raw materials, and the wastewater treatment process is characterized in that the treatment liquid 20 from which low-boiling organic matter is removed from the wastewater is transferred to a biological treatment plant for treatment. At this time, the stripper 18 is characterized by using a direct steam method.

이하 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail.

본 발명은 메틸아민 제조공정시 발생되는 폐수에서 저비점 유기물을 분리 회수하는 스트립퍼(18)와; 분리 회수된 저비점 유기물과 리사이클된 아민류가 합쳐져서 원료로 투입되는 리사이클 탱크를 포함하는 구성으로 이루어져서 상기 폐수(17)에서 저비점 유기물을 분리 회수하고, 유기물이 제거된 액은 생물학 처리장으로 보내는 공정에 있다. 특히, 원료예열기를 거쳐 나오는 폐수(17)에서 저비점 유기물을 분리 회수하기 위한 스트립퍼(18)를 가지는 것을 본 발명의 특징으로 한다.The present invention provides a stripper (18) for separating and recovering low-boiling organic matter from wastewater generated during the methylamine manufacturing process; The low boiling point organic matter and the recycled amines which are separated and recovered are combined to include a recycling tank which is added as a raw material. The low boiling point organic matter is separated and recovered from the waste water 17, and the organic matter is removed to a biological treatment plant. In particular, it is a feature of the present invention to have a stripper 18 for separating and recovering low-boiling organics from the wastewater 17 passing through the raw material preheater.

이와 같은 본 발명이 유기물의 분리 회수 및 폐수 처리공정을 첨부된 제2도에 의하여 상세히 설명하면 다음과 같다.When the present invention as described above is described in detail by the accompanying Figure 2 recovery and wastewater treatment process as follows.

원료예열기를 거쳐 나온 폐수는 폐수 주입라인을 통해 스트립퍼(18)로 들어간다. 스트립퍼에서 압력 5kg/㎠, 상부온도 110∼120℃, 하부온도 150∼155℃의 조건하에 직접 수증기법으로 유기물을 분리 회수한다. 이때 메탄올과 일부 메틸아민류가 물과의 끓는 점 차이가 크므로 대부분은 증류되어 회수된다. 저비점 유기물이 대부분 제거된 나머지 폐수는 생물학 처리장을 보내진다. 분리되어 회수된 저비점 유기물은 냉각을 거치지 않고 고온을 유지하면서 리사이클 탱크(21)로 보내진다. 리사이클 탱크(21)에서 리사이클된 모노메틸아민(MMA), 트리메틸아민(TMA)(9,10)와 합쳐져서 원료인 메탄올과 다시 반응기로 이송된다.Wastewater from the raw material preheater enters the stripper 18 through the wastewater injection line. The stripper is separated and recovered by direct steam method under the conditions of a pressure of 5 kg / cm 2, an upper temperature of 110 to 120 ° C., and a lower temperature of 150 to 155 ° C. At this time, since the boiling point difference between methanol and some methylamines is large, most are distilled and recovered. Most of the low-boiling organics are removed, and the wastewater is sent to biological treatment plants. The low boiling point organic matter separated and recovered is sent to the recycling tank 21 while maintaining a high temperature without undergoing cooling. The recycled tank 21 is combined with the recycled monomethylamine (MMA) and trimethylamine (TMA) (9, 10), and is transferred back to the reactor with methanol as a raw material.

본 발명은 메틸아민 제조공정에서 발생되는 폐수를 스트립핑의 방법으로 유기물을 제거시킴으로써, 생물학 처리장의 부하를 감소시키고, 폐기되던 원료를 재사용함으로써 환경오염을 줄일 뿐 아니라 공정의 경제성을 높이는 효과를 가져왔다.The present invention removes organic matter by stripping the wastewater generated in the methylamine manufacturing process, thereby reducing the load on the biological treatment plant and reusing waste materials, thereby reducing environmental pollution and improving the economics of the process. come.

상기 과정에 있어서 스트립핑이 잘 이루어질 경우, 발생되는 원폐수의 COD가 7,000∼10,000 ppm 이던 것이 200 ppm 이하로 낮아졌다. 또한 리사이클 되는 원료의 양은 순수한 원료의 약 2%에 달한다.When stripping was well performed in the above process, the COD of the generated wastewater was lowered to 200 ppm or less from 7,000 to 10,000 ppm. In addition, the amount of recycled raw materials amounts to about 2% of pure raw materials.

본 발명을 실시예에 의하여 상세히 설명하면 다음과 같다. 그러나 본 발명이 실시예에 의해 한정되는 것은 아니다.The present invention will be described in detail by way of examples. However, the present invention is not limited by the examples.

[실시예]EXAMPLE

메틸아민 제조공정에서 나오는 폐수가 아래의 표 1과 같은 조성을 가질 때 제2도에서의 공정과 같이 스트립퍼 조건, 압력 5kg/㎠, 상부온도 110∼120℃, 하부온도 150∼155℃에서 직접 수증기법으로 유기물을 분리 회수한다. 공정을 거친 후의 성분과 COD에 관한 결과는 다음의 표 2와 같다.When the wastewater from the methylamine manufacturing process has the composition shown in Table 1 below, the steam method is applied directly under stripper conditions, pressure 5kg / ㎠, upper temperature 110-120 ℃ and lower temperature 150-155 ℃ as in the process of FIG. Organic matter is separated and recovered. The result of the component and COD after the process is shown in Table 2 below.

[표 1]TABLE 1

폐수의 조성Composition of wastewater

Figure kpo00002
Figure kpo00002

[표 2]TABLE 2

분리된 저비점 유기물과 처리된 폐수의 조성Composition of Separated Low Boiling Organics and Treated Wastewater

Figure kpo00003
Figure kpo00003

본 발명에서 바로 폐수처리장으로 보내지던 폐수중의 유기물을 스트립핑을 이용하여 분리 회수하여 재사용하고, 유기물이 제거된 폐수를 생물학 처리함으로써 폐수처리장의 부하를 감소시키고, 원료이 재사용에 따른 경제적 효과를 얻고, 폐수 처리의 효율을 높여 폐액 처리비용 절감 효과가 있음을 알 수 있다.In the present invention, the organic matter in the wastewater, which is directly sent to the wastewater treatment plant, is recovered and reused by stripping, and the biological treatment of the wastewater from which the organic matter is removed reduces the load on the wastewater treatment plant, and obtains the economic effect of reusing raw materials. In addition, it can be seen that the efficiency of wastewater treatment is increased, thereby reducing the cost of treating wastewater.

Claims (2)

메틸아민 제조공정시 발생되는 폐수를 처리함에 있어서, 제조공정에서 생성되는 폐수(17)를 스트립퍼(18)를 통과시켜 저비점 유기물을 분리 회수하고, 분리 회수된 저비점 유기물(19)과 리사이클된 아민류가 합쳐져 원료로 투입시키고, 폐수에서 저비점 유기물이 제거된 처리액(20)을 생물학적 처리장으로 이송시켜 처리함을 특징으로 하는 폐수 처리공정.In treating the wastewater generated in the methylamine manufacturing process, the wastewater 17 generated in the manufacturing process is passed through a stripper 18 to separate and recover the low boiling organic matter, and the separated and recovered low boiling organic matter 19 and the recycled amines are Combined and introduced into the raw material, the wastewater treatment process characterized in that the treatment liquid 20 is removed from the wastewater to remove the boiling point organic matter to a biological treatment plant. 제1항에 있어서, 상기 스트립퍼(18)는 직접 수증기법을 사용함을 특징으로 하는 폐수중 처리공정.The process according to claim 1, wherein the stripper (18) uses a direct steam method.
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