KR20030018474A - Solvent recovery facility by the combination of extraction and distillation - Google Patents
Solvent recovery facility by the combination of extraction and distillation Download PDFInfo
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- KR20030018474A KR20030018474A KR1020010052579A KR20010052579A KR20030018474A KR 20030018474 A KR20030018474 A KR 20030018474A KR 1020010052579 A KR1020010052579 A KR 1020010052579A KR 20010052579 A KR20010052579 A KR 20010052579A KR 20030018474 A KR20030018474 A KR 20030018474A
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- 239000002904 solvent Substances 0.000 title claims abstract description 109
- 238000000605 extraction Methods 0.000 title claims abstract description 107
- 238000004821 distillation Methods 0.000 title claims abstract description 54
- 238000011084 recovery Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000002351 wastewater Substances 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 14
- 230000005484 gravity Effects 0.000 claims abstract description 11
- 238000007670 refining Methods 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 54
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- 238000001704 evaporation Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- 229940113088 dimethylacetamide Drugs 0.000 description 2
- 239000002649 leather substitute Substances 0.000 description 2
- 239000010887 waste solvent Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IYWCBYFJFZCCGV-UHFFFAOYSA-N formamide;hydrate Chemical compound O.NC=O IYWCBYFJFZCCGV-UHFFFAOYSA-N 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- -1 that is Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
추출법과 증류법을 병용한 용제회수방법이 개시된다. 그러한 용제회수방법은 물보다 비중이 높은 추출용매와 용제가 함유된 폐수를 추출탑에 유입시켜 추출에 의하여 추출액은 하부로 배출하고, 추잔액은 상부로 배출하는 추출단계와, 상기 추출탑을 거친 추출액을 증류탑에 유입시켜 증류시킴으로서 추출용매는 상부로 배출하고, 용제는 하부로 분리하는 증류단계와, 상기 증류탑에서 분리된 용제를 정제탑에 유입시켜 정제하여 회수하는 정제단계와, 그리고 상기 추출탑에서 배출되는 추잔액에 함유된 추출용매와 증류탑에서 발생된 추출용매를 회수하여 추출용매탱크에 저장하는 추출용매회수단계를 포함한다.Disclosed is a solvent recovery method using an extraction method and a distillation method. In such a solvent recovery method, the wastewater containing the extraction solvent and the solvent having a higher specific gravity than the water is introduced into the extraction tower, and the extraction liquid is discharged to the bottom by the extraction, and the extraction liquid is discharged to the top. The extraction solvent is discharged to the top by distillation by introducing the extract into the distillation column, and the distillation step of separating the solvent to the bottom, the purification step of refining and recovering the solvent separated from the distillation column into the purification tower, and the extraction tower And an extracting solvent recovery step of recovering the extraction solvent contained in the extract residue discharged from the distillation column and storing the extraction solvent generated in the extraction solvent tank.
Description
본 발명은 수용성 용제가 다량 함유된 폐수(수용성 폐용제)로부터 용제를 회수하는 방법에 관한 것으로, 더욱 상세하게는 용제 회수율을 높이면서 용제회수에 사용되는 에너지를 최소화 할 수 있는 용제회수방법에 관한 것이다.The present invention relates to a method for recovering a solvent from waste water (aqueous waste solvent) containing a large amount of water-soluble solvent, and more particularly, to a solvent recovery method capable of minimizing energy used for solvent recovery while increasing solvent recovery rate. will be.
일반적으로 유기 용제는 여러 산업 분야에서 제품의 가공·생산을 위해 널리 사용된다. 특히 합성피혁, 합성 섬유 제조 공정에서는 원료로 사용되는 폴리우레탄수지의 용제로 디메틸 포름아미드(DMF;Dimethyl Formamide; 이하, DMF), 디메틸 아세트아미드(DMAC;Dimethyl Acetamide; 이하, DMAC)등이 사용되며 원가 절감 및 환경 보전을 위해서도 사용된 유기 용제는 회수하여 다시 사용할 필요가 있다.In general, organic solvents are widely used for processing and production of products in various industries. Particularly in the manufacturing process of synthetic leather and synthetic fiber, dimethyl formamide (DMF), dimethyl acetamide (DMAC), etc. are used as solvents for polyurethane resins used as raw materials. Organic solvents used for cost reduction and environmental conservation also need to be recovered and reused.
일예로 습식 폴리우레탄 합성피혁 제조공정에서 사용된 DMF 용제는 물로 세정되며 세정수 속에 DMF가 녹아 폐수로 배출된다. 이 폐수 중의 DMF(약 15% 함유)는 지금까지 증류법으로 재생 회수되어 왔다.For example, the DMF solvent used in the wet polyurethane synthetic leather manufacturing process is washed with water, and DMF is dissolved in the washing water and discharged into the wastewater. DMF (containing about 15%) in this wastewater has been recovered by distillation until now.
도1 에는 이러한 증류법에 의한 용제 회수방법이 도시된다. 도시된 바와 같이, 증류법에 의한 용제회수 시스템은 제1 및 제2 증류탑(1,2), 그리고 정제탑(3)으로 이루어진다.1 shows a solvent recovery method by such a distillation method. As shown, the solvent recovery system by distillation consists of first and second distillation towers (1, 2), and a purification tower (3).
이러한 용제 회수 시스템에 있어서, 폐수가 상기 제1 증류탑(1)으로 유입되면 폐수중의 용제 DMF는 물과 반응하여 가수분해 반응을 일으키므로 개미산이 필수적으로 생성되며, 이러한 개미산은 DMF와 공비 혼합물을 만들게 된다. 따라서, 제2 증류탑(2)에서 공비 혼합물을 처리하며, 처리된 공비 혼합물은 최종적으로 정제탑(3)으로 공급되어 용제를 분리하게 된다.In such a solvent recovery system, when the wastewater flows into the first distillation column (1), the solvent DMF in the wastewater reacts with water to cause a hydrolysis reaction, and thus formic acid is essentially generated, and such formic acid forms an azeotropic mixture with DMF. Will be made. Therefore, the azeotropic mixture is treated in the second distillation column 2, and the treated azeotropic mixture is finally supplied to the purification tower 3 to separate the solvent.
그러나, 이러한 증류법에 의한 용제 회수 방법은 증류를 위해 열원이 필요하며 증발잠열이 높은 물을 증발시키기 위한 에너지 소모가 많은 문제점을 가지고 있다.However, the solvent recovery method by the distillation method has a problem that requires a heat source for distillation and energy consumption for evaporating the high latent heat of evaporation.
또한, 고온에서 증류탑이 운전되므로 물과 용제가 반응하는 가수 분해 반응이 일어나는 경우, 일부 용제가 분해되어 부산물이 생성되기 때문에 회수율이 떨어지고 제품의 순도가 떨어지는 문제점이 있다.In addition, when the distillation column is operated at a high temperature, when a hydrolysis reaction occurs in which water and a solvent react, there is a problem in that a recovery rate is lowered and product purity is lowered because some solvents are decomposed to produce by-products.
그리고, 다량의 물(약 85% 함유)을 증류법에 의해 분리하므로 에너지 소비가 많은 결점을 가지고 있는데, 이를 개선하기 위하여 제1증류탑에서 나온 증기를 제2증류탑의 재가열 열원으로 사용하는 2중 효용 증류법이 주로 적용되어 에너지 소비를 줄여주고 있으나 대략 15% DMF 폐수 1톤을 처리하는데 1.1톤 정도의 스팀을 사용하여야 하므로 에너지 절약 측면에서 볼 때 만족스러운 결과를 얻지 못하고 있는 실정이다.In addition, since a large amount of water (containing about 85%) is separated by a distillation method, energy consumption has a drawback, and a double-effect distillation method using steam from the first distillation tower as a reheating heat source for the second distillation column is used to improve this. This is mainly applied to reduce energy consumption, but since 1.1 tonnes of steam must be used to treat 1 tonne of 15% DMF wastewater, satisfactory results are not obtained in terms of energy saving.
따라서, 본 발명은 이러한 문제점을 극복하기 위하여 안출된 것으로서, 본 발명의 목적은 용제와 물의 가수분해 반응에 의한 부산물의 생성을 억제하여 회수율을 높이고, 에너지 사용량을 대폭 줄일 수 있는 용제 회수 방법을 제공하는데 있다.Accordingly, the present invention has been made to overcome these problems, an object of the present invention is to provide a solvent recovery method that can suppress the production of by-products by the hydrolysis reaction of the solvent and water to increase the recovery rate, significantly reducing the energy consumption It is.
도1 은 종래기술에 따른 용제 회수 공정을 설명하기 위한 도면.1 is a view for explaining a solvent recovery process according to the prior art.
도2 는 본 발명의 바람직한 실시예에 따른 용제 회수 방법을 설명하기 위한 도면.2 is a view for explaining a solvent recovery method according to a preferred embodiment of the present invention.
도3 은 용제를 회수하는 과정을 단계별로 도시하는 순서도.3 is a flow chart showing step by step the process of recovering the solvent.
상기와 같은 목적을 달성하기 위하여, 본 발명은 물보다 비중이 높은 추출용매와 용제가 함유된 폐수를 추출탑에 유입시켜 추출에 의하여 추출액은 하부로 배출하고, 추잔액은 상부로 배출하는 추출단계; 상기 추출탑을 거친 추출액을 증류탑에 유입시켜 증류시킴으로서 추출용매는 상부로 배출하고, 용제는 하부로 분리하는 증류단계; 상기 증류탑에서 분리된 용제를 정제탑에 유입시켜 정제하여 회수하는 정제단계; 그리고 상기 추출탑에서 배출되는 추잔액에 함유된 추출용매와 증류탑에서 발생된 추출용매를 회수하여 추출용매탱크에 저장하는 추출용매회수단계를 포함하는 용제회수방법을 제공한다.In order to achieve the above object, the present invention is to extract the waste liquid containing the solvent and solvent having a higher specific gravity than the water flow into the extraction column to extract the extraction liquid to the bottom, the extraction liquid is discharged to the top ; A distillation step of distilling the extract by passing through the extraction column into a distillation column to distill the extraction solvent to an upper portion, and separating the solvent into a lower portion; A purification step of purifying and recovering the solvent separated in the distillation column by flowing into the purification column; And it provides a solvent recovery method comprising an extraction solvent recovery step of recovering the extraction solvent contained in the extraction liquid discharged from the extraction tower and the extraction solvent generated in the distillation column and stored in the extraction solvent tank.
본 발명의 바람직한 실시예에 의하면, 상기 추출탑과 증류탑의 사이에 디켄터를 구비함으로써, 상기 추출탑의 하부로부터 배출된 추출액에 함유된 물을 걸러서 상기 추출탑으로 복귀시키고 추출용매와 용제만을 상기 증류탑으로 유입시킨다.According to a preferred embodiment of the present invention, by providing a decanter between the extraction tower and the distillation column, to filter the water contained in the extract liquid discharged from the bottom of the extraction column to return to the extraction tower and only the extraction solvent and solvent in the distillation column Inflow to
상기 추출탑과 상기 추출용매탱크의 사이에 탈거탑을 구비함으로써, 상기 추출탑의 상부로부터 배출된 추잔액에 함유된 추출용매를 스팀으로 탈거시켜 상기 추출용매탱크로 유입시킨다.By providing a stripping column between the extraction tower and the extraction solvent tank, the extraction solvent contained in the weight balance liquid discharged from the top of the extraction tower is stripped with steam and introduced into the extraction solvent tank.
상기 탈거탑에 일체로 연결되어 상기 탈거탑으로부터 배출되는 물의 온도를 낮추어서 외부로 배출시키는 이코노마이저를 포함한다.Is connected to the stripping tower integrally includes an economizer for lowering the temperature of the water discharged from the stripping tower to discharge to the outside.
이하, 첨부된 도면을 참조하여 본 발명의 바람직한 실시예에 따른 용제 회수 방법을 상세하게 설명한다.Hereinafter, a solvent recovery method according to a preferred embodiment of the present invention with reference to the accompanying drawings will be described in detail.
도2 및 도3 에 도시된 바와 같이, 본 발명이 제시하는 용제 회수방법은 물보다 비중이 높은 추출용매를 사용하여 추출에 의하여 물을 제거하는 추출단계 (S100)와, 상기 추출단계(S100)를 거친 추출액을 증류하여 용제를 분리하는 증류단계(S200)와, 분리된 용제를 정제하여 회수하는 정제단계(S300)를 포함한다. 그리고, 상기 추출단계 및 증류단계(S100,S200)에서 발생된 추출용매를 회수하는 추출용매회수단계(S400)를 추가로 포함한다.As shown in Figures 2 and 3, the solvent recovery method of the present invention is an extraction step (S100) and the extraction step (S100) to remove the water by the extraction using an extraction solvent having a higher specific gravity than water; And distillation step (S200) of separating the solvent by distilling the extracted extract, and a purification step (S300) of purifying and recovering the separated solvent. Further, the method may further include an extraction solvent recovery step S400 for recovering the extraction solvent generated in the extraction step and the distillation steps S100 and S200.
상기 추출단계(S100)에 있어서는, 먼저 추출용매와 수용성 폐용제가 함유된 폐수를 추출탑(10)에 유입시킨다. 이때, 상대적으로 비중이 큰 추출용매는 추출탑 (10)의 상부로 유입시키고 비중이 작은 폐수는 추출탑(10)의 하부로 유입시키는 것이 좋다.In the extraction step (S100), first, the wastewater containing the extraction solvent and the water-soluble waste solvent are introduced into the extraction tower 10. At this time, the relatively large specific gravity solvent is introduced to the top of the extraction tower 10, waste water having a small specific gravity is preferably introduced to the lower portion of the extraction tower (10).
그러면, 유입된 폐수의 비중은 1정도이고 추출 용매의 비중은 1.36 정도이므로 비중차이로 인하여 추출탑(10)에서 추출 용매는 상부(11)에서 하부로 이동하고 반대로 폐수는 추출탑(10) 하부(12)에서 상부(11)로 이동한다. 이렇게 하면 폐수와추출 용매간에는 추출탑(10) 내부에서 추출에 의하여 물질 이동이 일어난다.Then, since the specific gravity of the introduced wastewater is about 1 and the specific gravity of the extraction solvent is about 1.36, the extraction solvent in the extraction tower 10 moves from the upper portion 11 to the lower portion due to the difference in specific gravity. Move from 12 to top 11. In this case, mass transfer occurs between the wastewater and the extraction solvent by extraction in the extraction column 10.
즉, 폐수 중의 용제 DMF는 추출 용매 쪽으로 이동하여 추출 용매와 함께 추출탑(10)의 하부(12)로 이동하면서 배출된다. 이때, 이 액을 추출액이라고 정의한다. 그리고, 폐수 중 용제가 제거된 물은 추출탑(10)의 상부(11)로 배출되게 되는데 이 액을 추잔액이라고 정의한다.That is, the solvent DMF in the wastewater moves toward the extraction solvent and is discharged while moving to the lower portion 12 of the extraction column 10 together with the extraction solvent. At this time, this liquid is defined as an extract liquid. And, the water from which the solvent is removed from the waste water is discharged to the upper portion 11 of the extraction tower 10, this liquid is defined as the balance.
상기 과정에서, 추출 용매의 선택이 매우 중요한데, 추출용매는 원할한 추출이 가능하도록 물에 대한 용해도가 매우 낮은 동시에 회수하고자 하는 용제에 대한 용해도는 높아야 한다. 또한, 추출공정에서의 액액상 분리가 잘 되도록 물보다 비중이 5% 이상 높아야 한다. 그리고, 증발잠열이 물의 증발잠열(상압 100℃에서 539 kcal/kg)보다 훨씬 적어야 한다.In the above process, the selection of the extraction solvent is very important. The extraction solvent has to have a very low solubility in water and a high solubility in the solvent to be recovered at the same time in order to enable a smooth extraction. In addition, the specific gravity should be at least 5% higher than that of water in order to facilitate separation of the liquid phase in the extraction process. And the latent heat of evaporation should be much less than the latent heat of evaporation of water (539 kcal / kg at 100 ° C).
이러한 조건을 고려할 때, 추출용매로 메틸렌클로라이드가 가장 적합하다. 메틸렌클로라이드는 비중이 1.36이고, 증발열이 79 kcal/kg이다.Considering these conditions, methylene chloride is most suitable as an extraction solvent. Methylene chloride has a specific gravity of 1.36 and a heat of evaporation of 79 kcal / kg.
이와 같이 추출탑(10)의 하부로부터 배출된 추출액은 디켄터(13)로 유입된다. 상기 디켄터(13)로 유입된 추출액은 소량의 추잔액 즉, 물을 함유하게 되는데 상기 디켄터(13)에서 추출액과 물이 서로 분리된다. 그리고, 분리된 물은 다시 추출탑(10)으로 복귀하며, 물이 제거된 추출액은 증류탑(14)으로 공급된다.In this way, the extraction liquid discharged from the bottom of the extraction tower 10 is introduced into the decanter (13). The extract liquid introduced into the decanter 13 contains a small amount of the balance liquid, that is, water, and the extract liquid and the water are separated from each other in the decanter 13. Then, the separated water is returned to the extraction tower 10 again, the extract is removed from the water is supplied to the distillation column (14).
상기한 바와 같이 추출단계(S100)가 완료되면, 증류단계(S200)가 진행한다. 즉, 추출액이 증류탑(14)에 유입되며, 상기 증류탑(14)에서 추출액은 증류법에 의하여 추출 용매(메틸렌클로라이드)와 유기용제(DMF)로 분리된다. 그리고, 분리된 추출용매는 증류탑(14)의 상부(15)로, 유기용제(DMF)는 증류탑(14)의 하부(16)로이동한다.When the extraction step (S100) is completed as described above, the distillation step (S200) proceeds. That is, the extract is introduced into the distillation column 14, the extract is separated into an extraction solvent (methylene chloride) and the organic solvent (DMF) by the distillation method. The separated extraction solvent moves to the upper portion 15 of the distillation column 14, and the organic solvent (DMF) moves to the lower portion 16 of the distillation column 14.
상기한 바와 같이 증류단계(S200)후, 정제단계(S300)가 진행한다. 상기 정제단계(S300)에 있어서는, 증류탑(14)에서 처리된 유기용제가 정제탑(17)으로 공급된다. 그리고, 상기 정제탑(17)에서 회수 용제를 최종적으로 다시 한 번 정제시켜 불순물을 제거하고 회수 용제를 제품으로 얻는다.After the distillation step (S200) as described above, the purification step (S300) proceeds. In the purification step (S300), the organic solvent treated in the distillation tower 14 is supplied to the purification tower (17). In the purification tower 17, the recovery solvent is finally purified again to remove impurities and obtain a recovery solvent as a product.
한편, 상기 추출단계(S100) 및 증류단계(S200)에서는 추출탑(10)의 상부(11)로 추잔액과 함께 추출용매가 소량 배출되고, 증류탑(14)의 상부(15)로부터는 추출용매가 증류액으로 배출되는데, 이러한 추출용매를 회수하기 위한 추출용매회수단계(S400)가 상기 공정에 추가로 구비된다.Meanwhile, in the extraction step (S100) and the distillation step (S200), a small amount of the extraction solvent is discharged to the upper portion 11 of the extraction tower 10 together with the weight balance, and the extraction solvent from the upper portion 15 of the distillation column 14. Is discharged to the distillate, the extraction solvent recovery step (S400) for recovering such extraction solvent is further provided in the process.
상기한 바와 같이, 상기 추출탑(10)의 상부(11)에서는 추잔액이 배출되며, 이러한 추잔액은 이코노 마이저(18)를 거쳐 탈거탑(19)으로 공급된다. 그리고, 이 탈거탑(19)에서 추잔액에 함유된 미량의 추출 용매(메틸렌클로라이드)가 스팀에 의해 탈거되어 추잔액으로부터 분리된다.As described above, the weight balance is discharged from the upper portion 11 of the extraction tower 10, the weight balance is supplied to the stripping column 19 via the economizer (18). In the stripping column 19, a small amount of the extraction solvent (methylene chloride) contained in the weight balance liquid is stripped off by steam and separated from the weight balance liquid.
즉, 상기 탈거탑(19)의 하부에 스팀을 주입하여 소정 온도로 가열하면 상기 탈거탑(19)의 내부에 공급된 추잔액은 온도가 올라가고, 이 과정에서, 추잔액에 함유된 미량의 추출용매는 기화됨으로써 탈거탑(19)의 상부(20)로 배출된다.That is, when steam is injected into the lower part of the stripping column 19 and heated to a predetermined temperature, the balance remaining in the stripping column 19 is increased in temperature, and in this process, the trace amount contained in the balance is extracted. The solvent is vaporized and discharged to the upper portion 20 of the stripping column 19.
그리고, 탈거탑(19)의 상부(20)로 배출된 추출용매는 냉각 응축됨으로써 추출 용매탱크(22)로 회수된다. 이때, 추출용매가 제거된 물은 탈거탑(19)의 하부 (21)로 이동한다.Then, the extraction solvent discharged to the upper portion 20 of the stripping column 19 is recovered by the extraction solvent tank 22 by cooling condensation. At this time, the water from which the extraction solvent is removed moves to the lower portion 21 of the stripping column 19.
또한, 상기 증류탑(14)의 상부(15)로 배출된 추출용매는 마찬가지로 냉각 응축되어 상기 추출용매탱크(22)로 이송되어 저장됨으로써 회수된다.In addition, the extraction solvent discharged to the upper portion 15 of the distillation column 14 is recovered by being cooled and condensed and transferred to the extraction solvent tank 22.
상기한 바와 같이, 종래의 증류법에 의한 용제회수방법과 본 발명의 추출법과 증류법을 병용한 용제회수방법의 효율적인 차이를 다음 표에 의하여 비교하였다. 표예에서 보듯이 본 발명에 의한 추출법과 증류법을 병용한 용제 회수 방법이 종래의 증류법에 의한 용제 회수 방법보다 DMF 회수율, 제품의 순도, 에너지 사용량, 시설 투자비 등 여러 가지 항목에서 성능이 우수함을 알 수 있다.As described above, the effective difference between the solvent recovery method by the conventional distillation method and the solvent recovery method using the extraction method and the distillation method of the present invention was compared by the following table. As shown in the table, it can be seen that the solvent recovery method using the extraction method and the distillation method according to the present invention outperforms the conventional solvent recovery method by the distillation method in several items such as DMF recovery rate, product purity, energy usage, and facility investment cost. have.
표table
* DMF 폐수 중 DMF 농도 : 15 wt%* DMF concentration in DMF wastewater: 15 wt%
** DMF 폐수 기준 3 MT/h 처리 능력의 설비 기준** Facility standard of 3 MT / h treatment capacity based on DMF wastewater
이상과 같이, 본 발명의 바람직한 실시예에 따른 용제회수방법은 먼저 추출법을 적용하여 추출용매 쪽으로 회수하고자 하는 용제를 추출시킨 다음, 증발잠열이 물보다 훨씬 낮은 추출용매와 용제를 증류법으로 분리시켜 회수하므로 소요 에너지를 대폭 줄일 수 있고 부산물의 발생을 억제시키는 장점을 가진다.As described above, in the solvent recovery method according to a preferred embodiment of the present invention, by first extracting the solvent to be recovered toward the extraction solvent by applying an extraction method, the extraction solvent and solvent having a much lower latent heat of evaporation than water are recovered by distillation. Therefore, it can significantly reduce the energy required and has the advantage of suppressing the generation of by-products.
또한, 기존의 증류법에 의한 회수 설비와 비교할 때 스팀 사용량을 50% 이하로 줄이고, 증류탑에서의 용제 가수 분해 반응에 의한 부산물 발생을 원천적으로 제거하므로 제품의 품질이 좋아지며 부산물 제거를 위한 정제 설비를 생략할 수 있으므로 투자비를 20% 정도 절감할 수 있는 장점이 있다.In addition, compared to the conventional recovery equipment by distillation method, the steam consumption is reduced to 50% or less, and by-products generated by solvent hydrolysis reaction in the distillation column are removed in principle, so that the quality of the product is improved and the purification equipment for removing by-products is improved. Since it can be omitted, the investment cost can be reduced by about 20%.
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| KR20130101279A (en) * | 2012-03-05 | 2013-09-13 | 웅진케미칼 주식회사 | Method for separating and recovering dimethylformaide in industrial waste water |
| WO2015072740A1 (en) * | 2013-11-15 | 2015-05-21 | 김용환 | Method for treating organic waste liquid including sludge and waste water using solvent extraction |
| WO2020091391A1 (en) * | 2018-11-01 | 2020-05-07 | 주식회사 엘지화학 | Method for separating organic solvent from organic solvent-containing mixed solution |
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| FR2674245B1 (en) * | 1991-03-20 | 1994-05-27 | Inst Francais Du Petrole | PROCESS FOR SEPARATING BUTENES AND BUTANES BY EXTRACTIVE DISTILLATION. |
| KR950014000B1 (en) * | 1993-01-20 | 1995-11-20 | Choe Ki Su | Method for separating phenol formalin methanol and natrium chloride from waste water |
| US5399244A (en) * | 1993-12-06 | 1995-03-21 | Glitsch, Inc. | Process to recover benzene from mixed hydrocarbons by extractive distillation |
| JP3546210B2 (en) * | 1995-11-06 | 2004-07-21 | 帝人ファイバー株式会社 | Method for recovering acetic acid from wastewater containing acetic acid |
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| KR20130101279A (en) * | 2012-03-05 | 2013-09-13 | 웅진케미칼 주식회사 | Method for separating and recovering dimethylformaide in industrial waste water |
| WO2015072740A1 (en) * | 2013-11-15 | 2015-05-21 | 김용환 | Method for treating organic waste liquid including sludge and waste water using solvent extraction |
| WO2020091391A1 (en) * | 2018-11-01 | 2020-05-07 | 주식회사 엘지화학 | Method for separating organic solvent from organic solvent-containing mixed solution |
| CN111886062A (en) * | 2018-11-01 | 2020-11-03 | 株式会社Lg化学 | Method for separating organic solvent from mixed solution containing organic solvent |
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| US12251652B2 (en) | 2020-10-05 | 2025-03-18 | Lg Chem, Ltd. | Stripping device and stripping method |
| CN115159752A (en) * | 2021-04-06 | 2022-10-11 | 于筛成 | A kind of comprehensive treatment method of synthetic leather wastewater |
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| KR20230022034A (en) * | 2021-08-06 | 2023-02-14 | 주식회사 지티씨엔에스 | Continuous recovery method of dimethylformamide from the waste solution of polyimide production process |
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