KR20010092049A - Refining apparatus and its process for removing impurities of waste organic solvent by boiling with third material - Google Patents

Refining apparatus and its process for removing impurities of waste organic solvent by boiling with third material Download PDF

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KR20010092049A
KR20010092049A KR1020000013952A KR20000013952A KR20010092049A KR 20010092049 A KR20010092049 A KR 20010092049A KR 1020000013952 A KR1020000013952 A KR 1020000013952A KR 20000013952 A KR20000013952 A KR 20000013952A KR 20010092049 A KR20010092049 A KR 20010092049A
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column
service tank
organic solvent
impurities
waste organic
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KR1020000013952A
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Korean (ko)
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이범진
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이범진
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/36Azeotropic distillation

Abstract

PURPOSE: A distillatory apparatus for refining waste organic solvents is provided to separate impurities from waste organic solvent with increased efficiency. CONSTITUTION: The distillatory apparatus comprises a feeding pump(6) supplying raw materials into a service tank(5); a column into which raw materials from the service tank is introduced by gravitational force; a reboiler(1) which is installed in the lower bottom of the column to supply steam thereto; 1st cooler(3), 2nd cooler(4) and condensers(11,11) which are respectively installed in the upper part of the column; a distillation tower(100) on the inside of which two radiators(8,10), five flow sheets(9), and vacuum pump(12) are equipped. This apparatus is characterized in that an inlet port(101) is installed at a certain position to infuse a specific amount of water or other substance intermittently or periodically into the service tank so that impurities being carried along flow can be isolated.

Description

폐유기용제속의 불순물을 제3의 물질과 공비시켜 제거하는 정제장치 및 방법{REFINING APPARATUS AND ITS PROCESS FOR REMOVING IMPURITIES OF WASTE ORGANIC SOLVENT BY BOILING WITH THIRD MATERIAL}REFINING APPARATUS AND ITS PROCESS FOR REMOVING IMPURITIES OF WASTE ORGANIC SOLVENT BY BOILING WITH THIRD MATERIAL}

본 발명은 다단증류(多段烝溜)를 실시할 때 물성(物性)에 따라 공비비율(共沸比率)에 의거 제품화하고저 하는 물질(物質)에 공비되어 따라 다니는 불순물을 물 또는 제3의 물질로 분리 제거하는 폐유기용제속의 불순물을 제3의 물질과 공비시켜 제거하는 정제장치 및 방법에 관한 것이다.The present invention is a water or a third material to carry impurities azeotropically to the material to be commercialized according to the azeotropic ratio (따라 比 率) according to the physical properties when performing the multi-stage distillation The present invention relates to a refining apparatus and method for azeotropically removing impurities in a waste organic solvent to be separated and removed with a third material.

주지하고 있는 바와 같이 유기용제(宥機容劑)는 시험연구용시약과 원료의 약품 및 전자시약 등을 용해(溶解) 또는 희석(稀釋)시키는데 사용되는 유기성의 알콜 및 아세톤 등과 같은 액체화합물질(液體化合物質)이다.As is well known, organic solvents are liquid compounds such as organic alcohols and acetone used to dissolve or dilute test reagents, raw materials, and electronic reagents.化合物 質).

이와같이 다른 약품을 용해 또는 희석시키는데 사용된 폐유기용제 속에는 많은 불순물을 포함하고 있어서 이를 재생하여 폐유기용제가 발생된 제조공정에 다시 사용할 수 있게 하기 위한 증류방법(烝溜方法)에는 유기용제를 제조할때 끓여서 정제하는 단순증류방법(單純烝溜方法)과 다단증류방법(多段烝溜方法)을 이용하고 있다.As such, organic solvents can be prepared in the distillation method to recycle waste organic solvents used in dissolving or diluting other chemicals and to recycle them. Boil and purify simple distillation method (單純 烝 溜 方法) and multi-stage distillation method (多 段 烝 溜 方法) is used.

그런데 상기의 단순증류방법은 유기용제를 한번 끓여서 발생된 증기를 응축(凝縮)또는 냉각시켜 제품화하는 방법이며, 또 다단증류방법은 유기용제를 다단증류시설로 끓여서 매단(每段)으로 증기를 보내서 그 단에서 다시 끓게 한 후 높은 온도에서 끓은 물질을 액체상태로 하단(下段)으로 보내주고 낮은 온도에서 끓은 물질은 증기상태로 다음의 상단(上段)으로 상승하여 더 낮은 온도에서 끓은 물질을 끓여주는 과정이 모든 단수를 단계적으로 통과하여 낮은 온도에서 끓은 물질의 일부는 다시 환류(還流)(Column의 최상단에 액체상태로 응축된 물질을 다시 투입해주는 것)시켜 주므로서 불순물의 분리를 확실하게 하고 또 일부는 제품화 되어지는 방법이다.However, the simple distillation method is a method of commercializing the steam generated by boiling the organic solvent once and condensing or cooling the product, and the multi-stage distillation method is to boil the organic solvent to a multi-stage distillation facility and send the steam to each stage. After boiling again at that stage, the boiled material is sent to the lower part in a liquid state at a high temperature, and the boiled material is lowered to the next upper part in a vapor state to boil the boiled material at a lower temperature. The process passes through all the stages step by step to recirculate some of the boiled material at low temperature (reintroduce the liquid condensed material at the top of the column) to ensure the separation of impurities. Some are ways of becoming product.

그러나 두가지 이상의 물질이 혼화(混化)되어 있는 액체화합물질인 유기용제속에 포함된 불순물을 제거하는데는 주로 후자의 다단증류방법이 이용되고 있지만 이 방법 역시 유기용제에 용해된 불순물이 완전히 제거되지 않는 경우가 많았다.However, the latter multi-stage distillation method is mainly used to remove impurities contained in the organic solvent, a liquid compound in which two or more substances are mixed, but this method also does not completely remove impurities dissolved in the organic solvent. There were many cases.

특히 지정폐기물인 유기용제의 정제시 품질을 높이는데는 더더욱 어려움이많아 다량의 폐유기용제를 그대로 폐기하는데 따른 환경오염이 점차 더 심화하고 있는 실정이며 더우기 이를 소각처리할때도 유기용제를 사용하는 업소에서는 제조원가의 상승과 폐유기용제의 적정한 처리로 인한 많은 어려움을 격고 있는 실정이다.In particular, the quality of organic solvents, which are designated wastes, is much more difficult to improve. Therefore, the environmental pollution caused by the disposal of large amounts of organic wastes is intensifying. Moreover, businesses that use organic solvents even when incinerated There are many difficulties due to the rise in manufacturing cost and proper disposal of waste organic solvents.

본 발명에서는 상기와 같은 문제점을 해소하기 위하여 다단증류장치의 임의의 부위로 물 또는 제3의 물질을 투입하여 불순물로 공비되어 따라 다니는 물질을 제거하여 유기용제의 품질을 고순도로 정제할 수 있도록 함을 그 목적으로 한다.In the present invention, in order to solve the above problems, water or a third material is added to an arbitrary part of the multi-stage distillation apparatus to remove the azeotrope that is followed by the azeotrope as impurities, so that the quality of the organic solvent can be purified with high purity. For that purpose.

본 발명은 이와 같은 목적을 달성하기 위하여 다단증류장치의 서비스탱크가 위치한 부위나 기타임의의 부위에 설치한 투입구를 통해 투입되는 물 또는 제3의 물질을 물과 함께 공비시켜 중간 제품으로 하고 과량의 물은 불순물과 함께 증류장치의 하단부로 제거되게 하는 폐유기용제속의 불순물을 제3의 물질과 공비시켜 제거하는 정제장치 및 방법을 특징으로 한다.In order to achieve the above object, the present invention provides an intermediate product by azeotropically combining water or a third material introduced through the inlet installed at the site of the service tank of the multi-stage distillation unit or any other site with water to make an intermediate product. It is characterized in that the purification apparatus and method for removing azeotropes in the waste organic solvent with the third material by azeotropically removing the water together with the impurities to the lower end of the distillation apparatus.

도 1은 본 발명을 실시하기 위한 전체 처리공정도임.1 is an overall processing process diagram for practicing the present invention.

※도면의 주요부분에 대한 부호의 설명※※ Explanation of symbols about main part of drawing ※

1-리보일러 2-컬럼 3,4-제1 및 제2응축기1-reboiler 2-column 3,4-first and second condenser

5-서비스탱크 6-피팅펌프 7-분리기5-service tank 6-fitting pump 7-separator

8,10-냉각기 11,11-콘덴서 9-폴로시트8,10-Cooler 11,11-Capacitor 9-Polo Sheet

12-진공펌프 100-증류탑 101-투입구12-vacuum pump 100-distillation tower 101-inlet

이하, 본발명을 첨부된 도면을 참조하여 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

첨부된 도면은 본 발명을 실시하기 위한 전체처리공정도로서 원료를 서비스 탱크(Sevice Tank)(5)로 이송시켜 주는 피팅펌프(Feeding pump)(6)와; 상기 서비스탱크(5)로 부터 자연낙차시켜 투입되게 한 컬럼(Column)(2)과; 상기 컬럼(2)의 하부에서 스팀을 가할 수 있는 리보일러(Reboiler)(1)가 이에 설치되고 또 컬럼(2)의 상부는 제1응축기(1ST Cooler)(3) 및 제2응축기(2nd cooler)(4)와콘덴셔(Condenser)(11)(11), 그리고 냉각기(8)(10)로 구성되어 있는 증류탑(100)에는 폐유기용제의 흐름을 관찰할 수 있는 5개의 폴로시트(Flow sheet)(9)와 분리기(Separator)(7)및 진공펌프(Vaeum pump)(12)등을 갖추고 있다.The accompanying drawings are, as a whole process flow chart for carrying out the present invention and a feeding pump (6) for transferring the raw material to the service tank (Sevice Tank) (5); A column 2 which is naturally dropped from the service tank 5 and is introduced; A reboiler (1) capable of applying steam from the lower part of the column (2) is installed therein, and the upper part of the column (2) has a first condenser (1ST cooler) 3 and a second condenser (2nd cooler). (4) and condenser (11) (11) and cooler (8) (10) in the distillation column (100) has five polo sheets (Flow sheet) to observe the flow of the waste organic solvent (9), separator (7) and vacuum pump (12).

본 발명은 이와 같이 설치되어 있는 증류탑(100)의 서비스 탱크(5)부위나 또는 임의의 부위에 물 또는 제3의 물질을 투입할 수 있는 투입구(101)를 설치하여 불순물로 공비되어 따라 다니는 물질을 제거할 수 있게 한 구조이다.The present invention is installed in the service tank (5) of the distillation column 100 is installed in this way or any portion of the water inlet or any other material to the third material can be installed to azeotroped with impurities It is a structure that can be removed.

즉 상기의 투입구(101)로 다음 공정에서 제거하기 쉬운 물 또는 제3의 물질을 넣어 공비시키거나 불순물이 높은 온도에서 끓는 상태로 변화시켜 제거하므로서 얻고저 하는 유기용제의 품질을 고순도로 정제할 수 있고 또 이 과정에서 물 또는 제3의 물질은 얻고저 하는 물질의 특성과 제거하고저 하는 물질의 특성을 고려하여 이에 적합한 물질을 선택 사용하게 되는데 이때 선택하는 방법은 각종 문헌을 참고하여 각물질의 성질과 공비(共沸)의 조건을 고려하여 경우에 따라서는 실험적인 방법으로 사전에 실험하여 선택 사용할 수 있고 또한 제품의 품질수준은 요구하는 규격에 따라 조건을 조절하여 제품화하게 된다.That is, the inlet 101 can be purified with high purity by adding water or a third material which is easy to be removed in the next process or by azeotropically removing impurities by changing to a boiling state at a high temperature. In this process, water or a third substance is selected and used in consideration of the characteristics of the substance to be obtained and the substance to be removed and the substance to be removed. Considering the properties and conditions of azeotropy, in some cases, it can be experimented and used in advance by an experimental method, and the quality level of the product is manufactured by adjusting the conditions according to the required standard.

한편, 본 발명이 다단증류장치를 필요로 하는 이유는 단순증류장치의 경우는 1∼2회를 반복하여 찌꺼기를 제거하고 있지만 확실하게 분리가 이루워지지 않고 있기 때문에 분리하고저 하는 물질에 따라 그 높이와 단수(대략 60단)를 달리 구성할 수 있으므로 해서 보통의 액체화합물질의 경우 그 분리를 용이하게 할 수 있음에 기인한다.On the other hand, the present invention requires a multi-stage distillation apparatus in the case of a simple distillation apparatus to remove the residue by repeating once or twice, but since it is not reliably separated, depending on the material to be separated This is because the height and the number of stages (approximately 60 stages) can be configured differently so that the separation can be facilitated in the case of ordinary liquid compounds.

〈실시예〉<Example>

재생하고저 하는 폐유기용제 즉 메틸렌크로라이드 화합물질속에 미지의 고비점(高沸点)물질이 석여 있는 경우 물 또는 제3의 물질을 투입구(101)로 투입하면 미지의 고비점 물질은 물에 용해되어 증류탑(100)의 하부를 몰리게 되고 40.3℃에 끓은 메틸렌 크로라이드는 물 1.5%와 공비하여 비점이 38.5℃로 낮아져 증류시설의 상부로 몰리게 된다.If there is an unknown high boiling point substance in the waste organic solvent, i.e. methylene chloride compound, which is to be regenerated, water or a third substance is introduced into the inlet 101, and the unknown high boiling point substance is dissolved in water. The lower portion of the distillation column 100 is driven, and the methylene chromide boiled at 40.3 ° C. is azeotropic with 1.5% of water, and the boiling point is lowered to 38.5 ° C., thereby driving the upper part of the distillation unit.

이때 물과 공비되어 38.5℃에서 끓어나온 메틸렌크로라이드는 냉각시켰을 경우 물은 메틸렌크로라이드와 섞이지 아니하고 석출(析出)되어 비중이 상대적으로 낮아 메틸렌크로라이드에 의해 뜨게 되는 바 물을 제거하여 간단히 제품화되는데 물을 사용하지 않을 시에는 메틸렌크로라이드와 공비하여 제거되지 않는다.At this time, when the methylene chloride, which is azeotropic with water and boiled at 38.5 ° C., is cooled, water is not mixed with methylene chloride and precipitated (출 出) and its specific gravity is relatively low. When water is not used, it is not removed azeotropically with methylene chloride.

본 발명은 상기 실시예에 의거한 메틸렌크로라이드와 같은 물질에 한정하지 않고 시험연구용시약, 원료의약품 및 전자시약규격에 재사용할 수 있도록 폐유기용제속에 포함된 불순물을 제거하는데 광범위하게 적용될 수 있음은 물론이다.The present invention is not limited to a material such as methylene chromide according to the above embodiment, and can be widely applied to remove impurities contained in waste organic solvents so that they can be reused in test research reagents, raw material drugs, and electronic reagent standards. Of course.

이상에서 설명한 바와 같이 본 발명은 폐유기용제속에 포함된 불순물을 다단증류장치로 정제할 때 물성에 따라 공비율에 의거 불순물이 제품화하고저 하는 물질에 공비되어 따라 다니는 물 또는 제3의 물질을 투입하여 분리하기 어려운 불순물의 제거를 간단히 하므로서 폐유기용제의 가치를 극대화하고 품질을 고급화하므로서 그 이용범위를 넓히고 환경보전에 일조를 담당할 수 있는 일석삼조의 효과를 제공한다.As described above, in the present invention, when the impurities contained in the waste organic solvent are purified by a multi-stage distillation apparatus, water or a third substance which is followed by azeotropically to the material which is impregnated with impurities according to the physical properties according to the physical properties is added. By simplifying the removal of impurities that are difficult to separate, it maximizes the value of waste organic solvents and enhances the quality of the organic solvents.

Claims (2)

원료를 서비스탱크(5)로 이송시켜주는 피팅펌프(6)와; 상기 서비스탱크(5)로부터 자연낙차시켜 투입되게 한 컬럼(2)과; 상기 컬럼(2)의 하부에서 스팀을 가할 수 있는 리보일러(1)가 이에 설치되고 또 컬럼(2)의 상부는 제1응축기(3)및 제2응축기(4)와 콘덴서(11)(11); 그리고 냉각기(8)(10)를 갖고 5개의 플로시트(9)와 분리기(7) 및 진공펌프(12)를 구비하는 증류탑(100) 및 어떠한 형식의 증류시설에 있어서,A fitting pump 6 for transferring raw materials to the service tank 5; A column 2 which is naturally dropped from the service tank 5 and is introduced; A reboiler 1 capable of applying steam in the lower part of the column 2 is installed therein, and the upper part of the column 2 has a first condenser 3, a second condenser 4, and a condenser 11, 11. ); And in a distillation column 100 and any type of distillation system having a cooler 8, 10 and having five flow sheets 9, a separator 7 and a vacuum pump 12. 증류시설에 설치된 서비스 탱크(5)의 부위나 임의의 부위에 물 또는 제3의 물질을 투입할 수 있는 투입구(101)을 구비하여서 된 것을 특징으로 하는 폐유기용제속의 불순물을 제3의 물질과 공비시켜 제거하는 정제장치.Impurities in the waste organic solvent comprising an inlet 101 through which water or a third substance can be introduced into a part or any part of the service tank 5 installed in the distillation facility. Refiner to remove azeotropically. 증류탑(100)의 서비스 탱크(5)부위나 또는 임의의 부위에 설치되어 있는 투입구(101)를 통하여 필요한 량의 물 및 제3의 물질을 지속적으로 또는 간헐적으로 투입 조절하여 공비비율에 의거 불순물이 제품화하고저 하는 물질에 공비되어 따라 다니는 것을 제거할 수 있음을 특징으로 하는 폐유기용제속의 불순물을 제3의 물질과 공비시켜 제거하는 정제방법.Through the inlet 101 installed at the service tank 5 part of the distillation column 100 or at an arbitrary part, the required amount of water and the third material are continuously or intermittently adjusted to control impurities based on the azeotropy ratio. A method for purifying azeotropic impurities in a waste organic solvent with a third substance, characterized in that it can remove the azeotropic agent to a material to be commercialized.
KR1020000013952A 2000-03-20 2000-03-20 Refining apparatus and its process for removing impurities of waste organic solvent by boiling with third material KR20010092049A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3987121A (en) * 1975-08-26 1976-10-19 International Flavors & Fragrances Inc. Process for separating alpha-pinene from beta-pinene
US4070254A (en) * 1975-06-10 1978-01-24 Nippon Zeon Co., Ltd. Process for preparing a purified methacrylic acid ester
US4323432A (en) * 1979-07-06 1982-04-06 Mitsui Petrochemical Industries, Ltd. Process for isolating and recovering meta- and para-cresols from crude cresol-containing compositions composed of cresol components, unreacted cymene components and high-boiling by-products
US4359365A (en) * 1979-10-16 1982-11-16 Sumitomo Chemical Company, Limited Method of purification of β-phenylethyl alcohol
JPS63205101A (en) * 1987-02-20 1988-08-24 Daicel Chem Ind Ltd Separation of dimethyl carbonate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4070254A (en) * 1975-06-10 1978-01-24 Nippon Zeon Co., Ltd. Process for preparing a purified methacrylic acid ester
US3987121A (en) * 1975-08-26 1976-10-19 International Flavors & Fragrances Inc. Process for separating alpha-pinene from beta-pinene
US4323432A (en) * 1979-07-06 1982-04-06 Mitsui Petrochemical Industries, Ltd. Process for isolating and recovering meta- and para-cresols from crude cresol-containing compositions composed of cresol components, unreacted cymene components and high-boiling by-products
US4359365A (en) * 1979-10-16 1982-11-16 Sumitomo Chemical Company, Limited Method of purification of β-phenylethyl alcohol
JPS63205101A (en) * 1987-02-20 1988-08-24 Daicel Chem Ind Ltd Separation of dimethyl carbonate

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