WO2015016653A1 - Dispositif de raffinage et procédé de raffinage l'utilisant - Google Patents

Dispositif de raffinage et procédé de raffinage l'utilisant Download PDF

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Publication number
WO2015016653A1
WO2015016653A1 PCT/KR2014/007097 KR2014007097W WO2015016653A1 WO 2015016653 A1 WO2015016653 A1 WO 2015016653A1 KR 2014007097 W KR2014007097 W KR 2014007097W WO 2015016653 A1 WO2015016653 A1 WO 2015016653A1
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WIPO (PCT)
Prior art keywords
distillation column
raw material
flowing out
distillation
flow rate
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PCT/KR2014/007097
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English (en)
Korean (ko)
Inventor
이성규
신준호
Original Assignee
주식회사 엘지화학
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Application filed by 주식회사 엘지화학 filed Critical 주식회사 엘지화학
Priority to US14/783,715 priority Critical patent/US9770674B2/en
Priority to CN201480026915.8A priority patent/CN105229119B/zh
Priority to JP2016531533A priority patent/JP6238148B2/ja
Priority claimed from KR1020140098792A external-priority patent/KR101550150B1/ko
Publication of WO2015016653A1 publication Critical patent/WO2015016653A1/fr

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    • 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
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • 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
    • B01D3/007—Energy recuperation; Heat pumps
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G7/00—Distillation of hydrocarbon oils

Definitions

  • the present application relates to a purification apparatus and a purification method for distilling and purifying raw materials.
  • the present application relates to a refining apparatus and a refining method for distilling and refining a raw material, and provide a refining apparatus and a refining method for maximizing the use of an internal heat source in a distillation column to reduce external energy use.
  • the purification apparatus includes a first distillation unit, a second distillation unit and a heat exchanger.
  • 1 shows an exemplary purification apparatus 100.
  • the refining apparatus 100 of the present application has a first distillation tower 101 for distilling introduced raw materials with a first raw material supply port 103 into which raw materials are introduced, and the first distillation tower 101.
  • the first condenser 104 for condensing the overhead flow flowing out of the overhead region of the first column and returning a portion of the overhead stream to the first distillation column and the first outlet route 11 for transferring the substance to the lower portion of the first distillation column 101.
  • It may include a first distillation unit including.
  • the purification apparatus 100 of the present application has a second raw material supply port 105 through which the raw material is introduced, the second distillation column 102 for distilling the introduced raw material, and flows out from the top region of the second distillation column 102.
  • the second condenser 106 for condensing the overhead stream to be returned to the second distillation column 102 and the bottom stream flowing out from the bottom region of the second distillation column 102 are heated to replace the portion with the second distillation column (
  • a second distillation unit including a second reboiler 107 to reflux to a second and a second outlet route 12 for transferring the material flowing out to the bottom of the second distillation column 102.
  • the purification apparatus 100 of the present application is a top bottom region of the first distillation column 101 before the top flow flowing out of the top region of the second distillation column 102 is introduced into the second condenser 106. It may include a heat exchanger (108) for heat exchange with the bottoms flow flowing out from.
  • the bottom stream flowing out from the bottom region of the first distillation column 101 may be at least partially or refluxed to the bottom region of the first distillation column 101.
  • the heat exchanger 108 may transfer the heat of the high temperature overhead stream flowing out of the top region of the second distillation column 102 to the bottom stream flowing out of the bottom region of the first distillation column 101. have.
  • the overhead flow of the second distillation column 102 through the heat exchanger 108 may flow out to the second condenser 106.
  • the overhead flow of the second distillation column 102 can flow to the second condenser 106 at a lower temperature to save energy, and the bottom flow of the first distillation column 101 It may be heated to reflux to the first distillation column (101).
  • the agent for heating the bottom stream flowing out of the bottom region of the first distillation column 201 to reflux a portion of the first distillation column 201 1 may further include a reboiler (209).
  • the first reboiler 209 may heat another column bottom stream from the column bottom flow of the first distillation column 201 through the heat exchanger to reflux a portion of the first reboiler 201 to the first column 201. It is not limited to this.
  • the first reboiler 209 may heat at least a portion of the bottom stream of the first distillation column 201 through the heat exchanger to reflux at least a portion of the first distillation column 201.
  • the bottom stream passing through the first reboiler 209 may be refluxed to the first distillation column 201. Accordingly, the bottom stream of the first distillation column 201 is heated by receiving a heat source from the heat exchanger 208, thereby reducing the energy to be used for heating the bottom stream in the first reboiler 209.
  • the operating pressure P2 of the second distillation column 102 of the present application may be controlled to be higher than the operating pressure P1 of the first distillation column 101.
  • the pressure difference between the operating pressure P2 of the second distillation column and the operating pressure P1 of the first distillation column is 0.25 to 3.5 kg / cm 2 g, 1 to 3.3 kg / cm 2 g, 1.5 to 3.0 kg / cm 2 g, or from 2.0 to 2.8 kg / cm 2 g.
  • the ratio P1 / P2 of the operating pressure P1 of the first distillation column to the operating pressure P2 of the second distillation column is 0.02 to 0.85, 0.03 to 0.80, 0.05 to 0.73, 0.08 to 0.70, 0.10 To 0.67, 0.1 to 0.65, 0.1 to 0.60, or 0.1 to 0.55.
  • the process may be controlled such that a temperature difference of 18 ° C, or 18 ° C to 22 ° C occurs.
  • the ratio (T1 / T2) of the temperature T1 of the column bottom stream of the first distillation column to the temperature T2 of the column top flow of the second distillation column is 0.5 to 0.96, 0.53 to 0.95, 0.55 to 0.94, 0.57 to 0.93. , 0.60 to 0.92, 0.65 to 0.90, 0.70 to 0.90 or 0.75 to 0.85.
  • a method of controlling the pressure of the first distillation column or the second distillation column may be performed as described above, but is not limited thereto.
  • the operating pressure of the second distillation column is 1.5 to 3.5 kg / cm 2 g, 2.0 to 3.3 kg / cm 2 g, 2.3 to 3.0 kg / cm 2 g, or 2.5 to 2.9 kg / cm 2 g.
  • the operating pressure of the first distillation column is 0.1 to 1.5 kg / cm 2 g, 0.15 to 1.0 kg / cm 2 g, 0.2 to 0.8 kg / cm 2 g.
  • the operating pressure may be the operating pressure of the column top of the distillation column, unless otherwise specified.
  • the operating pressure is not particularly limited as long as it satisfies the ratio P1 / P2 of the operating pressure P1 of the first distillation column to the operating pressure P2 of the second distillation column.
  • heat exchange occurs between the flow, and through the heat exchange between existing processes instead of an external heat source, it is possible to improve the energy efficiency of the process.
  • the purification apparatus 300 of the present application is a recovery device 310 for recovering the material flowing out of the first outlet route 11 or the second outlet route 12. It may further include.
  • the recovery device 310 may recover some active ingredients from the substance leaked to the first outflow route 11 and / or the second outflow route 12.
  • the method of flowing out the top product of the first distillation column 101 to the bottom stream of the first distillation column 101 is not particularly limited, and may be performed through a general process in the art.
  • the flow rate through the first outlet route 11 of the first distillation column 101 as described below, the bottom of the top product of the first distillation column exits to the bottom flow or the first outlet route 11. Can be spilled into the effluent material, but is not limited thereto.
  • top product refers to a substance rich in a low boiling point component which is produced in the top region of the first or second distillation column and has a relatively low boiling point
  • top product refers to the first distillation column.
  • present invention refers to a material rich in a high boiling point component generated in the bottom region of the second distillation column and having a relatively high boiling point.
  • &quot rich substance having a low boiling point component " refers to a substance having a higher content of a low boiling point component and a relatively low boiling point component generated in the top region than the contents of the low boiling point component, the high boiling point component and the middle boiling point component included in the raw material.
  • the content of the low boiling point component included in the product may refer to a product having 80% by weight, 90% by weight, 95% by weight or 99% by weight or more.
  • a substance having a high boiling point component refers to a content of a high boiling point component generated in the bottom region and having a relatively higher boiling point than the content of each of the low boiling point component, the high boiling point component and the middle boiling point component contained in the raw material.
  • This higher material may mean, for example, a product having a high boiling point component contained in the product of at least 80% by weight, at least 90% by weight, at least 95% by weight or at least 99% by weight.
  • top region means the upper region of the first distillation column or the second distillation column, and specifically, the base of the column, based on the first raw material supply port or the second raw material supply port to which the raw material is supplied. It can mean the upper region.
  • bottom region means a lower region of the first distillation column or the second distillation column, and, specifically, refers to the first raw material supply port or the second raw material supply port to which the raw material is supplied. It may mean a lower region.
  • the ratio (V2 / V1) of the flow rate (V2) of the material flowing out of the first outlet route 11 to the flow rate (V1) of the raw material flowing into the first raw material supply port is 0.0009 to 0.005, 0.001 to 0.004, 0.0015 to 0.0035, 0.0016 to 0.0034, 0.0017 to 0.0033, 0.0018 to 0.0032, 0.0019 to 0.0031, 0.002 to 0.003, 0.0021 to 0.0029 or 0.0022 to 0.0028.
  • the ratio (V4 / V3) of the flow rate V4 of the substance flowing out of the second outlet route 12 to the flow rate V3 of the raw material flowing into the second raw material supply port is 0.0009 to 0.004, and 0.001 to 0.003. , 0.001 to 0.0025, 0.0011 to 0.0024, 0.0012 to 0.0023, 0.0013 to 0.0022, 0.0014 to 0.0021 or 0.0015 to 0.002.
  • the V2 / V1 value may be greater than the V4 / V3 value. That is, the flow rate of the substance flowing out to the bottom of the first distillation column can be controlled to be larger.
  • the ratio (V6 / V5) of the flow rate (V6) of the material recovered to the recovery device to the total flow rate (V5) of the raw materials flowing into the first raw material supply port and the second raw material supply port is 0.001 to 0.005, 0.0012 to 0.0045, 0.0013 to 0.004, 0.0014 to 0.0035, 0.0015 to 0.003 or 0.0016 to 0.0025.
  • the first distillation column by controlling the ratio (V2 / V1) of the flow rate (V2) of the substance flowing out of the first outlet route 11 with respect to the flow rate (V1) of the raw material flowing into the first raw material supply port.
  • V2 / V1 the ratio of the flow rate (V2) of the substance flowing out of the first outlet route 11 with respect to the flow rate (V1) of the raw material flowing into the first raw material supply port.
  • the effective material is It can collect
  • the purification apparatus of the present application may further include a connection route 13 connecting the vapor phase of the recovery device 310 to the bottom of the first distillation column 301.
  • the vapor phase of the upper portion of the recovery device 310 may transfer a heat source to the lower portion of the first distillation column 301. That is, the entire amount of energy supplied to the recovery device can be recovered and utilized. Through this, the vapor phase of the recovery device 310 is introduced into the lower portion of the first distillation column 301, so that the recovery device may play the same role as the reboiler.
  • the ratio V7 / V6 of the flow rate V7 of the material flowing into the bottom of the first distillation column via the connecting route 13 to the flow rate V6 of the material returned to the recovery device is 0.5 to 0.95. , 0.55 to 0.93, 0.60 to 0.90, 0.65 to 0.89, 0.67 to 0.88, 0.7 to 0.87, 0.75 to 0.86 or 0.77 to 0.85.
  • the flow rate of the material returned to the recovery device and the flow rate of the material flowing into the lower portion of the first distillation column through the connection route it is possible to implement an energy efficiency improvement of the entire process through the heat source of the recovery device.
  • the raw material is not particularly limited, and in one example, the first distillation column and the second distillation column of the present application may be a solvent recovery process, but are not limited thereto.
  • the purification apparatus of the present application may be applied without limitation as long as the chemical process separates the mixture. Therefore, some of the active ingredients recovered through the recovery device 310 may be a solvent, and the solvent may be n-hexane, but is not limited thereto.
  • the present application also relates to a method for purifying raw materials.
  • the purification method may be performed by the above-described purification device.
  • An exemplary method includes introducing a raw material into the first distillation column 101; Introducing a raw material into the second distillation column (102); Separating the introduced raw materials into a top stream and a bottom stream in the first distillation column 101 and the second distillation column 102, respectively; And heat-exchanging the overhead stream flowing out of the overhead region of the second distillation column 102 and the overhead stream flowing out of the bottom region of the first distillation tower 101.
  • by exchanging heat through the heat exchange step existing interprocess heat exchange may occur instead of an external heat source. Controlling the operating pressure or operating temperature of the first distillation column and / or the second distillation column may be performed as described above. In addition, controlling the flow rate of each flow of the first distillation column and / or the second distillation column may all be performed as described above.
  • the method of purifying the raw material of the present application may further include recovering the material flowing out to the bottom of the first or second distillation column. That is, the material flowing out to the lower portion of each distillation column through the first outlet route 11 of the first distillation column or the second outlet route 12 of the second distillation column may be recovered by the above-described recovery apparatus.
  • the purification method may further comprise the step of delivering the vapor phase generated in the recovery step to the bottom of the first distillation column. That is, the vapor phase may be transferred to the lower portion of the first distillation column through the connection route 13 of the recovery device. Purification method of the raw material of the present application may recover the solvent through the recovery step.
  • the purification method may exchange heat through the temperature difference between the bottom stream of the first distillation column 301 and the overhead stream of the second distillation column 302 as described above.
  • the bottom stream of the first distillation tower 301 or the second distillation column 302 is discharged by flowing out the bottom stream of the first distillation column 301 or the second distillation column 302 as described above.
  • the temperature of the overhead flow of 302 can be controlled.
  • the purification method of the present application is a method for heat exchange between the bottom stream of the first distillation column 101 and the overhead flow of the second distillation column 102, in addition to adjusting the pressure, the first distillation column 101
  • Some of the overhead product of the first distillation column 101 may include flowing out to the bottom stream.
  • the high temperature bottom stream of the lower part of the first distillation column 101 lowers the concentration of the high boiling point material in the bottom stream due to the mixing of a part of the low temperature column top product of the first distillation column, thereby reducing the concentration of the high boiling point material.
  • the temperature of the entire stream is lowered, and the above-described temperature ratio T1 / T2 may be satisfied in relation to the overhead flow of the second distillation column 102.
  • the method of flowing out the top product of the first distillation column 101 to the bottom stream of the first distillation column 101 is not particularly limited, and may be performed through a general process in the art. In one example, by controlling the flow rate as described above through the first outflow route 11 of the first distillation column 101, the top product of the first distillation column can flow out to the bottom flow, but is not limited thereto. .
  • Purification apparatus and purification method according to the present application it is possible to improve the energy efficiency of the entire process by maximizing the use of the internal heat source in the distillation column in the process of distilling the raw material and reducing the use of external heat source.
  • 1 to 3 is a view showing a purification device according to an embodiment of the present application.
  • FIG. 4 is a view showing a conventional purification device.
  • N-hexane was recovered using a purification apparatus as shown in FIG. Specifically, a separation process is performed by introducing a raw material including n-hexane into the purification apparatus, wherein the operating pressure of the top region of the first distillation column of the purification apparatus is about 0.3 Kg / cm 2 g, and the operating temperature is It was set at about 77 ° C. in the zone and at about 95 ° C. in the bottom zone. The operating pressure of the top column of the second distillation column was about 2.8 Kg / cm 2 g. It was made to be ° C. In addition, a portion of the bottom stream discharged to the bottom region of the first distillation column was refluxed to the first distillation column via a heat exchanger.
  • the flow rate V1 of the raw material flowing into the first raw material supply port is 22 ton / hr
  • the flow rate V2 of the material flowing out of the first outflow route is 0.05 ton / hr, flowing into the second raw material supply port.
  • the flow rate V3 of the raw material to be used was controlled to 45 ton / hr and the flow rate V4 of the substance flowing out to the second outflow route to 0.07 ton / hr.
  • the purification was performed in the same manner as in Example 1 except that the column bottom stream, which was passed through the heat exchanger of the first distillation column, was heated to a first column by refluxing by heating through a reboiler.
  • the apparatus further includes a recovery device for recovering material discharged from the bottom region of the first distillation column and the second distillation column, and a connection route connecting the recovery device and the lower portion of the first distillation column. Purification was carried out in the same manner as in Example 2.
  • the flow rate (V5) of the raw material flowing into the first raw material supply port and the second raw material supply port is 67 ton / hr
  • the flow rate (V6) of the material recovered to the recovery device is 0.12 ton / hr
  • the recovery device The flow rate (V7) of the material flowing into the bottom of the first distillation column through the connecting route at the top of was controlled to 0.1 ton / hr.
  • Example 2 Purification was carried out in the same manner as in Example 1 except that the feedstock flow rate of the first distillation column was supplied at 45 ton / hr, and the flow rate of the feedstock of the second distillation column was supplied at 22 ton / hr.
  • the flow rate V2 of the substance flowing out of the first distillation column through the first outlet route was 0.07 ton / hr
  • the flow rate V4 of the substance flowing out of the second distillation column through the second outlet route was 0.05 ton. / hr.
  • n-hexane was recovered by separately using the first distillation column 401 and the second distillation column 402. Purification was carried out in the same manner as in Example 2, except for the heat exchanger. Similarly, the first distillation column and the second distillation column of the refining apparatus were controlled to have an operating pressure of about 0.75 Kg / cm 2 g, an operating temperature of about 88 ° C. in the column top region, and about 115 ° C. in the bottom region.
  • Example 1 Example 2
  • Example 3 Example 4 Comparative Example 1 First Distillation Tower Energy Consumption (Gcal / hr) 2.5 2.5 2.5 2.5 1.3 2.2 Second Distillation Column Energy Consumption (Gcal / hr) 3.1 3.1 3.0 4.5 3.4 Recovery device energy consumption (Gcal / hr) 0.0 0.0 0.1 0.0 0.0 Energy recovery amount (Gcal / hr) 2.5 2.0 2.5 1.3 0.0 Total energy usage (Gcal / hr) 3.1 3.6 3.0 4.5 5.6 Energy savings (Gcal / hr) 2.5 2.0 2.6 1.1 - Energy saving rate (%) 44.6 35.7 46.4 19.6 -
  • Example 2 Example 3
  • Example 4 Comparative Example 1 First distillation tower Light 1.66 1.66 1.66 1.66 1.66 n-Hexane 98.32 98.32 98.32 98.32 Heavies 0.02 0.03 0.02 0.02 0.02 0.02 Second Distillation Tower Light 0.93 0.93 0.93 0.93 0.93 n-Hexane 99.05 99.05 99.05 99.05 99.05 Heavies 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02
  • the purification apparatus according to the embodiment of the present application can achieve energy saving while maintaining the purity of the product at the same level.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention porte sur un dispositif de raffinage et sur un procédé de raffinage l'utilisant. Plus précisément, la présente invention porte sur un dispositif de raffinage et un procédé de raffinage qui permettent, dans un processus de distillation de matière première, d'améliorer le rendement énergétique de tout le processus par l'augmentation au maximum de l'utilisation d'une source de chaleur interne et la réduction de l'utilisation d'une source de chaleur externe dans une colonne de distillation.
PCT/KR2014/007097 2013-08-01 2014-08-01 Dispositif de raffinage et procédé de raffinage l'utilisant WO2015016653A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US14/783,715 US9770674B2 (en) 2013-08-01 2014-08-01 Purification device and purification method using the same
CN201480026915.8A CN105229119B (zh) 2013-08-01 2014-08-01 纯化设备及使用该纯化设备的纯化方法
JP2016531533A JP6238148B2 (ja) 2013-08-01 2014-08-01 精製装置及びこれを利用した精製方法

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR20130091797 2013-08-01
KR10-2013-0091797 2013-08-01
KR10-2014-0098792 2014-08-01
KR1020140098792A KR101550150B1 (ko) 2013-08-01 2014-08-01 정제 장치 및 이를 이용한 정제 방법

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Publication Number Publication Date
WO2015016653A1 true WO2015016653A1 (fr) 2015-02-05

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5035776A (en) * 1990-03-29 1991-07-30 University Of Massachusetts Low energy extractive distillation process for producing anhydrous ethanol
KR100442501B1 (ko) * 1998-06-19 2004-07-30 스톤 앤드 웹스터 인코포레이티드 에틸벤젠/스티렌 탑의 캐스케이드식 리보일링
KR20080089961A (ko) * 2007-04-03 2008-10-08 (주)에이피에스티 추출증류를 이용한 무수 에탄올 생산방법
US20100051441A1 (en) * 2008-08-27 2010-03-04 Membrane Technology And Research, Inc. Membrane-augmented distillation with compression to separate solvents from water
US20130037404A1 (en) * 2010-04-21 2013-02-14 Saudi Basic Industries Corporation Distillation process and multi-column heat-integrated distillation system

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5035776A (en) * 1990-03-29 1991-07-30 University Of Massachusetts Low energy extractive distillation process for producing anhydrous ethanol
KR100442501B1 (ko) * 1998-06-19 2004-07-30 스톤 앤드 웹스터 인코포레이티드 에틸벤젠/스티렌 탑의 캐스케이드식 리보일링
KR20080089961A (ko) * 2007-04-03 2008-10-08 (주)에이피에스티 추출증류를 이용한 무수 에탄올 생산방법
US20100051441A1 (en) * 2008-08-27 2010-03-04 Membrane Technology And Research, Inc. Membrane-augmented distillation with compression to separate solvents from water
US20130037404A1 (en) * 2010-04-21 2013-02-14 Saudi Basic Industries Corporation Distillation process and multi-column heat-integrated distillation system

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