JP2022168249A - Separation method and apparatus of mixture - Google Patents

Separation method and apparatus of mixture Download PDF

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JP2022168249A
JP2022168249A JP2022145412A JP2022145412A JP2022168249A JP 2022168249 A JP2022168249 A JP 2022168249A JP 2022145412 A JP2022145412 A JP 2022145412A JP 2022145412 A JP2022145412 A JP 2022145412A JP 2022168249 A JP2022168249 A JP 2022168249A
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heat exchanger
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mixture
water
compressor
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JP2022168249A5 (en
JP7468587B2 (en
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幸一 山崎
Koichi Yamazaki
渊 唐
Yuan Tang
正康 那須
Masayasu Nasu
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Mitsubishi Chemical Engineering Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a separation method and an apparatus of a mixture where the heating cost of the mixture is inexpensive and the contamination of impurities in a product can be avoided.
SOLUTION: In a separation method and an apparatus of a mixture,: a raw material feed liquid including the mixture is evaporated in an evaporator 5; steam from the evaporator 5 is passed in a heat exchanger 9, heat-exchanged with a heat transfer medium (water) and condensed in a condenser 14; steam generated in the heat exchanger 9 is compressed by a compressor 20 and temperature is raised and the raw material feed liquid is heated in a heat exchanger 3; a part of steam from the compressor 20 is passed in a heat exchanger 6 for an evaporator bottom liquid and the raw material feed liquid is heated; and a part of the evaporator bottom liquid is passed in the heat exchanger 2 and the raw material feed liquid is heated.
SELECTED DRAWING: Figure 1
COPYRIGHT: (C)2023,JPO&INPIT

Description

本発明はエタノールと水、イソプロパノールと水などの、沸点の異なる複数成分の混合物を分離処理するための方法及び装置に関するものであり、好適には、混合物を蒸発缶で蒸発させた後、蒸発物から熱を回収する工程を有する混合物の分離方法及び装置に関する。 The present invention relates to a method and apparatus for separating a mixture of multiple components having different boiling points, such as ethanol and water or isopropanol and water. It relates to a method and apparatus for separating a mixture with the step of recovering heat from the

エタノール等のアルコールと水との混合物を蒸発させた後、膜等によってエタノール等と水とに分離する方法及び装置が特許文献１，２に記載されている。 Patent Documents 1 and 2 describe a method and an apparatus for separating ethanol or the like from water by means of a membrane or the like after evaporating a mixture of alcohol such as ethanol and water.

特許文献１では、エタノールおよび水の混合物をエバポレータに供給してエタノールおよび水の該混合物を蒸発させ、エタノールおよび水の気化混合物をコンプレッサにて加圧した後、膜ユニットに供給し、エタノールとエタノール・水混合物とに分離する。 In Patent Document 1, a mixture of ethanol and water is supplied to an evaporator to evaporate the mixture of ethanol and water, the vaporized mixture of ethanol and water is pressurized by a compressor, then supplied to a membrane unit, and ethanol and ethanol are - separates into a water mixture;

特許文献２には、アルコール等と水との混合物を蒸留塔に供給し、留出物を第２圧縮機にて加圧・昇温した後、膜分離器によりアルコール等と、アルコール・水混合物とに分離し、この混合物を蒸留塔に戻すことが記載されている。蒸留塔にはリボイラが設けられている。特許文献２では、蒸留塔留出物の一部を分取して第１圧縮機にて加熱加圧し、このリボイラに加熱源流体として供給し、その後、蒸留塔塔頂に返送する。 In Patent Document 2, a mixture of alcohol or the like and water is supplied to a distillation column, the distillate is pressurized and heated by a second compressor, and then the alcohol or the like is separated from the alcohol/water mixture by a membrane separator. and separating this mixture back into the distillation column. The distillation column is equipped with a reboiler. In Patent Document 2, part of the distillation column distillate is separated, heated and pressurized by a first compressor, supplied to this reboiler as a heat source fluid, and then returned to the top of the distillation column.

特許文献３には、ベンゼンとトルエンなどの混合液を熱交換器で加熱した後、蒸留塔で蒸留し、塔頂留出分をコンプレッサで加圧昇温した後、その一部を該混合液加熱用熱交換器に熱源流体として流通させることが記載されている。 In Patent Document 3, a mixed liquid such as benzene and toluene is heated with a heat exchanger, distilled with a distillation column, and the overhead distillate is pressurized and heated with a compressor. Circulating as a heat source fluid in a heat exchanger for heating is described.

特表２０１１－５１３０５６号公報Japanese Patent Publication No. 2011-513056 特開２０１２－１１０８３２号公報JP 2012-110832 A 特開２０１２－４５４４９号公報JP 2012-45449 A

特許文献１，２のように、エタノール等を含んだ蒸気をコンプレッサ（圧縮機）で加圧すると、コンプレッサにおいてオイル、グリース等の不純物が蒸気に混入し、製品の純度が低下するおそれがある。また、アルコール等の蒸気を加圧するコンプレッサには十分な防火、防爆機構が必要であると共に、コンプレッサに十分な防食性が必要となりコスト高となる。同様の課題は特許文献３でも生じる。特に塔頂留出分を回収目的成分とする場合に不純物混入が問題となる。 As in Patent Documents 1 and 2, when steam containing ethanol or the like is pressurized by a compressor, impurities such as oil and grease may be mixed into the steam in the compressor, which may reduce the purity of the product. In addition, a compressor for pressurizing vapor such as alcohol requires a sufficient fireproof and explosion-proof mechanism, and the compressor also needs a sufficient corrosion resistance, which increases the cost. A similar problem arises in Patent Document 3 as well. In particular, when the overhead distillate is used as the component to be recovered, contamination with impurities becomes a problem.

本発明は、混合物の加熱コストが安価であり、また製品への不純物混入を回避することができる混合物の分離方法及び装置を提供することを目的とする。 SUMMARY OF THE INVENTION An object of the present invention is to provide a method and an apparatus for separating a mixture which can reduce the heating cost of the mixture and avoid contamination of the product with impurities.

本発明の混合物の分離方法は、混合物よりなる原料フィード液を分離器（５）にて分離する分離工程と、分離器（５）からの蒸気を熱交換器（９）で伝熱媒体と熱交換させた後、取り出す工程と、該熱交換器（９）で熱交換した伝熱媒体をコンプレッサ（２０）で加圧昇温させる工程と、該コンプレッサ（２０）からの伝熱媒体の蒸気を原料フィード液加熱用熱交換器（３）に通して原料フィード液を加熱する工程と、該原料フィード液加熱用熱交換器（３）を通過した伝熱媒体を熱交換器（９）に戻す工程とを有するものである。 The method for separating a mixture of the present invention includes a separation step of separating a raw material feed liquid consisting of the mixture in a separator (5), and a heat transfer medium and heat After exchanging, a step of taking out, a step of pressurizing and heating the heat transfer medium heat-exchanged in the heat exchanger (9) with a compressor (20), and removing the steam of the heat transfer medium from the compressor (20) A step of heating the raw feed liquid by passing it through a heat exchanger (3) for heating the raw feed liquid, and returning the heat transfer medium that has passed through the heat exchanger (3) for heating the raw feed liquid to the heat exchanger (9). and a step.

本発明の混合物の分離装置は、混合物よりなる原料フィード液を蒸発させる分離器（５）と、分離器（５）からの蒸気を伝熱媒体と熱交換させる熱交換器（９）と、該熱交換器（９）で熱交換した伝熱媒体を加圧昇温させるコンプレッサ（２０）と、該コンプレッサ（２０）からの伝熱媒体の蒸気によって原料フィード液を加熱する原料フィード液加熱用熱交換器（３）とを有するものである。 The apparatus for separating a mixture of the present invention comprises a separator (5) for evaporating a raw material feed liquid comprising a mixture, a heat exchanger (9) for exchanging heat between the steam from the separator (5) and a heat transfer medium, and A compressor (20) for pressurizing and raising the temperature of the heat transfer medium heat-exchanged by the heat exchanger (9), and heat for heating the raw material feed liquid by means of the vapor of the heat transfer medium from the compressor (20). and an exchanger (3).

本発明の一態様では、前記分離器は蒸発缶（５）であり、該蒸発缶（５）の缶底液の一部を缶底液用熱交換器（６）で加熱する。 In one aspect of the present invention, the separator is an evaporator (5), and part of the bottom liquid of the evaporator (5) is heated by a bottom liquid heat exchanger (6).

本発明の一態様では、前記缶底液の残部を原料フィード液加熱用熱交換器（２）に通して原料フィード液を加熱する。 In one aspect of the present invention, the remaining portion of the bottom liquid is passed through a heat exchanger (2) for heating the raw feed liquid to heat the raw feed liquid.

本発明の一態様では、前記原料フィード液の一部を前記熱交換器（３）からの伝熱媒体が通される熱交換器（２Ａ）によって加熱し、前記原料フィード液の残部を、前記缶底液の残部が通される熱交換器（２Ｂ）によって加熱することを特徴とする。 In one aspect of the present invention, part of the raw material feed liquid is heated by a heat exchanger (2A) through which a heat transfer medium from the heat exchanger (3) passes, and the remainder of the raw material feed liquid is heated by the It is characterized by heating with a heat exchanger (2B) through which the remainder of the bottom liquid is passed.

本発明の一態様では、前記蒸発缶（５）からの蒸気を熱交換器（９）で降温させた後、その一部を蒸発缶（５）に供給する。 In one aspect of the present invention, after the temperature of the steam from the evaporator (5) is lowered by the heat exchanger (9), part of it is supplied to the evaporator (5).

本発明の一態様では、前記混合物は、メタノール・水、エタノール・水、イソプロパノール・水、ブタノール・水、酢酸・水、ＮＭＰ（Ｎ－メチル－２－ピロリドン）・水、ＤＭＦ（ジメチルホルムアミド）・水、ＤＭＡＣ（ジメチルアセトアミド）・水、アセトン・水、トルエン・水、ＴＨＦ（テトラヒドロフラン）・水、又は酢酸エチル・水の混合液であり、前記伝熱媒体は水であることを特徴とする。 In one aspect of the present invention, the mixture comprises methanol/water, ethanol/water, isopropanol/water, butanol/water, acetic acid/water, NMP (N-methyl-2-pyrrolidone)/water, DMF (dimethylformamide)/ Water, DMAC (dimethylacetamide)/water, acetone/water, toluene/water, THF (tetrahydrofuran)/water, or ethyl acetate/water, and the heat transfer medium is water.

本発明では、原料フィード液を原料フィード液加熱用熱交換器で加熱後、蒸発缶や膜分離器等の分離器で分離処理して目的成分の蒸気と、水蒸気等の他成分とに分離する。そして、この目的成分蒸気の保有熱でヒートポンプの伝熱媒体を加熱して気化させ、生じた伝熱媒体の蒸気をコンプレッサで加圧昇温させて、原料フィード液加熱用の熱交換器に循環供給するようにしている。本発明は、伝熱媒体の蒸気をコンプレッサで加圧昇温させるようにしたものであり、特許文献１，２のようにエタノール・水等の混合蒸気をコンプレッサで加圧昇温するものではない。そのため、目的成分への不純物の混入を回避できる。また、原料フィード液の加熱をヒートポンプ方式としているので、原料フィード液の加熱コストを低くすることができる。 In the present invention, the raw material feed liquid is heated by a heat exchanger for heating the raw material feed liquid, and then separated into a target component vapor and other components such as water vapor by a separator such as an evaporator or a membrane separator. . Then, the heat transfer medium of the heat pump is heated and vaporized by the heat contained in the target component vapor, and the generated heat transfer medium vapor is pressurized and heated by the compressor, and circulated to the heat exchanger for heating the raw material feed liquid. I am trying to supply. The present invention pressurizes and heats the steam of the heat transfer medium with a compressor, and does not pressurize and heat a mixed steam of ethanol, water, etc. with a compressor as in Patent Documents 1 and 2. . Therefore, contamination of the target component with impurities can be avoided. Moreover, since the heat pump system is used to heat the raw material feed liquid, the cost of heating the raw material feed liquid can be reduced.

また、本発明の一態様では、蒸発缶の缶底液を加熱する熱交換器の加熱源流体をコンプレッサで加圧昇温させるヒートポンプ方式としているため、蒸発缶の加熱コストを低くすることができる。 Further, in one aspect of the present invention, a heat pump system is used in which the heat source fluid of the heat exchanger that heats the bottom liquid of the evaporator is pressurized and heated by the compressor, so that the heating cost of the evaporator can be reduced. .

本発明の実施の形態を示す系統図である。BRIEF DESCRIPTION OF THE DRAWINGS It is a system diagram which shows embodiment of this invention. 別の実施の形態を示す系統図である。It is a system diagram which shows another embodiment. 別の実施の形態を示す系統図である。It is a system diagram which shows another embodiment.

以下、図面を参照して実施の形態について説明する。 Embodiments will be described below with reference to the drawings.

図１は本発明の一実施の形態を示す系統図であり、混合物（この実施の形態ではエタノール・水混合物）よりなる原料フィード液がポンプから配管１を介して熱交換器２，３に導入され、加熱された後、配管４を介して蒸発缶（エバポレータ）５に供給され、蒸発する。蒸発缶５の缶底液の一部が配管５ａ，５ｂを介して熱交換器６に導入され、加熱後、配管５ｃを介して蒸発缶５に戻される。また、缶底液の残部は、ポンプ５Ｐ、配管１６を介して熱交換器２に導入され、混合物を加熱後、配管１７を介して熱交換器１８で冷却され、系外に取り出される。 FIG. 1 is a system diagram showing one embodiment of the present invention, in which a raw material feed liquid composed of a mixture (a mixture of ethanol and water in this embodiment) is introduced from a pump through a pipe 1 into heat exchangers 2 and 3. After being heated, it is supplied to an evaporator 5 through a pipe 4 and evaporated. A part of the bottom liquid of the evaporator 5 is introduced into the heat exchanger 6 through the pipes 5a and 5b, heated, and then returned to the evaporator 5 through the pipe 5c. The remainder of the bottom liquid is introduced into the heat exchanger 2 through the pump 5P and the pipe 16, heats the mixture, is cooled in the heat exchanger 18 through the pipe 17, and is taken out of the system.

蒸発缶５からの留出分であるエタノール、水の混合蒸気は、配管８から熱交換器９に導入され、凝縮された後、配管１０を介して還流槽１１に導入され、還流槽１１からポンプ１２、配管１３及び熱交換器１４を経て、液体エタノールとして取り出される。ポンプ１２から送り出されたエタノール及び水の一部は、配管１３から分岐した配管１３ａに分流された後、熱交換器１５で冷却され、蒸発缶５の上部に返送される。 The mixed vapor of ethanol and water, which is the distillate from the evaporator 5, is introduced from the pipe 8 into the heat exchanger 9, condensed, and then introduced into the reflux tank 11 through the pipe 10. Through pump 12, pipe 13 and heat exchanger 14, it is taken out as liquid ethanol. A portion of the ethanol and water sent out from the pump 12 is diverted to a pipe 13 a branched from the pipe 13 , cooled by the heat exchanger 15 , and returned to the upper portion of the evaporator 5 .

熱交換器９へは、気液分離器２５内の伝熱媒体としての水が配管３１、ポンプ３２、配管３３を介して導入される。この水が熱交換器９で加熱されて水蒸気が発生し、この水蒸気が気液分離器２５に導入される。気液分離器２５からの水蒸気は、配管２６を介してコンプレッサ２０に送られ、加圧昇温した水蒸気が、配管２２を介して前述の混合物加熱用熱交換器３に供給される。熱交換器３で降温した水蒸気（及び生じた凝縮水）は、配管２３、減圧弁２４を介して気液分離器２５に循環される。 Water as a heat transfer medium in the gas-liquid separator 25 is introduced into the heat exchanger 9 via a pipe 31 , a pump 32 and a pipe 33 . This water is heated by the heat exchanger 9 to generate steam, which is introduced into the gas-liquid separator 25 . The steam from the gas-liquid separator 25 is sent to the compressor 20 through the pipe 26 , and the pressurized and heated steam is supplied through the pipe 22 to the mixture heating heat exchanger 3 . The water vapor (and condensed water produced) whose temperature has been lowered in the heat exchanger 3 is circulated to the gas-liquid separator 25 via the pipe 23 and the pressure reducing valve 24 .

コンプレッサ２０からの高温水蒸気の一部は、配管２１から分岐した配管２７を介して、前述の缶底液加熱用の熱交換器６に供給される。熱交換器６で降温した水蒸気（及び生じた凝縮水）は、配管２８、減圧弁２９を介して気液分離器２５に循環される。 A part of the high-temperature steam from the compressor 20 is supplied to the aforementioned heat exchanger 6 for heating the bottom liquid via a pipe 27 branched from the pipe 21 . The water vapor (and condensed water produced) whose temperature has been lowered in the heat exchanger 6 is circulated to the gas-liquid separator 25 via the pipe 28 and the pressure reducing valve 29 .

この実施の形態では、上記の通り、原料フィード液（エタノール・水混合物）を熱交換器２，３で加熱後、蒸発缶５で蒸発させ、生じた蒸気の保有熱で熱交換器９にてヒートポンプの加熱媒体である水を加熱して気化させ、生じた水蒸気を気液分離器２５及び配管２６を介してコンプレッサ２０で加圧昇温させ、配管２１，２２で混合物加熱用の熱交換器３に供給し、熱交換器３の流出水及び水蒸気を配管２３、減圧弁２４、気液分離器２５を介して熱交換器９に循環供給するようにしている。 In this embodiment, as described above, the raw material feed liquid (ethanol/water mixture) is heated by the heat exchangers 2 and 3 and then evaporated by the evaporator 5. Water, which is the heating medium of the heat pump, is heated and vaporized, and the generated steam is pressurized and heated by the compressor 20 through the gas-liquid separator 25 and the pipe 26, and is connected to the heat exchanger for heating the mixture by the pipes 21 and 22. 3, and the outflow water and steam from the heat exchanger 3 are circulated and supplied to the heat exchanger 9 via a pipe 23, a pressure reducing valve 24, and a gas-liquid separator 25.

このように、この実施の形態では、蒸発缶５で生じたエタノール蒸気と水蒸気との混合蒸気によって熱交換器９でヒートポンプの伝熱媒体（この実施の形態では水）を加熱した後、コンプレッサ２０で加圧昇温し、熱交換器３に導入するようにしており、特許文献１，２のようにエタノール・水の混合蒸気をコンプレッサで加圧昇温しない。そのため、コンプレッサでの不純物混入がなく、得られるエタノールが高純度のものとなる。また、このヒートポンプ方式は加熱コストが低いと共に、コンプレッサ２０は水蒸気を加圧するものであるため、防火、防爆機構が不要ないし簡易化される。 Thus, in this embodiment, after the heat transfer medium (water in this embodiment) of the heat pump is heated in the heat exchanger 9 by the mixed vapor of ethanol vapor and water vapor generated in the evaporator 5, the compressor 20 The mixed steam of ethanol and water is not pressurized and heated by a compressor as in Patent Documents 1 and 2. Therefore, there is no contamination of impurities in the compressor, and the obtained ethanol is of high purity. In addition, since the heat pump system has a low heating cost and the compressor 20 pressurizes steam, the fire prevention and explosion prevention mechanisms are unnecessary or simplified.

この実施の形態では、熱交換器６で缶底液を加熱するように、コンプレッサ２０で加圧昇温させた伝熱媒体（水蒸気）の一部を配管２７で熱交換器６に供給し、熱交換器６からの伝熱媒体を配管２８及び減圧弁２９を介して気液分離器２５に循環させている。 In this embodiment, part of the heat transfer medium (steam) pressurized and heated by the compressor 20 is supplied to the heat exchanger 6 through the pipe 27 so as to heat the bottom liquid in the heat exchanger 6, A heat transfer medium from the heat exchanger 6 is circulated to the gas-liquid separator 25 via a pipe 28 and a pressure reducing valve 29 .

このように、蒸発缶５の缶底液を加熱する熱交換器６の加熱源流体である水蒸気をコンプレッサ２０で加圧昇温させるヒートポンプ方式としているため、蒸発缶５の加熱コストを低くすることができる。 In this way, the heat pump system is adopted in which the compressor 20 pressurizes and raises the temperature of steam, which is the heat source fluid of the heat exchanger 6 that heats the bottom liquid of the evaporator 5, so that the heating cost of the evaporator 5 can be reduced. can be done.

図２，３を参照して別の実施の形態について説明する。 Another embodiment will be described with reference to FIGS.

図２では、原料フィード液の供給用配管１を途中で配管１Ａ，１Ｂに並列状に分岐させ、各配管１Ａ，１Ｂに熱交換器２Ａ，２Ｂを設置し、各配管１Ａ，１Ｂの末端を合流させて熱交換器３に接続している。熱交換器２Ａには熱交換器３の流出伝熱媒体が配管３ａを介して導入される。熱交換器２Ａから流出した伝熱媒体は配管２３及び減圧弁２４を介して気液分離器２５へ循環される。熱交換器２Ｂには、前記配管１６から缶底液の一部が導入される。熱交換器２Ｂから流出した缶底液は、配管１７、熱交換器１８の順に流れる。 In FIG. 2, a raw material feed liquid supply pipe 1 is branched in parallel into pipes 1A and 1B on the way, heat exchangers 2A and 2B are installed in each pipe 1A and 1B, and the ends of each pipe 1A and 1B are connected to each other. They are merged and connected to the heat exchanger 3 . The outflow heat transfer medium of the heat exchanger 3 is introduced into the heat exchanger 2A through a pipe 3a. The heat transfer medium that has flowed out of the heat exchanger 2A is circulated to the gas-liquid separator 25 via the pipe 23 and the pressure reducing valve 24 . A portion of the bottom liquid is introduced from the pipe 16 into the heat exchanger 2B. The bottom liquid that has flowed out of the heat exchanger 2B flows through the pipe 17 and the heat exchanger 18 in this order.

図２のその他の構成は図１と同一であり、同一符号は同一部分を示している。 Other configurations in FIG. 2 are the same as in FIG. 1, and the same reference numerals denote the same parts.

図３では、蒸発缶５がフラッシュドラムとなっている。図３では、図２において、熱交換器９及び熱交換器（凝縮器）１４で冷却されて生じた液体エタノールを凝縮液槽３５に導入し、ポンプ３６で送り出すようにしている。図３では缶底液を加熱するための熱交換器６は省略され、熱交換器６用の配管２７，２８も省略されている。また、フラッシュドラム５上部へのエタノール還流用の配管１３ａ及び熱交換器１５も省略されている。 In FIG. 3, the evaporator 5 is a flash drum. In FIG. 3, the liquid ethanol produced by being cooled by the heat exchanger 9 and the heat exchanger (condenser) 14 in FIG. In FIG. 3, the heat exchanger 6 for heating the bottom liquid is omitted, and the pipes 27 and 28 for the heat exchanger 6 are also omitted. Further, the pipe 13a for refluxing ethanol to the upper portion of the flash drum 5 and the heat exchanger 15 are also omitted.

図３のその他の構成は図２と同一であり、同一符号は同一部分を示している。 Other configurations in FIG. 3 are the same as in FIG. 2, and the same reference numerals denote the same parts.

上記実施の形態では分離器として蒸発缶又はフラッシュドラムが用いられているが、膜分離器、吸着分離器等であってもよい。 Although an evaporator or a flash drum is used as a separator in the above embodiments, a membrane separator, an adsorption separator, or the like may be used.

５ 蒸発缶又はフラッシュドラム
２０ コンプレッサ
２５ 気液分離器
5 evaporator or flash drum 20 compressor 25 gas-liquid separator

Claims (1)

混合物よりなる原料フィード液を分離器（５）にて分離する分離工程と、
分離器（５）からの蒸気を熱交換器（９）で伝熱媒体と熱交換させた後、取り出す工程と、
該熱交換器（９）で熱交換した伝熱媒体をコンプレッサ（２０）で加圧昇温させる工程と、
該コンプレッサ（２０）からの伝熱媒体の蒸気を原料フィード液加熱用熱交換器（３）に通して原料フィード液を加熱する工程と、
該原料フィード液加熱用熱交換器（３）を通過した伝熱媒体を熱交換器（９）に戻す工程と
を有する混合物の分離方法。
A separation step of separating a raw material feed liquid consisting of a mixture in a separator (5);
a step of extracting the steam from the separator (5) after exchanging heat with a heat transfer medium in a heat exchanger (9);
A step of pressurizing and heating the heat transfer medium heat-exchanged in the heat exchanger (9) with a compressor (20);
a step of passing the vapor of the heat transfer medium from the compressor (20) through a heat exchanger (3) for heating the raw feed liquid to heat the raw feed liquid;
and a step of returning the heat transfer medium that has passed through the heat exchanger (3) for heating the feed liquid to the heat exchanger (9).
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