JPH035431A - Method for dehydrating alcohol with propylene - Google Patents
Method for dehydrating alcohol with propyleneInfo
- Publication number
- JPH035431A JPH035431A JP13923689A JP13923689A JPH035431A JP H035431 A JPH035431 A JP H035431A JP 13923689 A JP13923689 A JP 13923689A JP 13923689 A JP13923689 A JP 13923689A JP H035431 A JPH035431 A JP H035431A
- Authority
- JP
- Japan
- Prior art keywords
- propylene
- distillation column
- alcohol
- heat
- pressurized
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims description 25
- 238000004821 distillation Methods 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 230000006835 compression Effects 0.000 claims abstract description 10
- 238000007906 compression Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract 3
- 239000007792 gaseous phase Substances 0.000 abstract 1
- 230000003134 recirculating effect Effects 0.000 abstract 1
- 238000000895 extractive distillation Methods 0.000 description 16
- 239000012071 phase Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 240000008042 Zea mays Species 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- -1 corn Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明はアルコールの４縮精製方法に関し、合成アルコ
ール、使用“済アルコール水溶液及び発酵アルコール等
から高純度のアルコールを省エネルギー的に濃縮精製す
るのに適した方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a four-condensation purification method for alcohol, and is a method for concentrating and refining highly pure alcohol from synthetic alcohol, used alcohol aqueous solution, fermented alcohol, etc. in an energy-saving manner. Regarding methods suitable for
−１「シょ、さつまいも、とうもろごし等の炭水化物を
原料とする発酵アルコールは飲料用及び工業用として重
要な出発原料であるが、発酵法及び合成法で得られるア
ルコール水？’ａ Ｗｌ、のアルコール濃度は１０〜２
０ｗＬ％♂低いため、約９５〜１００ ｗＬ％まで濃縮
する必要がある。-1 "Fermented alcohol made from carbohydrates such as corn, sweet potato, and corn is an important starting material for beverages and industrial use, but alcoholic water obtained by fermentation and synthesis methods?'a Wl , the alcohol concentration is 10-2
Since it is low at 0 wL%♂, it is necessary to concentrate it to about 95-100 wL%.
従来、この濃縮法として蒸留法が用いられてきたが、主
成分アルコール及び水の蒸発潜熱の回収が困難で経済的
に不利であり、これに替わる省エネルギー型のｆＡ縮法
の開発が望まれている。Conventionally, distillation has been used as this concentration method, but it is economically disadvantageous because it is difficult to recover the latent heat of vaporization of the main components alcohol and water, and there is a desire to develop an energy-saving fA reduction method instead. There is.
通常の蒸留法では１０−Ｌ％から９５１％にアルコール
を濃縮するのに約３，０００ ｋｃａｌ／ ｋｇ−アル
コールを要している。又、９５−１％から９９．２ｗｔ
％以上の無水アルコールに蒸留にて：ａｗｉするには、
ジエチルエーテル、ベンゼン、シクロヘキサンなどを用
いた共沸蒸留が行なわれており、約１０００〜２０００
ｋｃａ ｌ ／ ｋｇ−アルコールのエネルギーを要し
省エネルギーが望まれている。Conventional distillation methods require about 3,000 kcal/kg-alcohol to concentrate alcohol from 10-L% to 951%. Also, from 95-1% to 99.2wt
% or more of absolute alcohol by distillation: awi:
Azeotropic distillation is carried out using diethyl ether, benzene, cyclohexane, etc.
Since it requires energy of kcal/kg-alcohol, energy saving is desired.
一方、省エネルギー型の：ａ縮法として超臨界状態又は
擬臨界状態の炭酸ガスを用いてアルコールを水より抽出
・公刊して′ａｗｉする方法が提案されている。（特開
昭５６−５６２旧及び同５９−１４１５２８号公Ｑμ）
しかしながら、炭酸ガスを溶剤として用いた場合、比較
的多量の溶剤を必要とし、又、アルコールの選択的抽出
には限界があり、最大濃縮度しよ約９１ｗｔ％が限界で
あり、これ以−Ｅに濃縮することは不可能であることが
最近報告されている。On the other hand, as an energy-saving method of :a reduction, a method has been proposed in which alcohol is extracted from water using carbon dioxide gas in a supercritical or quasi-critical state and then published. (Japanese Unexamined Patent Publication Nos. 56-562 and 59-141528 Qμ) However, when carbon dioxide gas is used as a solvent, a relatively large amount of solvent is required, and there are limits to the selective extraction of alcohol. It has recently been reported that the maximum concentration is about 91 wt%, and that it is impossible to concentrate beyond this point.
本発明は、既存の蒸留法に較べて大幅に少ないエネルギ
ーで、アルコール濃度９９．２ｗＬ％（無水アルコール
濃度）以上に濃縮する方法を提供しようとするものであ
る。The present invention aims to provide a method for concentrating alcohol to an alcohol concentration of 99.2 wL% (anhydrous alcohol concentration) or higher using significantly less energy than existing distillation methods.
本発明者らは産業上有用な価値を有する純度９９ 、２
ｗ Ｌ％以上の無水エタノールを省エネルギー的に製造
する方法について鋭意検討した結果、原料のアルコール
水溶液に、プロピレン溶剤を抽出溶剤として添加して加
圧抽出蒸留を行なうことにより、容易に無水アルコール
が１７られること及び又、加圧抽出蒸留塔塔頂プロピレ
ンガスを再圧縮循環する際に発生する圧縮熱で加圧抽出
蒸留塔の熱源の大部分を補え、既存の蒸留法に較べて大
幅にエネルギーが節約できることを見出し、本発明を完
成するに至った。The present inventors have found that purity of 99,2 has industrially useful value.
As a result of intensive studies on energy-saving methods for producing anhydrous ethanol of w L% or more, we found that by adding a propylene solvent as an extraction solvent to an aqueous raw material alcohol solution and performing pressurized extractive distillation, anhydrous alcohol can be easily reduced to 17% by weight. Furthermore, the heat of compression generated when the propylene gas at the top of the pressurized extractive distillation column is recompressed and circulated can supplement most of the heat source of the pressurized extractive distillation column, and the energy consumption is significantly greater than that of existing distillation methods. They found that it was possible to save money and completed the present invention.
即ち、本発明はエタノール及び水を主成分とする原ｒ１
を第１蒸留塔の中部に供給し、第１蒸留塔の上部よりプ
ロピレン溶剤を供給し、該第１７Ａ留塔内でプロピレン
の液体と気体が同時に存在する温度、圧力に保持し、該
第１蒸留塔のド部より実質的に水分を含まないエタノー
ルと液体プロピレンを、又該第１蒸留塔上部より実質的
にエタノールを含まない水分と藩気プロピレンを取り出
すことを特徴とする無水アルコール製造方法である。That is, the present invention provides raw material r1 containing ethanol and water as main components.
is supplied to the middle part of the first distillation column, a propylene solvent is supplied from the upper part of the first distillation column, and the temperature and pressure are maintained such that propylene liquid and gas exist simultaneously in the 17A distillation column. A method for producing anhydrous alcohol, characterized in that ethanol and liquid propylene that do not contain substantially water are taken out from the bottom part of the distillation column, and water and liquid propylene that do not contain substantially ethanol are taken out from the upper part of the first distillation column. It is.
そして、上記方法において、第１蒸留塔上部のガス相を
加圧し、その圧縮熱を第１蒸留塔リポイラーの熱源とし
た後、第１蒸留塔上部へ還流すること、及び第１蒸留塔
下部の無水エタノール及びプｒ１ピレン混合液を第２蒸
留塔に導入し、プロピレン溶剤をストリッピングするに
際し、第２蒸留塔上部ガス相を加圧してその圧縮熱を第
２蒸留塔の熱源に用いた後、第２蒸留塔及び第１藩留塔
上部へ還流することを好ましい態様とするものである。In the above method, the gas phase in the upper part of the first distillation column is pressurized, the heat of compression is used as a heat source for the first distillation column repoiler, and then refluxed to the upper part of the first distillation column, and the gas phase in the lower part of the first distillation column is refluxed. After introducing the anhydrous ethanol and propylene mixture into the second distillation column and stripping the propylene solvent, the upper gas phase of the second distillation column is pressurized and the heat of compression is used as a heat source for the second distillation column. A preferred embodiment is to reflux the liquid to the upper part of the second distillation column and the first distillation column.
以下、本発明の一実施態様を第１図に従って詳述し、そ
の作用を明らかにする。Hereinafter, one embodiment of the present invention will be described in detail with reference to FIG. 1, and its operation will be clarified.
第１図において、供給ライン２よりの原料アルコール水
溶液は、製品無水アルコールと熱交換器３７で熱交換さ
れて予熱され、充填塔、多孔板塔、トレイ型塔などの加
圧抽出蒸留塔１の中部に供給される。原料アルコール濃
度は限定されないが、含水アルコール（アルコール４度
９５ｖｏ１％）を原ｒ１とする場合、本発明は最も効率
的となる。In FIG. 1, the raw alcohol aqueous solution from the supply line 2 is preheated by heat exchange with the product absolute alcohol in a heat exchanger 37, and is then preheated in a pressurized extractive distillation column 1 such as a packed column, perforated plate column, or tray type column. Supplied to central Japan. The raw material alcohol concentration is not limited, but the present invention is most efficient when the raw material r1 is hydrous alcohol (4% alcohol, 95 vol%).
加圧抽出蒸留塔１の気液接触部分は通常の蒸Ｗ／に用い
られる各種の充填物、多孔板、各種トレイなど寺用いる
ことができる。The gas-liquid contacting portion of the pressurized extractive distillation column 1 can use various packings, perforated plates, various trays, etc. used in ordinary steaming.
プロピレン溶剤はライン１５．１６より加圧抽出蒸留塔
ｌの上部に供給される。プロピレンのガスと液が共存す
る条件下にアルコール水溶液をおいた場合、アルコール
は親和力の差異により選択的に液体プロピレンに抽出さ
れ、更にアルコールに対して比較的液体プロピレンが多
縦にある条件下では、水分はプロピレン／アルコール６
１４合液体中へは殆ど溶解せず、プロピレンガス相中の
水分濃度が水の飽和濃度以下になるような条件を設定す
ると、水分はプロピレンガス相側へ選択的に移行させる
ことができる。かくしてアルコールと水との分離ができ
、無水アルコールが得られる。このように加圧抽出蒸留
塔１内でブｌ］ピレンのガスと液の両相が共存する条件
とするためには、温度はプロピレンの臨界温度′ｒｃ
＝９２．３°Ｃ以下で、圧力はこの温度における液相組
成に対応した飽和蒸気圧（最大値はブ［１ピレンの臨界
圧力Ｐｃ−４５ａＬ■）にずべきである。またプロピレ
ンのガスと液の比率は原料アルコール濃度及び製品無水
アルコール濃度により変えるべきで、これはプロピレン
のｌ１ｆｆｉ、加圧抽出蒸留塔１０段数及びリポイラー
６．７への熱量の与え方によって調整することができる
。Propylene solvent is fed to the top of the pressurized extractive distillation column 1 via lines 15, 16. When an alcohol aqueous solution is placed under conditions where propylene gas and liquid coexist, alcohol is selectively extracted into liquid propylene due to the difference in affinity. , water is propylene/alcohol 6
By setting conditions such that water hardly dissolves in the 14 mixture liquid and the water concentration in the propylene gas phase is equal to or lower than the saturation concentration of water, water can be selectively transferred to the propylene gas phase side. In this way, alcohol and water can be separated and anhydrous alcohol can be obtained. In order to achieve the conditions in which both the gas and liquid phases of pyrene coexist in the pressurized extractive distillation column 1, the temperature must be set at the critical temperature of propylene 'rc.
= 92.3 DEG C. or less, the pressure should shift to the saturated vapor pressure corresponding to the liquid phase composition at this temperature (the maximum value is the critical pressure of pyrene Pc-45aL). In addition, the ratio of propylene gas and liquid should be changed depending on the raw material alcohol concentration and product absolute alcohol concentration, and this should be adjusted by the l1ffi of propylene, the number of pressurized extractive distillation columns (10 stages), and the method of providing heat to the repoiler 6.7. I can do it.
加圧抽出蒸留塔ｌの塔頂ガス（プロピレンガスと水から
なり、実質的にアルコールは存在しない）はうイン３よ
り取出し、圧縮機４で再圧ｉ宿された後、ライン５を経
てリポイラー６に導き再圧縮によって発止する圧縮熱を
該リポイラー６の熱源として用いるのがよい。加圧抽出
蒸ｆ（ｉ塔１の塔頂と塔底の温度差はＩＯ”ｃ以下にし
ても燥業することができるので、圧縮機４での僅かな圧
縮、すなわち僅かな動力、で塔頂ガス温度を塔底温度以
上に断熱圧縮により昇温することができ、塔頂ガスの凝
縮潜熱をリポイラー６の熱源として十分利用することが
可能となり、既存の蒸留法に較べて大幅にエネルギーの
節約ができる。The top gas (consisting of propylene gas and water, substantially free of alcohol) of the pressurized extractive distillation column 1 is taken out from the inlet 3, recompressed by the compressor 4, and then passed through the line 5 to the repoiler. It is preferable to use the compression heat introduced into the repoiler 6 and generated by recompression as a heat source for the repoiler 6. Pressure extraction steaming f(i) Since drying can be carried out even if the temperature difference between the top and bottom of the column 1 is less than IO"c, the column can be operated with a small amount of compression in the compressor 4, that is, with a small amount of power. The temperature of the top gas can be raised above the bottom temperature by adiabatic compression, and the latent heat of condensation of the top gas can be fully utilized as a heat source for the repoiler 6, which significantly reduces energy consumption compared to existing distillation methods. You can save money.
リポイラー６で熱交換されたプロピレンと水の混合物は
ライン１０を経て水のデカンタ−１１に導入されて水分
とプロピレンに重力沈降分随される。水はうイン１２よ
り抜き出され、プロピレンはライン１３より減圧弁１４
を経てライン１５より加圧抽出蒸留塔ｌへ還流される。The mixture of propylene and water heat-exchanged in the repoiler 6 is introduced into a water decanter 11 through a line 10, where it is gravity-separated into water and propylene. Water is extracted from the inlet 12, and propylene is extracted from the line 13 through the pressure reducing valve 14.
It is then refluxed from line 15 to pressurized extractive distillation column 1.
次に、加圧抽出蒸留塔ｌの塔底液抜出しライン８からは
、実質的に水を含まない無水アルコールと液体プロピレ
ンの混合物が後出され、該混合物は加圧抽出蒸留塔１の
塔底レベル制」弁９を備えたうイン１７を経て熱交換３
１Ｂに導かれ、ここで昇温され、史にライン１９を経て
熱交換器２０に導かれて更に昇温された後、ライン２１
を経てストリッパー２２の中部に導入される。このスト
リッパー２２は加圧蒸留塔であり、気液接触部分は通常
蒸留で用いられる各種充填物、多孔板、各種トレイなど
を用いることができる。このストリンパ−２２の圧力は
加圧抽出蒸留塔ｌとの圧力差ができるだけ小さくなるよ
うにするのが好ましい。Next, a mixture of absolute alcohol and liquid propylene substantially free of water is discharged from the bottom liquid withdrawal line 8 of the pressure extractive distillation column 1; Heat exchanger 3 via inlet 17 with level system valve 9
1B, where it is heated, and then passed through line 19 to heat exchanger 20, where it is further heated, and then into line 21.
It is introduced into the middle part of the stripper 22 through the process. This stripper 22 is a pressurized distillation column, and the gas-liquid contact portion can use various packings, perforated plates, various trays, etc. that are normally used in distillation. It is preferable that the pressure of this stripper 22 is set such that the pressure difference between it and the pressure extractive distillation column 1 is as small as possible.
ストリッパー２２の塔頂ガス（実質的にアルコールヲ含
まないプロピレンガス）はうイン２３より取出され、前
記ライン１７の液体（無水アルコールと液体プロピレン
の混合物）温度より５〜】０°Ｃ以ト高瓜になるように
圧縮機２４で僅かに断熱圧縮され、ライン２５を経て前
記熱交Ｉ！Ｊ！器１８に導かれ、ここでライン２５のプ
ロピレンガスの凝縮層熱の大部分と顕熱の一部を前記ラ
イン１７の流体に与える。かくすることによってストリ
ッパー２２の熱源の大部分を補うことができる。熱交換
３１Ｂで昇４された流体はライン１９を経て更に熱交換
器２０により昇温され、ライン２１を経てストリッパー
２２の中部に供給される。The top gas of the stripper 22 (propylene gas that does not substantially contain alcohol) is taken out from the inlet 23 and is 5 to 0°C higher than the temperature of the liquid (mixture of absolute alcohol and liquid propylene) in the line 17. It is slightly adiabatic compressed by the compressor 24 so that it becomes a melon, and then passed through the line 25 to the heat exchanger I! J! 18, where it imparts most of the condensation bed heat and some of the sensible heat of the propylene gas in line 25 to the fluid in line 17. In this way, most of the heat source of the stripper 22 can be supplemented. The fluid raised in the heat exchanger 31B passes through a line 19, is further heated by a heat exchanger 20, and is supplied to the middle part of the stripper 22 via a line 21.
一方、熱交換器１８でライン１７の液体に熱を与えて降
温したライン２６のプロピレンはデカンタ−２７に導入
され、水はライン２８より抜出され、実質的に水を含ま
ないプロピレンは、ライン２９より取出され、ここでラ
イン３０とライン３１に分流され、ライン３０に分流さ
れたプロピレンは減圧弁３９を経て前記の加圧抽出蒸留
塔１の」二部にライン１６を介して循環され、ライン３
１に分流されたプロピレンは減圧弁３８を経てライン３
２を介してストリッパー２２の上部に還流される。On the other hand, the propylene in the line 26 whose temperature has been lowered by applying heat to the liquid in the line 17 in the heat exchanger 18 is introduced into the decanter 27, water is drawn out from the line 28, and propylene substantially free of water is transferred to the line 26. 29, where it is divided into lines 30 and 31, and the propylene divided into line 30 is circulated through the pressure reducing valve 39 to the second part of the pressurized extractive distillation column 1 through the line 16, line 3
The propylene branched to line 1 passes through pressure reducing valve 38 to line 3.
2 to the upper part of the stripper 22.
−・方、ストリッパー２２の塔底からは実質的にプロピ
レンを含まない無水アルコール（エタノール９９．２ｗ
Ｌ％以上）がライン３３より抜出される。- On the other hand, from the bottom of the stripper 22, anhydrous alcohol (ethanol 99.2 w
L% or more) is extracted from line 33.
ライン３３から抜出された無水アルコールの温度は、加
圧下のアルコールの沸点であり、約８０゛Ｃ以上である
ため、ライン３５を経て熱交換器２０に導かれ、ここで
前記ライン１９の流体の昇温に利用され、更に熱交換器
３７に導かれ、ここでライン２の原料アルコールの予熱
に利用されて熱回収され、常温の無水アルコールとなっ
てライン３６より製品として取出される。Since the temperature of the absolute alcohol extracted from line 33 is the boiling point of alcohol under pressure, which is about 80°C or higher, it is led to heat exchanger 20 via line 35, where the water in line 19 is The alcohol is used to raise the temperature of the alcohol, and is further led to the heat exchanger 37, where it is used to preheat the raw alcohol in the line 2 and recovers the heat, becoming anhydrous alcohol at room temperature and taken out as a product from the line 36.
なお３４はストリッパー２２のりボイラーであって、ラ
イン３３より抜出されたストリッパー２２の塔底液の一
部が該リポイラー３４を経由してストリッパー２２に還
流されるようになっている。Note that 34 is a boiler for the stripper 22, and a part of the bottom liquid of the stripper 22 extracted from the line 33 is refluxed to the stripper 22 via the repoiler 34.
以下、本発明の実施例をあげて本発明の詳細な説明する
。Hereinafter, the present invention will be explained in detail by giving examples of the present invention.
（実施例１）
内径１００ｍｍ 、高さ４ｍの充填塔式加圧抽出蒸留塔
において、原料（エタノール９５−１％、水５ｗＬ％）
を１００ ｇ ／ ｂで中部より供給し、プロピレン液
体をｓ、ｏｏｏｇ／ｈで上部より供給し、圧力’） ｋ
ｇ ／ ｃ＋＊”Ｇの条件下で加圧抽出蒸留を行なった
。この結果、塔底は温度２５°Ｃ１塔頂は温度２０°Ｃ
となり温度差は僅かに５ ’Ｃにすることができた。(Example 1) In a packed column type pressurized extractive distillation column with an inner diameter of 100 mm and a height of 4 m, raw materials (ethanol 95-1%, water 5 wL%)
is supplied from the middle at 100 g/b, propylene liquid is supplied from the top at s,ooog/h, and the pressure is ')k.
Pressure extractive distillation was carried out under the conditions of g/c+*”G. As a result, the temperature at the bottom of the column was 25°C, and the temperature at the top was 20°C.
Therefore, the temperature difference could be reduced to just 5'C.
又、塔底及び塔頂からの抜出し量は次のとおりであった
。In addition, the amounts extracted from the bottom and top of the tower were as follows.
塔底液は、プロピレンを容易に分離でき、その結果、専
売法及びＪＩＳ規格を満たす純度の無水エタノールが得
られた。Propylene could be easily separated from the bottom liquid, and as a result, anhydrous ethanol with a purity that met the proprietary method and JIS standards was obtained.
（実施例２）
実施例１の結果をもとに、第１図に示すプロセスの最適
化を行ない、所要エネルギーを求めた。(Example 2) Based on the results of Example 1, the process shown in FIG. 1 was optimized and the required energy was determined.
（＋１ 操作条件
加圧抽出蒸留塔Ｉ
圧 力 ９ ｋｇ ／ ｃｍ”Ｇ温 度
２０℃ （塔頂）
２５”Ｃ（塔底）
原 料 １００ｇ ／ ｈ（９５ｗＬ％エタノール）
プロピレン ５０００ ｇ／ｈ （ライン１５と１６
の合計）
・ストリッパー２２
圧 力
温度
８ ｋｇ ／ ｃｍ”Ｇ
１６“Ｃ（塔頂）
１５０°Ｃ（塔底）
０．５（ライン２９に対するライ
ン３１流量比）
還流比
・圧縮機４
人［１３
出口５
温 度 ２０℃
圧 力 ９ ｋｇ ／ ｃｓ”Ｇ温 度 ３
５℃
圧 力 １３ｋｇ ／ ｃｔｍ”Ｇ−圧縮機２４
人口２３ 温 度 １６°Ｃ
圧 力 ８ ｋｇ ／ ＣＩＩ”Ｇ出口２５ ４
度 ５２°Ｃ
圧 力 １９ｋｇ／ｃｍ’（。(+1 Operating conditions Pressure extractive distillation column I Pressure 9 kg/cm"G Temperature
20℃ (tower top) 25”C (tower bottom) Raw material 100g/h (95wL% ethanol)
Propylene 5000 g/h (lines 15 and 16
・Stripper 22 Pressure Temperature 8 kg/cm"G 16"C (tower top) 150°C (tower bottom) 0.5 (line 31 flow rate ratio to line 29) Reflux ratio ・Compressor 4 people [13 Outlet 5 Temperature 20℃ Pressure 9 kg/cs”G Temperature 3
5℃ Pressure 13kg/ctm"G-Compressor 24 Population 23 Temperature 16°C Pressure 8kg/CII"G outlet 25 4
Degree: 52°C Pressure: 19kg/cm' (.
（２）無水エタノール１ｋｇを製造するに必要なエネル
ギーは、
となり、既存の蒸留法の約１７５〜Ｉ／ｌｏの所要エネ
ルギーであった。(2) The energy required to produce 1 kg of absolute ethanol is as follows, which is the energy required by the existing distillation method of about 175 to I/lo.
（実施例３）
実施例１において、圧力を種々変化させたテストを行な
い以Ｆの結果をＩＪた。(Example 3) In Example 1, tests were conducted with various pressure changes, and the following results were obtained.
果を奏する。play the fruit.
第１図は本発明を実施ずのためのプロセスフローである
。
いずれの条件下でも、塔頂と塔底の温度差は小さく、か
つ専売法及びＪＩＳ ＭＪ、格の濃度９９．２ｉｙＬ％
を満たず無水エタノールが１１られた。
（発明の効果）FIG. 1 is a process flow for implementing the present invention. Under all conditions, the temperature difference between the top and bottom of the column was small, and the concentration was 99.2iyL% according to the proprietary law and JIS MJ.
11% of absolute ethanol was used. (Effect of the invention)
Claims (3)
塔の中部に供給し、第１蒸留塔の上部よりプロピレン溶
剤を供給し、該第１蒸留塔内でプロピレンの液体と気体
が同時に存在する温度、圧力に保持し、該第１蒸留塔の
下部より実質的に水分を含まないエタノールと液体プロ
ピレンを、又該第１蒸留塔上部より実質的にエタノール
を含まない水分と蒸気プロピレンを取り出すことを特徴
とするプロピレンによるアルコールの脱水方法。(1) A raw material mainly composed of ethanol and water is supplied to the middle of the first distillation column, and a propylene solvent is supplied from the upper part of the first distillation column, so that the propylene liquid and gas are simultaneously produced in the first distillation column. ethanol and liquid propylene that do not contain substantially water from the lower part of the first distillation column, and water and vapor propylene that does not contain substantially ethanol from the upper part of the first distillation column. A method for dehydrating alcohol using propylene, which is characterized by removing alcohol.
第１蒸留塔リポイラーの熱源とした後、第１蒸留塔上部
へ還流する特許請求範囲第（１）項に記載の方法。(2) The method according to claim 1, in which the gas phase in the upper part of the first distillation column is pressurized, the heat of compression is used as a heat source for the first distillation column repoiler, and then the gas phase is refluxed to the upper part of the first distillation column. .
混合液を第２蒸留塔に導入し、プロピレン溶剤をストリ
ッピングするに際し、第２蒸留塔上部ガス相を加圧して
その圧縮熱を第２蒸留塔の熱源に用いた後、第２蒸留塔
及び第１蒸留塔上部へ還流する特許請求範囲第（１）項
記載の方法。(3) When the anhydrous ethanol and propylene mixture at the bottom of the first distillation column is introduced into the second distillation column and the propylene solvent is stripped, the gas phase at the top of the second distillation column is pressurized and the heat of compression is transferred to the second distillation column. The method according to claim (1), wherein the method is used as a heat source for the column and then refluxed to the second distillation column and the upper part of the first distillation column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13923689A JPH035431A (en) | 1989-06-02 | 1989-06-02 | Method for dehydrating alcohol with propylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13923689A JPH035431A (en) | 1989-06-02 | 1989-06-02 | Method for dehydrating alcohol with propylene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH035431A true JPH035431A (en) | 1991-01-11 |
Family
ID=15240645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13923689A Pending JPH035431A (en) | 1989-06-02 | 1989-06-02 | Method for dehydrating alcohol with propylene |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH035431A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5294304A (en) * | 1989-11-14 | 1994-03-15 | Ministry Of International Trade And Industry | Process for the recovery of absolute ethanol by vapor compression extractive distillation |
| US7699961B2 (en) | 2001-10-19 | 2010-04-20 | Mitsubishi Chemical Corporation | Apparatus for concentrating water-soluble organic material |
| JP2015134321A (en) * | 2014-01-17 | 2015-07-27 | 東洋エンジニアリング株式会社 | Distillation tower |
-
1989
- 1989-06-02 JP JP13923689A patent/JPH035431A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5294304A (en) * | 1989-11-14 | 1994-03-15 | Ministry Of International Trade And Industry | Process for the recovery of absolute ethanol by vapor compression extractive distillation |
| US7699961B2 (en) | 2001-10-19 | 2010-04-20 | Mitsubishi Chemical Corporation | Apparatus for concentrating water-soluble organic material |
| JP2015134321A (en) * | 2014-01-17 | 2015-07-27 | 東洋エンジニアリング株式会社 | Distillation tower |
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