JP2003170001A - Thin film evaporator - Google Patents
Thin film evaporatorInfo
- Publication number
- JP2003170001A JP2003170001A JP2001373671A JP2001373671A JP2003170001A JP 2003170001 A JP2003170001 A JP 2003170001A JP 2001373671 A JP2001373671 A JP 2001373671A JP 2001373671 A JP2001373671 A JP 2001373671A JP 2003170001 A JP2003170001 A JP 2003170001A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- film evaporator
- evaporator
- wall surface
- main body
- 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
- 239000010409 thin film Substances 0.000 title claims abstract description 60
- 239000007788 liquid Substances 0.000 claims abstract description 70
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 230000008020 evaporation Effects 0.000 claims abstract description 14
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 15
- 150000002148 esters Chemical class 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 abstract 1
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 8
- 239000003112 inhibitor Substances 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- -1 2-ethylhexyl Chemical group 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- CYUZOYPRAQASLN-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid Chemical compound OC(=O)CCOC(=O)C=C CYUZOYPRAQASLN-UHFFFAOYSA-N 0.000 description 1
- 101710192523 30S ribosomal protein S9 Proteins 0.000 description 1
- 102100032768 Complement receptor type 2 Human genes 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 101000941929 Homo sapiens Complement receptor type 2 Proteins 0.000 description 1
- 101000917858 Homo sapiens Low affinity immunoglobulin gamma Fc region receptor III-A Proteins 0.000 description 1
- 101000917839 Homo sapiens Low affinity immunoglobulin gamma Fc region receptor III-B Proteins 0.000 description 1
- 102100029185 Low affinity immunoglobulin gamma Fc region receptor III-B Human genes 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 101100219325 Phaseolus vulgaris BA13 gene Proteins 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- XPLSDXJBKRIVFZ-UHFFFAOYSA-L copper;prop-2-enoate Chemical compound [Cu+2].[O-]C(=O)C=C.[O-]C(=O)C=C XPLSDXJBKRIVFZ-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229910001026 inconel Inorganic materials 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229950000688 phenothiazine Drugs 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、内部に攪拌翼が取
り付けられた回転軸を有する薄膜蒸発器に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thin film evaporator having a rotary shaft inside which a stirring blade is attached.
【０００２】[0002]
【従来の技術】外面に加熱手段、上部に液供給口と蒸気
抜出口、下部に残渣排出口を有している、主体部が円筒
状の蒸発器本体と、その内部に設置されている回転軸
と、これに取り付けられていて蒸発器本体の内壁面に沿
って周方向に移動する攪拌翼とを有する縦型薄膜蒸発器
は公知である。この薄膜蒸発器では、加熱手段の設けら
れている外面に対応する内面が伝熱面であり、上部の液
供給口より供給された被処理液は、回転する攪拌翼によ
って円筒内壁面上に膜状に押し広げられ、この液膜が重
力によって落下する過程で、加熱手段により供給された
熱により被処理液中の低沸点成分を蒸発させるというも
のである。この装置は、被処理液中の低沸点成分を短時
間で蒸発させることが可能なため、熱に対して敏感な物
質、例えば昜重合性化合物を含んだ液を処理するには好
適である。また、処理液が回転する攪拌翼によって強力
に攪拌され、伝熱面と接する液が常に新しい液と更新さ
れるため、被処理液が局部的に過熱されて、液の焦げ付
きやスケーリングが発生しにくいという利点がある。2. Description of the Related Art An evaporator main body having a cylindrical main body having a heating means on the outer surface, a liquid supply port and a vapor discharge port on the upper part, and a residue discharge port on the lower part, and a rotation installed inside the evaporator main body. A vertical thin film evaporator having a shaft and a stirring blade attached to the shaft and moving in the circumferential direction along the inner wall surface of the evaporator body is known. In this thin film evaporator, the inner surface corresponding to the outer surface on which the heating means is provided is a heat transfer surface, and the liquid to be treated supplied from the upper liquid supply port forms a film on the inner wall surface of the cylinder by a rotating stirring blade. The liquid having a low boiling point in the liquid to be treated is vaporized by the heat supplied by the heating means in the process of being spread in a circular shape and dropping the liquid film by gravity. This apparatus can evaporate low-boiling components in the liquid to be treated in a short time, and is therefore suitable for treating a liquid containing a substance sensitive to heat, for example, a sol-polymerizable compound. Further, the processing liquid is strongly stirred by the rotating stirring blades, and the liquid in contact with the heat transfer surface is constantly updated with a new liquid, so that the liquid to be processed is locally overheated, causing the liquid to burn or scale. It has the advantage of being difficult.
【０００３】回転軸への攪拌翼の取り付け方には多くの
方式があるが、たとえば可動翼式では攪拌翼は支点、ま
たはスプリングを介して回転軸に取り付けられ、回転軸
に関して円周方向に動くことが出来るようになっている
ため、回転軸の回転により、遠心力によって円筒の内壁
面と接触しながら、或いはこれとわずかな隙間を保ちな
がら回転する。There are many methods for attaching the stirring blade to the rotary shaft. For example, in the movable blade type, the stirring blade is attached to the rotary shaft via a fulcrum or a spring and moves in the circumferential direction with respect to the rotary shaft. Therefore, the rotation of the rotating shaft causes the centrifugal force to rotate while being in contact with the inner wall surface of the cylinder, or while maintaining a slight gap therebetween.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、（メ
タ）アクリル酸やそのエステル（本明細書において（メ
タ）アクリル酸とはアクリル酸及びメタクリル酸の両者
を意味する。）の蒸留精製に際し、蒸留塔の塔底から排
出される（メタ）アクリル酸やそのエステルを含む重質
成分から、薄膜蒸発器を用いて（メタ）アクリル酸やそ
のエステルを回収しようとすると、薄膜蒸発器の集液部
の出口部分や液抜出管がしばしば閉塞を起こすという問
題がある。本発明者らはその原因を追究した結果、薄膜
蒸発器の内壁面上を流下してきた液が、攪拌翼の下端よ
りも下方の内壁面上で重合すること、及び薄膜蒸発器に
導入された液が濃縮されることにより、予め添加されて
いた（メタ）アクリル酸やそのエステル用の重合防止剤
が析出すること、によるものであることを見いだした。
すなわち薄膜蒸発器では、蒸発が起こる伝熱面上の液膜
を攪拌翼が攪拌するように構成されており、伝熱面より
下方の内壁面部分、特に円筒状部分に続く逆円錐形状、
又は逆円錐形と円筒形とを組み合わせた漏斗状の集液部
には攪拌翼の設置がされていない。従って、この部分で
は、流下する液は低沸点成分が大部分除去されており本
来的に流動性が良くないことに加えて、攪拌翼による攪
拌がないので、内壁面と接している液は新しい液と更新
され難い。その結果、内壁面と接している液の帯留時間
が異常に長くなり、液中に残存している（メタ）アクリ
ル酸やそのエステルが徐々に重合して液が重質化する。
これにより、この液の流動性はますます小さくなり、内
壁面上に重合物が堆積するようになる。また液が濃縮さ
れることにより、予め添加されていた（メタ）アクリル
酸やそのエステル用の重合防止剤が析出するようにな
る。堆積した重合物及び析出物は、液の流れを阻害する
だけでなく、これらが内壁面から剥離すると集液部の出
口部分やこれに続く液抜出管を閉塞する。従って、本発
明はこの様な閉塞を生じない薄膜蒸発器を提供すること
を目的とする。However, when distilling and purifying (meth) acrylic acid or its ester (in this specification, (meth) acrylic acid means both acrylic acid and methacrylic acid), a distillation column is used. When attempting to recover (meth) acrylic acid and its ester from a heavy component containing (meth) acrylic acid and its ester discharged from the bottom of the column using a thin film evaporator, There is a problem that the outlet part and the liquid extraction pipe often block. As a result of investigating the cause, the inventors have found that the liquid flowing down on the inner wall surface of the thin film evaporator is polymerized on the inner wall surface below the lower end of the stirring blade, and is introduced into the thin film evaporator. It was found that the concentration of the liquid causes precipitation of a polymerization inhibitor for (meth) acrylic acid or its ester that had been added in advance.
That is, in the thin film evaporator, the stirring blade is configured to agitate the liquid film on the heat transfer surface where evaporation occurs, and the inner wall surface portion below the heat transfer surface, particularly the inverted cone shape following the cylindrical portion,
Alternatively, a stirring blade is not installed in the funnel-shaped liquid collecting section that is a combination of an inverted conical shape and a cylindrical shape. Therefore, in this part, most of the low-boiling components are removed from the liquid flowing down, and the fluidity is inherently poor, and since there is no stirring by the stirring blade, the liquid in contact with the inner wall surface is new. It is hard to be updated with liquid. As a result, the retention time of the liquid in contact with the inner wall surface becomes abnormally long, and the (meth) acrylic acid and its ester remaining in the liquid gradually polymerize to become heavy.
As a result, the fluidity of this liquid becomes smaller and smaller, and the polymer is deposited on the inner wall surface. Further, by concentrating the liquid, the polymerization inhibitor for (meth) acrylic acid or its ester that has been added in advance is deposited. The deposited polymer and precipitate not only hinder the flow of the liquid, but when they are separated from the inner wall surface, they block the outlet part of the liquid collecting part and the liquid drain pipe that follows it. Therefore, it is an object of the present invention to provide a thin film evaporator that does not cause such blockage.
【０００５】[0005]
【課題を解決するための手段】本発明に係る薄膜蒸発器
は、攪拌翼の下端よりもさらに下方の内壁面部分にも、
この内壁面に接して周方向に移動するワイパーを有する
ことを特徴とするものである。これにより薄膜蒸発器の
攪拌翼の下端よりもさらに下方の内壁面上に堆積物が生
ずるのを防止し、薄膜蒸発器を長期間安定して運転させ
ることができる。The thin film evaporator according to the present invention has an inner wall surface portion further below the lower end of the stirring blade.
It is characterized by having a wiper which is in contact with the inner wall surface and moves in the circumferential direction. As a result, it is possible to prevent deposits from being formed on the inner wall surface below the lower end of the stirring blade of the thin film evaporator, and to operate the thin film evaporator stably for a long period of time.
【０００６】[0006]
【発明の実施の形態】本発明に係る薄膜蒸発器は、公知
の薄膜蒸発器と同じく、外面に加熱手段、上部に液供給
口と蒸気抜出口、下部に残渣排出口を有している、主体
部が円筒状の蒸発器本体と、その内部に設置されている
回転軸と、これに取り付けられていて蒸発器本体の内壁
面に沿って周方向に移動する攪拌翼とを有している。こ
の様な薄膜蒸発器の代表的な例としては、スミス式薄膜
蒸発器やＬｕｗａ薄膜蒸発器などが挙げられる。薄膜蒸
発器本体部の下部にある集液部の形状は、蒸発残渣がス
ムーズに残渣排出口から液抜出管に流入するように、蒸
発面に対して傾斜を持つ様な形状とするのが望ましいと
されており、集液部の形状が逆円錐状や逆円錐形と円筒
形の形状を組み合わせた漏斗状の形状のものが実用化さ
れている。BEST MODE FOR CARRYING OUT THE INVENTION The thin film evaporator according to the present invention has a heating means on the outer surface, a liquid supply port and a vapor discharge port on the upper part, and a residue discharge port on the lower part, like a known thin film evaporator. The main body has a cylindrical evaporator main body, a rotary shaft installed inside the main body, and a stirring blade attached to the main body and moving in the circumferential direction along the inner wall surface of the evaporator main body. . Representative examples of such a thin film evaporator include a Smith type thin film evaporator and a Luwa thin film evaporator. The shape of the liquid collecting section at the bottom of the thin film evaporator main body should be a shape that is inclined with respect to the evaporation surface so that the evaporation residue can smoothly flow into the liquid extraction pipe from the residue discharge port. It is considered to be desirable, and the shape of the liquid collecting portion has been put into practical use in the shape of an inverted cone or a funnel shape in which an inverted cone shape and a cylindrical shape are combined.
【０００７】本発明に係る薄膜蒸発器は、この様な公知
の薄膜蒸発器において、回転軸に取り付けられている攪
拌翼の下端に対応する内壁面よりもさらに下方の内壁面
に接して、周方向に移動するワイパーを備えている。攪
拌翼は液膜からの蒸発を促進する為のものであるから、
通常は伝熱面に対応する位置に有り、攪拌翼の下端は伝
熱面の下端とほぼ同じ位置になる。The thin-film evaporator according to the present invention is such a known thin-film evaporator that the inner wall surface further lower than the inner wall surface corresponding to the lower end of the stirring blade attached to the rotary shaft is contacted with the peripheral wall. Equipped with a wiper that moves in the direction. Since the stirring blade is for promoting evaporation from the liquid film,
Usually, it is located at a position corresponding to the heat transfer surface, and the lower end of the stirring blade is almost at the same position as the lower end of the heat transfer surface.
【０００８】従って、本発明においてはワイパーは伝熱
面より下方の非伝熱面に対応するように取り付ける。例
えば、円筒状の薄膜蒸発器本体の下部が非伝熱面となっ
ている場合には、この部分に対応するようにワイパーを
取り付ける。円筒状の薄膜蒸発器本体に、逆円錐状や逆
円錐形と円筒形とを組み合わせた漏斗状の集液部が接続
されている場合には、この集液部に対応するようにワイ
パーを取り付ける。取り付けるワイパーは１個であって
も良く、また幾つかに分割されていても良い。なお、ワ
イパーは通常、これらの部分の全面に対応するように取
り付けるのが好ましいが、非伝熱面上に蒸発残渣が堆積
するのを防止するというワイパーの目的が達成される限
り、必ずしも全面に取り付ける必要はない。ワイパーは
通常、薄膜形成の為の攪拌翼が取り付けられている回転
軸、ないしはそれを下方に延長した軸上に取り付ける。
これにより、攪拌翼とワイパーの駆動源を共用すること
ができ、装置の構造を簡単にすることができる。また、
ワイパーの取り付け方式は任意であるが、攪拌翼と同じ
く、支点またはスプリングを介して回転軸に取り付け、
回転軸に関して円周方向に動くことが出来るような可動
翼式で取り付けるのが望ましい。Therefore, in the present invention, the wiper is attached so as to correspond to the non-heat transfer surface below the heat transfer surface. For example, when the lower part of the cylindrical thin film evaporator main body has a non-heat transfer surface, the wiper is attached so as to correspond to this part. If a cylindrical thin-film evaporator body is connected to a funnel-shaped collection part that is an inverted conical shape or a combination of an inverted conical shape and a cylindrical shape, install a wiper to correspond to this collection part. . The wiper to be attached may be one piece or may be divided into several pieces. Although it is usually preferable to install the wiper so as to correspond to the entire surface of these portions, as long as the purpose of the wiper to prevent the evaporation residue from being deposited on the non-heat transfer surface is achieved, it is not necessary to install the wiper on the entire surface. No need to install. The wiper is usually mounted on a rotating shaft to which a stirring blade for forming a thin film is attached, or on a shaft extending downward.
As a result, the stirring blade and the wiper drive source can be shared, and the structure of the device can be simplified. Also,
The method of attaching the wiper is arbitrary, but like the stirring blade, it is attached to the rotating shaft via a fulcrum or spring,
It is desirable to mount the movable blades so that they can move in the circumferential direction about the rotation axis.
【０００９】ワイパーを構成する材質としては、薄膜蒸
発器で処理する被処理液の物性に合わせた材質を選定す
ればよい。例えば、被処理液がアクリル酸等の腐食性の
高い液である場合には、ＳＵＳ３０４、ＳＵＳ３１６、
ＳＵＳ３１６Ｌ、ＳＵＳ３１７、ＳＵＳ３１７Ｌ、ＳＵ
Ｓ３２９ＪＬ、ＳＵＳ３２９Ｊ２Ｌ等のステンレス鋼、
或いはハステロイ類、インコネル類等のニッケル合金類
を挙げることが出来るが、耐食性、経済性の点からＳＵ
Ｓ３０４、ＳＵＳ３１６、ＳＵＳ３１６Ｌが好ましい。
また、ワイパーの薄膜蒸発器内面と物理的に接触する部
分の材質としては、薄膜蒸発器の内壁面を傷つけないよ
うな材質のものを用いるのが望ましい。好ましくはカー
ボンに樹脂や金属を真空加圧含浸させ、機械的強度及び
耐シール性を向上させた、高温下においても使用可能な
ハイブリットカーボン、例えば、日本カーボン（株）製
のスライディングコンポジットカーボン ＮＣ−０７Ｅ
や、テフロン（登録商標）等の薄膜蒸発器内壁面を傷つ
けず、腐食に強いものを用いる。中でも好ましいのは長
期形状安定性に優れ、高温下においても使用可能なハイ
ブリットカーボンである。The material for the wiper may be selected according to the physical properties of the liquid to be treated in the thin film evaporator. For example, when the liquid to be treated is a highly corrosive liquid such as acrylic acid, SUS304, SUS316,
SUS316L, SUS317, SUS317L, SU
Stainless steel such as S329JL and SUS329J2L,
Alternatively, nickel alloys such as hastelloys and inconel can be mentioned, but in view of corrosion resistance and economy, SU
S304, SUS316, and SUS316L are preferable.
Further, as the material of the portion of the wiper that physically contacts the inner surface of the thin film evaporator, it is desirable to use a material that does not damage the inner wall surface of the thin film evaporator. Preferably, carbon is vacuum-impregnated with a resin or a metal to improve mechanical strength and seal resistance, and hybrid carbon that can be used even under high temperature, for example, sliding composite carbon NC- manufactured by Nippon Carbon Co., Ltd. 07E
Also, a material such as Teflon (registered trademark) that does not damage the inner wall surface of the thin film evaporator and is resistant to corrosion is used. Among these, hybrid carbon is preferable because it has excellent long-term shape stability and can be used even at high temperatures.
【００１０】本発明に係る薄膜蒸発器は、常用の薄膜蒸
発器と同じく、種々の被処理液から低沸点成分を蒸発さ
せるのに用いることができるが、特に熱により重合し易
い成分を含む被処理液から低沸点成分を蒸発させるのに
好適である。この様な被処理液としては（メタ）アクリ
ル酸やそのエステルを蒸留精製するに際し、塔底から排
出される（メタ）アクリル酸やそのエステルが残存して
いる重質成分が挙げられる。（メタ）アクリル酸エステ
ルの例としてはメチル、エチル、ブチル、イソブチル、
ターシャリーブチル、２−エチルヘキシル、２−ヒドロ
キシエチル、２−ヒドロキシプロピル、メトキシエチル
等を挙げることができる。The thin film evaporator according to the present invention can be used to evaporate low-boiling components from various liquids to be treated, like the conventional thin film evaporators. It is suitable for evaporating low-boiling components from the treatment liquid. Examples of such a liquid to be treated include a heavy component in which (meth) acrylic acid and its ester are discharged from the bottom of the column when distilling and purifying (meth) acrylic acid and its ester. Examples of (meth) acrylic acid ester include methyl, ethyl, butyl, isobutyl,
Examples thereof include tertiary butyl, 2-ethylhexyl, 2-hydroxyethyl, 2-hydroxypropyl, methoxyethyl and the like.
【００１１】また、これらの重合し易いものの蒸留精製
に際しては、一般に液中に重合防止剤を添加することが
行われている。例えばアクリル酸の蒸留精製に際して
は、ハイドロキノン、ハイドロキノンモノメチルエーテ
ル等のフェノール系の重合防止剤や、フェノチアジン、
Ｎ−オキシル化合物など有機物や、ジアルキルジチオカ
ルバミン酸銅、アクリル酸銅、酢酸銅等の銅塩が一般に
用いられている。従って蒸留塔の塔底から排出される塔
底液にはこれらの重合防止剤が濃縮されている。重合防
止剤が濃縮されている塔底液を薄膜蒸発器で処理する
と、重合防止剤が更に濃縮されて析出し、壁面上に堆積
したり蒸発残渣の流動性を悪化させるので、通常の薄膜
蒸発器では円滑な処理が困難であるが、本発明に係る薄
膜蒸発器によれば、容易に処理することができる。When distilling and refining these substances that are easily polymerized, a polymerization inhibitor is generally added to the liquid. For example, in the case of distillation and purification of acrylic acid, hydroquinone, a phenolic polymerization inhibitor such as hydroquinone monomethyl ether, or phenothiazine,
Organic substances such as N-oxyl compounds and copper salts such as copper dialkyldithiocarbamate, copper acrylate and copper acetate are generally used. Therefore, these polymerization inhibitors are concentrated in the bottom liquid discharged from the bottom of the distillation column. If the bottom liquid with concentrated polymerization inhibitor is treated with a thin film evaporator, the polymerization inhibitor will be further concentrated and deposited, and it will be deposited on the wall surface and deteriorate the fluidity of the evaporation residue. Although smooth treatment is difficult with a vessel, the thin film evaporator according to the present invention enables easy treatment.
【００１２】図１〜４に本発明に係る回転スライダー式
薄膜蒸発器の１例の概略図を示すが、本発明はその要旨
を越えない限り、この例に限定されるものではない。本
装置は外面に加熱用ジャケット（１）を有する円筒形の
主体部（２）を持つ薄膜蒸発器であり、内部の回転軸
（３）と、それを回転させるモーター（４）を有してい
る。回転軸（３）には攪拌翼（５）が取り付けられてお
り、攪拌翼は、主体部の内壁とごくわずかに隙間を保ち
ながら回転する。薄膜蒸発器上部の液供給口（６）より
供給された被処理液は、回転する攪拌翼によって主体部
の内壁に沿って、膜状に押し広げられつつ、重力により
流下する。この流下する過程で、加熱用ジャケットから
の熱によって被処理液中の低沸点成分が蒸発する。蒸発
した低沸点成分は薄膜蒸発器の上部にある蒸気抜出口
（７）より系外へ導かれ、低沸点成分の大部分が除去さ
れて流動性が悪くなった蒸発残渣は集液部（９）に導か
れる。そして、回転軸に取り付けられたワイパー（１
０）、（１１）が集液部の壁面に接して回転することに
より、この集液部に流入した蒸発残渣は内壁面上より定
常的に除去され、薄膜蒸発器の下部にある残渣排出口
（８）より抜き出される。これにより、従来の集液部に
おいて発生していた、蒸発残渣による集液部の出口部分
やこれに続く液抜出管の閉塞を防止することができ、薄
膜蒸発器の長期間安全運転が可能となる。1 to 4 show schematic views of an example of a rotary slider type thin film evaporator according to the present invention, but the present invention is not limited to this example unless the gist thereof is exceeded. This device is a thin film evaporator having a cylindrical main body (2) having a heating jacket (1) on the outer surface, and has an inner rotating shaft (3) and a motor (4) for rotating it. There is. A stirring blade (5) is attached to the rotating shaft (3), and the stirring blade rotates while keeping a slight gap from the inner wall of the main body. The liquid to be treated supplied from the liquid supply port (6) on the upper part of the thin film evaporator flows down by gravity while being spread in a film shape along the inner wall of the main body by the rotating stirring blade. During this flowing process, the low boiling point component in the liquid to be treated is evaporated by the heat from the heating jacket. The evaporated low boiling point component is guided to the outside of the system through the vapor outlet (7) at the upper part of the thin film evaporator, and most of the low boiling point component is removed, and the evaporation residue whose fluidity has deteriorated is collected in the liquid collecting section (9). ). Then, the wiper (1
By rotating 0) and (11) in contact with the wall surface of the liquid collecting part, the evaporation residue flowing into this liquid collecting part is constantly removed from the inner wall surface, and the residue discharge port at the bottom of the thin film evaporator is It is extracted from (8). As a result, it is possible to prevent clogging of the outlet part of the liquid collecting part and the subsequent liquid withdrawal pipe due to evaporation residue, which has occurred in the conventional liquid collecting part, and long-term safe operation of the thin film evaporator is possible. Becomes
【００１３】本発明に係る薄膜蒸発器を用いて易重合性
成分を含む被処理液を処理した１例を示すと、 図１〜
図４に示すような、集液部の逆円錐状部分及び円筒状部
分のそれぞれに対応する箇所にワイパーを持つ本発明に
係る薄膜蒸発器を用いて、アクリル酸の蒸留精製工程
で、蒸留塔の塔底から排出された塔底液（アクリル酸６
９．４重量％、アクリル酸２量体２０．９重量％、無水
マレイン酸６．９重量％、その他２．８重量％）からア
クリル酸を回収する操作を行ったところ、１０ヶ月間の
連続運転を達成することができた。これに対し、ワイパ
ーが取り付けられていないこと以外は、全く同一の薄膜
蒸発器を用いて同様の運転を行ったところ、５ヶ月を経
過したところで残渣排出口の配管ラインが閉塞し、運転
を停止せざるを得なかった。An example of treating a liquid to be treated containing an easily polymerizable component using the thin film evaporator according to the present invention is shown in FIG.
In the distillation purification step of acrylic acid, the thin film evaporator according to the present invention, which has wipers at the positions corresponding to the inverted conical portion and the cylindrical portion of the liquid collecting portion, as shown in FIG. Bottom liquid (acrylic acid 6
9.4% by weight, acrylic acid dimer 20.9% by weight, maleic anhydride 6.9% by weight, and other 2.8% by weight), the operation of recovering acrylic acid was carried out, and it was continued for 10 months. I was able to achieve driving. On the other hand, when the same operation was performed using the same thin film evaporator except that the wiper was not attached, the pipe line of the residue discharge port was blocked after 5 months and the operation was stopped. I had to do it.
【００１４】[0014]
【発明の効果】本発明に係る薄膜型蒸発器によれば、蒸
発器内部における重合物の発生を抑止することができ、
また重合物や析出物が発生した場合においても、それら
の堆積を防止することができ、薄膜蒸発器の長期安定運
転が可能である。これにより生産の安定化を図ることが
できる。よって、本発明に係る薄膜蒸発器は工業上非常
に有用な機器であるといえる。According to the thin film type evaporator of the present invention, it is possible to suppress the generation of a polymer in the evaporator,
Further, even when a polymer or a precipitate is generated, it is possible to prevent the accumulation of the polymer and the precipitate, and the long-term stable operation of the thin film evaporator is possible. This makes it possible to stabilize production. Therefore, it can be said that the thin film evaporator according to the present invention is an industrially very useful device.
【図１】本発明に係る薄膜蒸発器の１例の概念図。FIG. 1 is a conceptual diagram of an example of a thin film evaporator according to the present invention.
【図２】図１の薄膜蒸発器底部の拡大図。2 is an enlarged view of the bottom of the thin film evaporator of FIG.
【図３】図２の逆円錐部に対応して取り付けられている
ワイパーの取り付け状態を示す図。FIG. 3 is a view showing a mounting state of a wiper attached so as to correspond to the inverted conical portion of FIG.
【図４】図２の円筒部に対応して取り付けられているワ
イパーの取り付け状態を示す図。FIG. 4 is a view showing a mounting state of a wiper attached corresponding to the cylindrical portion of FIG.
１：加熱用ジャケット、２：主体部、３：回転軸、４：
モーター、５：攪拌翼、６：液供給口、７：蒸気抜出
口、８：残渣排出口、９：集液部、１０：ワイパー、１
１：ワイパー、１２：ワイパー取り付け腕、１３：スプ
リング1: heating jacket, 2: main body part, 3: rotating shaft, 4:
Motor, 5: stirring blade, 6: liquid supply port, 7: vapor outlet, 8: residue discharge port, 9: liquid collecting part, 10: wiper, 1
1: Wiper, 12: Wiper mounting arm, 13: Spring
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ０７Ｃ 69/54 Ｃ０７Ｃ 69/54 Ｚ (72)発明者 小川 寧之 三重県四日市市東邦町１番地 三菱化学株 式会社内 (72)発明者 鈴木 芳郎 三重県四日市市東邦町１番地 三菱化学株 式会社内 Ｆターム(参考） 4D076 AA06 AA07 AA24 BA13 CA19 CD03 CD16 CD21 DA10 FA31 FA37 GA03 HA03 HA11 JA02 JA03 4H006 AA02 AD11 BS10 ─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. 7 Identification code FI theme code (reference) C07C 69/54 C07C 69/54 Z (72) Inventor Yasuyuki Ogawa 1 Toho-cho, Yokkaichi-shi, Mie Mitsubishi Chemical In-company (72) Inventor Yoshiro Suzuki 1 Toho-cho, Yokkaichi-shi, Mie Mitsubishi Chemical In-company F-term (reference) 4D076 AA06 AA07 AA24 BA13 CA19 CD03 CD16 CD21 DA10 FA31 FA37 GA03 HA03 HA11 JA02 JA03 4H006 AA02 AD11 BS10
Claims (8)
抜出口、下部に残渣排出口を有している、主体部が円筒
状の蒸発器本体と、その内部に設置されている回転軸
と、これに取り付けられていて蒸発器本体の内壁面に沿
って周方向に移動する攪拌翼とを有する縦型薄膜蒸発器
において、攪拌翼の下端と残渣排出口との間の内壁面に
接して周方向に移動するワイパーを有することを特徴と
する薄膜蒸発器。1. An evaporator main body having a cylindrical main body, having a heating means on the outer surface, a liquid supply port and a vapor discharge port on the upper part, and a residue discharge port on the lower part, and a rotation installed inside thereof. In a vertical thin film evaporator having a shaft and a stirring blade attached to the shaft and moving in a circumferential direction along the inner wall surface of the evaporator main body, an inner wall surface between a lower end of the stirring blade and a residue discharge port is provided. A thin film evaporator comprising a wiper that is in contact with and moves in a circumferential direction.
抜出口、下部に残渣排出口を有している、主体部が円筒
状で、その下部が逆円錐状の集液部となっている蒸発器
本体と、その内部に設置されている回転軸と、これに取
り付けられていて蒸発器本体の内壁面に沿って周方向に
移動する攪拌翼とを有する縦型薄膜蒸発器において、逆
円錐状の集液部の内壁面に接して周方向に移動するワイ
パーを有することを特徴とする薄膜蒸発器。2. A liquid collector having a heating means on the outer surface, a liquid supply port and a steam outlet on the upper part, and a residue discharge port on the lower part, the main part being cylindrical and the lower part being an inverted conical shape. In a vertical thin-film evaporator having an evaporator main body, a rotary shaft installed therein, and a stirring blade attached to the main shaft and moving in a circumferential direction along an inner wall surface of the evaporator main body, A thin-film evaporator comprising a wiper that moves in a circumferential direction in contact with an inner wall surface of an inverted conical liquid collecting portion.
抜出口、下部に残渣排出口を有している、主体部が円筒
状で、その下部が逆円錐形と円筒形の形状を組み合わせ
た漏斗状の集液部となっている蒸発器本体と、その内部
に設置されている回転軸と、これに取り付けられていて
蒸発器本体の内壁面に沿って周方向に移動する攪拌翼と
を有する縦型薄膜蒸発器において、漏斗状の集液部の内
壁面に接して、周方向に移動するワイパーを有すること
を特徴とする薄膜蒸発器。3. A main body having a cylindrical shape and a lower part having an inverted conical shape and a cylindrical shape having a heating means on an outer surface, a liquid supply port and a vapor discharge port on an upper part, and a residue discharge port on a lower part. An evaporator main body which is a combined funnel-shaped liquid collecting section, a rotary shaft installed therein, and an agitating blade attached to the evaporator main body that moves in the circumferential direction along the inner wall surface of the evaporator main body. A vertical thin film evaporator having: a thin film evaporator having a wiper that moves in a circumferential direction in contact with an inner wall surface of a funnel-shaped liquid collecting portion.
内面が伝熱面となっており、上部に液供給口と蒸気抜出
口、下部に残渣排出口を有している、主体部が円筒状の
蒸発器本体と、その内部に設置されている回転軸と、こ
れに取り付けられていて蒸発器本体の内壁面に沿って周
方向に移動する攪拌翼とを有する縦型薄膜蒸発器におい
て、蒸発器本体下部の非伝熱面である内壁面に接して周
方向に移動するワイパーを有することを特徴とする薄膜
蒸発器。4. A main body having a heating means on an outer surface, a corresponding inner surface serving as a heat transfer surface, a liquid supply port and a steam outlet on an upper part, and a residue discharge port on a lower part. A vertical thin film evaporator having a cylindrical evaporator body, a rotating shaft installed therein, and a stirring blade attached to the body and moving in a circumferential direction along an inner wall surface of the evaporator body. The thin film evaporator according to claim 1, further comprising a wiper that moves in a circumferential direction in contact with an inner wall surface that is a non-heat transfer surface of a lower portion of the evaporator body.
回転軸と同一の回転軸上に取り付けられていることを特
徴とする請求項１ないし４のいずれかに記載の薄膜蒸発
器。5. The thin film evaporator according to claim 1, wherein the wiper is mounted on the same rotary shaft as the rotary shaft on which the stirring blade is mounted.
する請求項１ないし５のいずれかに記載の薄膜蒸発器。6. The thin film evaporator according to claim 1, wherein the wiper is of a movable blade type.
膜蒸発器に、上部の液供給口から易重合性成分を含む液
を供給して内壁面上を流下させ、発生した蒸気を上部の
蒸気抜出口から外部に抜き出し、蒸発残渣は下部の残渣
排出口から外部に抜き出すことを特徴とする、易重合性
成分を含む液を蒸気と蒸発残渣とに分離する方法。7. The thin film evaporator according to any one of claims 1 to 6, wherein a liquid containing an easily polymerizable component is supplied from an upper liquid supply port to flow down on an inner wall surface, and the generated vapor is transferred to the upper part. The method for separating a liquid containing an easily polymerizable component into steam and evaporation residue, which is characterized in that the evaporation residue is extracted to the outside from the steam extraction outlet and the evaporation residue is extracted to the outside from the lower residue discharge port.
膜蒸発器に、その上部の液供給口から（メタ）アクリル
酸又はそのエステルを含む液を供給して内壁面上を流下
させ、発生した（メタ）アクリル酸又はそのエステルの
蒸気を上部の蒸気抜出口から外部に抜き出し、蒸発残渣
は下部の残渣排出口から外部に抜き出すことを特徴とす
る（メタ）アクリル酸又はそのエステルの蒸留残渣から
の（メタ）アクリル酸又はそのエステルの回収方法。8. The thin film evaporator according to claim 1, wherein a liquid containing (meth) acrylic acid or its ester is supplied from an upper liquid supply port to make it flow down on the inner wall surface. The distillation of (meth) acrylic acid or its ester is characterized in that the generated vapor of (meth) acrylic acid or its ester is extracted to the outside from the vapor outlet of the upper part, and the evaporation residue is extracted to the outside from the residue outlet of the lower part. A method for recovering (meth) acrylic acid or its ester from the residue.
Priority Applications (14)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001373671A JP2003170001A (en) | 2001-12-07 | 2001-12-07 | Thin film evaporator |
| CN200410069866.4A CN1267397C (en) | 2001-10-30 | 2002-10-30 | Refining method of acrylic acid or methacrylic acid |
| AU2002344613A AU2002344613A1 (en) | 2001-10-30 | 2002-10-30 | Method for purifying (meth)acrylic acid |
| CN200410069865.XA CN1572781A (en) | 2001-10-30 | 2002-10-30 | Refining method of (meth)acrylic acid |
| PCT/JP2002/011308 WO2003045890A1 (en) | 2001-10-30 | 2002-10-30 | Method for purifying (meth)acrylic acid |
| CNB2004100698645A CN100389848C (en) | 2001-10-30 | 2002-10-30 | Thin film evaporator and application thereof in (methyl) acrylic acid refining method |
| CN200410069863.0A CN1288126C (en) | 2001-10-30 | 2002-10-30 | Refining method of (meth)acrylic acid |
| CN200410069867.9A CN1263725C (en) | 2001-10-30 | 2002-10-30 | Refining method of (meth)acrylic acid |
| CN02821954.6A CN1582268A (en) | 2001-10-30 | 2002-10-30 | Refining method of (meth)acrylic acid |
| US10/834,075 US7414150B2 (en) | 2001-10-30 | 2004-04-29 | Method for purifying (meth)acrylic acid |
| US11/103,617 US7265241B2 (en) | 2001-10-30 | 2005-04-12 | Method for purifying (meth)acrylic acid |
| US11/103,622 US20050176998A1 (en) | 2001-10-30 | 2005-04-12 | Method for purifying (meth)acrylic acid |
| US11/226,360 US20060009657A1 (en) | 2001-10-30 | 2005-09-15 | Method for purifying (meth)acrylic acid |
| US12/014,186 US20080245652A1 (en) | 2001-10-30 | 2008-01-15 | Method for purifying (meth)acrylic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001373671A JP2003170001A (en) | 2001-12-07 | 2001-12-07 | Thin film evaporator |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003170001A true JP2003170001A (en) | 2003-06-17 |
Family
ID=19182347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001373671A Pending JP2003170001A (en) | 2001-10-30 | 2001-12-07 | Thin film evaporator |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2003170001A (en) |
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| JP2010155797A (en) * | 2008-12-26 | 2010-07-15 | Toagosei Co Ltd | Method for producing (meth)acrylate |
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| JP2010155797A (en) * | 2008-12-26 | 2010-07-15 | Toagosei Co Ltd | Method for producing (meth)acrylate |
| CN101912690A (en) * | 2010-08-06 | 2010-12-15 | 爱阔特(上海)清洗设备制造有限公司 | Distillation tank |
| WO2013136874A1 (en) * | 2012-03-16 | 2013-09-19 | 三菱レイヨン株式会社 | Vertical centrifugal thin film evaporator and monomer purification method |
| CN104168972A (en) * | 2012-03-16 | 2014-11-26 | 三菱丽阳株式会社 | Vertical centrifugal thin film evaporator and monomer purification method |
| JPWO2013136874A1 (en) * | 2012-03-16 | 2015-08-03 | 三菱レイヨン株式会社 | Vertical centrifugal thin film evaporator and monomer purification method |
| KR101604940B1 (en) * | 2012-03-16 | 2016-03-18 | 미쯔비시 레이온 가부시끼가이샤 | Vertical centrifugal thin film evaporator and monomer purification method |
| US9981201B2 (en) | 2012-03-16 | 2018-05-29 | Mitsubishi Chemical Corporation | Vertical centrifugal thin film evaporator and monomer purification method |
| CN110665243A (en) * | 2019-11-14 | 2020-01-10 | 杭州富春食品添加剂有限公司 | Evaporator for producing high-purity low-glycerol molecular distillation monoglyceride |
| CN110665243B (en) * | 2019-11-14 | 2024-05-10 | 浙江金棕榈科技股份有限公司 | Evaporator for producing high-purity low-glycerol molecular distillation monoglyceride |
| CN113713411A (en) * | 2021-09-23 | 2021-11-30 | 宜昌诚凯化工科技有限公司 | Phosphorous acid film evaporation system |
| CN113713411B (en) * | 2021-09-23 | 2024-02-09 | 宜昌诚凯化工科技有限公司 | Phosphorous acid film evaporation system |
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