JP2001046802A - Method and apparatus for refining of organic compound containing easily blockable substance - Google Patents
Method and apparatus for refining of organic compound containing easily blockable substanceInfo
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- JP2001046802A JP2001046802A JP2000168001A JP2000168001A JP2001046802A JP 2001046802 A JP2001046802 A JP 2001046802A JP 2000168001 A JP2000168001 A JP 2000168001A JP 2000168001 A JP2000168001 A JP 2000168001A JP 2001046802 A JP2001046802 A JP 2001046802A
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- liquid
- gas
- baffle plate
- substance
- refining
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- 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】本発明は易閉塞性物質を含む
有機化合物の精製方法及び精製装置に関し、詳細にはス
ラリーや重合物の如き不溶性の固形物（粘稠性物質を含
む）を含む液状の有機化合物、例えば（メタ）アクリル
酸，（メタ）アクリル酸エステル，フタル酸，マレイン
酸等の精製に好適な精製装置及び精製方法に関するもの
である。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for purifying an organic compound containing an easily occlusive substance, and more particularly, to a liquid containing an insoluble solid (including a viscous substance) such as a slurry or a polymer. The present invention relates to a purification apparatus and a purification method suitable for the purification of organic compounds such as (meth) acrylic acid, (meth) acrylic acid ester, phthalic acid, and maleic acid.
【０００２】[0002]
【従来の技術】複数成分の混合物から特定成分を精製す
る際に用いられる精製装置としては、気液接触方法の違
いにより、(a) 十字流接触型，(b) 向流接触型，(c) シ
ャワー接触型等のその他の型に分類できる。例えば図１
（ａ）に示す様に、(a) 十字流接触型では、精製装置の
内部にダウンカマー３を介してトレイ１が多数段設けら
れており、各トレイ１には多数の気体貫通用の開孔部１
ａが形成されると共に、堰２によって被処理液（または
スラリー）の滞留部Ｒが形成されている。そして、精製
装置の上方から被処理液を流下させると共に、下方から
気体を上昇流で流すと、上記開孔部１ａを通して上昇す
る気体が、前記滞留部Ｒ内に溜まった被処理液中を通過
する際に気液接触が行なわれる。また滞留している被処
理液は堰２を越えて下段へ溢流する。2. Description of the Related Art Purification apparatuses used for purifying a specific component from a mixture of a plurality of components include (a) cross-flow contact type, (b) countercurrent contact type, and (c) ) It can be classified into other types such as shower contact type. For example, FIG.
As shown in (a), (a) in the cross-flow contact type, a plurality of trays 1 are provided inside the refining device via downcomers 3, and each tray 1 has a large number of openings for gas penetration. Hole 1
a is formed, and the weir 2 forms a stagnant portion R of the liquid to be treated (or slurry). When the liquid to be treated is caused to flow down from above the refining device and the gas is caused to flow from below, the gas rising through the opening 1a passes through the liquid to be treated accumulated in the retaining portion R. The gas-liquid contact is performed at the time. The retained liquid to be processed overflows the weir 2 to the lower stage.
【０００３】また(b) 向流接触型では、図１（ｂ）に示
す如く、多数の開孔部４ａを設けたトレイ４が精製装置
の水平方向全面に亘って、且つ上下方向に適当な間隔を
あけて多数段配設されており、前記開孔部４ａを通して
流下する被処理液と同開孔部４ａを通して上昇する気体
との間で気液接触が行われる。(B) In the counter-current contact type, as shown in FIG. 1 (b), a tray 4 provided with a large number of apertures 4a extends along the entire horizontal surface of the refining apparatus and is suitable for the vertical direction. A large number of stages are arranged at intervals, and gas-liquid contact is made between the liquid to be processed flowing down through the opening 4a and the gas rising through the opening 4a.
【０００４】また(c)シャワー接触型では、図１（ｃ）
に示す如く、被処理液が上側のバッフル板５から下側の
バッフル板６に滝状で流下する際に、該液流を潜って上
昇する気体との間で気液接触が行われる。(C) In the case of a shower contact type, FIG.
When the liquid to be treated flows down from the upper baffle plate 5 to the lower baffle plate 6 in a waterfall manner, gas-liquid contact is made between the liquid and the gas rising under the liquid flow.
【０００５】従って、上記(a)〜(c)に示したタイプの精
製装置の気液接触効率を比較すると、(a)の十字流接触
型が最も優れており、次に(b)の向流接触型が優れてい
ることから、汎用精製装置の殆どはこれら２つの型式の
ものが採用されている。Therefore, comparing the gas-liquid contact efficiencies of the refining apparatuses of the types (a) to (c) above, the cross-flow contact type of (a) is the most excellent, followed by the direction of (b). Because of the superiority of the flow contact type, most of the general-purpose purification devices adopt these two types.
【０００６】しかし、精製の対象となる被処理液が易閉
塞性物質を含む有機化合物である場合には、トレイ１
（またはトレイ４）に開口された前記開孔部１ａ（また
は開孔部４ａ）が該易閉塞性物質によって閉塞されるこ
とがあり、こうした開孔部１ａ（または開孔部４ａ）の
閉塞が起こると、十字流や向流での気液接触効率が低下
するばかりでなく、被処理液の流下および気体の上昇が
阻害されて連続操業自体が困難になる。従ってこの様な
閉塞が生じたときは、運転を中止して精製装置内に蓄積
した閉塞物を人為的に取り除くか、或いは薬剤により化
学的に除去する等の処置が不可欠となる。However, when the liquid to be treated to be purified is an organic compound containing an easily clogging substance, the tray 1
The opening 1a (or opening 4a) opened in the tray (or the tray 4) may be closed by the easily-closable substance, and such opening 1a (or opening 4a) may be closed. When this occurs, not only does the gas-liquid contact efficiency in the cross flow or countercurrent decrease, but also the flow of the liquid to be treated and the rise of the gas are hindered, making continuous operation itself difficult. Therefore, when such a blockage occurs, it is indispensable to take measures such as stopping the operation and artificially removing the blockage accumulated in the purification apparatus, or chemically removing the blockage with a chemical.
【０００７】[0007]
【発明が解決しようとする課題】本発明は上記事情に着
目してなされたものであり、精製されるべき被処理液
が、易閉塞性物質を含む有機化合物の場合であっても、
運転を中止することなく長期に亘って連続的に精製を行
うことのできる精製方法及び精製装置を提供しようとす
るものである。SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and even when the liquid to be purified is an organic compound containing an easily occluding substance,
An object of the present invention is to provide a refining method and a refining apparatus capable of continuously performing refining for a long time without stopping operation.
【０００８】[0008]
【課題を解決するための手段】上記課題を解決した本発
明の精製装置とは、該装置内を降下する被処理液と該装
置内を上昇する気体との接触により該被処理液の精製を
行なうシャワー接触型の精製装置であって、上記精製装
置内には、ウインドウ部を有するバッフル板が多数段配
設され、且つ該バッフル板には全面に気体貫通用の開孔
部が形成されてなることを要旨とするものである。According to the present invention, there is provided a purification apparatus comprising: a purifying apparatus for purifying a liquid to be treated by contacting a liquid to be treated descending in the apparatus with a gas rising in the apparatus; A purifying apparatus of a shower contact type, wherein a plurality of baffle plates having windows are arranged in the purifying apparatus, and an opening for gas penetration is formed on the entire surface of the baffle plate. The point is to become.
【０００９】上記開孔部の孔径としては３〜３０ｍｍの
範囲が好ましく、その開孔部の面積の合計は、バッフル
板の上部面積に対し１０〜５０％の範囲となる様に設計
することが望ましく、また前記ウインドウ部の面積は、
前記装置の横断面積に対し１０％〜７０％の範囲とする
ことが好ましく、更には、前記装置内に配設される上下
で隣接するバッフル板で形成されるカーテン部面積は、
前記装置の横断面積に対し１０％〜１２０％の範囲とな
るように設計することが望ましく、この様に設計された
精製装置は、装置内での易閉塞性物質による閉塞事故を
可及的に抑えることができるので、被処理液として易閉
塞性物質を含む有機化合物を使用した場合にその特徴が
より効果的に発揮される。The hole diameter of the opening is preferably in the range of 3 to 30 mm, and the total area of the opening is designed to be in the range of 10 to 50% with respect to the upper area of the baffle plate. Preferably, the area of the window portion is
It is preferable to set the range of 10% to 70% with respect to the cross-sectional area of the device, and furthermore, the area of the curtain portion formed by the vertically adjacent baffle plates disposed in the device,
It is desirable to design the apparatus so as to be in the range of 10% to 120% with respect to the cross-sectional area of the apparatus. Since this can be suppressed, when an organic compound containing an easily-closable substance is used as the liquid to be treated, the characteristics are more effectively exhibited.
【００１０】また本発明にかかる精製法とは、上記構成
の精製装置を使用し、易閉塞性物質を含む液状の有機化
合物、例えば（メタ）アクリル酸や（メタ）アクリル酸
エステルを、気液接触により効率よく精製するところに
要旨を有している。[0010] The purification method according to the present invention means that a liquid organic compound containing an easily occlusive substance, such as (meth) acrylic acid or (meth) acrylic acid ester, is purified by gas-liquid The gist lies in the fact that it is efficiently purified by contact.
【００１１】尚、上記ウインドウ部とは、例えば図２に
示す様に、トレイ２１と精製装置内壁の間の空間領域２
８のことであり、即ちバッフル板が形成されていない切
欠部である。The window portion is, for example, as shown in FIG. 2, a space area 2 between the tray 21 and the inner wall of the purifier.
8. That is, a notch in which a baffle plate is not formed.
【００１２】また上記ウインドウ部とは、例えば図３に
示す様に、上側トレイ２１のウインドウ部側端部と下側
トレイ２２の間に形成される領域２９のことであり、灌
液流面積である。The window is, for example, as shown in FIG. 3, an area 29 formed between the end of the upper tray 21 on the side of the window and the lower tray 22. is there.
【００１３】[0013]
【発明の実施の形態】本発明によれば、シャワー接触型
の精製装置を基本構成とし、該精製装置内に設けられる
バッフル板の構成を前述の様に工夫することにより、易
閉塞性物質を含む液状の有機化合物を、閉塞事故を生じ
ることなく長期間に亘って効率よく精製操業を継続する
ことが可能となる。DESCRIPTION OF THE PREFERRED EMBODIMENTS According to the present invention, a shower contact type purifying apparatus is basically used, and the structure of a baffle plate provided in the purifying apparatus is devised as described above, so that easily occlusive substances can be removed. It becomes possible to efficiently continue the refining operation of a liquid organic compound containing the compound over a long period of time without causing a blockage accident.
【００１４】本発明において精製装置とは、例えば精製
塔、即ち蒸留塔，吸収塔，放散塔など目的物の精製用い
られる各種塔を含む意味であり、これら各塔は円筒形を
有する塔であることが望ましい。以下、本発明に係る精
製装置及び精製方法を精製塔を用いて説明するが、本発
明はこれらに限定される趣旨ではない。In the present invention, the term "purifying apparatus" means, for example, a purifying column, that is, a column having a cylindrical shape, such as a distillation column, an absorption column, and a stripping column, each column being used for purifying a target substance. It is desirable. Hereinafter, the purification apparatus and the purification method according to the present invention will be described using a purification tower, but the present invention is not limited to these.
【００１５】本発明の精製塔に導入される被処理液とし
ては、通常の（メタ）アクリル酸，フタル酸，マレイン
酸の製造過程における、接触気相酸化で得られた反応ガ
ス凝縮液，溶剤捕集液などが例示されるがこれらに限定
されず、被処理液が易閉塞性物質を含む有機化合物であ
ってもよく、例えば（メタ）アクリル酸，（メタ）アク
リル酸エステル，フタル酸，マレイン酸などの有機化合
物に好適に用いることができる。（メタ）アクリル酸に
含まれる易閉塞性物質としてはポリマー，テレフタル
酸，フマル酸などの析出物、フタル酸，マレイン酸に含
まれる易閉塞性物質としてはアルデヒド重合物やキノン
縮合物などのタール状物質が例示される。The liquid to be treated to be introduced into the purification column of the present invention includes a reaction gas condensate obtained by catalytic gas phase oxidation, a solvent, and a solvent in a usual process for producing (meth) acrylic acid, phthalic acid and maleic acid. The liquid to be treated may be an organic compound containing an easily occlusive substance. Examples of the liquid to be treated include, but are not limited to, (meth) acrylic acid, (meth) acrylic acid ester, phthalic acid, and the like. It can be suitably used for organic compounds such as maleic acid. Polymers, terephthalic acid, fumaric acid, and other precipitates included in (meth) acrylic acid include easily occlusive substances, and phthalic acid, maleic acid include easily occlusive substances, such as aldehyde polymers and quinone condensates. Substances are exemplified.
【００１６】また本発明の精製塔に導入される気体とし
てはリボイラ等から発生した蒸気，上記接触気相酸化で
得られた反応ガスなどを導入することができ、特に限定
されない。The gas introduced into the purification tower of the present invention may be, for example, steam generated from a reboiler or the like, or a reaction gas obtained by the above-mentioned catalytic gas phase oxidation, and is not particularly limited.
【００１７】図４は、シャワー接触型精製塔内にバッフ
ル板を配設した精製塔の概略説明図であり、精製塔１０
の上部に設けられた被処理液供給手段（ディストリビュ
ータ）１１から、易閉塞性物質を含む被処理液がバッフ
ル板２１上に供給される。そして供給された被処理液
は、バッフル板２２、２３、……と、下方のバッフル板
に逐次流下しつつ、下方から上昇してくる気体（リボイ
ラより発生した蒸気など）と気液接触することによって
精製が行われる。FIG. 4 is a schematic explanatory view of a refining tower in which a baffle plate is disposed in a shower contact type refining tower.
The liquid to be treated containing the easily-closable substance is supplied onto the baffle plate 21 from the liquid to be treated supply means (distributor) 11 provided on the top of the baffle plate 21. The supplied liquid to be treated flows down the baffle plates 22, 23,... Sequentially into the lower baffle plate, and comes into gas-liquid contact with a gas (such as steam generated from a reboiler) rising from below. Purification is performed.
【００１８】但しシャワー接触型精製塔の場合、前述の
如くウインドウ部から滝状で流れる被処理液とその液膜
を潜って上昇する気体との間で気液接触するだけである
から、前述した十字流接触型や向流接触型の精製塔に比
べると気液接触効率は低い。However, in the case of the shower contact type refining tower, since the liquid to be treated flowing in a waterfall form from the window portion and the gas rising under the liquid film only come into gas-liquid contact as described above, The gas-liquid contact efficiency is lower than that of the cross-flow contact type or countercurrent contact type purification tower.
【００１９】そこで本発明では、気液接触効率を高める
ための手段として、例えば図５に示す如く、塔内に配設
されるバッフル板の全面に亘って多数の開孔部３０を形
成し、該開孔部３０を通して上昇する気体を被処理液と
気液接触させることによって精製効率を高める。即ち従
来のシャワー接触型精製塔（図１（ｃ））では、内部に
配設されるバッフル板には開孔部が形成されておらず、
前述したウインドウ部から滝状に流下する被処理液膜を
気体が通過する際に気液接触が行われるだけであるのに
対し、本発明では、こうした滝状液膜を通過する際の気
液接触に加えて、各バッフル板に開口された開孔部３０
を通して流下する被処理液と該開孔部内を上昇する気体
との間でも気液接触が行われるので、全体としての気液
接触効率は大幅に高められ、精製効率を著しく高めるこ
とができる。Therefore, in the present invention, as means for improving the gas-liquid contact efficiency, for example, as shown in FIG. 5, a large number of apertures 30 are formed over the entire surface of a baffle plate provided in a tower. The purification efficiency is enhanced by bringing the gas rising through the opening 30 into gas-liquid contact with the liquid to be treated. That is, in the conventional shower contact type refining tower (FIG. 1 (c)), the baffle plate disposed inside does not have an opening formed therein,
While the gas-liquid contact is only made when the gas passes through the liquid film to be processed flowing down from the window portion in a waterfall shape, the present invention provides the gas-liquid In addition to the contact, an opening 30 opened in each baffle plate
Gas-liquid contact is also performed between the liquid to be treated flowing down through the gas and the gas rising in the opening, so that the gas-liquid contact efficiency as a whole can be greatly increased, and the purification efficiency can be significantly increased.
【００２０】しかも本発明では、基本的にシャワー接触
型を採用しており、各バッフル板に開口された開孔部３
０が多少閉塞を起こすことがあっても、被処理液の下降
流や気体の上昇流は各バッフル板のウインドウ部２８に
よって確保されているので、それらの流れが阻害された
り塔内が閉塞するといった問題は一切生じない。Further, in the present invention, a shower contact type is basically adopted, and an opening 3 is formed in each baffle plate.
Even if 0 may cause some blockage, the downward flow of the liquid to be treated and the upward flow of the gas are secured by the window portions 28 of each baffle plate, so that those flows are obstructed or the inside of the column is blocked. Such a problem does not occur at all.
【００２１】尚、バッフル板の全面に形成される開孔部
３０は、前述の如く該開孔部３０を通過する被処理液と
気体を気液接触させる機能を果たすもので、孔径が小さ
すぎると易閉塞性物質が詰まり易くなるので、直径が３
ｍｍ程度以上、より好ましくは１２ｍｍ程度以上にする
ことが望ましい。しかし、逆に孔径が大きすぎると、ウ
イーピングが起こり気液接触効率が低下してくるので、
３０ｍｍ程度以下、より好ましくは２５ｍｍ程度以下と
することが望ましい。The aperture 30 formed on the entire surface of the baffle plate has a function of bringing the liquid to be processed and the gas passing through the aperture 30 into gas-liquid contact as described above, and has a too small diameter. And the easily occlusive material is easily clogged,
It is desirable that the thickness be about mm or more, more preferably about 12 mm or more. However, conversely, if the pore size is too large, weeping will occur and the gas-liquid contact efficiency will decrease,
It is desirable that the thickness be about 30 mm or less, more preferably about 25 mm or less.
【００２２】尚、この開孔部は全て同一形状、同一サイ
ズであってもよく、或いは異形、易サイズのものであっ
ても構わないが、安定して高い気液接触効率を確保する
には同一形状、同一サイズのものを各バッフル板の全面
に万遍なく形成しておくことが望ましい。また、閉塞防
止の観点からすると真円形のものが最も好ましいが、場
合によっては楕円形や卵形、あるいは多角形のものであ
ってもよく、それらの場合の開口サイズは前述した真円
の直径相当サイズと考えればよい。The openings may have the same shape and the same size, or may have different shapes and sizes. However, in order to stably ensure a high gas-liquid contact efficiency. It is desirable to uniformly form the same shape and the same size on the entire surface of each baffle plate. From the viewpoint of preventing occlusion, a perfect circular shape is most preferable, but in some cases, an oval shape, an oval shape, or a polygonal shape may be used. You can think of it as a considerable size.
【００２３】また、該開孔部３０の総開孔面積がバッフ
ル板の上部面積に対して好ましくは１０％以上、より好
ましくは２０％以上とし、また好ましくは５０％以下、
より好ましくは４０％以下の範囲となる様に各開孔部の
サイズと開口数を設計すれば、開孔部内への易閉塞性物
質の詰りを抑えつつ気液接触効率を一層効果的に高める
ことができるので好ましい。The total area of the openings 30 is preferably 10% or more, more preferably 20% or more, and preferably 50% or less with respect to the upper area of the baffle plate.
More preferably, if the size and the numerical aperture of each opening are designed so as to be within the range of 40% or less, the gas-liquid contact efficiency can be more effectively improved while the clogging of the easily occlusive material into the opening is suppressed. It is preferable because it can be used.
【００２４】被処理液の下降流路および気体の上昇流路
を構成する前記ウインドウ部２８（一般に切欠部とも呼
ばれる：図２の符号２８参照）の精製塔横断面積に対す
る開口面積比率（ウィンドウ面積比率）も、気液接触効
率を高める上で重要であり、精製塔の横断面積（内径）
に対して通常は１０％以上，より好ましくは２０％以
上、好ましくは７０％以下，より好ましくは４５％以下
の範囲となるように設計することが望ましい。１０％未
満だとガス通過口が小さすぎ、ガス通過速度が大きくな
るためフラッディングを起こし易くなる。また７０％超
では、ショートパスが起こり易く、効率低下を起こす可
能性があり、満足な気液接触効率が得られなくなる。な
お、各バッフル板の前記ウィンドウ面積比率は全てが同
じであってもよいが（その際は５０％以下とすることが
望ましい）、異なるウィンドウ部面積比率のバッフル板
を組み合わせて（例えば１０％と７０％等の組合わせ
で）配設してもよい。The opening area ratio (window area ratio) of the window section 28 (generally also referred to as a notch section: see reference numeral 28 in FIG. 2) constituting the descending flow path of the liquid to be treated and the ascending flow path of the gas with respect to the cross-sectional area of the purification tower. ) Is also important in increasing the gas-liquid contact efficiency, and the cross-sectional area (inner diameter) of the purification tower
In general, it is desirable to design so as to be in a range of 10% or more, more preferably 20% or more, preferably 70% or less, more preferably 45% or less. If it is less than 10%, the gas passage is too small and the gas passage speed becomes high, so that flooding easily occurs. On the other hand, if it exceeds 70%, a short path is likely to occur, and there is a possibility that the efficiency may be reduced, so that satisfactory gas-liquid contact efficiency cannot be obtained. The window area ratio of each baffle plate may be the same (preferably 50% or less in that case), but baffle plates having different window part area ratios are combined (for example, 10% and 10%). 70%).
【００２５】更に、上下で隣接するバッフル板で形成さ
れるカーテン部面積（一般に被処理液溢流面積とも呼ば
れる：図３の符号２９参照）の面積比率は、塔の横断面
積に対し１０％以上、１２０％以下の範囲とすることが
望ましく、シャワー接触効率を高める上で特に好ましい
のは２０％以上、１１０％以下の範囲である。Furthermore, the area ratio of the curtain area (generally also referred to as the overflow area of the liquid to be treated: see reference numeral 29 in FIG. 3) formed by the baffle plates adjacent vertically is 10% or more with respect to the cross-sectional area of the tower. , 120% or less, and particularly preferably from 20% to 110% in order to increase the shower contact efficiency.
【００２６】１０％未満ではフラッディングを起こしや
すく、１２０％を超えると気液接触効率の向上はそれほ
ど期待できず、装置が大型化するのみで好ましくない。If it is less than 10%, flooding is liable to occur, and if it exceeds 120%, the improvement of gas-liquid contact efficiency cannot be expected so much, which is not preferable because the apparatus becomes large.
【００２７】バッフル板の形式は様々であり、図６
（ａ）に示す様なディスク・ドーナッツ式や図６（ｂ）
〜６（ｄ）に示す様なセグメンタル・バッフル式などを
適宜選択して採用できる。またセグメンタル・バッフル
式の具体例としては、図６（ｃ）に示す様なツーフロー
タイプのものや、図６（ｄ）に示すマルチフロータイプ
のものを採用しても構わない。いずれの場合も、バッフ
ル板にはその上面に溜り部ができないようウインドウ部
の縁に堰を設置しない方が望ましい。但し、バッフルを
下方勾配をつけて設置する際には(図７(ａ))、バッフル
上の液ホールドアップが減少するため、ウインドウ部に
沿って堰を設置することが望ましい。堰は一般に用いら
れる直線堰，ノッチ付き堰の何れも適用でき、特に限定
されない。また堰の高さも特に限定されないが、堰高さ
は段間隔に対して好ましくは５％以上、より好ましくは
１０％以上、最も好ましくは１５％以上であり、好まし
くは４０％以下、より好ましくは３５％以下、最も好ま
しくは３０％以下とすることが望ましい。またバッフル
板の傾斜は塔横断面に対して１０°以下の勾配とするこ
とが好ましい。尚、堰を設けてバッフル板上面に溜り部
ができると、その部分に易閉塞性物質が堆積し、当該部
分に開口された開孔部を閉塞し易くなるので堰の高さと
勾配の関係は図７（ｃ）に示されるが如く、トレイ接合
部と堰上面とが同一高さとなる様にすることが望まし
い。There are various types of baffle plates.
Disc donut type as shown in (a) or Fig. 6 (b)
A segmental baffle method as shown in FIGS. As a specific example of the segmental baffle type, a two-flow type shown in FIG. 6C or a multi-flow type shown in FIG. 6D may be adopted. In any case, it is desirable not to install a weir at the edge of the window so that the baffle plate does not have a pool on the upper surface. However, when the baffle is installed with a downward slope (FIG. 7 (a)), it is desirable to install a weir along the window because the liquid hold-up on the baffle is reduced. The weir can be any of a generally used straight weir and a notch weir, and is not particularly limited. Also, the height of the weir is not particularly limited, but the weir height is preferably at least 5%, more preferably at least 10%, most preferably at least 15%, preferably at most 40%, more preferably at most 40%, relative to the step spacing. It is desirable that the content be 35% or less, most preferably 30% or less. Further, it is preferable that the inclination of the baffle plate is 10 ° or less with respect to the cross section of the tower. When a weir is provided and a reservoir is formed on the top surface of the baffle plate, the easily-closable substance accumulates in that part, and it becomes easy to close the opening part opened in the part, so the relationship between the height and the slope of the weir is As shown in FIG. 7 (c), it is desirable that the tray junction and the upper surface of the weir have the same height.
【００２８】各バッフル板上面への易閉塞性物質の付着
堆積をより確実に抑え、高い気液接触効率を得るには、
各バッフル板を少なくとも水平に配設し、しかも液体が
上側バッフル板から下側バッフル板に流下し受け止める
様に設置することが望ましく、例えば図６（ａ）〜
（ｄ）及び図８（ａ）〜（ｃ）で示す様に設置すること
が望ましく、特に上下で隣接するバッフル板の一部が重
なり合う様に設置することが推奨される。In order to more reliably suppress the adhesion and deposition of the easily occlusive substance on the upper surface of each baffle plate and obtain a high gas-liquid contact efficiency,
It is desirable to arrange each baffle plate at least horizontally, and to install so that liquid flows down from the upper baffle plate to the lower baffle plate and receives it.
It is desirable to install as shown in (d) and FIGS. 8 (a) to 8 (c), and it is particularly recommended to install so that the upper and lower adjacent baffle plates partially overlap.
【００２９】精製塔の温度は、目的物（即ち（メタ）ア
クリル酸，フタル酸，或いはマレイン酸）の融点以上で
気液接触操作の可能な温度域とすることが推奨される。
例えば（メタ）アクリル酸（エステル）の場合、好まし
くは２０〜１５０℃，より好ましくは４０〜１００℃と
することが好ましい。It is recommended that the temperature of the purification tower be in a temperature range above the melting point of the target substance (ie, (meth) acrylic acid, phthalic acid, or maleic acid) and in which gas-liquid contact operation is possible.
For example, in the case of (meth) acrylic acid (ester), the temperature is preferably 20 to 150 ° C, more preferably 40 to 100 ° C.
【００３０】尚、精製装置内に配設するバッフル板の数
は精製装置の処理能力など種々の要因に基づいて適宜決
定可能な技術事項であり、所望の目的に適合する様にバ
ッフル板の数を決定することができる。The number of baffle plates provided in the refining device is a technical matter that can be appropriately determined based on various factors such as the processing capacity of the refining device. Can be determined.
【００３１】本発明は以上の様に構成されており、易閉
塞性物質を含む様々の液状有機化合物の精製に有効に活
用できる。The present invention is configured as described above, and can be effectively used for purifying various liquid organic compounds including easily occlusive substances.
【００３２】[0032]
【実施例】以下、本発明を実施例によって更に詳細に説
明するが、下記実施例は本発明を限定する性質のもので
はなく、前・後記の趣旨に適合し得る範囲で適当に設計
を変更して実施することはいずれも本発明の技術的範囲
に含まれる。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following Examples are not intended to limit the present invention, and the design is appropriately changed within a range that can be adapted to the above and subsequent points. Any of such operations is included in the technical scope of the present invention.
【００３３】〔実施例１〕下記表１に示す構成のバッフ
ル板を設けたシャワー接触型精製塔Ａを使用し、テレフ
タル酸スラリー等の易閉塞性物質を含む下記組成のメタ
クリル酸水溶液を塔頂部（ディストリビューター１１）
から１２ｍ3／ｈで供給すると共に、塔底部（ガス入口
１６）からは重合防止剤として空気を２Ｎｍ3／ｈの速
度でリボイラ（図示せず）を通じて供給して上昇流を形
成し、塔頂圧力：２６７００Ｐａ、塔頂温度：６８℃、
溜出量／フィード量＝４％、塔底圧力：２８０００Ｐａ
で気液接触させて精製を行った。塔底部（液出口１７）
から得られる精製物の組成は下記の通りであり、この精
製操業を１年間連続して行なったが、精製塔閉塞の問題
は全く生じなかった。 Example 1 Using a shower contact type purification tower A provided with a baffle plate having the structure shown in Table 1 below, an aqueous methacrylic acid solution having the following composition containing an easily obstructive substance such as terephthalic acid slurry was added to the top of the tower. (Distributor 11)
From supplies at 12m 3 / h, to form the upward flow is supplied through the bottom of the tower reboiler air as the polymerization inhibitor from the (gas inlet 16) at a rate of 2 Nm 3 / h (not shown), the top Pressure: 26700 Pa, overhead temperature: 68 ° C.
Distillation amount / feed amount = 4%, tower bottom pressure: 28000 Pa
And gas-liquid contact for purification. Tower bottom (liquid outlet 17)
The composition of the purified product obtained from the above was as follows. This purification operation was carried out continuously for one year, but no problem of clogging of the purification tower occurred.
【００３４】[0034]
【表１】 [Table 1]
【００３５】〔実施例２〕上記表１の精製塔Ｂを使用
し、易閉塞性物質を含むメタクリル酸を含むガスの冷却
を行なった。供給ガス（メタクリル酸２ｖｏｌ％，メタ
クロレイン０．６ｖｏｌ％，水１２ｖｏｌ％，その他８
５．４ｖｏｌ％）を、１０２０Ｎｍ3／ｈでバッフル板
に供給し、１９ｍ3／ｈのメタクリル酸１９ｗｔ％水溶
液と塔底液５００ｍ3／ｈとを塔頂よりフィードし、ガ
スの吸収（冷却）を行なった。尚、操作は塔頂１２４０
００ＫＰａ，７１℃で実施した。その結果、１年間の連
続稼動が可能であり、塔底より実施例１のフィード液を
得た。Example 2 A gas containing methacrylic acid containing an easily-closable substance was cooled using the purification tower B shown in Table 1 above. Supply gas (methacrylic acid 2 vol%, methacrolein 0.6 vol%, water 12 vol%, other 8
5.4 vol%) was supplied to a baffle plate at 1020 Nm 3 / h, and a 19 m 3 / h 19 wt% aqueous solution of methacrylic acid and a bottom liquid 500 m 3 / h were fed from the top of the column to absorb gas (cooling). Was performed. The operation was performed at the tower top 1240.
The test was performed at 00 KPa and 71 ° C. As a result, continuous operation for one year was possible, and the feed solution of Example 1 was obtained from the bottom of the column.
【００３６】〔実施例３〕上記表1の精製塔Ｃを使用
し、易閉塞性物質を含むメタクリル酸水溶液を塔頂部か
らの供給量を０．５ｍ3／ｈに代えた以外は上記実施例
１と同様にして精製を行なったところ、やはり１年間の
連続稼動が可能であった。Example 3 The same procedure as in Example 1 was carried out except that the purification column C shown in Table 1 above was used, and the supply amount of the aqueous methacrylic acid solution containing the easily-closable substance from the top of the column was changed to 0.5 m 3 / h. Purification was carried out in the same manner as in Example 1. As a result, continuous operation for one year was possible.
【００３７】〔比較例１〕開孔部を全く形成していない
バッフル板（図１（ｃ）参照）を配置した以外は前記実
施例１と全く同様にして精製塔の連続運転を行なった。
その結果、１年間の連続稼働は可能であったが、精製効
率は下記の通りであり、前記実施例に比べてかなり劣っ
ていることが確認された。 Comparative Example 1 The continuous operation of the purification column was carried out in exactly the same manner as in Example 1 except that a baffle plate (see FIG. 1 (c)) having no openings was arranged.
As a result, continuous operation for one year was possible, but the purification efficiency was as follows, and it was confirmed that the purification efficiency was considerably inferior to that of the above example.
【００３８】〔比較例２〕前記図１（ｂ）に示した様な
向流接触型の精製塔（直径：１０ｍｍの開孔部を全面に
均一に開口したトレイを配設）を使用し、前記実施例１
と同様にして精製塔の連続操業を行なった。その結果、
塔底圧力が３０７００Ｐａまで上昇し、約１週間未満で
トレイの開孔部が不溶物で閉塞され、運転を停止せざる
を得なかった。[Comparative Example 2] A countercurrent contact type purification tower as shown in FIG. 1 (b) was used (a tray having a 10 mm diameter opening was uniformly opened over the entire surface). Example 1
Continuous operation of the refining tower was performed in the same manner as described above. as a result,
The pressure at the bottom of the tower increased to 30700 Pa, and the opening of the tray was blocked with insoluble matter in less than about one week, and the operation had to be stopped.
【００３９】[0039]
【発明の効果】本発明は以上の様に構成されており、被
処理液（被精製液）として、易閉塞性物質を含む有機化
合物を使用した場合でも、塔内閉塞を生じることなく長
期に亘って精製操業を効率よく連続的に行うことのでき
る精製装置および精製法を提供し得ることになった。The present invention is constituted as described above. Even when an organic compound containing an easily clogging substance is used as the liquid to be treated (liquid to be purified), it can be used for a long time without clogging in the tower. Thus, a refining apparatus and a refining method capable of efficiently and continuously performing a refining operation can be provided.
【図１】気液接触方法を示す説明図である。FIG. 1 is an explanatory diagram showing a gas-liquid contact method.
【図２】ウインドウ部の位置の説明図である。FIG. 2 is an explanatory diagram of a position of a window unit.
【図３】カーテン開口部の位置の説明図である。FIG. 3 is an explanatory diagram of a position of a curtain opening.
【図４】本発明方法に採用することのできる精製装置を
示す概略説明図である。FIG. 4 is a schematic explanatory view showing a purification apparatus that can be employed in the method of the present invention.
【図５】本発明装置に好適なバッフル板の代表例を示す
説明図である。FIG. 5 is an explanatory view showing a typical example of a baffle plate suitable for the device of the present invention.
【図６】シャワー接触型のトレイ形式を示す説明図であ
る。FIG. 6 is an explanatory view showing a tray type of a shower contact type.
【図７】本発明装置に適用可能なバッフル板の変形態様
を示す説明図である。FIG. 7 is an explanatory view showing a modified embodiment of a baffle plate applicable to the device of the present invention.
【図８】本発明装置のバッフル板の配設例を示す説明図
である。FIG. 8 is an explanatory view showing an example of the arrangement of a baffle plate of the apparatus of the present invention.
１，４ トレイ １ａ 気体貫通用開孔部 ４ａ,３０ 気液貫通用開孔部 ５,６,２１，２２,２３,３５ バッフル板 ２，３６ 堰 ３ ダウンカマー １０ 精製塔 １１ ディストリビューター １５ ガス出口 １６ ガス入口 １７ 液出口 ２７ 精製塔本体 ２８ ウインドウ部 ２９ カーテン部 1,4 Tray 1a Opening for gas penetration 4a, 30 Opening for gas-liquid 5,6,21,22,23,35 Baffle plate 2,36 Weir 3 Downcomer 10 Purification tower 11 Distributor 15 Gas outlet 16 Gas inlet 17 Liquid outlet 27 Purification tower main body 28 Window part 29 Curtain part
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 // Ｃ０７Ｂ 63/00 Ｃ０７Ｂ 63/00 Ｂ Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat II (reference) C07C 69/54 C07C 69/54 Z // C07B 63/00 C07B 63/00 B
Claims (6)
上昇する気体との接触により該被処理液の精製を行なう
シャワー接触型の精製装置であって、該精製装置内に
は、ウインドウ部を有するバッフル板が多段数配設さ
れ、且つバッフル板には全面に気液貫通用の開孔部が形
成されていることを特徴とする精製装置。1. A shower contact type purifier for purifying a liquid to be treated by contacting a liquid to be treated descending in the apparatus with a gas rising in the apparatus, wherein the purifier has: A refining apparatus comprising: a plurality of baffle plates each having a window portion; and a baffle plate having an opening for gas-liquid penetration on the entire surface.
り、その開孔部の面積の合計がバッフル板の上部面積に
対して１０〜５０％である請求項１に記載の精製装置。2. The refining apparatus according to claim 1, wherein the aperture has a hole diameter of 3 to 30 mm, and the total area of the apertures is 10 to 50% of the upper area of the baffle plate.
横断面積に対し１０〜７０％である請求項１または２に
記載の精製装置。3. The refining device according to claim 1, wherein the area of the window portion is 10 to 70% of the cross-sectional area of the device.
バッフル板で形成されるカーテン部の面積が、前記装置
の横断面積に対して１０〜１２０％である請求項１〜３
に記載の精製装置。4. An apparatus according to claim 1, wherein the area of the curtain formed by the vertically adjacent baffle plates disposed in the apparatus is 10 to 120% with respect to the cross-sectional area of the apparatus.
The purification device according to item 1.
置を用いることを特徴とする易閉塞性物質を含む有機化
合物の精製方法。5. A method for purifying an organic compound containing an easily-closable substance, comprising using the purifying apparatus according to claim 1. Description:
（メタ）アクリル酸，（メタ）アクリル酸エステル，フ
タル酸，マレイン酸のいずれかである請求項５に記載の
精製方法。6. The organic compound containing the easily occlusive substance,
The purification method according to claim 5, which is any one of (meth) acrylic acid, (meth) acrylate, phthalic acid, and maleic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000168001A JP4514901B2 (en) | 1999-06-03 | 2000-06-05 | Purification method for (meth) acrylic acid, etc. |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11-156655 | 1999-06-03 | ||
| JP15665599 | 1999-06-03 | ||
| JP2000168001A JP4514901B2 (en) | 1999-06-03 | 2000-06-05 | Purification method for (meth) acrylic acid, etc. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001046802A true JP2001046802A (en) | 2001-02-20 |
| JP4514901B2 JP4514901B2 (en) | 2010-07-28 |
Family
ID=26484340
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000168001A Expired - Lifetime JP4514901B2 (en) | 1999-06-03 | 2000-06-05 | Purification method for (meth) acrylic acid, etc. |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003103106A (en) * | 2001-09-28 | 2003-04-08 | Sumitomo Chem Co Ltd | Distillation method for easily polymerizable substance |
| WO2015072536A1 (en) * | 2013-11-14 | 2015-05-21 | 株式会社日本触媒 | Process for producing water-absorbing polyacrylic acid (salt) resin |
| JP2017113688A (en) * | 2015-12-22 | 2017-06-29 | 三菱化学株式会社 | Gas-liquid contact method |
| CN113413731A (en) * | 2021-06-28 | 2021-09-21 | 天津大学 | Gas-liquid contact device |
| WO2023162183A1 (en) * | 2022-02-25 | 2023-08-31 | 株式会社大栄製作所 | Gas replacement device |
| JP7462319B2 (en) | 2020-12-24 | 2024-04-05 | 株式会社大栄製作所 | Gas Replacement Device |
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| WO1995031278A1 (en) * | 1994-05-11 | 1995-11-23 | Urea Casale S.A. | Reactor for two-phase reactions, in particular for urea synthesis at high pressure and temperature |
| JPH1076103A (en) * | 1996-08-14 | 1998-03-24 | Basf Ag | Method for transferring material in plate column and device therefor |
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| GB763684A (en) * | 1954-01-07 | 1956-12-12 | Bataafsche Petroleum | Improvements in or relating to gas-liquid contacting columns |
| JPS4915153B1 (en) * | 1969-06-06 | 1974-04-12 | ||
| JPS5365855U (en) * | 1976-11-08 | 1978-06-02 | ||
| EP0158851A2 (en) * | 1984-03-21 | 1985-10-23 | MoDo-Chemetics Aktiebolag | Cross-flow diffusion column |
| WO1995031278A1 (en) * | 1994-05-11 | 1995-11-23 | Urea Casale S.A. | Reactor for two-phase reactions, in particular for urea synthesis at high pressure and temperature |
| JPH1076103A (en) * | 1996-08-14 | 1998-03-24 | Basf Ag | Method for transferring material in plate column and device therefor |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003103106A (en) * | 2001-09-28 | 2003-04-08 | Sumitomo Chem Co Ltd | Distillation method for easily polymerizable substance |
| WO2015072536A1 (en) * | 2013-11-14 | 2015-05-21 | 株式会社日本触媒 | Process for producing water-absorbing polyacrylic acid (salt) resin |
| US9682362B2 (en) | 2013-11-14 | 2017-06-20 | Nippon Shokubai Co., Ltd. | Process for producing water-absorbing polyacrylic acid (salt) resin |
| JP2017113688A (en) * | 2015-12-22 | 2017-06-29 | 三菱化学株式会社 | Gas-liquid contact method |
| JP7462319B2 (en) | 2020-12-24 | 2024-04-05 | 株式会社大栄製作所 | Gas Replacement Device |
| CN113413731A (en) * | 2021-06-28 | 2021-09-21 | 天津大学 | Gas-liquid contact device |
| WO2023162183A1 (en) * | 2022-02-25 | 2023-08-31 | 株式会社大栄製作所 | Gas replacement device |
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| Publication number | Publication date |
|---|---|
| JP4514901B2 (en) | 2010-07-28 |
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