JPH05237333A - Method for recovering solvent - Google Patents
Method for recovering solventInfo
- Publication number
- JPH05237333A JPH05237333A JP4076039A JP7603992A JPH05237333A JP H05237333 A JPH05237333 A JP H05237333A JP 4076039 A JP4076039 A JP 4076039A JP 7603992 A JP7603992 A JP 7603992A JP H05237333 A JPH05237333 A JP H05237333A
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- Japan
- Prior art keywords
- gas
- solvent
- adsorption
- flow path
- adsorbent
- 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.)
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- Treating Waste Gases (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は吸着により溶剤等を含む
ガスからその溶剤等を除去して清浄なガスを得るととも
に、さらにその溶剤等を濃縮回収する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for removing a solvent or the like from a gas containing the solvent or the like by adsorption to obtain a clean gas and further concentrating and recovering the solvent or the like.
【０００２】[0002]
【従来の技術】化学工場等では溶剤やその他の有害な気
体を含有する空気やガスが発生するためそうしたガスか
ら溶剤等を除去して空気やガスの浄化を行なう必要があ
る。また除去された成分が溶剤のごとく価値のある成分
の場合にはこれを回収して再使用に供することが省資源
の見地からも重要である。このようなガス中から微量の
成分を除去する方法として従来より吸着法が用いられて
いる。2. Description of the Related Art In a chemical factory or the like, air or gas containing a solvent or other harmful gas is generated. Therefore, it is necessary to remove the solvent or the like from the gas to purify the air or gas. Further, when the removed component is a valuable component such as a solvent, it is important from the viewpoint of resource saving to recover the component and reuse it. An adsorption method has been conventionally used as a method for removing a trace amount of components from such a gas.
【０００３】吸着法には種々の方法があるが最も一般的
に行なわれてきたのは活性炭に溶剤等を吸着させた後そ
の活性炭に水蒸気を直接吹き込んで吸着成分を脱離さ
せ、得られた蒸気混合物を冷却凝縮して溶剤等を回収す
る方法である。この方法は非常に簡単な操作で効率よく
溶剤等を回収できる優れた方法ではあるが一方で溶剤等
の回収にともなって、使用した水蒸気の凝縮水がかなり
の量生成する。こうした凝縮水には溶剤等の成分を含む
ことが多く排水処理を要する場合もある。また回収成分
が水溶性である場合には凝縮水との分離が容易ではなく
水蒸気脱離方法は適しない。こうした理由から凝縮水に
溶剤等の回収成分が混入しない、すなわち吸着成分の脱
離に直接水蒸気を使用しない処理方法または装置が必要
とされる。There are various adsorption methods, but the most commonly used method is obtained by adsorbing a solvent or the like on activated carbon and then directly blowing steam onto the activated carbon to desorb the adsorbed components. In this method, the vapor mixture is cooled and condensed to recover the solvent and the like. This method is an excellent method that can efficiently recover the solvent and the like with a very simple operation, but on the other hand, a considerable amount of the condensed water of the used steam is generated with the recovery of the solvent and the like. Such condensed water often contains components such as a solvent and may require wastewater treatment. Also, when the recovered component is water-soluble, separation from condensed water is not easy and the steam desorption method is not suitable. For these reasons, there is a need for a treatment method or apparatus that does not mix recovered components such as solvents into condensed water, that is, that does not directly use steam for desorption of adsorbed components.
【０００４】吸着成分の脱離に水蒸気を用いない方式と
しては空気などを再生ガスとして用いるガス脱離方式が
ある。これは吸着成分の脱離に水蒸気の代わりに高温の
ガスを用いるものである。一般に溶剤等を回収するため
には脱離した溶剤等の蒸気を凝縮させる必要がある。し
かしながら、ガス脱離方式の場合には再生ガスは非凝縮
性ガスを含むので、溶剤等の蒸気を凝縮させるためには
凝縮温度における溶剤等の飽和蒸気圧以上の分圧を有す
るようなかなり高濃度の再生ガスを得る必要がある。高
濃度の再生ガスを得るには極力少ない量の再生ガス中で
極力多くの溶剤等を脱離させなければならない。As a method that does not use water vapor for desorbing the adsorbed components, there is a gas desorption method that uses air as a regeneration gas. This uses a high-temperature gas instead of steam for desorption of adsorbed components. Generally, in order to recover the solvent and the like, it is necessary to condense the vapor of the desorbed solvent and the like. However, in the case of the gas desorption system, the regenerated gas contains a non-condensable gas, and therefore, in order to condense the vapor of the solvent or the like, it has a considerably high partial pressure equal to or higher than the saturated vapor pressure of the solvent or the like at the condensation temperature. It is necessary to obtain a concentration of regeneration gas. In order to obtain a high-concentration regenerated gas, it is necessary to desorb as much solvent as possible in the regenerated gas in the smallest amount possible.
【０００５】ところで溶剤等の脱離には所定の熱量が必
要である。ガス脱離方式ではその熱量は回収ガスの保有
する顕熱によって与えられるから、多くの溶剤を脱離さ
せるには多くの熱量を与えなければならない。そのため
には再生ガスの温度を上げるかあるいは再生ガス量を多
くしなければならない。再生ガス温度を高くすると吸着
体の耐久性や回収すべき溶剤の分解が問題になるため一
定の限界があり、また再生ガス量を多くすると再生ガス
濃度は低下する。このように通常のガス脱離方式では得
られる再生ガス濃度には限界があるため、ある程度溶剤
等の濃縮はできるが溶剤を凝縮回収することはかなり困
難である。By the way, a predetermined amount of heat is required to remove the solvent and the like. In the gas desorption system, the amount of heat is given by the sensible heat of the recovered gas, so a large amount of heat must be given to desorb many solvents. For that purpose, it is necessary to raise the temperature of the regeneration gas or increase the amount of regeneration gas. If the temperature of the regenerating gas is increased, the durability of the adsorbent and the decomposition of the solvent to be recovered become problems, so there is a certain limit, and if the amount of the regenerating gas is increased, the concentration of the regenerating gas decreases. As described above, since the concentration of the regenerated gas obtained by the usual gas desorption system is limited, the solvent and the like can be concentrated to some extent, but it is quite difficult to condense and recover the solvent.
【０００６】さらにまた可燃性溶剤等を処理する場合、
水蒸気による直接脱離方式では問題ないがガス脱離方式
では爆発燃焼の危険性を避けるため高濃度となる回収工
程は窒素ガス等の不活性ガス雰囲気下で実施する必要が
あるが、吸着工程から回収工程への移行にともなう効率
的な窒素ガス等の置換は一般に非常に難しい。When treating a flammable solvent, etc.,
Although there is no problem in the direct desorption method using water vapor, in the gas desorption method the recovery process with a high concentration must be carried out in an inert gas atmosphere such as nitrogen gas in order to avoid the risk of explosive combustion. Efficient replacement of nitrogen gas or the like with the shift to the recovery step is generally very difficult.
【０００７】[0007]
【発明が解決しようとする課題】水蒸気による直接脱離
方式以外の方法で、溶剤等を含有する空気等のガスから
溶剤等を除去しかつ除去した溶剤等を効率よく濃縮回収
すること、またこれは可燃性溶剤等の処理にも応用でき
るものであってかつその際窒素ガス等の不活性ガスの使
用量をできる限り少なくすることが本発明が解決しよう
とする課題である。The solvent and the like are removed from a gas such as air containing the solvent by a method other than the direct desorption method using water vapor, and the removed solvent and the like are efficiently concentrated and recovered. Is applicable to the treatment of flammable solvents, and the problem to be solved by the present invention is to reduce the amount of inert gas such as nitrogen gas used as much as possible.
【０００８】[0008]
【課題を解決するための手段】前記したような課題に関
し鋭意検討した結果以下に示すように特殊な構造を有し
た吸着体を使用して間接熱交換による脱離方式を行なう
ことにより解決できることを見い出した。Means for Solving the Problems As a result of intensive studies on the above problems, it can be solved by performing a desorption method by indirect heat exchange using an adsorbent having a special structure as shown below. I found it.
【０００９】すなわち本発明は、吸着、再生ガスの通流
する吸着剤を含む流路層Ａとこれとは別の流体流路であ
る流路層Ｂとが交互に積層され、かつ流路層Ａは波形の
シート状物により独立した多数の小流路に分割された構
造の吸着体を用いた吸着塔において、流路層Ａに溶剤等
を含む原ガスを通流させて溶剤等を吸着させる吸着工
程、および流路層Ｂに高温の流体を通流させながら流路
層Ａに少量のパージガスを通流させて吸着した溶剤等を
脱離させ、その脱離した溶剤等を冷却、凝縮、分離する
回収工程を交互に実施する操作を基本とし、複数の吸着
塔による前記吸着工程および回収工程を順次切り替えて
実施し連続的に原ガスを処理する。That is, according to the present invention, a flow path layer A containing an adsorbent through which an adsorption / regeneration gas flows and a flow path layer B which is a fluid flow path different from this are alternately laminated, and A is an adsorption tower using an adsorbent having a structure in which a plurality of small channels are divided into independent small channels by a corrugated sheet, and a raw gas containing a solvent is passed through the channel layer A to adsorb the solvent. And an adsorbing step in which the adsorbed solvent or the like is desorbed by passing a small amount of purge gas through the channel layer A while allowing a high temperature fluid to flow through the channel layer B, and the desorbed solvent or the like is cooled and condensed. On the basis of the operation of alternately carrying out the collecting step for separation, the adsorption step and the collecting step by a plurality of adsorption towers are sequentially switched and carried out to continuously treat the raw gas.
【００１０】また溶剤等が可燃性の場合には、原ガスの
吸着終了後、流路層Ａを含む流路Ａを不活性ガスでパー
ジし、その際パージガスは原ガスに合流させ、流路Ａ内
の酸素濃度が溶剤等の燃焼範囲以下になった後、やはり
パージガスに不活性ガスを用いて前記回収工程を実施す
る。さらに本発明を有利に実施する方法として、少なく
とも３基の吸着塔を設け前記吸着工程、回収工程を順次
連続的に行うに際し、前記回収工程からの未凝縮ガス
を、吸着工程を終了しかつ回収工程を開始する前の段階
にある吸着塔に通流させ、未凝縮ガス中の溶剤等をその
吸着塔内の吸着体に吸着せしめ、その後再び回収工程の
パージガスとして用いる。この方法は再生ガスとして不
活性ガス（特に窒素ガス）を使用する場合に特に有効で
ある。こうした方法により前記課題を解決するという目
的が達せられる。When the solvent or the like is flammable, after the adsorption of the raw gas is completed, the flow passage A including the flow passage layer A is purged with an inert gas, and the purge gas is merged with the raw gas at this time. After the oxygen concentration in A falls below the combustion range of the solvent and the like, the above-mentioned recovery step is carried out using an inert gas as the purge gas. Further, as a method for carrying out the present invention in an advantageous manner, when at least three adsorption towers are provided and the adsorption step and the recovery step are successively performed in sequence, uncondensed gas from the recovery step is terminated and recovered. The solvent in the uncondensed gas is adsorbed by the adsorbent in the adsorption tower after passing through the adsorption tower at the stage before starting the step, and then used again as the purge gas in the recovery step. This method is particularly effective when an inert gas (particularly nitrogen gas) is used as the regeneration gas. The purpose of solving the above problems can be achieved by such a method.
【００１１】[0011]
【作用】本発明に用いる吸着体の一例を図２に示すが、
処理されるべき原ガスや脱離時のパージガスが通流する
流通層Ａ（３１）と再生時の加熱流体等が通流する流路
層Ｂ（３２）とが隔離されている。なお３６はシール枠
である。また図３に示すのが吸着塔の概要図であるが、
吸着塔は主に１個または複数個の吸着体とそれらに各流
体を分配するためのダクト等からなる分配室（３３、３
４、３５、３６）で構成されていて、分配室３３、３４
は吸着体の流路層Ａ側に通じており、分配室３５、３６
は流路層Ｂ側に通じていてそれぞれの流路層に対し別々
に流体を供給できるようになっている。また吸着体の流
路層Ａ、それに通じる分配室および前後の導管を合わせ
て流路Ａと呼ぶ。流路Ｂについても同様である。2 shows an example of the adsorbent used in the present invention.
The flow layer A (31) through which the raw gas to be treated and the purge gas at the time of desorption flow and the flow path layer B (32) through which the heating fluid and the like flow during regeneration are separated. Reference numeral 36 is a seal frame. Further, FIG. 3 is a schematic diagram of the adsorption tower,
The adsorption tower is mainly composed of one or a plurality of adsorbents and a distribution chamber (33, 3 or 3) composed of ducts or the like for distributing each fluid to them.
4, 35, 36), and the distribution chambers 33, 34
Is connected to the flow path layer A side of the adsorbent, and the distribution chambers 35, 36
Is connected to the flow path layer B side so that the fluid can be separately supplied to each flow path layer. Further, the flow path layer A of the adsorbent, the distribution chamber leading to the adsorbent, and the front and rear conduits are collectively referred to as a flow path A. The same applies to the flow path B.
【００１２】つぎに本発明の基本的な操作を説明する。
溶剤等を含んだ原ガスはまず一つの吸着塔に導入されそ
の内部の吸着体の流路層Ａに通流される。原ガスに含ま
れる溶剤等は吸着体の流路層Ａに含まれる吸着剤に吸着
除去された清浄ガスとして吸着体の他端から排出され
る。吸着体に吸着された溶剤等の濃度は徐々に増加して
行くが吸着破過が生じる前に吸着操作が停止される。原
ガスは別の吸着塔に切り替えられそこで引き続き吸着工
程が行われる。前記吸着を停止した吸着塔は回収工程に
移る。Next, the basic operation of the present invention will be described.
A raw gas containing a solvent and the like is first introduced into one adsorption tower and passed through the flow path layer A of the adsorbent therein. The solvent and the like contained in the raw gas are discharged from the other end of the adsorbent as clean gas that has been adsorbed and removed by the adsorbent contained in the flow path layer A of the adsorbent. The concentration of the solvent or the like adsorbed on the adsorbent gradually increases, but the adsorption operation is stopped before the adsorption breakthrough occurs. The raw gas is switched to another adsorption tower where the adsorption process continues. The adsorption tower that has stopped the adsorption moves to the recovery step.
【００１３】回収工程では流路層Ａに再生ガスとして少
量のパージガスが通流されるとともにこれとは隔離され
た流路層Ｂに加熱流体が通流されることにより溶剤等が
脱離され非常に高濃度の溶剤等含有ガスが得られるので
これを冷却凝縮させて溶剤等を回収することができるの
である。もちろん再生ガスをパージの前に予熱しておい
てもよい。吸着体の再生温度は一般に８０〜１５０℃で
あるが吸着体の材質によってはそれ以上の温度でも可能
である。In the recovery step, a small amount of purge gas is passed through the flow path layer A as a regeneration gas, and the heating fluid is passed through the flow path layer B, which is separated from the purge gas, so that the solvent and the like are desorbed and the temperature is very high. Since a gas containing a solvent or the like having a concentration is obtained, the solvent or the like can be recovered by cooling and condensing the gas. Of course, the regeneration gas may be preheated before purging. The regeneration temperature of the adsorbent is generally 80 to 150 ° C., but depending on the material of the adsorbent, a higher temperature can be used.
【００１４】前記吸着体は交互に多数積層された流路層
Ａと流路層Ｂから成っている。その構成の一例を図４に
示す。流路層Ａは通常波形の吸着性シート４２と平板状
の吸着性シート４１を積み重ねたいわゆるハニカム状を
なし多数の独立した小流路を有するように構成される。
吸着性シートの波形のピッチや波高は小さいほど吸着剤
の充填密度が高くなり吸着容量が大きくなるが反面、ガ
スが通流する場合の圧力損失が大きくなるので適当なピ
ッチが採用されなければならない。ピッチ、波高は通常
１〜５ｍｍ程度にとることが可能であるがピッチについ
ては２〜３ｍｍが好ましく、波高については１〜３ｍｍ
が好ましい。吸着性シートは吸着剤と骨材とをバインダ
ーを用いて抄紙したものが用いられ、吸着材には活性炭
素繊維、粉末活性炭、各種ゼオライト、吸着性樹脂等
が、また骨材にはパルプ、ガラス繊維、アスベスト繊
維、アラミド繊維が使用可能である。もちろん流路層Ａ
は、例えば突起を持った吸着性シートを重ねるなど吸着
性物質で構成されかつガスの適度の流通性があればよく
上記の構成にこだわらない。The adsorbent is composed of a plurality of flow channel layers A and B alternately laminated. An example of the configuration is shown in FIG. The flow path layer A has a so-called honeycomb shape in which a corrugated adsorptive sheet 42 and a flat plate-like adsorptive sheet 41 are stacked and has a large number of independent small channels.
The smaller the corrugated pitch or wave height of the adsorptive sheet, the higher the packing density of the adsorbent and the larger the adsorption capacity, but on the other hand, the pressure loss when the gas flows increases, so an appropriate pitch must be adopted. .. The pitch and wave height can usually be set to about 1 to 5 mm, but the pitch is preferably 2 to 3 mm, and the wave height is 1 to 3 mm.
Is preferred. The adsorptive sheet is made of a paper made of an adsorbent and an aggregate using a binder.The adsorbent is activated carbon fiber, powdered activated carbon, various zeolites, adsorbent resin, or the like, and the aggregate is pulp or glass. Fibers, asbestos fibers and aramid fibers can be used. Of course, the flow path layer A
Is not limited to the above structure as long as it is made of an adsorbent substance and has an appropriate gas flowability, for example, by stacking an adsorbent sheet having protrusions.
【００１５】なお一つの流路層Ａ内では波形と平板状シ
ートの組合せは１組であってもよく、またその流路層Ａ
内の熱伝達に支障のない範囲で２組以上にしてもよい。
図６は流路層Ａ内の波形と平板状シートの組合せを２組
にした例である。流路層Ｂは隣接する流路層Ａの間の間
隔を保ち流体が通流する構造であればなんでもよく例え
ば流路層Ａと同じような波形シートを用いてもよい。図
２や図６は波形シートを用いた例であり、図４は山形ス
ペーサー４４を用いた例である。ただしこれらはできる
だけ熱容量の小さい素材で構成することが好ましくペー
パー、樹脂や金属が用いられる。In one channel layer A, the combination of corrugations and flat sheet may be one set, and the channel layer A
There may be two or more pairs within a range that does not hinder heat transfer inside.
FIG. 6 shows an example in which the combination of the corrugations in the flow path layer A and the flat sheet is two. The flow path layer B may have any structure as long as the fluid flows through while keeping the space between the adjacent flow path layers A, and for example, a corrugated sheet similar to the flow path layer A may be used. 2 and 6 show an example using a corrugated sheet, and FIG. 4 shows an example using a chevron spacer 44. However, these are preferably composed of materials having a heat capacity as small as possible, and paper, resin or metal is used.
【００１６】流路層Ａと流路層Ｂの間は極力熱伝達がよ
く、かつ良好な隔離性すなわちガスの透過漏洩の極力少
ない隔壁４３で仕切られていることが必要である。従っ
てその隔壁としては例えばアルミや銅などの金属シート
やその他樹脂フィルム等を用いることができる。図５は
小突起を形成するように加工した金属シートを隔壁の片
方に使用してスペーサーと隔壁を兼ねさせた例である。
流路層Ａと流路層Ｂは上述のように別々の流路を形成し
なければならないので通常は吸着体の互いに直交した位
置に出入口端面が設けられシール枠で相互にシールされ
る。吸着塔内には１個または複数個の前記吸着体がある
が、流路Ａは各吸着体のそれぞれの流路層Ａガスが通流
するように、また流路Ｂについても同様に流路層Ｂに流
体が通流するように設置される。It is necessary that the heat transfer between the flow path layer A and the flow path layer B is as good as possible, and the partition wall 43 has good isolation, that is, gas permeation leakage is minimal. Therefore, as the partition wall, for example, a metal sheet such as aluminum or copper or other resin film can be used. FIG. 5 shows an example in which a metal sheet processed so as to form small protrusions is used as one of the partition walls to serve as both the spacer and the partition wall.
Since the flow path layer A and the flow path layer B have to form separate flow paths as described above, the inlet / outlet end faces are usually provided at positions orthogonal to each other on the adsorbent and are sealed with each other by the seal frame. There is one or a plurality of the adsorbents in the adsorption tower, but the flow path A is such that the gas of each flow path layer A of each adsorbent flows through, and the flow path B is also the same. The fluid is set to flow through the layer B.
【００１７】本発明のガス処理方法では吸着後の回収工
程において再生用のパージガスと脱離のための熱量を供
給する加熱用の流体とを分離することができる。従って
再生ガス量に関係なく加熱流体量を供給することができ
るため従来のガス脱離方法よりもはるかに高い濃度の再
生ガスをうることができるのである。また熱交換が用意
であるから吸着工程において吸着熱を除去して吸着を促
進させるために流路層Ｂに冷却流体を通流することもで
きる。In the gas treatment method of the present invention, the purge gas for regeneration and the heating fluid for supplying the amount of heat for desorption can be separated in the recovery step after adsorption. Therefore, since the amount of the heating fluid can be supplied regardless of the amount of the regeneration gas, it is possible to obtain the regeneration gas having a much higher concentration than the conventional gas desorption method. Further, since heat exchange is ready, a cooling fluid can be passed through the flow path layer B in order to remove the heat of adsorption and promote adsorption in the adsorption step.
【００１８】また回収工程を終了した吸着塔をそのまま
吸着工程に移行して原ガスを通流すると、吸着体は高温
であるため初期の吸着不良が生じ清浄ガス中の溶剤等の
濃度が高くなる場合がある。その場合は回収工程終了後
流路層Ｂに冷却流体を通流させて吸着体の温度を所定の
温度まで冷却してから吸着工程に移行させることができ
る。回収工程で濃縮後冷却して、含有溶剤等を凝縮、分
離した後の再生ガスは量は少ないが凝縮温度での飽和蒸
気圧の溶剤を有しかなりの高濃度であるため別途処理工
程を設けてもよいが普通は原ガスと合流させて吸着工程
に戻す。When the adsorption tower after the recovery step is transferred to the adsorption step as it is, and the raw gas is passed through, the initial adsorption failure occurs because the adsorbent is at a high temperature, and the concentration of the solvent and the like in the clean gas increases. There are cases. In that case, after completion of the recovery process, a cooling fluid can be caused to flow through the flow path layer B to cool the temperature of the adsorbent to a predetermined temperature, and then the adsorption process can be started. The concentration of the regenerated gas after condensation and cooling in the recovery process after condensing and separating the contained solvent, etc. is small, but there is a solvent with a saturated vapor pressure at the condensation temperature and a considerably high concentration, so a separate treatment process is provided. Although it may be used, it is usually combined with the raw gas and returned to the adsorption step.
【００１９】次にそうした操作方法の例として吸着塔が
２基の場合につき図１に従って説明する。送風機４によ
り原ガスライン１０から原ガスが、第一吸着塔１にその
流路Ａ側の導管１１から供給される。この原ガスは流路
Ａに連絡している吸着体の各流路層Ａに通流され含有す
る溶剤等が吸着される。溶剤等の除去されたガスは清浄
ガスとして導管１３より大気中に排出される。この吸着
操作において必要な場合には冷却流体循環手段９により
導管２１から第一吸着塔の流路Ｂに冷却流体が供給され
導管２３を通って元に戻る。この冷却流体は吸着体の各
流路層Ｂを通り、これにより流路層Ａで生成する吸着熱
が隔壁を通して除去される。Next, as an example of such an operating method, a case where there are two adsorption towers will be described with reference to FIG. The raw gas is supplied from the raw gas line 10 by the blower 4 to the first adsorption tower 1 from the conduit 11 on the flow path A side. This raw gas is passed through each flow path layer A of the adsorbent communicating with the flow path A, and the solvent contained therein is adsorbed. The gas from which the solvent and the like have been removed is discharged into the atmosphere through the conduit 13 as a clean gas. When necessary in this adsorption operation, the cooling fluid circulating means 9 supplies the cooling fluid from the conduit 21 to the flow path B of the first adsorption tower and returns to the original state through the conduit 23. This cooling fluid passes through each flow path layer B of the adsorbent, and thereby the heat of adsorption generated in the flow path layer A is removed through the partition walls.
【００２０】これら第一吸着塔で吸着体が破過する前に
吸着工程を終了させ、原ガスの処理は第二吸着塔２に切
り替えられる。すなわち原ガスが送風機から導管１２を
通って第二吸着塔の流路Ａに供給され、そこで吸着工程
が引続きおこなわれる。一方第一吸着塔は回収工程に移
る。加熱流体循環手段８から導管２１、２３により第一
吸着塔の流路Ｂに加熱流体が供給され、吸着体の各流路
層Ｂに通流される。それとともに導管１５、１３を通っ
て少量の再生ガスが流路Ａに吸着時とは逆方向に供給さ
れる。The adsorption process is terminated before the adsorbent breaks through in the first adsorption tower, and the processing of the raw gas is switched to the second adsorption tower 2. That is, the raw gas is supplied from the blower through the conduit 12 to the flow path A of the second adsorption tower, and the adsorption process continues there. On the other hand, the first adsorption tower moves to the recovery process. The heating fluid is supplied from the heating fluid circulation means 8 to the channels B of the first adsorption tower by the conduits 21 and 23, and is flowed to the respective channel layers B of the adsorbent. At the same time, a small amount of regeneration gas is supplied to the channel A through the conduits 15 and 13 in the direction opposite to that at the time of adsorption.
【００２１】流路層Ｂの加熱流体の熱量が流路層Ｂから
流路層Ａにその間にある隔壁を通して伝えられ流路層Ａ
に吸着された溶剤等を脱離する。吸着体の各流路層Ａか
ら脱離された溶剤等により濃度の高い再生ガスを生じ
る。この再生ガスは流路層Ａから取り出され導管１１、
１７を通って凝縮器６に導かれ冷却されて、含まれる溶
剤等の一部が凝縮され溶剤等として分離され回収容器７
に回収される。なお未凝縮の溶剤等を含むガスは導管２
０から送風機の吸入側に戻され、原ガスに合流されて吸
着工程で処理される。流路層Ａから十分に溶剤等の脱離
が行なわれると加熱流体の供給が停止され、また必要に
より冷却流体循環手段から導管２１、２３を通って流路
Ｂに冷却流体が循環され吸着体が冷却され、その温度が
十分に低下した時点で冷却流体を停止し第一吸着塔の回
収工程を終了する。The heat quantity of the heating fluid of the flow path layer B is transmitted from the flow path layer B to the flow path layer A through the partition walls between the flow path layer A and the flow path layer A.
Desorb the solvent, etc. adsorbed on. A regenerated gas having a high concentration is generated by the solvent and the like desorbed from each flow path layer A of the adsorbent. This regeneration gas is taken out from the flow path layer A, the conduit 11,
It is guided to the condenser 6 through 17 and cooled, and a part of the contained solvent and the like is condensed and separated as the solvent and the like, and the recovery container 7
Will be collected. In addition, the gas containing uncondensed solvent etc. is in the conduit 2
It is returned from 0 to the suction side of the blower, merged with the raw gas, and processed in the adsorption step. When the solvent or the like is sufficiently desorbed from the flow path layer A, the supply of the heating fluid is stopped, and if necessary, the cooling fluid is circulated from the cooling fluid circulating means to the flow path B through the conduits 21 and 23 to adsorb the adsorbent. Is cooled, and the cooling fluid is stopped at the time when the temperature is sufficiently lowered, and the recovery process of the first adsorption tower is completed.
【００２２】そして第二吸着塔での吸着工程が終了した
時点で原ガスはこの第一吸着塔に切り替えられて吸着工
程に入り、第二吸着塔は回収工程に移行する。図１に示
すように加熱流体循環手段、冷却流体循環手段から各吸
着塔へはそれぞれ別個に独立して循環できるように導管
回路が設けられている。また吸着塔が３基以上ある場合
も同様に吸着工程を第一吸着塔から第二吸着塔へ、第二
から第三へと順次切り替えていき、吸着工程の終了した
吸着塔は、他の吸着塔で吸着工程が実施されている間に
回収工程が行なわれる。When the adsorption step in the second adsorption tower is completed, the raw gas is switched to the first adsorption tower to enter the adsorption step, and the second adsorption tower moves to the recovery step. As shown in FIG. 1, a conduit circuit is provided so that the heating fluid circulating means and the cooling fluid circulating means can individually and independently circulate to each adsorption tower. Similarly, when there are three or more adsorption towers, the adsorption step is sequentially switched from the first adsorption tower to the second adsorption tower, and then from the second to the third adsorption tower, and the adsorption tower after the adsorption step is completed by another adsorption tower. The recovery process is performed while the adsorption process is performed in the tower.
【００２３】溶剤等が可燃性である場合には回収工程で
の濃縮で再生ガス濃度が爆発燃焼範囲に入る可能性があ
って危険なため窒素ガス等の不活性ガスの雰囲気下で操
作をする必要があるので次のような操作を行なう。第一
吸着塔での吸着工程はこれまでに示したような通常の操
作で行なう。次に回収工程に入る前に導管１５、導管１
３を通って第一吸着塔の流路Ａに吸着時とは反対方向に
不活性ガスをパージして吸着塔内の流路層Ａを含む流路
Ａを不活性ガスで置換する。この間のパージ後のガスは
導管１７、酸素濃度計５、導管１９、２０を通って原ガ
スに還流されて別の吸着工程にある吸着塔にて処理され
る。When the solvent or the like is flammable, the concentration of the regenerated gas may be in the explosive combustion range due to the concentration in the recovery step, and it is dangerous. Therefore, the operation is performed in an atmosphere of an inert gas such as nitrogen gas. You need to perform the following operations. The adsorption step in the first adsorption tower is carried out by the usual operation as described above. Next, before entering the recovery process, conduit 15 and conduit 1
The inert gas is purged into the flow path A of the first adsorption tower through 3 in the direction opposite to that at the time of adsorption to replace the flow path A including the flow path layer A in the adsorption tower with the inert gas. The purged gas during this period is returned to the raw gas through the conduit 17, the oxygen concentration meter 5, and the conduits 19 and 20, and is processed in the adsorption tower in another adsorption step.
【００２４】そして酸素濃度計により系内酸素そが溶剤
塔の爆発燃焼範囲以下の安全な濃度に低下したのを確認
してから不活性ガスパージを中止して回収工程に移行す
る。一般的には可燃性溶剤等の燃焼範囲は酸素濃度１０
％（ｖｏｌ）以上である。従ってそれ以下の酸素濃度で
あれば一応安全といえるが実際には安全をみて５〜６％
程度以下に保持するのが好ましい。回収工程では再生ガ
スとしてはやはり不活性ガスを使用し、加熱流体循環手
段から流路Ｂに加熱流体を循環供給して流路層Ａから溶
剤等を脱離させ、それらを冷却して溶剤等を凝縮分離回
収する。また未凝縮のガスは原ガスに還流させ吸着工程
にある他の吸着塔で処理される。Then, after confirming that the oxygen concentration in the system has decreased to a safe concentration below the explosive combustion range of the solvent tower with an oxygen concentration meter, the inert gas purge is stopped and the process proceeds to the recovery step. Generally, the burning range of flammable solvents is oxygen concentration 10
% (Vol) or more. Therefore, if the oxygen concentration is lower than that, it is safe to say that it is actually 5-6%.
It is preferable to keep it at a degree or less. In the recovery step, an inert gas is still used as the regenerated gas, and the heating fluid is circulated and supplied from the heating fluid circulating means to the channel B to desorb the solvent and the like from the channel layer A and cool them to remove the solvent and the like. Are condensed, separated and collected. Further, the uncondensed gas is returned to the raw gas and treated in another adsorption tower in the adsorption step.
【００２５】本発明に使用する吸着体の流路層Ａは流路
方向に多数の小透孔を有する、いわゆるハニカム構造な
のでデッドスペースが少なくピストン流れが得られやす
い。従って非常に効率よく不活性ガスによる置換ができ
る。流路層Ａを不活性ガス雰囲気下で操作する場合、流
路層Ｂに通流する加熱流体あるいは冷却流体は空気を使
用してもよいが、吸着体の構造やシール部分からの漏洩
等による空気と再生ガスの混合が生じる可能性がある。
そのために常に流路層Ａよりも流路層Ｂ側の圧力を高め
に保って操作し流路層Ｂの空気中への濃厚な溶剤等含有
ガスの侵入を阻止するのがよい。なお流路層Ａへは再生
ガスとして不活性ガスがパージされるのでいくらかの空
気が流路層Ｂより漏洩しても補えるわけである。この場
合酸素分析計によって常時酸素濃度を監視するのが好ま
しい。また流路層Ｂにおいても不活性ガスを使用すれば
なお好ましい。なお不活性ガスとしては窒素ガスが最も
一般的であるがそれ以外に反応オフガスなど酸素濃度の
低いガスを利用することもできる。Since the flow path layer A of the adsorbent used in the present invention has a so-called honeycomb structure having a large number of small through holes in the flow path direction, the dead space is small and a piston flow is easily obtained. Therefore, the replacement with the inert gas can be performed very efficiently. When the flow channel layer A is operated in an inert gas atmosphere, air may be used as the heating fluid or cooling fluid flowing in the flow channel layer B, but due to the structure of the adsorbent or leakage from the seal portion. Mixing of air and regeneration gas can occur.
For this reason, it is preferable that the pressure on the flow path layer B side is higher than that on the flow path layer A at all times to prevent the inflow of a gas containing a rich solvent or the like into the air of the flow path layer B. In addition, since an inert gas is purged into the flow path layer A as a regeneration gas, even if some air leaks from the flow path layer B, it can be supplemented. In this case, it is preferable to constantly monitor the oxygen concentration with an oxygen analyzer. It is more preferable to use an inert gas also in the flow path layer B. Nitrogen gas is most commonly used as the inert gas, but a gas having a low oxygen concentration such as a reaction off gas can also be used.
【００２６】不活性ガスとして窒素ガスを使用する場
合、再生ガスとしてのパージ量は少量とはいいながら空
気を使用する場合に比べて運転コストが高くなる。そこ
で次のような方法によりパージ用窒素ガスを循環再使用
して節約することもできる。すなわち吸着塔を３塔以上
使用し、回収工程にある吸着塔からの再生ガスから溶剤
等を回収した後の未凝縮ガスを、吸着工程終了後の窒素
ガス置換後であってかつ回収工程前の吸着塔の流路Ａに
供給して、未凝縮で残留している溶剤等をさらに吸着さ
せる。これにより清浄になったガスを回収工程に還流さ
せ再生用のパージガスとして用いる。図７はその場合の
運転系統図である。また図８は実際の各吸着塔の作動状
況を示す工程図である。When nitrogen gas is used as the inert gas, the operating cost is higher than when air is used, although the amount of purge as the regeneration gas is small. Therefore, the purging nitrogen gas can be circulated and reused by the following method to save the cost. That is, using three or more adsorption towers, the uncondensed gas after recovering the solvent and the like from the regeneration gas from the adsorption tower in the recovery step is replaced with nitrogen gas after the adsorption step and before the recovery step. It is supplied to the flow path A of the adsorption tower to further adsorb the uncondensed residual solvent and the like. The gas thus cleaned is returned to the recovery step and used as a purge gas for regeneration. FIG. 7 is an operation system diagram in that case. In addition, FIG. 8 is a process diagram showing an actual operating state of each adsorption tower.
【００２７】第一吸着塔は吸着工程にあり溶剤等を含ん
だ原ガスを処理している。この際冷却流体循環手段（図
示せず）よりその流路Ｂに冷却流体を通流させてもよ
い。第三吸着塔は回収工程にあり加熱流体循環手段（図
示せず）による流路Ｂに加熱流体を通流しながら再生ガ
スを流路Ａに通流させて流路層Ａから溶剤等を脱離させ
凝縮器にて冷却し溶剤等を凝縮分離している。The first adsorption tower is in the adsorption step and processes the raw gas containing the solvent and the like. At this time, the cooling fluid may be caused to flow through the flow passage B by a cooling fluid circulating means (not shown). The third adsorption tower is in the recovery step and the regeneration gas is passed through the flow passage A while the heating fluid is being passed through the flow passage B by the heating fluid circulation means (not shown) to desorb the solvent and the like from the flow passage layer A. Then, it is cooled in a condenser to condense and separate the solvent.
【００２８】第二吸着塔は吸着工程を終了して窒素ガス
置換が行なわれる。この窒素ガス置換時の排出ガスは原
ガスに合流され吸着工程にある第一吸着塔で処理され
る。それから第三吸着塔での回収工程で溶剤等が冷却凝
縮分離された後の未凝縮ガスが供給され流路層Ａの吸着
体に残留溶剤が吸着される。溶剤が除かれて清浄になっ
た未凝縮ガスは第三吸着塔に還流され再生ガスとして使
用される。この第二吸着塔での工程を未凝縮ガス処理工
程という。なおこの未凝縮ガス処理工程でも吸着熱除去
のため流路層Ｂに冷却流体循環手段（図示せず）から冷
却流体を循環させてもよい。第一吸着塔での吸着工程が
終了すれば吸着工程は第三吸着塔に、また回収工程は第
二吸着塔に移る。第一吸着塔は窒素ガス置換されてから
未凝縮ガス処理工程に移り第二吸着塔での回収工程から
生じる未凝縮ガスの吸着に供せられる。In the second adsorption tower, the adsorption process is completed and the nitrogen gas is replaced. The exhaust gas at the time of this nitrogen gas replacement is combined with the raw gas and processed in the first adsorption tower in the adsorption step. Then, in the recovery step in the third adsorption tower, the uncondensed gas after the solvent and the like are cooled and condensed and separated is supplied, and the residual solvent is adsorbed on the adsorbent of the flow path layer A. The uncondensed gas, which has been cleaned by removing the solvent, is returned to the third adsorption tower and used as a regeneration gas. This process in the second adsorption tower is called an uncondensed gas treatment process. Even in this uncondensed gas treatment step, the cooling fluid may be circulated from the cooling fluid circulation means (not shown) in the channel layer B for removing the adsorption heat. When the adsorption step in the first adsorption tower is completed, the adsorption step is moved to the third adsorption tower and the recovery step is moved to the second adsorption tower. After the first adsorption tower is replaced with nitrogen gas, it moves to the uncondensed gas treatment step and is used for adsorption of the uncondensed gas generated in the recovery step in the second adsorption tower.
【００２９】回収工程での未凝縮ガス量は少量ではある
が溶剤等の濃度が原ガスよりもはるかに高い。従って原
ガスによる吸着工程の後であってもさらに吸着が行なわ
れる。しかもこの操作を行なうと吸着体の溶剤等の吸着
濃度は単に原ガスを吸着させた場合よりも高くなるので
回収工程でより高い濃度の再生ガスがえられ溶剤等の回
収効率がよくなるという利点もある。これを原ガスに還
流させず未凝縮ガス処理工程を通すことにより吸着工程
の負荷を軽減でき溶剤除去率の向上に貢献できる。Although the amount of uncondensed gas in the recovery step is small, the concentration of solvents and the like is much higher than that of the raw gas. Therefore, further adsorption is performed even after the adsorption step using the raw gas. Moreover, when this operation is performed, the adsorption concentration of the solvent or the like of the adsorbent becomes higher than that when the raw gas is simply adsorbed, so that there is an advantage that a higher concentration of regenerated gas is obtained in the recovery step and the recovery efficiency of the solvent is improved. is there. By passing this through the uncondensed gas treatment process without returning it to the raw gas, the load of the adsorption process can be reduced and the solvent removal rate can be improved.
【００３０】本発明によって処理できるものは有機溶剤
類が最も一般的であり例えば各種フロンやトリクロルエ
チレン、１・１・１−トリクロルエタンなどの塩素系溶
剤、ベンゼン、トルエンなどの芳香族類、アセトン、メ
チルイソブチルケトンなどのケトン類、酢酸メチル、酢
酸エチルなどのエステル類、エタンール、イソプロパノ
ールなどのアルコール類、ガソリン、灯油などの石油類
などが回収できる。もちろんこれらに限定されるもので
はなく吸着可能な成分であれば処理が可能である。また
本発明の方法は回収工程における冷却、凝縮操作を行な
わず単にガス中の希薄な成分の濃縮に応用することもで
きる。Organic solvents are most commonly used in the present invention. For example, various fluorocarbons, trichloroethylene, chlorine-based solvents such as 1.1.1-trichloroethane, aromatics such as benzene and toluene, and acetone. , Ketones such as methyl isobutyl ketone, esters such as methyl acetate and ethyl acetate, alcohols such as ethanol and isopropanol, petroleum such as gasoline and kerosene can be recovered. Of course, the components are not limited to these, and any component that can be adsorbed can be treated. The method of the present invention can also be applied to simply concentrate a dilute component in a gas without performing cooling and condensation operations in the recovery step.
【００３１】[0031]
（実施例１）図１のフローで示される装置を用いて１・
１・１−トリクロロエタンを２０００ｐｐｍ含む３０℃
の空気を１ｍ3 ／ｍｉｎの割合で処理した。図４の構造
の吸着体を用いた。流路層Ａの吸着剤は活性炭素繊維
（比表面積１５ｍ2 ／ｇ）を７５％含む目付１２０ｇ／
ｍ2 のペーパーおよびそれを波形加工したものである。
波形の波長ピッチは３ｍｍ、また波高は２．５ｍｍであ
る。隔壁はアルミシートを使用した。流路層Ｂにはアル
ミシートを加工した山形スペーサーを１０ｍｍピッチで
挿入し隔壁の間隔を２．５ｍｍに保持した。吸着体内で
の流速を０．４ｍ／ｓｅｃとし一つの吸着塔での吸着工
程の時間を３０分とした。まず最初に原ガスを導管１１
から第一吸着塔１に送り吸着処理後清浄になった空気は
導管１３より大気中に排出する（吸着工程）。この間第
一吸着塔における吸着体の流路層Ｂに冷却流体循環手段
９より導管２１を通って常温の空気を通流した。(Example 1) Using the apparatus shown in the flow chart of FIG.
30 ℃ containing 2000 ppm of 1.1-trichloroethane
Air was treated at a rate of 1 m 3 / min. The adsorbent having the structure shown in FIG. 4 was used. The adsorbent of the flow path layer A contains a activated carbon fiber (specific surface area 15 m 2 / g) of 75% and a basis weight of 120 g /
It is a m 2 paper and a corrugated product.
The waveform has a wavelength pitch of 3 mm and a wave height of 2.5 mm. An aluminum sheet was used for the partition. In the flow path layer B, mountain-shaped spacers made by processing an aluminum sheet were inserted at a pitch of 10 mm and the distance between the partition walls was kept at 2.5 mm. The flow rate in the adsorbent was 0.4 m / sec, and the adsorption step time in one adsorption tower was 30 minutes. First of all, the raw gas conduit 11
The air that has been sent to the first adsorption tower 1 and has been cleaned after the adsorption treatment is discharged into the atmosphere through the conduit 13 (adsorption step). During this time, normal temperature air was passed through the conduit 21 from the cooling fluid circulation means 9 to the flow path layer B of the adsorbent in the first adsorption tower.
【００３２】上記吸着工程終了後原ガスは第二吸着塔へ
切り替え第一吸着塔吸着体の流路層Ｂには加熱流体循環
手段８より１３０℃に加熱された空気を循環させるとと
もに、一方導管１５、１３より空気を１０リットル／分
で第一吸着塔の流路Ａ側を吸着工程時とは逆方向に通流
パージさせた。このパージガスは導管１７にて凝縮器６
に導き溶剤容器７に溶剤を回収した（回収工程）。この
際の凝縮器温度は３℃である。これら回収工程の時間は
約１５分である。また凝縮器での未凝縮ガスは導管２０
を通って送風機４の吸入側に還流させ原ガスに混合し
た。After completion of the adsorption step, the raw gas is switched to the second adsorption tower, and the air heated to 130 ° C. by the heating fluid circulating means 8 is circulated in the flow path layer B of the first adsorption tower adsorber, while the one conduit is provided. From 15 and 13, air was flown and purged at a rate of 10 liters / minute on the flow path A side of the first adsorption tower in the direction opposite to that in the adsorption step. This purge gas is supplied to the condenser 6 through the conduit 17.
And the solvent was collected in the solvent container 7 (collection step). The condenser temperature at this time is 3 ° C. The time for these recovery steps is about 15 minutes. The uncondensed gas in the condenser is the conduit 20.
It was flowed back to the suction side of the blower 4 and mixed with the raw gas.
【００３３】回収工程終了後第一吸着塔吸着体の流路層
Ｂに冷却流体循環手段より常温の空気を約１０分循環さ
せて吸着体を冷却した。かくして第二吸着塔の吸着工程
の終了後また吸着工程を第一吸着塔に切り替えるといっ
た操作を繰り返した。各所の濃度などは時間的に変動す
るが３時間以上の連続運転における平均値はつぎのよう
であった。 清浄ガス濃度 ３０ ｐｐｍ 溶剤除去率 ９８．５ ％ （１−清浄ガス濃
度／原ガス濃度） 回収溶剤量 ６２５ ｇ／ｈ 溶剤回収率 ９７．０ ％ （回収溶剤量／原
ガス含有溶剤量）After the recovery step was completed, the adsorbent was cooled by circulating air at room temperature for about 10 minutes through the cooling fluid circulating means in the flow path layer B of the adsorbent in the first adsorption tower. Thus, after the end of the adsorption step of the second adsorption tower, the operation of switching the adsorption step to the first adsorption tower was repeated. Concentrations at various places fluctuate with time, but the average value in continuous operation for 3 hours or more was as follows. Clean gas concentration 30 ppm Solvent removal rate 98.5% (1-clean gas concentration / original gas concentration) Recovery solvent amount 625 g / h Solvent recovery rate 97.0% (recovered solvent amount / original gas content solvent amount)
【００３４】（実施例２）次に溶剤としてトルエンを用
いて同様のテストを行なった。実施例１と同じ装置を用
いてトルエンを２０００ｐｐｍ含む３０℃の空気を１ｍ
3 ／ｍｉｎの割合で処理した。吸着体内での流速、吸着
工程の時間、その他の主な運転条件も実施例１と同様で
ある。まず第一吸着塔で吸着工程を行なう。吸着工程の
間、第一吸着塔における吸着体の流路層Ｂには冷却流体
循環手段９より導管２１を通って常温の窒素ガスを循環
させた。上記吸着工程終了後原ガスは第二吸着塔へ切り
替えた。(Example 2) Next, a similar test was conducted using toluene as a solvent. Using the same equipment as in Example 1, 1 m of air at 30 ° C. containing 2000 ppm of toluene
The treatment was performed at a rate of 3 / min. The flow rate in the adsorbent, the time of the adsorption step, and other main operating conditions are the same as in Example 1. First, the adsorption step is performed in the first adsorption tower. During the adsorption step, the nitrogen gas at room temperature was circulated through the conduit 21 from the cooling fluid circulation means 9 in the flow path layer B of the adsorbent in the first adsorption tower. After completion of the adsorption step, the raw gas was switched to the second adsorption tower.
【００３５】第一吸着塔では導管１５、１３より窒素ガ
スを３０リットル／分の流量で吸着工程時とは逆方向に
パージし流路Ａ側を窒素ガス置換した。そのパージガス
は導管１７から酸素濃度計５に導き系内の酸素濃度を測
定した。３分で酸素濃度は約１％になった。なおその間
のパージガスはバイパス導管１９から導管２０を通って
原ガスに還流させた。それから第一吸着塔吸着体の流路
層Ｂには加熱流体循環手段８より１３０℃に加熱された
窒素ガスを循環させるとともに、やはり導管１５、１３
より窒素ガスを１０リットル／分で第一吸着塔の流路Ａ
側を吸着工程時とは逆方向に通流パージさせた。このパ
ージガスは導管１７にて凝縮器６に導き冷却し凝縮した
溶剤を溶剤容器７に回収した。In the first adsorption tower, nitrogen gas was purged from the conduits 15 and 13 at a flow rate of 30 liters / minute in the direction opposite to that in the adsorption step, and the flow path A side was replaced with nitrogen gas. The purge gas was introduced from the conduit 17 to the oxygen concentration meter 5 to measure the oxygen concentration in the system. The oxygen concentration became about 1% in 3 minutes. The purge gas during that time was returned from the bypass conduit 19 to the raw gas through the conduit 20. Then, the nitrogen gas heated to 130 ° C. is circulated by the heating fluid circulating means 8 in the flow path layer B of the adsorbent of the first adsorption tower, and the conduits 15 and 13 are also provided.
Nitrogen gas at a flow rate of 10 L / min in the first adsorption tower
The side was flow-purged in the direction opposite to that in the adsorption step. The purge gas was introduced into the condenser 6 through the conduit 17 and cooled to collect the condensed solvent in the solvent container 7.
【００３６】凝縮器での未凝縮ガスは導管２０を通って
送風機４の吸入側に還流させ原ガスに混合した。回収工
程終了後第一吸着塔吸着体の流路層Ｂに冷却流体循環手
段８より常温の空気を約１０分間循環させて吸着体を冷
却した。以後吸着塔を順次切り替え、連続運転を行なっ
た。連続運転における平均値はつぎのようであった。 清浄ガス濃度 １６ ｐｐｍ 溶剤除去率 ９９．２ ％ 回収溶剤量 ４３５ ｇ／ｈ 溶剤回収率 ９８．０ ％The uncondensed gas in the condenser was refluxed to the suction side of the blower 4 through the conduit 20 and mixed with the raw gas. After the recovery step, the cooling fluid circulating means 8 circulated normal temperature air through the flow path layer B of the first adsorption tower adsorbent for about 10 minutes to cool the adsorbent. After that, the adsorption towers were sequentially switched, and continuous operation was performed. The average values in continuous operation were as follows. Clean gas concentration 16 ppm Solvent removal rate 99.2% Recovered solvent amount 435 g / h Solvent recovery rate 98.0%
【００３７】（実施例３）実施例２と同じ原ガスを図７
のように３基の吸着塔を用いて処理しパージ窒素ガスを
回収した。個々の吸着塔、凝縮器、その他の機器類は実
施例１と同じである。トルエンを２０００ｐｐｍ含む３
０℃の空気を１ｍ3 ／ｍｉｎの割合で処理した。吸着体
内での流速、吸着工程の時間、その他の主な運転条件も
実施例２と同様である。まず第一段階では第一吸着塔は
吸着工程にあり原ガスを処理している。第一吸着塔にお
ける吸着体の流路層Ｂに冷却流体循環手段（図示せず）
より常温の窒素ガスを循環させている。(Embodiment 3) The same raw gas as in Embodiment 2 is shown in FIG.
As described above, the treatment was performed using three adsorption towers, and the purged nitrogen gas was recovered. The individual adsorption tower, condenser, and other equipment are the same as in Example 1. Contains 2000 ppm of toluene 3
Air at 0 ° C. was treated at a rate of 1 m 3 / min. The flow rate in the adsorbent, the time of the adsorption step, and other main operating conditions are also the same as in Example 2. First, in the first stage, the first adsorption tower is in the adsorption process and is processing the raw gas. Cooling fluid circulating means (not shown) in the flow path layer B of the adsorbent in the first adsorption tower
Nitrogen gas at a room temperature is circulated.
【００３８】第二吸着塔は第一吸着塔が吸着工程に入る
前に吸着工程にあったが吸着工程終了後、前記窒素ガス
置換を行なった後回収工程にある第三吸着塔からの溶剤
回収後の未凝縮ガスが供給されている。窒素ガス置換条
件は実施例２と同様に、窒素ガスを３０リットル／分の
流量で吸着工程時とは逆方向に３分間パージし流路Ａ側
を窒素ガス置換した。そのパージガスは原ガスに還流さ
せた。第二吸着塔における吸着体の流路層Ｂにも、冷却
流体循環手段（図示せず）より常温の窒素ガスを循環さ
せている。第二吸着塔で溶剤を除去された未凝縮ガスは
第三吸着塔へ還流され再生用ガスとして使用される。The second adsorption tower was in the adsorption step before the first adsorption tower entered the adsorption step, but after the adsorption step was completed, the solvent was recovered from the third adsorption tower in the recovery step after performing the nitrogen gas replacement. The later uncondensed gas is being supplied. The nitrogen gas replacement conditions were the same as in Example 2, except that nitrogen gas was purged at a flow rate of 30 liters / minute for 3 minutes in the direction opposite to the adsorption step to replace the flow path A side with nitrogen gas. The purge gas was returned to the raw gas. In the flow path layer B of the adsorbent in the second adsorption tower, the nitrogen gas at room temperature is also circulated by the cooling fluid circulation means (not shown). The uncondensed gas from which the solvent has been removed in the second adsorption tower is returned to the third adsorption tower and used as a regeneration gas.
【００３９】第三吸着塔では吸着体の流路層Ｂに加熱流
体循環手段より１３０℃に加熱された窒素ガスを循環さ
せるとともに、窒素ガスおよび第二吸着塔での未凝縮ガ
ス処理工程の排出ガス１０リットル／分を流路Ａ側を吸
着工程時とは逆方向に通流パージさせた。このパージガ
スは凝縮器６に導き冷却し凝縮した溶剤を回収した。凝
縮器での未凝縮ガスは前記第二吸着塔に還流した。次に
第二段階では吸着工程は第三吸着塔に、回収工程は第二
吸着塔に、そして未凝縮ガス処理工程は窒素ガス置換後
の第一吸着塔に移り同様な操作を続ける。第三段階では
さらに各工程を一つずつずらせ、以後吸着塔を順次切り
替え連続運転を行なった。In the third adsorption tower, the nitrogen gas heated to 130 ° C. is circulated through the flow path layer B of the adsorbent by the heating fluid circulating means, and the nitrogen gas and the uncondensed gas treatment step in the second adsorption tower are discharged. A flow rate of 10 liter / min of gas was passed through the flow path A side in the direction opposite to that in the adsorption step and purged. This purge gas was introduced into the condenser 6 and cooled to collect the condensed solvent. The uncondensed gas in the condenser was refluxed to the second adsorption tower. Next, in the second stage, the adsorption process is moved to the third adsorption column, the recovery process is moved to the second adsorption column, and the uncondensed gas treatment process is moved to the first adsorption column after nitrogen gas replacement, and the same operation is continued. In the third stage, each process was further shifted one by one, and thereafter the adsorption towers were sequentially switched to perform continuous operation.
【００４０】連続運転における平均値はつぎのようであ
った。 清浄ガス濃度 ２４ ｐｐｍ 溶剤除去率 ９８．８ ％ 回収溶剤量 ４３５ ｇ／ｈ 溶剤回収率 ９８．０ ％ 本実施例では回収工程のパージ用窒素ガスが実施例２に
くらべて約２５０リットル／ｈ節約できることがわかっ
た。The average values in continuous operation were as follows. Clean gas concentration 24 ppm Solvent removal rate 98.8% Recovered solvent amount 435 g / h Solvent recovery rate 98.0% In this example, the nitrogen gas for purging in the recovery step was saved about 250 liters / h compared to Example 2. I knew I could do it.
【００４１】[0041]
【発明の効果】本発明の方法によれば、再生ガス量とは
関係なく吸着した溶剤等の脱離に必要な熱量を独立して
与えることができるため、再生ガス量を少なくすること
により容易に高い濃縮率が得られ溶剤等を凝縮して回収
することができる。しかも水蒸気による脱離のように多
量の凝縮水が回収溶剤に混合することもない。また吸着
体内の不活性ガス置換が容易なことから可燃製溶剤等の
回収も可能であり、さらにその際再生ガスを循環使用で
きるので不活性ガスとして窒素ガスを使用する場合でも
その消費量が少なくてすむ。According to the method of the present invention, the amount of heat necessary for desorbing the adsorbed solvent and the like can be independently provided regardless of the amount of the regenerated gas, and therefore it is easy to reduce the amount of the regenerated gas. A very high concentration rate can be obtained, and the solvent and the like can be condensed and recovered. In addition, a large amount of condensed water does not mix with the recovered solvent unlike desorption due to water vapor. In addition, it is possible to recover combustible solvents, etc. because it is easy to replace the inert gas in the adsorbent body, and at that time, the regeneration gas can be circulated and used, so the consumption amount is small even when nitrogen gas is used as the inert gas. End
【図１】本発明の溶剤回収システムのフロー図。FIG. 1 is a flow chart of a solvent recovery system of the present invention.
【図２】原ガス及びパージガスが通流する流路層Ａと再
生時の加熱ガスが通流する流路Ｂが交互に積層されてい
る吸着体の一例。FIG. 2 is an example of an adsorbent in which a flow path layer A through which a raw gas and a purge gas flow and a flow path B through which a heating gas during regeneration flows are alternately stacked.
【図３】吸着体と各流体を分離するためのダクト等から
なる分配室で構成される吸着塔の概要図。FIG. 3 is a schematic diagram of an adsorption tower including a distribution chamber including an adsorbent and a duct for separating each fluid.
【図４〜６】流路層Ａ、流路層Ｂが複数積層された吸着
体の一例。4 to 6 are examples of adsorbents in which a plurality of flow channel layers A and B are stacked.
【図７】３基の吸着塔を用いた場合の運転系統図。FIG. 7 is an operation system diagram when three adsorption towers are used.
【図８】３基の吸着塔を用いた場合の各吸着塔の工程
図。FIG. 8 is a process diagram of each adsorption tower when three adsorption towers are used.
１ 第一吸着塔 ２ 第二吸着塔 ３ 清浄ガス ４ 送風機 ５ 酸素濃度計 ６ 凝縮器 ７ 回収容器 ８ 加熱流体循環手段 ９ 冷却流体循環手段 １０ 原ガスライン １１〜１４ 導管 １５、１６ パージガス（窒素）用導管 １７〜２４ 導管 ３０ 吸着体 ３１ 流路層Ａ ３２ 流路層Ｂ ３３〜３５ 分配室 ３６ シール枠 ４１、４２ 吸着性シート ４３ 隔壁 ４４ スペーサー ４５ 第三吸着塔 ４６ 窒素ガス ４７ 原ガス ４８ 回収溶剤 DESCRIPTION OF SYMBOLS 1 1st adsorption tower 2 2nd adsorption tower 3 Clean gas 4 Blower 5 Oxygen concentration meter 6 Condenser 7 Recovery container 8 Heating fluid circulation means 9 Cooling fluid circulation means 10 Raw gas lines 11-14 Pipes 15 and 16 Purge gas (nitrogen) For conduit 17-24 Conduit 30 Adsorbent 31 Channel layer A 32 Channel layer B 33-35 Distribution chamber 36 Seal frame 41, 42 Adsorbent sheet 43 Partition wall 44 Spacer 45 Third adsorption tower 46 Nitrogen gas 47 Raw gas 48 Recovery solvent
Claims (2)
剤を含む流路層Ａとこれとは別の流体流路である流路層
Ｂとが交互に積層され、かつ流路層Ａが波形のシート状
物により独立した多数の小流路に分割された構造の吸着
体を用いた吸着塔において、流路層Ａに溶剤等を含む原
ガスを通流させて溶剤等を吸着させる吸着工程、および
流路層Ｂに高温の流体を通流させながら流路層Ａに少量
のパージガスを通流させて吸着した溶剤等を脱離させ、
その脱離した溶剤等を冷却、凝縮、分離する回収工程と
を交互に実施する方法であり、かつ複数の前記吸着塔に
より前記吸着工程および回収工程を順次切り替えて実施
し連続的に原ガスを処理することを特徴とする溶剤等の
回収方法。1. A flow path layer A containing an adsorbent through which an adsorbed gas and a regeneration gas flow and a flow path layer B which is a different fluid flow path from the adsorbent are alternately laminated, and the flow path layer A is In an adsorption tower using an adsorbent having a structure in which a large number of independent small channels are divided by a corrugated sheet-like material, adsorption in which a raw gas containing a solvent or the like is passed through the channel layer A to adsorb the solvent or the like. Step, and while passing a high temperature fluid through the flow path layer B, a small amount of purge gas is passed through the flow path layer A to desorb the adsorbed solvent and the like,
It is a method of alternately performing a recovery step of cooling, condensing and separating the desorbed solvent and the like, and continuously switching the adsorption step and the recovery step by a plurality of the adsorption towers to continuously carry out a raw gas. A method for recovering a solvent or the like characterized by treating.
る方法において、前記吸着工程、回収工程を順次連続的
に行うに際し、前記回収工程からの未凝縮ガスを、吸着
工程を終了しかつ回収工程を開始する前の段階にある吸
着塔に通流させ、未凝縮ガス中の溶剤等をその吸着塔内
の吸着体に吸着せしめ、その後再び回収工程のパージガ
スとして用いる溶剤等の回収方法。2. A method of using at least three adsorption towers according to claim 1, wherein when the adsorption step and the recovery step are successively performed, uncondensed gas from the recovery step is terminated and recovered. A method for recovering a solvent or the like to be used as a purge gas in the recovery step after causing the solvent or the like in the uncondensed gas to be adsorbed by the adsorbent in the adsorption tower by allowing the solvent or the like in the uncondensed gas to flow through the adsorption tower at the stage before starting the process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07603992A JP3282676B2 (en) | 1992-02-26 | 1992-02-26 | Recovery method for solvents, etc. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07603992A JP3282676B2 (en) | 1992-02-26 | 1992-02-26 | Recovery method for solvents, etc. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05237333A true JPH05237333A (en) | 1993-09-17 |
| JP3282676B2 JP3282676B2 (en) | 2002-05-20 |
Family
ID=13593669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP07603992A Expired - Fee Related JP3282676B2 (en) | 1992-02-26 | 1992-02-26 | Recovery method for solvents, etc. |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3282676B2 (en) |
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|---|---|---|---|---|
| JP2003071235A (en) * | 2001-08-30 | 2003-03-11 | Sumitomo Chem Co Ltd | Method for separating combustible organic solvent in gas to be treated |
| JP2007050379A (en) * | 2005-08-19 | 2007-03-01 | Air Liquide Japan Ltd | Recovery process for volatile organic compound |
| JP2007050378A (en) * | 2005-08-19 | 2007-03-01 | Air Liquide Japan Ltd | Recovery process for volatile organic compound |
| JP4530945B2 (en) * | 2005-08-19 | 2010-08-25 | 日本エア・リキード株式会社 | Recovery process for volatile organic compounds |
| JP2010527755A (en) * | 2007-05-18 | 2010-08-19 | エクソンモービル リサーチ アンド エンジニアリング カンパニー | Method for removing target gas from a mixture of gases by thermal swing adsorption |
| JP2009061402A (en) * | 2007-09-06 | 2009-03-26 | Nippon Oil Corp | Pier facilities and hydrocarbon recovery system |
| JP2013540573A (en) * | 2010-08-27 | 2013-11-07 | インヴェンティス サーマル テクノロジーズ インコーポレイテッド | Adsorbed gas separation method using thermally conductive contactor structure |
| CN114225644A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Device and method for treating trichloroethane tail gas in sucralose production |
| CN114225644B (en) * | 2021-11-23 | 2024-05-03 | 安徽金禾实业股份有限公司 | Trichloroethane tail gas treatment device and method in sucralose production |
| WO2023190088A1 (en) * | 2022-03-30 | 2023-10-05 | 東洋紡エムシー株式会社 | Gas treatment device and gas treatment method |
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