JPH0622654B2 - Adsorption method of removing halogenated hydrocarbon gas - Google Patents

Adsorption method of removing halogenated hydrocarbon gas


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JPH0622654B2 JP27546685A JP27546685A JPH0622654B2 JP H0622654 B2 JPH0622654 B2 JP H0622654B2 JP 27546685 A JP27546685 A JP 27546685A JP 27546685 A JP27546685 A JP 27546685A JP H0622654 B2 JPH0622654 B2 JP H0622654B2
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activated carbon
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JPS62132523A (en )
武士 岸元
進 朝倉
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【発明の詳細な説明】 [産業上の利用分野] 本発明は、ハロゲン化炭化水素系ガスを含有する混合ガスから該ハロゲン化炭化水素系ガス(以下Hal−CH DETAILED DESCRIPTION OF THE INVENTION [FIELD OF THE INVENTION The present invention, the halogenated hydrocarbon gas from a mixed gas containing a halogenated hydrocarbon gas (hereinafter Hal-CH
ガスと記す)を効率良く吸着除去することのできる方法に関するものである。 It referred to as gas) to a method capable of efficiently adsorb and remove.

[従来の技術] 有機溶剤を取扱う業界でしばしば問題となるのは揮発溶剤が作業員に与える健康障害である。 Often it becomes a problem in the industry to deal with the [prior art] the organic solvent is a health disorder that volatile solvent is applied to the workers. この為最近では有機溶剤取扱い建屋の建設に当たって排気ダクトの完備が義務付けられており、且つ大気中への溶剤蒸気の放散を防止する為溶剤吸着除去設備の付設も要請されている。 Therefore recently are obliged conditioning of the exhaust duct when the construction of the organic solvent handling building, are and requested for also attached solvent adsorption removal system for preventing the dissipation of solvent vapor into the atmosphere.
この様な溶剤吸着除去に最も広く実用化されている吸着剤は活性炭であり、普通は併設された2基以上の吸着塔に活性炭を充填しておき、バルブ操作によって吸着と着脱再生を交互に繰り返すことによって溶剤の吸着除去を連続的に行なっている。 The most widely practically used adsorbents are to such solvent adsorbed and removed is activated carbon, usually leave filled with activated carbon features have been 2 group or more adsorption towers, alternately detachable adsorption and regeneration by valving and performing suction removal of the solvent continuously by repeating.

[発明が解決しようとする問題点] ところがフレオン(商品名、米国デュポン社製)や塩化メチレン、四塩化炭素、クロロホルム等に代表される低沸点(特に沸点100℃以下)のHal−CHガスは吸着剤に対する吸着性が乏しく、多くのHal−CHガスが未吸着のままで放出され作業雰囲気や大気汚染を引き起こすという問題がある。 [INVENTION Problems to be Solved] However freon (trade name, DuPont, USA) and methylene tetrachloride, Hal-CH gases carbon tetrachloride, low boiling typified by chloroform (especially boiling point 100 ° C. or less) it is poor adsorptivity for the adsorbent, many Hal-CH gas but also causes released working atmosphere and air pollution remain unadsorbed.

即ち上記の様なHal−CHガスは冷媒、溶剤、抽出剤、エローゾル噴霧剤等として広範囲の用途を有しており、引火性を有していないという利点もあって利用範囲は多岐に亘っているが、揮発性に富むものであるから雰囲気汚染を生じ易く、各種吸着剤に対する吸着性が乏しいこともあってその除去に苦慮しているのが実情である。 That Hal-CH gas, such as the refrigerant, solvent, extraction agent, have a wide range of applications as Erozoru propellant such, utilization range is diversified there is also the advantage that does not have a flammable it is, but tend to cause atmosphere pollution from those rich in volatile, are you struggling to its removal there is also the poor adsorptivity for various adsorbent is in reality.

本発明はこの様な状況のもとで、Hal−CHガスを含む混合ガスからHal−CHガスを効率良く吸着除去することのできる方法を提供しようとするものである。 The present invention seeks to provide a process capable of efficiently adsorbing and removing Hal-CH gas from a mixed gas containing Under these circumstances, the Hal-CH gas.

[問題点を解決する為の手段] 本発明に係る吸着除去方法の構成は、Hal−CHガスを含有する混合ガス中の該Hal−CHガスを活性炭によって吸着除去する方法において、吸着処理に先立ち前記混合ガスを加熱処理に付して相対湿度を50%以下としておくところに要旨を有するものである。 [Means for solving the problems] configuration of adsorption removing method according to the present invention is a method of removing adsorbed the Hal-CH gas in the mixed gas containing Hal-CH gas by the activated carbon, prior to the adsorption process the relative humidity subjected mixed gas to heat treatment and has a gist where to keep 50% or less.

[作用] 周知の様にHal−CHガスは吸着剤による吸着除去が困難であるとされており、こうした傾向は吸着力の優れた活性炭を吸着剤として使用した場合も例外ではない。 [Operation] known Hal-CH gas as is to be difficult to suction removal by the adsorbent, this trend is not an exception when used as an adsorbent excellent activated carbon adsorption force.
そこでHal−CHガスが活性炭に吸着され難い理由を明確にすべく色々の実験を繰り返すうち、次の様な事実が明らかとなってきた。 So out of Hal-CH gases repeated various experiments in order to clarify the reason why hardly adsorbed on the activated carbon, following such facts it has been revealed. 即ち活性炭は水分に対しても優れた吸着能を有しており、水分とHal−CHガスは活性炭吸着に関する限り拮抗的に作用する。 That activated carbon has an adsorption ability which is excellent against water, moisture and Hal-CH gas acts only antagonistically related activated carbon adsorption. しかも一般的には水分の方が吸着され易いという傾向があった。 Moreover generally towards the water tended being easily adsorbed. 従って水分が一旦活性炭に吸着されるとHal−CHガスに対する活性炭の吸着能が低下するばかりでなく、水分とHal−CHガスの親和性が乏しいことからHal−C Thus water not only once adsorption capacity of the activated carbon for Hal-CH gas when adsorbed to the activated carbon is decreased, moisture and Hal-C from the poor affinity of Hal-CH Gas
Hガスに対する吸着能は一段と乏しくなり、Hal−C Adsorption capacity for H gas becomes increasingly poor, Hal-C
Hガス吸着除去の目的を果たし得なくなる。 Not obtained serves the purpose of H gas adsorption removal. 殊に我国は温暖多湿気候であり、しかも四方が海に囲まれていることもあって非常に湿度が高く室内外の湿度は年間を通じて殆んどが60%以上を示すと言われている。 Especially our country is a warm and humid climate, moreover indoor and outdoor humidity very humidity is higher there and that they are surrounded by all sides the sea is most of them are said to exhibit more than 60% throughout the year. その為被処理ガス中には相当量の湿気が混在しており、この湿気が活性炭に優先的に吸着しHal−CHガスの吸着を阻害しているものと考えられる。 Therefore a substantial amount of moisture has been mixed in the treated gas, the moisture is considered that inhibit the adsorption of preferentially adsorbed Hal-CH gas by the activated carbon.

そこで本発明者等は、Hal−CHガスと水分の活性炭に対する吸着平衡について種々検討し、これらの差を利用する手段について研究を進めた。 The present inventors have variously studied the adsorption equilibrium for the activated carbon of Hal-CH gas and water, we were researching the means for utilizing these differences. その結果該混合ガスを相対湿度が50%以下となるまで加熱処理した後で活性炭に吸着させれば、Hal−CHガスを極めて効率良く吸着除去し得ることが確認された。 If ask result adsorbed on the activated carbon after the mixture gas relative humidity was heated until 50% or less, it was confirmed that the Hal-CH gas can very efficiently adsorbed and removed.

ちなみに第1図は、Hal−CHガスの吸着性が水分の吸着性を上回り、前者としてフレオン113(CCl 2 F − Incidentally Figure 1 is above the adsorption of the adsorption of Hal-CH gas moisture, Freon 113 as the former (CCl 2 F -
CClF 2 )ガスを選択して活性炭による吸着実験を行ない、該Hal−CHガス含有混合ガス(残部ガスは空気)の相対湿度がフレオン113及び水分の平衡吸着量にどの様な影響を及ぼすかを調べた結果を示すものであり、実験法は下記の通りとした。 CClF 2) subjected to adsorption experiments by selecting the gas with activated carbon, the relative humidity of the Hal-CH gas-containing mixed gas (balance gas air) what kind of influence on the equilibrium adsorption amount of Freon 113 and water and it shows the results of examining the experimental method was as follows.

〈実験法〉 (1)第2図に略示する如く100の透明密閉容器Vに下記無機塩の飽和水溶液Sを装入し、器内の調湿(at2 <Experimental Method> (1) was charged with a saturated aqueous solution S of the transparent airtight container V below inorganic salts schematically as 100 in FIG. 2, the humidity control in the converter (at2
5℃)を行なう。 5 ℃) perform.

K 2 CO 3飽和水溶液 :40% NH 4 NO 3飽和水溶液 :61〜64% (NH 4 ) 2 SO 4飽和水溶液:81〜83% (2)絶乾状態(120℃×3hr以上処理後)の活性炭(約2g)ACを上記密閉容器V内へ入れ、飽和水分率となるまで吸着させる。 K 2 CO 3 saturated aqueous: 40% NH 4 NO 3 saturated aqueous: 61 to 64% (NH 4) 2 SO 4 saturated solution: a 81 to 83% (2) absolute dry condition (after 120 ° C. × 3 hr further processing) activated carbon (about 2 g) AC put into the closed vessel V, is adsorbed to a saturation moisture content.

(3)活性炭ACが飽和水分率に到達した後、該密閉容器V内にフレオン113を7.8 g/100注入し、攪拌機Iにより攪拌して容器V内にフレオン113を均一に分散させ(フレオン濃度10,300 ppm)た後、約1時間放置する。 (3) After the activated carbon AC reaches the saturated moisture content, the Freon 113 7.8 g / 100 injected into the closed vessel V, stirred uniformly disperse the Freon 113 into the vessel V with a stirrer I (Freon concentration 10,300 ppm) after was allowed to stand for about 1 hour.

(4)その後密封容器V内の相対湿度及びフレオン113 (4) relative humidity then sealed vessel V and Freon 113
濃度を測定し、初期濃度より減少して安定化したときの安定化濃度を差引いて活性炭ACへの吸着量を求めた。 To determine the concentration, it was determined adsorption amount of activated carbon AC by subtracting the stabilization concentration when stabilized reduced from the initial concentration.

(5)尚比較の為トルエンについても同様にして相対湿度と平衡吸着量の関係を調べた。 (5) It should be noted also toluene for comparison was examined to relate the relative humidity and the equilibrium adsorption amount similarly.

第1図からも明らかな様に相対湿度が50%以下である場合Ha−CHガスはむしろ水分よりも優先的に活性炭に吸着されるが、相対湿度が50%を超えると水分の吸着量が急激に増大すると共にHal−CHガスの吸着量は急激に低下してくる。 While preferentially adsorbed by the activated carbon than the rather moisture Ha-CH gas when the relative humidity as is clear is 50% or less from Figure 1, the adsorption amount of moisture when the relative humidity exceeds 50% adsorption amount of Hal-CH gas together rapidly increase comes rapidly decreases. こうした傾向からも明らかな様に、Hal−CHガスは活性炭に対する吸着能が必ずしも乏しいと言う訳ではなく、一定量以上の水分の存在によって活性炭に対する吸着能が激減するものと考えられた。 As is apparent from this trend, Hal-CH gas is not necessarily to say that necessarily poor adsorption capacity for the activated carbon, the adsorption capacity for the activated carbon is believed to depleted by the presence of certain amount or more of water. 換言するとHal−CHガス混合ガスを予め加熱し相対湿度を低下させた後に活性炭による吸着処理を行なえば、Hal−CHガスの効果的な吸着除去が可能となる。 By performing the adsorption treatment with activated carbon after reducing the other words the preheated relative humidity Hal-CH gas mixed gas, it is possible to effectively adsorb and remove the Hal-CH gas. 尚トルエンについては、相対湿度による吸着量の低減傾向が非常に小さいことが分かる。 Note The toluene, it can be seen reduced tendency for adsorption by the relative humidity is very small.

本発明はこうした知見を基になされたものであって、H The present invention was made based on these findings, H
al−CHガスを含む混合ガスを活性炭により吸着除去するに先立って、該混合ガスを加熱するところに特徴を有するものであって、加熱の程度は第1図に示した実験結果より、活性炭への水分の吸着量が急増する相対湿度50%を基準として該値以下(より好ましくは40%以下)と定めた。 A mixed gas containing al-CH gases prior to adsorption removal by activated carbon include those having a characterized in that heating the mixed gas, the degree of heating than the experimental results shown in FIG. 1, the activated carbon (more preferably 40% or less) of the said value below the relative humidity of 50% adsorption amount is rapidly increased moisture basis was defined as.

[実施例] 第3図に示す実験装置を使用し、活性炭充填塔へ供給するガス中のフレオン113濃度及び相対湿度を色々変化させ、所定時間吸着処理を行なった場合における活性炭充填塔通過ガス中のフレオン113濃度の変化を調べた。 [Example] Using the experimental apparatus shown in FIG. 3, the Freon 113 concentration and the relative humidity of the gas supplied to the activated carbon packed column is variously changed, the activated carbon packed column passes gas in case of performing a predetermined time adsorption treatment It examined the Freon 113 changes in the concentration of. 即ち第3図に示す如く模擬ガス発生装置4内のヒート5上に設置した蒸発皿6内にフレオン113を装入して加熱蒸発させ、該蒸気を空気と共にライン8及びファン9を通して吸着塔1a(又は1b)へ送り込む。 That charged was vaporized by heating and the Freon 113 to install the evaporating dish 6 on Heat 5 of simulant gas generator 4 as shown in Figure 3, the adsorption tower 1a care the evaporated through line 8 and fan 9 together with the air fed to (or 1b). このとき該供給ガスに、ヒータ11を通して加熱させ調湿装置10を通して相対湿度を変化させた空気を合流させて供給ガスの相対湿度を様々に変化させるものとし、且つ吸着塔入側ガスの温度をTCA、湿度をHCで夫々検知しつつヒータ11の上記弁を開閉することによって供給ガスの温度及び相対湿度を調整する。 To the feed gas at this time, by merging the varying relative humidity air shall be variously change the relative humidity of the feed gas through the allowed humidity control apparatus 10 heated through the heater 11, and the temperature of the adsorption tower inlet side gas TCA, to adjust the temperature and relative humidity of the feed gas by opening and closing the valve of the heater 11 while respectively detecting the humidity in HC. そして各条件毎に吸着塔1a(又は1b)通過前・後におけるガス中のフレオン113濃度をハイドロカーボンメータXIによって調べた。 And examined Freon 113 concentration in the gas after the adsorption tower 1a (or 1b) pass the front and the hydrocarbon meter XI for each condition. 実験条件は下記の通りとした。 The experimental conditions were as follows.

<実験条件> 大気条件: 28℃,90% 原料ガス中の フレオン113 濃度:約50,000 ppm 原料ガス送給量:14.4 Nm 3 /分 処理温度: 35〜40℃ 第4図は1バッチ目終了時における吸着塔通過ガス中のフレオン113濃度と5バッチ目終了時における同ガス中のフレオン113濃度を示したものであり、これらの結果より次の様に考えることができる。 <Experimental Conditions> atmospheric conditions: 28 ° C., Freon 113 concentration in the 90% material gas: about 50,000 ppm raw gas feed rate: 14.4 Nm 3 / min treatment temperature: 35-40 ° C. at Figure 4 is the first batch ends and it shows the Freon 113 concentration of the gas in Freon 113 concentration and 5 batched at the end of the adsorption tower passing gas in, can be considered as follows from these results.

(1)供給ガスの相対湿度が50%を超えると、フレオン113濃度が高い場合はもとより、フレオン113濃度が低い場合でも少ない処理回数で活性炭のフレオン吸着活性が低下し、出口ガス中のフレオン113濃度は著しく高くなっている。 (1) when the relative humidity of the feed gas is more than 50%, well if Freon 113 concentration is high, and decreases Freon adsorption activity of the activated carbon with a small number of processing times even when Freon 113 concentration is low, Freon 113 in the outlet gas concentration is significantly higher.

(2)これに対し供給ガスの相対湿度を50%以下に低下させておくと出口ガス中のフレオン113濃度は初回吸着処理時よりも5回の吸着処理を行なった後の方が低くなっている。 (2) In contrast Freon 113 concentration when the relative humidity allowed to drop below 50% the outlet gas of the feed gas becomes lower in the after performing five adsorption treatment than at the first adsorption treatment there. 即ち本実験は約65%RHの外気雰囲気で実験を行なったものであり、こうした条件のもとでは吸着塔内の活性炭は若干吸湿しているものと考えられ、初回吸着処理時は吸着水分の影響を受けて若干低めの吸着活性しか発揮しないが、供給ガスの相対湿度を50%以下にしておくと、吸着塔内に充填された活性炭の吸着水分が供給ガスの通過により逆に放出されて活性炭のフレオン113吸着活性が高まり、初回吸着処理時よりもむしろフレオン113吸着除去効率が向上してきたものと考えられる。 That this experiment are those experiments were performed at ambient atmosphere of RH 65%, in the adsorption tower under these conditions the activated carbon is considered to have slightly hygroscopic, the first time the adsorption process of the adsorbed water slightly affected but not exert only low adsorption activity and keep the relative humidity of the feed gas to 50% or less, adsorbed water of the activated carbon filled in the adsorption tower is discharged into reverse by the passing of the feed gas increased Freon 113 adsorption activity of activated carbon is considered to what has been rather improved Freon 113 adsorption and removal efficiency than the first time the adsorption process. 何れにしても供給ガスの相対湿度を50% In any the relative humidity of the feed gas be 50%
以下としておくことによって、該供給ガス中のフレオン113を極めて効率良く吸着除去することができる。 By keeping the following, it can be very efficiently adsorb and remove Freon 113 of the feed gas.

[発明の効果] 本発明は以上の様に構成されているが、要するにHal [Effect of the Invention] The present invention is constructed as described above but, in short Hal
−CHガスを含む混合ガスを予め加熱してその相対湿度を50%以下としておくことにより、活性炭のHal− By previously the relative humidity of 50% or less by preheated mixed gas containing -CH gas, activated carbon Hal-
CHガス吸着性能を最大限に発揮させることができ、H CH gas adsorption performance can be maximized to, H
al−CHガスを効率良く吸着除去することができる。 The al-CH gas can be efficiently adsorbed and removed.


第1図は混合ガスの相対湿度がフレオン又はトルエンの吸着活性に及ぼす影響を調べた結果を示すグラフ、第2 Graph Figure 1 is showing the results of relative humidity of the mixed gas was studied the effect on the adsorption activity of Freon or toluene, second
図は吸着活性試験法を示す説明図、第3図は実施例で用いた装置を示す説明図、第4図は供給ガスの相対湿度と吸着塔出口ガスのフレオン濃度変化を示すグラフである。 Figure is an explanatory view showing an adsorption activity test method, FIG. 3 is an explanatory diagram showing an apparatus used in Example, Fig. 4 is a graph showing the Freon concentration change of the adsorption tower outlet gas and the relative humidity of the feed gas. 1a,1b……活性炭充填塔 4……模擬ガス発生装置、5……ヒータ 6……蒸発皿、10……調湿装置 1a, 1b ...... activated carbon packed column 4 ...... simulated gas generator, 5 ...... heater 6 ...... evaporating dish, 10 ...... humidity controller

Claims (1)

    【特許請求の範囲】 [The claims]
  1. 【請求項1】ハロゲン化炭化水素系ガスを含有する混合ガス中の該ハロゲン化炭化水素系ガスを活性炭によって吸着除去する方法において、吸着処理に先立ち前記混合ガスを加熱処理に付して相対湿度を50%以下としておくことを特徴とするハロゲン化炭化水素系ガスの吸着除去方法。 1. A method for the halogenated hydrocarbon gas in the mixed gas containing a halogenated hydrocarbon gas adsorbed and removed by the activated carbon, relative humidity and subjected to heat treatment of the mixed gas prior to the adsorption process adsorption method of removing halogenated hydrocarbon gas, characterized in that to keep 50% or less.
JP27546685A 1985-12-06 1985-12-06 Adsorption method of removing halogenated hydrocarbon gas Expired - Lifetime JPH0622654B2 (en)

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