JPS59232175A - Refining of gas - Google Patents
Refining of gasInfo
- Publication number
- JPS59232175A JPS59232175A JP10661283A JP10661283A JPS59232175A JP S59232175 A JPS59232175 A JP S59232175A JP 10661283 A JP10661283 A JP 10661283A JP 10661283 A JP10661283 A JP 10661283A JP S59232175 A JPS59232175 A JP S59232175A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- hydrogenation
- coke oven
- oven gas
- temperature
- 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.)
- Granted
Links
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- Catalysts (AREA)
- Industrial Gases (AREA)
Abstract
Description
【発明の詳細な説明】
〔発明の利用分野〕
本発明はコークス炉ガスから不純物成分を除去する方法
に係り、特にコークス炉ガス中に含有するジエン類、酸
素、オレフィン類、硫黄化合物を除去するのに好適なガ
スの精製法に関する。[Detailed Description of the Invention] [Field of Application of the Invention] The present invention relates to a method for removing impurity components from coke oven gas, particularly for removing dienes, oxygen, olefins, and sulfur compounds contained in coke oven gas. This invention relates to a gas purification method suitable for.
従来のコークス炉ガスの精製プロセスでは、ニッケルー
モリブデン系触媒又はコバルト−モリブデン系触媒を用
いて不純物であるジエン類、酸素、オレフィン類及び硫
黄化合物を除去していたが、触媒活性が悪いという欠点
があった。In conventional coke oven gas purification processes, impurities such as dienes, oxygen, olefins, and sulfur compounds are removed using nickel-molybdenum catalysts or cobalt-molybdenum catalysts, but the drawback is that the catalyst activity is poor. was there.
本発明の目的は、ニッケルーモリブデン系触媒又はコバ
ルト−モリブデン系触媒を用いたときよりも水添活性を
高めることができるガスの精製方法を提供することにあ
る。An object of the present invention is to provide a gas purification method that can increase hydrogenation activity more than when using a nickel-molybdenum catalyst or a cobalt-molybdenum catalyst.
本発明はガスの精製法の発明であって、不純物としてジ
エン類、酸素、オレフィン類及び硫黄化合物を含有する
コークスかガスを精製する方法において、該不純物を、
触媒として白金族金属を担持した触媒の存在下で水添す
る工程、及び前記水添工程より水素化処理されたコーク
ス炉ガス中の硫化水素を吸着除去する硫化水素除去工程
の各工程を包含することを特徴とする。The present invention is a method for purifying gas, and is a method for refining coke or gas containing dienes, oxygen, olefins, and sulfur compounds as impurities.
It includes the steps of hydrogenating in the presence of a catalyst supporting a platinum group metal as a catalyst, and the hydrogen sulfide removal step of adsorbing and removing hydrogen sulfide in the coke oven gas hydrogenated from the hydrogenation step. It is characterized by
更に詳しく述べれば、コークス炉ガス中の不純物を除去
する方法において、コークス炉ガス中のジエン類、酸素
、オレフィン類、硫黄化合物を同時に水添し、ジエン類
、オレフィン類はパラフィン、酸素は水に変換し、更に
硫黄化合物は硫化水素に変換した後硫化水素除去装置で
分離除去する方法である。More specifically, in a method for removing impurities from coke oven gas, dienes, oxygen, olefins, and sulfur compounds in the coke oven gas are simultaneously hydrogenated, and the dienes and olefins are replaced by paraffin, and the oxygen is replaced by water. In this method, the sulfur compound is converted into hydrogen sulfide, and then separated and removed using a hydrogen sulfide removal device.
本発明で水添反応に使用する触媒の例には、白金及び／
又はパラジウムを例えばアルミナ、チタ１
ニア又はマグネシア等の担体に担持したものがあり、そ
の水添性能は画期的に優れている。上記水添触媒は製造
工程において、還元状態になっているのでこのまま使用
される。還元状態において、金属成分の量は触媒全重量
に対して、０．０１〜５重量％が水添活性向上に役立つ
。上記の特殊な水添触媒を用いて行われる水添反応の温
度は５０〜４５０Ｃ，好ましくは１５０〜３５０Ｃであ
る。Examples of catalysts used in the hydrogenation reaction in the present invention include platinum and/or
or palladium, e.g. alumina, titanium
There are some supported on carriers such as nia or magnesia, and their hydrogenation performance is revolutionary. The above-mentioned hydrogenation catalyst is in a reduced state during the manufacturing process and is therefore used as is. In a reduced state, the amount of metal component from 0.01 to 5% by weight based on the total weight of the catalyst is useful for improving hydrogenation activity. The temperature of the hydrogenation reaction carried out using the above-mentioned special hydrogenation catalyst is 50 to 450C, preferably 150 to 350C.
コークス炉ガス中には酸素が０．１〜２容量チ含有する
が、酸素が１容ｉ％反応すると、１５０Ｃの温度上昇が
ある。また、コークス炉ガス中にはオＶフィン類瀘３〜
５容量チ含有するが、オレフィン類が１容量チ反応する
と、３０Ｃの温度上昇がある。したがってコークス炉ガ
ス中のオレフィン類、酸素濃度の変化により、触媒層内
の温度は５００Ｃ以上に達することがしばしばある。水
添触媒が５００Ｃを超えると触媒の半融現象による失活
、反応器の損傷となる。反応熱を制御するには触媒層の
温度上昇を監視して、硫化水素除去工程からの精製ガス
の一部を水添工程の入口へ再循環させ、入口の酸素、オ
レフィン濃度を希釈してやることにより、水添工程の温
度が４５００を超えないように調節を行うと良い。また
、水添工程の入口温度を５０〜３００ｃの範囲内に調節
することも効果的である。Coke oven gas contains 0.1 to 2 volumes of oxygen, and when 1 volume i% of oxygen reacts, the temperature rises by 150C. In addition, coke oven gas contains O-V fins.
Although it contains 5 volumes of hydrogen, when olefins react with 1 volume of hydrogen, there is a temperature rise of 30C. Therefore, due to changes in the olefins and oxygen concentrations in the coke oven gas, the temperature within the catalyst layer often reaches 500C or higher. If the temperature of the hydrogenation catalyst exceeds 500C, the catalyst will be deactivated due to a half-melting phenomenon and the reactor will be damaged. The heat of reaction can be controlled by monitoring the temperature rise of the catalyst bed and recirculating a portion of the purified gas from the hydrogen sulfide removal process to the inlet of the hydrogenation process to dilute the oxygen and olefin concentrations at the inlet. It is preferable to adjust the temperature in the hydrogenation step so that it does not exceed 4,500 ℃. It is also effective to adjust the inlet temperature of the hydrogenation step within the range of 50 to 300c.
更に、従来用いられていたニッケルーモリブデン触媒の
場合、硫黄化合物を除去するためには、水添工程の入口
の温度を高くする必要があり、温度を高くすれはジエン
類と酸素及び−酸化窒素の重合物が析出しやすいという
不都合な点が見られた。本発明で使用する触媒により、
低い入口温度でも、硫黄化合物、オレフィン類の水添が
可能であり、且つジエン類や酸素も同時に水添できる。Furthermore, in the case of the conventionally used nickel-molybdenum catalyst, in order to remove sulfur compounds, it is necessary to increase the temperature at the inlet of the hydrogenation process, and increasing the temperature causes dienes, oxygen, and nitrogen oxides to The disadvantage was that polymers of With the catalyst used in the present invention,
Even at low inlet temperatures, sulfur compounds and olefins can be hydrogenated, and dienes and oxygen can also be hydrogenated at the same time.
水添工！へのコークス炉ガスの供給速度はｓ■（空間速
度）で、５００ ｈ ” 〜５０，０００ ｈ −１が
良（，５００ｈ−１未満では触媒量が多くなって経済的
ではなく、また５０，０ＯＯｈ”’を超えると水添活性
が低下してしまう。水添反応を行う圧力は、２〜１００
気圧で良いが特に限定されない。Hydrogen work! The supply rate of coke oven gas to the coke oven gas is s (space velocity), and 500 h'' to 50,000 h-1 is good (if it is less than 500 h-1, the amount of catalyst becomes large and it is not economical, and If it exceeds 0OOh"', the hydrogenation activity will decrease.The pressure for carrying out the hydrogenation reaction is 2 to 100
Atmospheric pressure may be used, but there is no particular limitation.
硫化水素の除去は、吸着除去法としても公知の方法がい
ずれも使用されうる。例を挙げればＺｎｏ、Ｆｅ２Ｏ３
、ＣｕＯなどの固体吸着剤である。To remove hydrogen sulfide, any known adsorption removal method may be used. Examples are Zno, Fe2O3
, CuO, and other solid adsorbents.
次に本発明を実施するためのプロセスを図面によって具
体的に説明する。すなわち第１図は、本発明の一実施の
態様を示す工程図であり、１はコークス炉ガス、２は水
添塔、３は硫化水素吸着塔、そして５は精製ガスを意味
する。また、第２図は、本発明において精製ガスの一部
を水添工程の入口へ再循環させた場合の一実施の態様を
示す工程図であり、１〜３及び５は第１図と同義であり
、４は循環ラインを意味する。図面は本発明を理解する
ために必要な主要部のみを含み、それ以外のポンプ、冷
却器、測定器及び制御装置、その他の装置は省略されて
いる。Next, a process for carrying out the present invention will be specifically explained with reference to the drawings. That is, FIG. 1 is a process diagram showing an embodiment of the present invention, in which 1 represents coke oven gas, 2 represents a hydrogenation tower, 3 represents a hydrogen sulfide adsorption tower, and 5 represents purified gas. Moreover, FIG. 2 is a process diagram showing an embodiment in which a part of the purified gas is recirculated to the inlet of the hydrogenation step in the present invention, and 1 to 3 and 5 have the same meaning as in FIG. 1. and 4 means a circulation line. The drawings include only the main parts necessary for understanding the present invention, and other devices such as a pump, a cooler, a measuring device, a control device, and other devices are omitted.
次に本発明を実施例により更に説明するが、本発明はこ
れにより限定されない。Next, the present invention will be further explained with reference to Examples, but the present invention is not limited thereto.
実施例
第１図において、コークス炉ガス１は約１５０〜２００
Ｃの温度に加熱されて水添塔２に導入さレル。コークス
炉ガスの主な成分の組成は、Ｈ２が５３．２５チ、ｃｏ
が５．８９チ、ＣＯ２が２．２０チ、ＣＨ４カ３０．６
７％、Ｃ２Ｈ４カ１．６０ ％ 、ＣａＨａカ１．６０
チ、０２が０．５０チ、Ｃ４ＨＩＩが０．１０チ、硫黄
化合物が０．０１ ％、Ｎｌｌが４．１８ ％である。Embodiment In FIG. 1, the coke oven gas 1 is about 150 to 200
The reactor is heated to a temperature of C and introduced into the hydrogenation tower 2. The composition of the main components of coke oven gas is 53.25 H2, co
is 5.89 inches, CO2 is 2.20 inches, CH4 is 30.6 inches
7%, C2H4 1.60%, CaHa 1.60
H, 02 is 0.50 H, C4HII is 0.10 H, sulfur compound is 0.01%, and Nll is 4.18%.
水添触媒はアルミナ担体にパラジウムとして約０．５重
量％担持した触媒を用いる。水添塔の出口におけるガス
組成は、Ｎ２が５３．５２％、Ｃｏが５．９２俤、Ｃ０
２が２２１チ、Ｃ）Ｔ４が３０．８２％、Ｃ２Ｈ・が１
．６１チ、Ｃ５Ｈｓが１．６１％、Ｃ４Ｈ１゜が０．１
０チ、Ｎ２が４．２０チ、Ｈａｓが０．０１チであった
。この結果からもわかるようにブタジェンはブタンに変
換され、酸素は水となって除去され、エチレン、プロピ
レンはエタン、プロパンに変換され、硫黄化合物は硫化
水素に変換されている。As the hydrogenation catalyst, a catalyst in which about 0.5% by weight of palladium is supported on an alumina carrier is used. The gas composition at the exit of the hydrogenation tower is 53.52% N2, 5.92% Co, and C0
2 is 221chi, C) T4 is 30.82%, C2H・ is 1
．． 61chi, C5Hs 1.61%, C4H1° 0.1
0ch, N2 was 4.20ch, and Has was 0.01ch. As can be seen from these results, butadiene is converted to butane, oxygen is converted to water and removed, ethylene and propylene are converted to ethane and propane, and sulfur compounds are converted to hydrogen sulfide.
上記生成ガスは２７０〜３５０Ｃの温度で水添塔を出る
。The product gas leaves the hydrogenation tower at a temperature of 270-350C.
水添塔を出たガスは約３５０Ｃの温度で硫化水素吸、着
塔３に導入される。硫化水素吸着塔ではガス中の硫化水
素が除去される。このようにして精′ 製され
たガス５の組成は、Ｎ２が５３．５３１ＸＣ０が５．９
２チ、Ｃ０２が２．２１チ、ＣＨ４が３０．８３％、Ｃ
２Ｈ５が１．６１％、Ｃ５Ｈｓが１．６１ ％ 、Ｃ４
Ｈｔ。The gas leaving the hydrogenation tower is introduced into the hydrogen sulfide adsorption and deposition tower 3 at a temperature of about 350C. Hydrogen sulfide in the gas is removed in the hydrogen sulfide adsorption tower. The composition of the gas 5 purified in this way is 53.531 N2 x 5.9 C0.
2chi, C02 is 2.21chi, CH4 is 30.83%, C
2H5 is 1.61%, C5Hs is 1.61%, C4
Ht.
が０．１０チ、Ｎ２が４．２０チであった。was 0.10 inches, and N2 was 4.20 inches.
この実施例においてはジエン類としてブタジェン、オレ
フィン類としてエチレン及びプロピレン、硫黄化合物と
してはチオフェン等を含むガスについて述べているが、
他のジエン類、オレフィン類や硫黄化合物に対しても有
効であることはもちろんのことである。This example describes a gas containing butadiene as a diene, ethylene and propylene as olefins, and thiophene as a sulfur compound.
Of course, it is also effective against other dienes, olefins, and sulfur compounds.
第２図に示した精製ガスの一部を水添塔の入口に循環す
る場合においても、先の実施例と同様に効率よくコーク
ス炉ガスの精製が行われる。すなわちコークス炉ガス中
の酸素、オレフィン濃度が変動して、水添反応により水
添塔の温度が４５０Ｃを超える場合には未然に反応器の
温度を監視して、循環ライン４を作動させて循環ガスの
一部を水添塔入口に循環することによシ、水添塔入口の
酸素、オレフィン濃度は希釈される。循環ガスの循環比
は原料コークス炉ガスに対し１０〜１０００チの範囲で
可能である。Even when part of the purified gas shown in FIG. 2 is circulated to the inlet of the hydrogenation column, the coke oven gas is efficiently purified as in the previous embodiment. That is, if the oxygen and olefin concentrations in the coke oven gas fluctuate and the temperature of the hydrogenation tower exceeds 450C due to hydrogenation reaction, the temperature of the reactor is monitored in advance and the circulation line 4 is activated to restart the circulation. By circulating a portion of the gas to the hydrogenation tower inlet, the oxygen and olefin concentrations at the hydrogenation tower inlet are diluted. The circulation ratio of the circulating gas to the raw coke oven gas is possible in the range of 10 to 1000 g.
以上詳細な説明から明らかなように、本発明によれば、
水添性能が画期的に優れた触媒の使用により、コークス
炉ガス中に含まれるジエン類、酸素、オレフィン類及び
硫黄化合物等の不純物を同時に水素化するという効果を
持っている。従来用いられていたニッケルーモリブデン
触媒の場合、硫黄化合物を除去するためには、水添工程
の入口の温度を高くする必要があり、温度を高くすると
ジエン類と酸素及び−酸化窒素の重合物が析出しやすい
という不都合な点が見られた。本発明で使用する触媒に
より、低い入口温度でも、硫黄化合物、オレフィン類の
水添が可能であり、且つジエン類や酸素も同時に水添で
きるという顕著な効果がある。As is clear from the detailed description above, according to the present invention,
By using a catalyst with dramatically superior hydrogenation performance, it has the effect of simultaneously hydrogenating impurities such as dienes, oxygen, olefins, and sulfur compounds contained in coke oven gas. In the case of the conventionally used nickel-molybdenum catalyst, in order to remove sulfur compounds, it is necessary to raise the temperature at the entrance of the hydrogenation process, and when the temperature is raised, polymers of dienes, oxygen, and nitrogen oxides are formed. The disadvantage was that it was easy to precipitate. The catalyst used in the present invention has the remarkable effect of being able to hydrogenate sulfur compounds and olefins even at low inlet temperatures, and also hydrogenating dienes and oxygen at the same time.
第１図は本発明の一実施の態様を示す工程図、第２図は
本発明において、精製ガスの一部を再循環させた場合の
一実施の態様を示す工程図である。
１・・・コークス炉ガス、２・・・水添塔、３・・・硫
化水素吸着塔、４・・・循環ライン、５・・・精製ガス
。
代理人 弁理士 中本 宏
（９）
４８７
菊１ 図FIG. 1 is a process diagram showing an embodiment of the present invention, and FIG. 2 is a process diagram showing an embodiment in which a part of the purified gas is recirculated in the present invention. 1... Coke oven gas, 2... Hydrogenation tower, 3... Hydrogen sulfide adsorption tower, 4... Circulation line, 5... Purified gas. Agent Patent Attorney Hiroshi Nakamoto (9) 487 Chrysanthemum 1 Figure
Claims (1)
黄化合物を含有するコークス炉ガスを精製する方法にお
いて、該不純物を、触媒として白金族金属を担持した触
媒の存在下で水添する工程、及び前記水添工程により水
素化処理されたコークス炉ガス中の硫化水素を吸着除去
する硫化水素除去工程の各工程を包含することを特徴と
するガスの精製法。 ２、該水添工程の入口温度を５０〜３００Ｃの範囲内の
温度に調節する特許請求の範囲第１項記載のガスの精製
法。 ３、該水添工程に使用する触媒が白金族金属を０．０１
〜５重量％、担体を９９．９９〜９５重量−の割合で含
有するものである特許請求の範囲第１項又は第２項記載
のガスの精製法。 ４、硫化水素除去工程からの精製ガスの一部を水添工程
の入口へ再循環させ、水添工程の温度が４５０Ｃを超え
ないように調節する特許請求の範囲第１項記載のガスの
精製法。[Claims] 1. A method for purifying coke oven gas containing dienes, oxygen, olefins, and sulfur compounds as impurities, in which the impurities are purified by water in the presence of a catalyst supporting a platinum group metal. and a hydrogen sulfide removal step of adsorbing and removing hydrogen sulfide in the coke oven gas that has been hydrogenated in the hydrogenation step. 2. The gas purification method according to claim 1, wherein the inlet temperature of the hydrogenation step is adjusted to a temperature within the range of 50 to 300C. 3. The catalyst used in the hydrogenation step contains 0.01 platinum group metal.
The gas purification method according to claim 1 or 2, wherein the gas purification method contains the carrier in a proportion of 99.99 to 95% by weight. 4. Gas purification according to claim 1, wherein a part of the purified gas from the hydrogen sulfide removal step is recirculated to the inlet of the hydrogenation step, and the temperature of the hydrogenation step is adjusted so as not to exceed 450C. Law.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10661283A JPS59232175A (en) | 1983-06-16 | 1983-06-16 | Refining of gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10661283A JPS59232175A (en) | 1983-06-16 | 1983-06-16 | Refining of gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59232175A true JPS59232175A (en) | 1984-12-26 |
| JPH0229711B2 JPH0229711B2 (en) | 1990-07-02 |
Family
ID=14437939
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10661283A Granted JPS59232175A (en) | 1983-06-16 | 1983-06-16 | Refining of gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59232175A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6189294A (en) * | 1984-10-09 | 1986-05-07 | Kawasaki Steel Corp | Method of purifying coke oven gas |
| JP2008239892A (en) * | 2007-03-28 | 2008-10-09 | Mitsubishi Chemicals Corp | Method and system for purification of source gas |
| DE102016116306A1 (en) | 2016-09-01 | 2018-03-01 | Thyssenkrupp Ag | Method and apparatus for removing organic sulfur compounds from hydrogen-rich gases |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5573785A (en) * | 1978-11-29 | 1980-06-03 | Hitachi Ltd | Purification of hydrocarbon oil or gas |
-
1983
- 1983-06-16 JP JP10661283A patent/JPS59232175A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5573785A (en) * | 1978-11-29 | 1980-06-03 | Hitachi Ltd | Purification of hydrocarbon oil or gas |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6189294A (en) * | 1984-10-09 | 1986-05-07 | Kawasaki Steel Corp | Method of purifying coke oven gas |
| JPH0349960B2 (en) * | 1984-10-09 | 1991-07-31 | Kawasaki Seitetsu Kk | |
| JP2008239892A (en) * | 2007-03-28 | 2008-10-09 | Mitsubishi Chemicals Corp | Method and system for purification of source gas |
| DE102016116306A1 (en) | 2016-09-01 | 2018-03-01 | Thyssenkrupp Ag | Method and apparatus for removing organic sulfur compounds from hydrogen-rich gases |
| CN109641176A (en) * | 2016-09-01 | 2019-04-16 | 蒂森克虏伯工业解决方案股份公司 | Method and apparatus for removing organosulfur compound from hydrogen-rich gas |
| JP2019529306A (en) * | 2016-09-01 | 2019-10-17 | ティッセンクルップ インダストリアル ソリューションズ アクツィエンゲゼルシャフトＴｈｙｓｓｅｎＫｒｕｐｐ Ｉｎｄｕｓｔｒｉａｌ Ｓｏｌｕｔｉｏｎｓ ＡＧ | Method and apparatus for removing organic sulfur compounds from hydrogen enriched gas |
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| Publication number | Publication date |
|---|---|
| JPH0229711B2 (en) | 1990-07-02 |
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