JPH0791546B2 - Method for removing mercury in hydrocarbon oils - Google Patents
Method for removing mercury in hydrocarbon oilsInfo
- Publication number
- JPH0791546B2 JPH0791546B2 JP63012287A JP1228788A JPH0791546B2 JP H0791546 B2 JPH0791546 B2 JP H0791546B2 JP 63012287 A JP63012287 A JP 63012287A JP 1228788 A JP1228788 A JP 1228788A JP H0791546 B2 JPH0791546 B2 JP H0791546B2
- Authority
- JP
- Japan
- Prior art keywords
- copper
- mercury
- hydrocarbon
- activated carbon
- oil
- 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.)
- Expired - Lifetime
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/40—Ethylene production
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
【発明の詳細な説明】 ＜産業上の利用分野＞ 本発明は、炭化水素系油中に混在する水銀の除去方法に
関し、特に固−液接触機構を利用した水銀の選択的、効
率的除去方法に関する。TECHNICAL FIELD The present invention relates to a method for removing mercury mixed in a hydrocarbon oil, and more particularly to a method for selectively and efficiently removing mercury using a solid-liquid contact mechanism. Regarding
＜従来の技術＞ 水添等によって、ナフサ等の炭化水素系油を改質する場
合には、パラジウム担持アルミナ系等の触媒が用いられ
る。ところが、炭化水素系油中には不純物として水銀が
存在すると、触媒が被毒して反応が充分行われない。<Prior Art> When reforming a hydrocarbon oil such as naphtha by hydrogenation or the like, a palladium-supported alumina catalyst or the like is used. However, if mercury is present as an impurity in the hydrocarbon oil, the catalyst is poisoned and the reaction is not sufficiently carried out.
このため、従来から以下のような水銀の除去方法が行わ
れている。Therefore, the following mercury removal methods have been conventionally performed.
ａ）活性炭、モレキュラシーブ、シリカゲル、ゼオライ
ト、アルミナ等の多孔質吸着剤を用いる物理吸着方法。a) Physical adsorption method using a porous adsorbent such as activated carbon, molecular sieve, silica gel, zeolite or alumina.
ｂ）金属硫化物、あるいは多孔質吸着剤に硫黄を添加
し、水銀と硫黄との反応／吸着によって水銀を除去する
方法。b) A method in which sulfur is added to a metal sulfide or a porous adsorbent and mercury is removed by a reaction / adsorption of mercury and sulfur.
しかし、ａ）の物理吸着方法では、炭化水素系油中の重
質分やガム質は効率良く除去されるものの、水銀の除去
率は30〜70wt％と低い。また、ｂ）の反応／吸着方法で
は、反応／吸着後の濾別が困難であると同時に、ａ）の
物理吸着方法と同様水銀の除去率が低い。However, in the physical adsorption method of a), although the heavy components and gums in the hydrocarbon-based oil are efficiently removed, the removal rate of mercury is as low as 30 to 70 wt%. Further, in the reaction / adsorption method of b), filtration after reaction / adsorption is difficult, and at the same time, the removal rate of mercury is low as in the physical adsorption method of a).
このため、炭化水素系油中の水銀を選択的かつ効率良く
除去する方法が望まれている。Therefore, a method for selectively and efficiently removing mercury in hydrocarbon-based oil is desired.
＜発明が解決しようとする課題＞ 本発明の目的は、炭化水素系油中の微量の水銀を選択的
かつ効率良く除去し、しかも反応後、触媒物質との分離
が容易な炭化水素系油中の水銀の除去方法を提供せんと
する。<Problems to be Solved by the Invention> An object of the present invention is to remove a trace amount of mercury in a hydrocarbon-based oil selectively and efficiently, and yet to separate it from a catalyst substance after the reaction in a hydrocarbon-based oil. The method for removing mercury in
＜課題を解決するための手段＞ 本発明は、銅を担持した活性炭に、水銀を含む炭化水素
系油を接触させることを特徴とする炭化水素系油中の水
銀の除去方法を提供する。<Means for Solving the Problems> The present invention provides a method for removing mercury in a hydrocarbon-based oil, which is characterized by bringing a hydrocarbon-based oil containing mercury into contact with activated carbon carrying copper.
ここで、前記銅が銅ハロゲン化物を含むのが良い。Here, the copper preferably contains a copper halide.
また、前記活性炭が、平均細孔径10〜500Å比表面積100
〜1500m2/gであるのが良い。Further, the activated carbon has an average pore size of 10 to 500 Å specific surface area of 100.
It should be ~ 1500 m 2 / g.
＜発明の構成＞ 以下に本発明の構成を詳述する。<Structure of the Invention> The structure of the present invention will be described in detail below.
本発明方法を適用する炭化水素系油は、常温で液体の炭
化水素であればいかなるものでもよい。The hydrocarbon-based oil to which the method of the present invention is applied may be any hydrocarbon as long as it is a liquid hydrocarbon at room temperature.
原油、直留ナフサ、灯油、軽油、減圧留出物、常圧残存
油、エチレンプラントの熱分解装置で副生される熱分解
ガソリン、熱処理を受けた炭化水素油、接触分解装置で
生成されたナフサ留分、リサイクル油などが例示され
る。Crude oil, straight-distilled naphtha, kerosene, light oil, vacuum distillate, atmospheric residual oil, pyrolysis gasoline by-produced in a thermal cracker of an ethylene plant, hydrocarbon oil subjected to heat treatment, produced in a catalytic cracker Examples include naphtha fraction and recycled oil.
特に、天然ガスより液化石油ガス（LPG）を除いたnatur
al gas liquid（NGL）特にNGL中でも低沸点成分である
重質天然ガスリキッド中の水銀除去に好適に用いられ
る。In particular, natur, which is the natural gas excluding liquefied petroleum gas (LPG)
Al gas liquid (NGL) Particularly suitable for removing mercury in heavy natural gas liquid, which is a low boiling point component of NGL.
本発明方法では、除去される炭化水素系油中の水銀の存
在形態は、単体水銀、無機水銀、有機水銀等いかなる形
態で存在してもよいが、常温で液体である炭化水素系油
中に存在する有機水銀に対して特に有効である。In the method of the present invention, the existing form of mercury in the hydrocarbon-based oil to be removed may be any form such as elemental mercury, inorganic mercury, and organic mercury, but in a hydrocarbon-based oil that is liquid at room temperature. It is particularly effective against the organic mercury present.
炭化水素系油中の水銀濃度は、特に限定されるものでは
ないが、400〜600ppb以下、好ましくは100〜150ppb以下
であると反応効率が良い。The concentration of mercury in the hydrocarbon-based oil is not particularly limited, but the reaction efficiency is good when it is 400 to 600 ppb or less, preferably 100 to 150 ppb or less.
必要な場合は、炭化水素系油中のスラッジ等を、あらか
じめ濾過膜やフィルター等で濾過し、スラッジとともに
濾別される水銀を除去しておくのが良い。If necessary, it is advisable to previously filter the sludge in the hydrocarbon-based oil with a filter membrane or a filter to remove the mercury that is filtered off together with the sludge.
本発明方法に用いる活性炭は、一般に用いられる粒状ま
たは粉末状の活性炭が用いられ、水蒸気賦活活性炭を用
いることもよい。The activated carbon used in the method of the present invention is generally used granular or powdery activated carbon, and steam activated carbon may be used.
特に、細孔径10〜500Å好ましくは10〜100Å、比表面積
100〜1500m2/g好ましくは、800〜1200m2/gの活性炭がよ
い。In particular, pore size 10-500Å, preferably 10-100Å, specific surface area
100 to 1500 m 2 / g, preferably 800 to 1200 m 2 / g activated carbon.
この範囲の物性を持つ活性炭を用いると、水銀の除去率
が向上するという効果があるからである。This is because the use of activated carbon having physical properties in this range has the effect of improving the mercury removal rate.
また活性炭への銅（銅化合物）の担持量は担体（活性
炭）重量に対して0.1〜30重量％が好ましい。The amount of copper (copper compound) supported on the activated carbon is preferably 0.1 to 30% by weight based on the weight of the carrier (activated carbon).
上記の活性炭に担持させる銅は、好ましくは以下の銅ま
たはこれらの混合物を用いる。As the copper to be supported on the above activated carbon, the following copper or a mixture thereof is preferably used.
これらの銅は、活性炭上で、銅、銅イオン、銅化合物ま
たはこれらの溶媒和物等で存在すると考えられるが詳細
な形態は不明であり、本発明ではこれらの総称として
「銅」を用いる場合もある。These copper, on the activated carbon, copper, copper ions, it is considered to be present in the copper compound or a solvate thereof, etc., but the detailed form is unknown, and in the present invention, when "copper" is used as a generic term for these. There is also.
（１）ハロゲン化銅 ハロゲン化銅としては、CuCl、CuCl2が好ましく、これ
らのハロゲン化銅を、水溶液、塩酸溶液、塩化アルカリ
溶液またはアンモニア水溶液等の適切な無機溶媒または
アセトン、アルコールなどの有機溶媒に溶解して溶液と
し、この溶液に活性炭を浸漬し、エバポレーターで溶媒
を除いた後乾燥焼成して、銅担持活性炭を調整する。(1) Copper Halogen As the copper halide, CuCl and CuCl 2 are preferable, and these copper halides are used as an appropriate inorganic solvent such as an aqueous solution, a hydrochloric acid solution, an alkali chloride solution or an aqueous ammonia solution, or an organic solvent such as acetone or alcohol. A copper-supported activated carbon is prepared by dissolving it in a solvent to form a solution, immersing the activated carbon in this solution, removing the solvent with an evaporator, and then drying and firing.
（２）酸化銅 銅溶液に活性炭を浸漬し、上述のように乾燥した後に、
酸素雰囲気中で焼成し、酸化銅として用いてもよい。(2) Copper oxide After immersing activated carbon in a copper solution and drying as described above,
It may be fired in an oxygen atmosphere and used as copper oxide.
銅担持活性炭と、炭化水素系油との接触方法は、各種の
固液接触方式を用いることができ、例えば固定床方式、
移動床方式、移動床方式がある。As the method for contacting the copper-supported activated carbon with the hydrocarbon oil, various solid-liquid contact methods can be used, for example, a fixed bed method,
There are moving floor system and moving bed system.
好ましくは、以下の反応装置等を用いるが、これらには
限定されない。The following reactors and the like are preferably used, but not limited to these.
第１図には、銅担持活性炭２を固定床に用いた吸着塔
３、４を備えた装置を示す。FIG. 1 shows an apparatus equipped with adsorption towers 3 and 4 using a copper-loaded activated carbon 2 as a fixed bed.
第１吸着塔３は、中心部に銅担持活性炭２の固定床を設
えた円筒状反応塔で上部にポンプ６を介して原料１を供
給する原料供給口が設けられ、下部に精製品取出ライン
９が設けられる。The first adsorption tower 3 is a cylindrical reaction tower having a fixed bed of the copper-supporting activated carbon 2 in the center, and a raw material supply port for supplying the raw material 1 via a pump 6 is provided in the upper portion and a purified product take-out line in the lower portion. 9 is provided.
好ましくは、吸着塔は多段に設けられる。第１図には、
第１吸着塔３と第２吸着塔４が２段に設けられた例を示
す。Preferably, the adsorption tower is provided in multiple stages. In Figure 1,
An example in which the first adsorption tower 3 and the second adsorption tower 4 are provided in two stages is shown.
炭化水素系油等の原料１は、第１吸着塔３へ供給され、
銅担持活性炭２の固定床を流下し、流下時に炭化水素系
油中の微量の水銀は銅担持活性炭２に吸着、除去され
る。水銀を除去された炭化水素系油は、精製品取出ライ
ン９からさらに第２吸着塔４へ供給され、第１吸着塔３
と同様に炭化水素系油中の水銀が除去される。Raw material 1 such as hydrocarbon oil is supplied to the first adsorption tower 3,
A fixed bed of the copper-supporting activated carbon 2 is flown down, and a small amount of mercury in the hydrocarbon-based oil is adsorbed and removed by the copper-supporting activated carbon 2 during the flow down. The hydrocarbon-based oil from which mercury has been removed is further supplied to the second adsorption tower 4 from the purified product take-out line 9, and the first adsorption tower 3
The mercury in the hydrocarbon oil is removed in the same manner as in.
SV値は、0.5hr-1〜5.0hr-1特に0.5hr-1〜2.0hr-1が好ま
しい。SV value is preferably 0.5hr -1 ~5.0hr -1 particularly 0.5hr -1 ~2.0hr -1.
第２図は、撹拌器７を有する吸着槽10、11を備えた装置
を示す。FIG. 2 shows an apparatus equipped with adsorption tanks 10 and 11 having a stirrer 7.
炭化水素系油等の原料１は、吸着槽10に供給され、一方
銅担持活性炭２も吸着槽10に適宜供給される。吸着槽２
内で撹拌器７により撹拌されつつ、原料１と銅担持活性
炭２が接触し、炭化水素系油中の微量の水銀が銅担持活
性炭２に吸着されて除去される。The raw material 1 such as hydrocarbon oil is supplied to the adsorption tank 10, while the copper-supported activated carbon 2 is also appropriately supplied to the adsorption tank 10. Adsorption tank 2
While being stirred by the stirrer 7 inside, the raw material 1 and the copper-supporting activated carbon 2 come into contact with each other, and a trace amount of mercury in the hydrocarbon oil is adsorbed by the copper-supporting activated carbon 2 and removed.
原料１に含まれる固型分が多い場合には、吸着塔３、
４、吸着槽10、11等の保護のためのスラッジ等をあらか
じめ取除くためのプレフィルターないしは濾過装置を用
いるのが良い。濾過材は固型分を取除くものであればい
かなるものでもよい。When the solid content contained in the raw material 1 is large, the adsorption tower 3,
4. It is preferable to use a prefilter or a filtration device for removing sludge and the like for protecting the adsorption tanks 10 and 11 in advance. Any filtering material may be used as long as it removes solid components.
＜実施例＞ 以下に実施例により、具体的に説明する。<Examples> Examples will be specifically described below.
（実施例１〜３） 重質天然ガスリキッド（Ｈ−NGL）100mlを 0.2μｍのミリポアフィルターで濾過した。濾別した
スラッジ組成は下記であった。(Examples 1 to 3) 100 ml of heavy natural gas liquid (H-NGL) was filtered with a 0.2 μm Millipore filter. The sludge composition filtered out was as follows.
Fe 10.0wt％ Si 18.3wt％ Hg 3.1wt％ Ｓ 2.3wt％ 濾液中の水銀濃度は130ppbであった。Fe 10.0 wt% Si 18.3 wt% Hg 3.1 wt% S 2.3 wt% The mercury concentration in the filtrate was 130 ppb.
この濾液100mlを、活性炭（比表面積1050、平均細孔径2
0Å、東洋カルゴンCAL）に表１に示す銅を吸着させた銅
担持活性炭0.8gと撹拌しながら１時間吸着反応処理し、
処理後の水銀濃度と水銀除去率を表１に示した。100 ml of this filtrate was added to activated carbon (specific surface area 1050, average pore size 2
0 Å, Toyo Calgon CAL) was adsorbed for 1 hour while stirring with 0.8 g of copper-supported activated carbon on which copper shown in Table 1 was adsorbed,
Table 1 shows the mercury concentration and the mercury removal rate after the treatment.
活性炭は、表１に示す銅溶液中に浸漬し、濾過、水洗、
濾過後、130℃乾燥器で、空気中、３時間乾燥処理して
用いた。Activated carbon was immersed in the copper solution shown in Table 1, filtered, washed with water,
After filtration, it was dried in a dryer at 130 ° C. for 3 hours and used.
得られた銅担持活性炭中の銅化合物の含有量を表１に示
した。The content of the copper compound in the obtained copper-supported activated carbon is shown in Table 1.
（比較例） べつに比較として、表１に示す銅を担持しない実施例と
同様の活性炭と、FeCl2、FeCl3、LiCl、NaCl、ZnCl2を
担持した実施例と同様の活性炭を用いて、実施例と同様
の処理を行い結果を表１に示した。(Comparative Example) As a comparison, an activated carbon similar to the example shown in Table 1 which does not support copper and an activated carbon similar to the example supporting FeCl 2 , FeCl 3 , LiCl, NaCl and ZnCl 2 were used. The same treatment as in the example was performed and the results are shown in Table 1.
＜発明の効果＞ 本発明方法は、炭化水素系油と銅担持活性炭を固−液接
触して、炭化水素系油中の水銀を除去するので、炭化水
素系油中に混在する水銀が選択的に効率良く除去でき、
しかも処理後の精製物の分離が容易である。 <Effect of the Invention> In the method of the present invention, the hydrocarbon in the hydrocarbon-based oil and the copper-supported activated carbon are brought into solid-liquid contact with each other to remove the mercury in the hydrocarbon-based oil. Can be removed efficiently,
Moreover, the purified product after the treatment can be easily separated.
水銀を除去された炭化水素系油は、触媒被毒成分を含ま
ないので、水添反応等の触媒使用反応に広く利用でき
る。Since the hydrocarbon-based oil from which mercury has been removed does not contain a catalyst poisoning component, it can be widely used for a reaction using a catalyst such as a hydrogenation reaction.
第１図は、本発明方法を実施する装置の１例を示す線図
である。 第２図は、本発明方法を実施する他の装置の例を示す線
図である。 符号の説明 １……原料、２……銅担持活性炭、 ３……第１吸着塔、４……第２吸着塔、 ５……配管、６……ポンプ、 ７……撹拌器、 ９……精製品取出ライン、 10、11……吸着槽FIG. 1 is a diagram showing an example of an apparatus for carrying out the method of the present invention. FIG. 2 is a diagram showing an example of another apparatus for carrying out the method of the present invention. DESCRIPTION OF SYMBOLS 1 ... Raw material, 2 ... Copper-loaded activated carbon, 3 ... First adsorption tower, 4 ... Second adsorption tower, 5 ... Piping, 6 ... Pump, 7 ... Stirrer, 9 ... Purified product take-out line, 10, 11 ... Adsorption tank
Claims (3)
素系油を接触させることを特徴とする炭化水素系油中の
水銀の除去方法。1. A method for removing mercury from a hydrocarbon-based oil, which comprises bringing a hydrocarbon-based oil containing mercury into contact with activated carbon carrying copper.
範囲第１項に記載の炭化水素系油中の水銀の除去方法。2. The method for removing mercury in a hydrocarbon oil according to claim 1, wherein the copper contains a copper halide.
積100〜1500m2/gである特許請求の範囲第１項または第
２項のいずれかに記載の炭化水素系油中の水銀の除去方
法。3. The mercury in the hydrocarbon oil according to claim 1, wherein the activated carbon has a pore size of 10 to 500Å and a specific surface area of 100 to 1500 m 2 / g. Removal method.
Priority Applications (10)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63012287A JPH0791546B2 (en) | 1988-01-22 | 1988-01-22 | Method for removing mercury in hydrocarbon oils |
| AU28619/89A AU607037B2 (en) | 1988-01-22 | 1989-01-19 | Method of removing mercury from hydrocarbon oils |
| CA000588678A CA1325992C (en) | 1988-01-22 | 1989-01-19 | Method of removing mercury from hydrocarbon oils |
| US07/299,025 US4946582A (en) | 1988-01-22 | 1989-01-19 | Method of removing mercury from hydrocarbon oils |
| ES198989300567T ES2034604T3 (en) | 1988-01-22 | 1989-01-20 | A METHOD OF ELIMINATION OF MERCURY FROM A HYDROCARBON OIL. |
| AT89300567T ATE78861T1 (en) | 1988-01-22 | 1989-01-20 | PROCESS FOR REMOVAL OF MERCURY FROM HYDROCARBON OILS. |
| DE8989300567T DE68902239T2 (en) | 1988-01-22 | 1989-01-20 | METHOD FOR REMOVING MERCURY FROM HYDROCARBON OILS. |
| EP89300567A EP0325486B1 (en) | 1988-01-22 | 1989-01-20 | Method of removing mercury from hydrocarbon oils |
| KR1019890000630A KR910005348B1 (en) | 1988-01-22 | 1989-01-21 | Method of removing mercury from hydrocarbon oils |
| GR920402104T GR3005782T3 (en) | 1988-01-22 | 1992-09-24 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63012287A JPH0791546B2 (en) | 1988-01-22 | 1988-01-22 | Method for removing mercury in hydrocarbon oils |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01188586A JPH01188586A (en) | 1989-07-27 |
| JPH0791546B2 true JPH0791546B2 (en) | 1995-10-04 |
Family
ID=11801138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63012287A Expired - Lifetime JPH0791546B2 (en) | 1988-01-22 | 1988-01-22 | Method for removing mercury in hydrocarbon oils |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0791546B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5202301A (en) * | 1989-11-22 | 1993-04-13 | Calgon Carbon Corporation | Product/process/application for removal of mercury from liquid hydrocarbon |
| JPH07116445B2 (en) * | 1992-03-19 | 1995-12-13 | 日揮株式会社 | Method for decomposing and removing mercury compound in hydrocarbon |
| JP3405556B2 (en) * | 1993-01-20 | 2003-05-12 | 住友ベークライト株式会社 | Method for producing activated carbon composition |
| JP5192653B2 (en) * | 2006-03-31 | 2013-05-08 | 日本インスツルメンツ株式会社 | Mercury reduction catalyst, mercury conversion unit, and total mercury measurement device in exhaust gas using the same |
-
1988
- 1988-01-22 JP JP63012287A patent/JPH0791546B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01188586A (en) | 1989-07-27 |
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