JP2947369B2 - Method for removing mercury and mercury compounds from hydrocarbon oil - Google Patents
Method for removing mercury and mercury compounds from hydrocarbon oilInfo
- Publication number
- JP2947369B2 JP2947369B2 JP3062032A JP6203291A JP2947369B2 JP 2947369 B2 JP2947369 B2 JP 2947369B2 JP 3062032 A JP3062032 A JP 3062032A JP 6203291 A JP6203291 A JP 6203291A JP 2947369 B2 JP2947369 B2 JP 2947369B2
- Authority
- JP
- Japan
- Prior art keywords
- mercury
- hydrocarbon oil
- extract
- compounds
- pressure
- 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
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- Extraction Or Liquid Replacement (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は、炭化水素油中の水銀お
よび水銀化合物の除去方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for removing mercury and mercury compounds in a hydrocarbon oil.
【0002】[0002]
【従来の技術】原油および天然ガスに含まれているコン
デンセートには、一部の産地のものから数十ppbオーダ
ーの水銀および水銀化合物が存在することが知られてい
る。これらの水銀および水銀化合物は、銅等の金属材料
と容易にアマルガムを生成して、石油精製処理や化学原
料として利用する際の触媒反応における触媒の活性低
下、化学機器に用いられる金属材料の腐食、強度低下等
を起こす原因となる。この水銀および水銀化合物の除去
方法としては、活性炭を用いて吸着除去する方法、また
は銅、アルミニウムおよびこれらの化合物との接触によ
り除去する方法が試みられている。2. Description of the Related Art It is known that condensate contained in crude oil and natural gas contains mercury and mercury compounds on the order of several tens of ppb from some localities. These mercury and mercury compounds easily produce amalgam with metal materials such as copper, and reduce the activity of the catalyst in the catalytic reaction when used as a petroleum refinery or chemical raw material, and corrode metal materials used in chemical equipment. , Causing a decrease in strength. As a method of removing mercury and a mercury compound, a method of removing the mercury by adsorption using activated carbon or a method of removing the mercury and the compound by contact with copper, aluminum, and these compounds have been attempted.
【0003】[0003]
【発明が解決しようとする課題】しかしながら、活性炭
を用いて吸着除去する方法では、炭化水素油がベンゼ
ン、トルエン等の芳香族炭化水素類であると、水銀およ
び水銀化合物を十分に除去することができない。また、
銅、アルミニウムおよびこれらの化合物との接触によ
り、水銀および水銀化合物を除去する方法では、その処
理に高温を要するため、装置も複雑であり、コスト上も
問題である。本発明は、上記のような従来の課題を解決
し、簡便な手段によって、効率よく炭化水素油から水銀
および水銀化合物を除去する方法を提供することを目的
とするものである。However, in the method of adsorption removal using activated carbon, if the hydrocarbon oil is an aromatic hydrocarbon such as benzene or toluene, mercury and mercury compounds can be sufficiently removed. Can not. Also,
In the method of removing mercury and mercury compounds by contacting with copper, aluminum and their compounds, the treatment requires a high temperature, so that the apparatus is complicated and the cost is problematic. An object of the present invention is to solve the conventional problems as described above and to provide a method for efficiently removing mercury and a mercury compound from hydrocarbon oil by simple means.
【0004】[0004]
【課題を解決するための手段】本発明者らは鋭意検討し
た結果、上記のような課題を解決することができた。す
なわち本発明は、水銀および/または水銀化合物を含有
する炭化水素油と、水より高沸点の有機溶媒を0.01
〜50容量%含む水溶液とを接触させて、撹拌・混合し
ながら、0.01〜10kg/cm2のゲージ圧下で、80〜
130℃に加熱し、炭化水素油中の水銀および/または
水銀化合物を抽出することを特徴とする、炭化水素油中
の水銀および水銀化合物の除去方法を提供するものであ
る。Means for Solving the Problems As a result of intensive studies, the present inventors have solved the above-mentioned problems. That is, the present invention provides a hydrocarbon oil containing mercury and / or a mercury compound and an organic solvent having a higher boiling point than water.
Contacting with an aqueous solution containing 5050% by volume, stirring and mixing, under a gauge pressure of 0.01 to 10 kg / cm 2 , and
It is intended to provide a method for removing mercury and a mercury compound in a hydrocarbon oil, wherein the method is heated to 130 ° C. to extract mercury and / or a mercury compound in the hydrocarbon oil.
【0005】以下に、本発明をさらに詳細に説明する。
本発明によって水銀および水銀化合物を除去できる炭化
水素油とは、あらゆる炭化水素油であって、とくに限定
するものではない。例えば、ベンゼン、トルエン等の炭
化水素油、ガソリン、燈油、軽油、天然ガスコンデンセ
ート等を挙げることができる。Hereinafter, the present invention will be described in more detail.
The hydrocarbon oils from which mercury and mercury compounds can be removed according to the present invention are all hydrocarbon oils, and are not particularly limited. Examples thereof include hydrocarbon oils such as benzene and toluene, gasoline, kerosene, light oil, natural gas condensate, and the like.
【0006】炭化水素油中の水銀および/または水銀化
合物を抽出する抽出液は、水より高沸点の有機溶媒を
0.01〜50容量%含む水溶液である。水より高沸点
の有機溶媒としては、とくに制限しないが、例えばエチ
レングリコール、トリメチレングリコール、ポリエチレ
ングリコール、グリセリンあるいはこれらの部分エステ
ル化物を挙げることができる。その添加量は、炭化水素
油1容に対し、通常0.1〜5容、好ましくは0.5〜2
容がよい。水の沸点より高沸点を有する有機溶媒を水に
溶解せしめることにより、操作中の蒸気圧を低くする効
果と、水銀化合物の水溶液への分配比を大きくする効果
とを付与することができる。An extract for extracting mercury and / or a mercury compound in a hydrocarbon oil is an aqueous solution containing 0.01 to 50% by volume of an organic solvent having a higher boiling point than water. Examples of the organic solvent having a higher boiling point than water include, but are not particularly limited to, ethylene glycol, trimethylene glycol, polyethylene glycol, glycerin, and partially esterified products thereof. The addition amount is usually 0.1 to 5 volumes, preferably 0.5 to 2 volumes per 1 volume of hydrocarbon oil.
It is good. By dissolving an organic solvent having a boiling point higher than the boiling point of water in water, the effect of lowering the vapor pressure during operation and the effect of increasing the distribution ratio of the mercury compound to the aqueous solution can be provided.
【0007】本発明の方法においては、水銀および/ま
たは水銀化合物を含有する炭化水素油と、抽出液とを接
触させる。水による抽出は、抽出温度を高くする程、水
銀化合物の水への分配比が大きくなる利点を有するが、
温度の上昇は、水銀の蒸気圧が上昇し、炭化水素油層に
入り込むことにより、除去率が低下する可能性を有す
る。この相反する2条件を満たすには最適の抽出温度が
存在する。検討によれば、130℃を超えると見かけ
上、炭化水素油からの水銀化合物抽出量が増加しなくな
る。さらに温度上昇は、圧力上昇につながり、その圧力
上昇は、温度の上昇に対し指数的に上昇するので、抽出
容器の耐圧性維持からもこれ以上の昇温は有利とならな
い。本発明の方法においては、接触温度は、通常80〜
130℃、好ましくは90〜110℃がよい。80℃未
満の温度では、水銀化合物の除去が不十分となり、また
130℃を超える温度では、上記のとおり水銀類の抽出
量の増加には効果がなく、使用する耐圧性容器の劣化の
原因ともなり好ましくない。、また抽出時の圧力は、大
気圧よりも高い圧力、例えばゲージ圧として通常0.0
1〜10kg/cm2、好ましくは0.1〜3kg/cm2がよ
い。0.01kg/cm2未満のゲージ圧では、水銀化合物の
除去が不十分となり、また10kg/cm2を超えるゲージ
圧を用いても、容器の耐圧を高くする必要があり好まし
くない。水銀および/または水銀化合物を含有する炭化
水素油と、抽出液との混合物を上記のような所定の温度
・圧力下で激しく撹拌して両液を接触させる。その方法
としては、例えば、炭化水素油と抽出液の混合物を、オ
ートクレーブ中で撹拌・接触させる方法、あるいは撹拌
機を有するか充填材を充填した流通式の加圧槽を通して
両液を接触させる方法等を挙げることができる。[0007] In the method of the present invention, a hydrocarbon oil containing mercury and / or a mercury compound is brought into contact with an extract. Extraction with water has the advantage that the higher the extraction temperature, the greater the distribution ratio of mercury compounds to water,
Increasing the temperature has the potential to increase the vapor pressure of the mercury and penetrate the hydrocarbon oil layer, thereby reducing the removal rate. There is an optimal extraction temperature to satisfy these two contradictory conditions. According to the study, when the temperature exceeds 130 ° C., the amount of mercury compound extracted from the hydrocarbon oil does not seem to increase. Furthermore, a rise in temperature leads to a rise in pressure, and the rise in pressure increases exponentially with a rise in temperature. Therefore, further maintenance of the pressure resistance of the extraction vessel is not advantageous. In the method of the present invention, the contact temperature is usually from 80 to
130 ° C, preferably 90 to 110 ° C. At a temperature lower than 80 ° C., the removal of mercury compounds becomes insufficient. At a temperature higher than 130 ° C., as described above, there is no effect on the increase in the amount of mercury extracted, which may cause deterioration of the pressure-resistant container used. It is not preferable. The pressure at the time of extraction is higher than atmospheric pressure, for example, usually 0.0 as a gauge pressure.
1 to 10 kg / cm 2 , preferably 0.1 to 3 kg / cm 2 is good. The 0.01 kg / cm 2 less than the gauge pressure, the removal of mercury compounds becomes insufficient, also be used a gauge pressure of greater than 10 kg / cm 2, it is necessary to increase the withstand voltage of the vessel undesirably. A mixture of a hydrocarbon oil containing mercury and / or a mercury compound and an extract is vigorously stirred under the above-mentioned predetermined temperature and pressure to bring the two liquids into contact. Examples of the method include a method in which a mixture of a hydrocarbon oil and an extract is stirred and contacted in an autoclave, or a method in which both liquids are contacted through a flow-type pressurized tank having a stirrer or filled with a filler. And the like.
【0008】撹拌・混合が完了した後、静置させて、主
として炭化水素油からなる上層と、主として抽出液から
なる下層とに分離させる。静置分離する際の温度は、通
常0〜80℃、好ましくは室温〜60℃がよい。After completion of the stirring and mixing, the mixture is allowed to stand and separated into an upper layer mainly composed of a hydrocarbon oil and a lower layer mainly composed of an extract. The temperature at the time of stationary separation is usually 0 to 80 ° C, preferably room temperature to 60 ° C.
【0009】[0009]
【実施例】以下、実施例によって本発明をさらに説明す
る。実施例1 炭化水素油として、n−ヘプタン40容量%、イソオク
タン50容量%およびエチルベンゼン10容量%からな
る混合物に対し、水銀として400W/Vppbとなるように
塩化水銀(II)を添加した。抽出液として、10容量%の
エチレングリコールを調製した。上記の調製した炭化水
素油300mlを、内容積1l、耐圧100kg/cm2のオー
トクレーブに入れ、これに抽出液150mlを加え、電磁
誘導撹拌装置を用いて撹拌・混合しながら、表1に示す
ような温度および圧力とした。この状態を10分間保っ
た。この後、オートクレーブから炭化水素油と抽出液と
の混合物を取り出し、10分間静置させ、主として炭化
水素油からなる上層と、抽出液を主体とする下層とに分
離させた。上層(炭化水素油層)を約50ml抜き出し、
25℃まで冷却させた後、原子吸光法により水銀含有量
を測定した。その結果を表1に示す。The present invention will be further described with reference to the following examples. Example 1 Mercury (II) chloride was added to a mixture of 40% by volume of n-heptane, 50% by volume of isooctane and 10% by volume of ethylbenzene as a hydrocarbon oil so as to obtain 400 W / Vppb as mercury. As an extract, 10% by volume of ethylene glycol was prepared. 300 ml of the above-prepared hydrocarbon oil was placed in an autoclave having an internal volume of 1 l and a pressure resistance of 100 kg / cm 2 , and 150 ml of the extract was added thereto. While stirring and mixing using an electromagnetic induction stirrer, as shown in Table 1, Temperature and pressure. This state was maintained for 10 minutes. Thereafter, the mixture of the hydrocarbon oil and the extract was taken out of the autoclave and allowed to stand for 10 minutes to separate into an upper layer mainly composed of the hydrocarbon oil and a lower layer mainly composed of the extract. About 50 ml of the upper layer (hydrocarbon oil layer) is extracted,
After cooling to 25 ° C., the mercury content was measured by the atomic absorption method. Table 1 shows the results.
【0010】[0010]
【表1】 表 1 ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━ 抽出温度 圧力(ゲージ圧) 上層(炭化水素油層)中の (℃) (kg/cm2) 水銀含有量 (W/Vppb) ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━ 80 <0.01 80 90 <0.01 65 100 0.04 40 110 0.80 25 120 1.80 20 130 2.45 30 ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━[Table 1] ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━ Extraction temperature Pressure (gauge pressure) In upper layer (hydrocarbon oil layer) (° C) (kg / cm 2 ) Mercury content (W / Vppb) 80 80 < 0.01 80 90 <0.01 65 100 0.04 40 110 0.80 25 120 1.80 20 130 2.45 30 ━━━━━━━━━━━━━━━━━━━━ ━━━━━━━━━━
【0011】実施例2 実施例1と同じ水銀濃度の炭化水素油を調製した。抽出
液として、10容量%のエチレングリコール、ジエチレ
ングリコール、トリエチレングリコールおよびグリセリ
ンをそれぞれ調製した。上記の調製した炭化水素油30
0mlを、実施例1で使用したオートクレーブに入れ、こ
れに上記の各抽出液150mlを加え、電磁誘導撹拌装置
を用いて撹拌・混合しながら、120℃まで昇温させ、
且つ表2に示すような圧力とした。この状態を10分間
保った。この後、オートクレーブから炭化水素油と抽出
液との混合物を取り出し、10分間静置させ、主として
炭化水素油からなる上層と、抽出液を主体とする下層と
に分離させた。上層(炭化水銀油層)および下層(抽出
液層)をそれぞれ約50ml抜き出し、25℃まで冷却さ
せた後、原子吸光法により水銀含有量を測定した。その
結果を表2に示す。 Example 2 A hydrocarbon oil having the same mercury concentration as in Example 1 was prepared. As the extract, 10% by volume of ethylene glycol, diethylene glycol, triethylene glycol and glycerin were respectively prepared. The above-prepared hydrocarbon oil 30
0 ml was placed in the autoclave used in Example 1, 150 ml of each of the above extracts was added thereto, and the mixture was heated to 120 ° C. while stirring and mixing using an electromagnetic induction stirrer.
The pressure was set as shown in Table 2. This state was maintained for 10 minutes. Thereafter, the mixture of the hydrocarbon oil and the extract was taken out of the autoclave and allowed to stand for 10 minutes to separate into an upper layer mainly composed of the hydrocarbon oil and a lower layer mainly composed of the extract. About 50 ml of each of the upper layer (mercury carbonized oil layer) and the lower layer (extracted liquid layer) was extracted and cooled to 25 ° C., and the mercury content was measured by an atomic absorption method. Table 2 shows the results.
【0012】[0012]
【表2】 表 2 ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━ 添加した 圧力(ゲージ圧) 上層中の水銀 下層中の水銀 有機溶媒類 (kg/cm2) 含有量(W/Vppb) 含有量(W/Vppb) ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━ エチレングリコール 1.80 20 380 ジエチレングリコール 1.70 25 375 トリエチレングリコール 1.55 25 370 グリセリン 1.50 30 370 ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━[Table 2] Table 2 ━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━ Added pressure (gauge pressure) In upper layer Mercury in the lower layer Mercury in the lower layer Organic solvents (kg / cm 2 ) Content (W / Vppb) Content (W / Vppb) ━━━━━━━━━━━━━━━━━━━━━エ チ レ ン Ethylene glycol 1.80 20 380 Diethylene glycol 1.70 25 375 Triethylene glycol 1.55 25 370 Glycerin 1.50 30 370━━━━━━━━━ ━━━━━━━━━━━━━━━━━━━━━━━━━━
【0013】実施例3 水銀を650W/Vppb含み、且つ100℃以下で沸騰する
低沸点物を除去した、天然ガスに同伴されるコンデンセ
ート300mlに、抽出液として10容量%のエチレング
リコールを150ml添加し、オートクレーブ中で撹拌・
混合しながら120℃まで昇温し、圧力を2.2kg/cm2
として、この状態を10分間保った。続いて10分間静
置させた後、コンデンセートを主体とする上層(コンデ
ンセート層)および抽出液を主体とする下層(抽出液
層)をそれぞれ約50ml抜き出し、25℃まで冷却させ
た後、原子吸光法により水銀含有量を測定した。その結
果、下層(抽出液層)中の水銀濃度は620W/Vppbであ
り、上層(コンデンセート層)中の水銀濃度は30W/Vp
pbであった。 EXAMPLE 3 150 ml of 10% by volume ethylene glycol was added as an extract to 300 ml of condensate containing 650 W / Vppb of mercury and containing low-boiling substances boiling below 100 ° C. and accompanied by natural gas. Stirring in an autoclave
The temperature was raised to 120 ° C. while mixing, and the pressure was increased to 2.2 kg / cm 2.
This state was maintained for 10 minutes. Subsequently, after allowing to stand for 10 minutes, about 50 ml of each of the upper layer (condensate layer) mainly composed of condensate and the lower layer (extract layer) mainly composed of the extract is cooled, cooled to 25 ° C., and then subjected to atomic absorption spectrometry. Was used to determine the mercury content. As a result, the mercury concentration in the lower layer (extract layer) was 620 W / Vppb, and the mercury concentration in the upper layer (condensate layer) was 30 W / Vpb.
pb.
【0014】[0014]
【発明の効果】本発明によって、簡便な手段で、効率よ
く炭化水素油から水銀および水銀化合物を除去すること
ができる。According to the present invention, mercury and mercury compounds can be efficiently removed from hydrocarbon oil by simple means.
Claims (1)
る炭化水素油と、水より高沸点の有機溶媒を0.01〜
50容量%含む水溶液とを接触させて、撹拌・混合しな
がら、0.01〜10kg/cm2のゲージ圧下で、80〜1
30℃に加熱し、炭化水素油中の水銀および/または水
銀化合物を抽出することを特徴とする、炭化水素油中の
水銀および水銀化合物の除去方法。1. A hydrocarbon oil containing mercury and / or a mercury compound and an organic solvent having a boiling point higher than that of water are used in an amount of from 0.01 to
An aqueous solution containing 50% by volume is brought into contact with the solution and stirred and mixed under a gauge pressure of 0.01 to 10 kg / cm 2 to 80 to 1
A method for removing mercury and a mercury compound in a hydrocarbon oil, comprising heating to 30 ° C. to extract mercury and / or a mercury compound in the hydrocarbon oil.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3062032A JP2947369B2 (en) | 1991-03-26 | 1991-03-26 | Method for removing mercury and mercury compounds from hydrocarbon oil |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3062032A JP2947369B2 (en) | 1991-03-26 | 1991-03-26 | Method for removing mercury and mercury compounds from hydrocarbon oil |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH04296391A JPH04296391A (en) | 1992-10-20 |
JP2947369B2 true JP2947369B2 (en) | 1999-09-13 |
Family
ID=13188423
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3062032A Expired - Lifetime JP2947369B2 (en) | 1991-03-26 | 1991-03-26 | Method for removing mercury and mercury compounds from hydrocarbon oil |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2947369B2 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ATE175596T1 (en) * | 1994-07-20 | 1999-01-15 | Gfr Aufbereitung Reststoffe | METHOD FOR THE CONTINUOUS PROCESSING AND RECYCLING OF OIL AND WATER CONTAINING SOLIDS |
-
1991
- 1991-03-26 JP JP3062032A patent/JP2947369B2/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
JPH04296391A (en) | 1992-10-20 |
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