JPH01201391A - Recovery of tar acid from hydrocarbon oil containing the same - Google Patents
Recovery of tar acid from hydrocarbon oil containing the sameInfo
- Publication number
- JPH01201391A JPH01201391A JP2465288A JP2465288A JPH01201391A JP H01201391 A JPH01201391 A JP H01201391A JP 2465288 A JP2465288 A JP 2465288A JP 2465288 A JP2465288 A JP 2465288A JP H01201391 A JPH01201391 A JP H01201391A
- Authority
- JP
- Japan
- Prior art keywords
- oil
- tar
- acidic
- hydrocarbon oil
- acidic 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.)
- Pending
Links
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 18
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 18
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 17
- 239000011289 tar acid Substances 0.000 title abstract 3
- 238000011084 recovery Methods 0.000 title description 7
- 230000002378 acidificating effect Effects 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 abstract description 11
- 230000003068 static effect Effects 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000011269 tar Substances 0.000 abstract description 3
- 238000005119 centrifugation Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 239000002641 tar oil Substances 0.000 description 16
- 239000000839 emulsion Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000000926 separation method Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 239000002612 dispersion medium Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Working-Up Tar And Pitch (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
石炭乾留時に回収されるコールタールの蒸留工業におい
て、タール油の如き酸性油を含有する炭化水素油より、
酸性油を回収する方法に関する。[Detailed Description of the Invention] <Industrial Application Field> In the coal tar distillation industry recovered during coal carbonization, from hydrocarbon oil containing acidic oil such as tar oil,
Relating to a method for recovering acidic oil.
〈従来の技術〉
タール油等酸性油を含有する炭化水素油から酸性油を分
離する方法としては、タール油に苛性ソーダ水溶液など
のアルカリ液を加えて接触、混合し、酸性油を酸性油ア
ルカリ塩として水溶液側へ抽出、穆行させて分離、精製
する方法が一般的である（例えば、特公昭２４−４１１
９号公報参照）。<Prior art> A method for separating acidic oil from a hydrocarbon oil containing acidic oil such as tar oil is to add an alkaline solution such as an aqueous solution of caustic soda to tar oil, contact and mix, and convert the acidic oil into an acidic oil alkaline salt. A common method is to extract and purify the aqueous solution by separating and purifying it (for example, Japanese Patent Publication No.
(See Publication No. 9).
〈発明が解決しようとする課題〉
しかしながら、このような分離方法では、タール油とア
ルカリ液との接触、混合時の剪断力により主としてＷｌ
ｏ （油中水）型のエマルションを形成するので、炭化
水素油とアルカリ液の二相を静置分離する際の滞留時間
が短い場合には、酸性油を分離した炭化水素油の蒸留工
程において、水分混入による熱量消費及び酸性油混入に
よる純度低下の原因となるとともに、酸性油収率の低下
をひきおこす。 また、剪断力によるエマルション発生
を緩和しようとすれば、接触及び混合不足によりアルカ
リ液側への酸性油抽出収率が低下するという問題点があ
った。<Problem to be solved by the invention> However, in such a separation method, Wl is mainly
o (water-in-oil) type emulsion is formed, so if the residence time is short when statically separating the two phases of hydrocarbon oil and alkaline liquid, in the distillation process of hydrocarbon oil from which acidic oil has been separated. This causes consumption of heat due to moisture contamination and a decrease in purity due to contamination with acidic oil, as well as a decrease in acidic oil yield. Moreover, if an attempt is made to alleviate the generation of emulsion due to shearing force, there is a problem in that the extraction yield of acidic oil to the alkaline solution side decreases due to insufficient contact and mixing.
すなわち、酸性油を含有するタール浦とアルカリ液とを
接触、混合して、油水二相の分離操作を静置式で行なう
場合、酸性油のアルカリ液への移行を良好にするために
接触、混合を強化すれば剪断力が大きくなってエマルシ
ョン生成量が多くなり、エマルションがＷｌｏ（油中水
）型である故に油側に分散し、アルカリ液側の酸性油回
収率が低下し、逆に接触、混合を緩和すればエマルショ
ン量は減少するが接触、混合が不充分となり、酸性油の
回収率が低下する。 従って、工程を安定化させるため
には酸性油ロスをある程度許容して操業する必要があり
、かつ静置槽も充分大きくする必要があり経済的でない
。That is, when a tar pond containing acidic oil and an alkaline liquid are brought into contact and mixed, and an oil-water two-phase separation operation is performed in a stationary manner, the contact and mixing are carried out in order to improve the transition of the acidic oil to the alkaline liquid. If it is strengthened, the shear force will increase and the amount of emulsion produced will increase, and since the emulsion is of the WLO (water-in-oil) type, it will be dispersed on the oil side, and the recovery rate of acidic oil on the alkaline side will decrease, and conversely, the amount of emulsion produced will increase. If the mixing is relaxed, the amount of emulsion will be reduced, but the contact and mixing will be insufficient and the recovery rate of acidic oil will decrease. Therefore, in order to stabilize the process, it is necessary to operate with a certain amount of acidic oil loss allowed, and the standing tank also needs to be sufficiently large, which is not economical.
本発明者は、エマルション化した油水を遠心力を用いて
比重差を大きくして破壊することにより二相に分離でき
るという知見から、種々の遠心力及び滞留時間でタール
油及びアルカリ液のエマルションの破壊実験を試み、通
常工業的に行われる攪拌翼あるいはスタティックミキサ
ー等による混合で生成するエマルションの主要な滴径と
破壊に必要な遠心力の関係を明らかにすることにより、
酸性油回収率を向上させ、かつ分離を良好にする条件を
得た。Based on the knowledge that emulsified oil and water can be separated into two phases by increasing the difference in specific gravity using centrifugal force and breaking it, the present inventor has developed an emulsion of tar oil and alkaline liquid using various centrifugal forces and residence times. By conducting destruction experiments and clarifying the relationship between the main droplet diameters of emulsions produced by mixing using stirring blades or static mixers, which are usually carried out industrially, and the centrifugal force required for destruction,
Conditions were obtained to improve acid oil recovery and improve separation.
本発明は、遠心分離法により酸性油含有炭化水素油中の
酸性油を効率よく分離、回収する方法を提供することを
目的としている。An object of the present invention is to provide a method for efficiently separating and recovering acidic oil in acidic oil-containing hydrocarbon oil by centrifugation.
く課題を解決するための手段〉
上記目的を達成するために、本発明によれば、酸性油含
有炭化水素油にアルカリ液を加えて酸性油を酸性油アル
カリ液として抽出、分離する方法において、前記酸性油
アルカリ液を遠心分離することを特徴とする酸性油含有
炭化水素油中の酸性油の回収方法が提供される。Means for Solving the Problems> In order to achieve the above object, according to the present invention, in a method for adding an alkaline liquid to an acidic oil-containing hydrocarbon oil to extract and separate the acidic oil as an acidic oil alkaline liquid, A method for recovering acidic oil in an acidic oil-containing hydrocarbon oil is provided, which comprises centrifuging the acidic oil-alkaline solution.
以下に、本発明により酸性油を回収する方法の一例を示
すフロー図に基づき、本発明をさらに詳細に説明する。The present invention will be explained in more detail below based on a flow diagram showing an example of a method for recovering acidic oil according to the present invention.
第１図において、酸性油含有炭化水素油を原料タンク１
に入れその所定量をポンプ２によりスタティックミキサ
ー３に導入する。 アルカリ液タンク４からアルカリ液
をポンプ５によりスタティックミキサー３に導入して所
定時間攪拌、混合したのち、混合液を遠心分離機６に導
入し、６０００Ｇ以上の遠心力で混合液を脱酸炭化水素
油と酸性油塩及びアルカリ液混合物とに分離し、脱酸炭
化水素油タンク７及び混合物タンク８にそれぞれ排出す
る。In Figure 1, acidic oil-containing hydrocarbon oil is stored in raw material tank 1.
A predetermined amount of the mixture is introduced into the static mixer 3 by the pump 2. After introducing the alkaline liquid from the alkaline liquid tank 4 into the static mixer 3 using the pump 5 and stirring and mixing for a predetermined time, the mixed liquid is introduced into the centrifugal separator 6, and the mixed liquid is deoxidized into hydrocarbons using a centrifugal force of 6000 G or more. The oil is separated into an acidic oil salt and alkaline liquid mixture and discharged into a deoxidized hydrocarbon oil tank 7 and a mixture tank 8, respectively.
上記フローにおいて、スタティックミキサー３内での攪
拌、混合によって生成するエマルションは、油中に分散
する型のＷｌｏ （油中水）型エマルションであり、１
つの粒子（滴）とした時の分離速度Ｕは、ストークス式
より下記のように表わせる。In the above flow, the emulsion generated by stirring and mixing in the static mixer 3 is a Wlo (water-in-oil) emulsion that is dispersed in oil.
The separation speed U when the particles are separated into one particle (droplet) can be expressed as follows using the Stokes equation.
ここに、
Ｕ：分離速度（ｍ／ｓｅｃ ）
ｒ：滴径 （ｍ）
ρ：エマルションの密度（ｋｇ／ｍ３）ρ。：分散媒（
油）の密度（ｋｇ／ｍ’ ）η：分散媒（油）の粘度（
ｋｇ／ｍ−５ｅｃ）Ｚ：遠心力（Ｇ）
一方、遠心分離機の回転の中心から油・水二相の分離界
面までの距離をｅ （ｍ）とし、分離に必要な滞留時間
をθ（ｓｅｃ）とすれば、分離条件は下記のように表わ
せる。Here, U: Separation speed (m/sec) r: Droplet diameter (m) ρ: Emulsion density (kg/m3) ρ. : Dispersion medium (
Density (kg/m') η of dispersion medium (oil): Viscosity (oil) of dispersion medium (oil)
kg/m-5ec) Z: Centrifugal force (G) On the other hand, let the distance from the center of rotation of the centrifuge to the separation interface of the two phases of oil and water be e (m), and the residence time required for separation be θ( sec), the separation conditions can be expressed as follows.
Ｕ・θ≧ｅ ・・・・・・（２）
また、上記エマルションの破壊実験に用いた遠心分離機
のｅ値とエマルション及び分散媒であるタール油の物性
は表−１の通りであった。U・θ≧e (2) In addition, the e value of the centrifugal separator used in the above emulsion destruction experiment and the physical properties of the emulsion and the dispersion medium, tar oil, are as shown in Table 1. .
表−１
種々の遠心力及び滞留時間で実験した結果、分離良の脱
酸タール油、すなわち酸性油分及び水分を含まない脱酸
タール油が得られたものを、第２図にＯ印で示した。
なお、図中の各曲線は上記式（１）及び（２）と表−１
の値から得たものである。 また、矢印は分列良好側を
示す。Table 1 As a result of experiments with various centrifugal forces and residence times, the deacidified tar oil that was obtained with good separation, that is, the deacidified tar oil that does not contain acidic oil and water, is indicated by the O mark in Figure 2. Ta.
In addition, each curve in the figure is based on the above formulas (1) and (2) and Table 1.
It is obtained from the value of . Further, the arrow indicates the good separation side.
第２図からタール油とアルカリ液を接触、混合して生成
するエマルションの主要な滴径は４〜７μｍであり、こ
れらを分離するためには遠心力６０００Ｇ以上、滞留時
間５０秒以上を要し、好ましくは遠心力１２０００Ｇ以
上が必要であることがわかる。From Figure 2, the main droplet diameter of the emulsion produced by contacting and mixing tar oil and alkaline liquid is 4 to 7 μm, and separating them requires a centrifugal force of 6000 G or more and a residence time of 50 seconds or more. , preferably a centrifugal force of 12,000 G or more is required.
に酸性油の回収率は表−２の通りであった。The recovery rate of acidic oil was as shown in Table 2.
〈実施例〉 以下に、本発明を実施例に基づき具体的に説明する。<Example> The present invention will be specifically explained below based on Examples.
（実施例１〜３）
石炭乾留時に回収されたコールタールの分留によって得
られた酸性油を含有するタール油（比重１．０１、蒸留
範囲１９０℃〜２９０℃、酸性油分２．３重量％のもの
）と１０重量％苛性ソーダ水溶液とを第１図のフローに
従って表−２の比率で接触、混合し、遠心分離して得ら
れた脱酸タール油中の酸性油分及び水分並びに酸性油の
回収率は表−２の通りであった。(Examples 1 to 3) Tar oil containing acidic oil obtained by fractional distillation of coal tar recovered during coal carbonization (specific gravity 1.01, distillation range 190°C to 290°C, acidic oil content 2.3% by weight) Recovery of acidic oil and moisture in deacidified tar oil obtained by contacting and mixing 10% by weight caustic soda aqueous solution with a 10% by weight aqueous solution of caustic soda at the ratio shown in Table 2 according to the flow shown in Fig. 1, and centrifuging the mixture. The rates are shown in Table-2.
なお、遠心分離機のｅ値及び原料タール油の特性は表−
１の通りである。The e-value of the centrifuge and the characteristics of the raw material tar oil are shown in Table-
As per 1.
（比較例１〜２）
実施例１〜３で用いたタール油に酸性油を添加して表−
２に示す酸性油含有タール油を調製し１０重量％苛性ソ
ーダ水溶液を表−２の割合で配合して接触、混合し、３
０分間静置して得られた脱酸タール油中の酸性油分及び
水分並び実施例はいずれも比較例にくらべ原料タール油
中の酸性油が少ないにもかかわらず短時間で脱酸タール
油が得られ、かつ油中の酸性油分及び水分は共に極めて
少なく、脱酸率は極めて高率であった。(Comparative Examples 1-2) Acidic oil was added to the tar oil used in Examples 1-3 and the
Prepare tar oil containing acidic oil shown in 2 and mix with 10% by weight caustic soda aqueous solution in the proportions shown in Table 2, contact and mix.
The acidic oil content and water content in the deacidified tar oil obtained after standing for 0 minutes, and the examples are all compared to the comparative example, despite the fact that the raw material tar oil contains less acidic oil, the deacidified tar oil can be deoxidized in a short time. The acidic oil content and water content in the obtained oil were both extremely low, and the deoxidation rate was extremely high.
〈発明の効果〉
本発明は、以上説明したように構成されているので、酸
性油含有炭化水素油中の酸性油を効率よく分離、回収し
、かつ得られる脱酸炭化水素油中の酸性油分及び水分が
極めて少ないため後工程の安定操業と省熱量操業が達成
される。<Effects of the Invention> Since the present invention is configured as described above, the acidic oil in the acidic oil-containing hydrocarbon oil can be efficiently separated and recovered, and the acidic oil content in the obtained deoxidized hydrocarbon oil can be reduced. And since the water content is extremely low, stable operation and heat saving operation in the post-process can be achieved.
また、酸性油の回収率を極めて高率にできる。Moreover, the recovery rate of acidic oil can be made extremely high.
第１図は本発明の一例を示すフロー図である。
第２図は遠心分離操作における遠心力と滞留時間の関係
とエマルションの分離状態を示す図である。
符号の説明
１・・・原料タンク、 ２・・・ポンプ、３・・
・スタティックミキサー、
４・・・アルカリ液タンク、５・・・ポンプ、６・・・
遠心分離機、
７・・・脱酸炭化水素油タンク、
８・・・混合物タンク
ＦＩＧ、１
ＦＩＧ、２
違Ｉ述力（Ｇ）FIG. 1 is a flow diagram showing an example of the present invention. FIG. 2 is a diagram showing the relationship between centrifugal force and residence time in a centrifugal separation operation, and the separation state of an emulsion. Explanation of symbols 1...Raw material tank, 2...Pump, 3...
・Static mixer, 4...alkaline liquid tank, 5...pump, 6...
Centrifugal separator, 7... Deoxidized hydrocarbon oil tank, 8... Mixture tank FIG, 1 FIG, 2 Differential force (G)
Claims (1)
油を酸性油アルカリ液として抽出、分離する方法におい
て、前記酸性油アルカリ液を遠心分離することを特徴と
する酸性油含有炭化水素油中の酸性油の回収方法。(1) A method for adding an alkaline liquid to an acidic oil-containing hydrocarbon oil to extract and separate the acidic oil as an acidic oil-alkaline liquid, characterized in that the acidic oil-alkaline liquid is centrifuged. How to recover the acidic oil inside.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2465288A JPH01201391A (en) | 1988-02-04 | 1988-02-04 | Recovery of tar acid from hydrocarbon oil containing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2465288A JPH01201391A (en) | 1988-02-04 | 1988-02-04 | Recovery of tar acid from hydrocarbon oil containing the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01201391A true JPH01201391A (en) | 1989-08-14 |
Family
ID=12144071
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2465288A Pending JPH01201391A (en) | 1988-02-04 | 1988-02-04 | Recovery of tar acid from hydrocarbon oil containing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01201391A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304385A (en) * | 2011-08-12 | 2012-01-04 | 华东理工大学 | Straight-run diesel oil deacidification method and device for achieving same |
-
1988
- 1988-02-04 JP JP2465288A patent/JPH01201391A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304385A (en) * | 2011-08-12 | 2012-01-04 | 华东理工大学 | Straight-run diesel oil deacidification method and device for achieving same |
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