JP2018002937A - Recover method of oil content in crude oil sludge - Google Patents
Recover method of oil content in crude oil sludge Download PDFInfo
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本発明は、原油が貯蔵されている原油タンク内に堆積した原油スラッジ中から原油と同等の品質を有する油分を回収する方法に関する。 The present invention relates to a method for recovering an oil component having a quality equivalent to that of crude oil from crude oil sludge accumulated in a crude oil tank in which the crude oil is stored.
原油タンクに堆積した原油スラッジは、原油タンクから取り出された後、一般的には、産業廃棄物として処理されるが、その廃棄処理には高い費用を要する。一方で、原油スラッジは、多くの場合３０〜８０体積％程度の油分を含んでいるため、原油スラッジ中の油分の回収のニーズも大きい。 After the crude oil sludge accumulated in the crude oil tank is taken out from the crude oil tank, it is generally treated as industrial waste, but its disposal requires high costs. On the other hand, since crude oil sludge often contains about 30 to 80% by volume of oil, there is a great need for recovery of oil in crude oil sludge.
そこで、従来、真空蒸留法、加熱分離法、遠心分離法等により、原油スラッジから油分を回収する試みが行われてきた（例えば、特許文献１〜３）。 Thus, conventionally, attempts have been made to recover oil from crude oil sludge by vacuum distillation, heating separation, centrifugation, or the like (for example, Patent Documents 1 to 3).
しかし、上記の方法、例えば、真空蒸留法や加熱分離法では設備投資が大規模になる。また、遠心分離法は小規模な設備投資で実施出来るが、原油と同程度の品質を有する油分を回収するためには、多量の油分溶解用の炭化水素で希釈する必要があり、分離工程での処理量が増加し、経済性の低下を招く。そのため、原油スラッジから遠心分離法を用いて回収された油分は、直接、安価な燃料油として使用されることが多い。 However, capital investment is large in the above-described methods, for example, the vacuum distillation method and the heat separation method. In addition, the centrifugal separation method can be implemented with small-scale capital investment, but in order to recover an oil component having the same quality as that of crude oil, it is necessary to dilute with a large amount of hydrocarbon for dissolving the oil component. The processing amount increases, and the economic efficiency decreases. Therefore, oil recovered from crude oil sludge using a centrifugal separation method is often used directly as an inexpensive fuel oil.
ここで、原油スラッジから回収した油分を原油に混合すれば、安価な燃料油ではなく、より価格の高い原油として販売することが可能となる。ところが、本発明者らが検討したところ、原油スラッジから遠心分離法を用いて回収した油分は、高分子炭化水素からなるアスファルテンや残留炭素分を多く含んでいるため、石油精製プロセスにおいて処理される原油に、原油スラッジから回収した油分を原油に混合すると、熱交換器や配管の汚れの原因となることが分かった。 Here, if the oil component recovered from the crude oil sludge is mixed with the crude oil, it can be sold as a crude oil having a higher price rather than an inexpensive fuel oil. However, as a result of studies by the present inventors, oil recovered from crude sludge using a centrifugal separation method is processed in an oil refining process because it contains a large amount of asphaltene and residual carbon that are composed of polymer hydrocarbons. It was found that mixing the crude oil with the oil recovered from the crude oil sludge causes the heat exchanger and piping to become dirty.
従って、本発明の課題は、油分溶解用の炭化水素の使用量を抑えながら、且つ原油スラッジから回収した油分中に含まれる高分子炭化水素含有量を原油品質と同等まで少なくすることができる原油スラッジ中の油分の回収方法を提供することにある。 Accordingly, an object of the present invention is to provide a crude oil capable of reducing the content of polymer hydrocarbons contained in oil recovered from crude oil sludge to the same level as that of crude oil while suppressing the amount of hydrocarbon used for oil dissolution. An object of the present invention is to provide a method for recovering oil in sludge.
上記課題は、以下の本発明により解決される。
すなわち、本発明は、油分を含有する原油スラッジ（Ａ）から油分を回収する方法であって、該原油スラッジ（Ａ）に、芳香族性指数が２０以下の油分溶解用炭化水素（Ｂ）を混合し、原油スラッジ（Ａ）と該油分溶解用炭化水素（Ｂ）との混合物を６０〜９５℃で加熱攪拌し、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）との加熱攪拌処理物を得る第一工程と、該加熱攪拌処理物を遠心分離することにより、軽液と重分とを分離して、軽液を得る第二工程と、を有することを特徴とする原油スラッジ中の油分の回収方法を提供するものである。
The above problems are solved by the present invention described below.
That is, the present invention is a method for recovering oil from crude oil sludge (A) containing oil, wherein the crude oil sludge (A) is provided with an oil-dissolving hydrocarbon (B) having an aromaticity index of 20 or less. Mix, heat and stir the mixture of crude oil sludge (A) and the oil-dissolving hydrocarbon (B) at 60-95 ° C., and heat and stir the crude oil sludge (A) and the oil-dissolving hydrocarbon (B). In a crude oil sludge comprising: a first step of obtaining a product; and a second step of separating a light liquid and a heavy component by centrifuging the heat-stirred product to obtain a light liquid. A method for recovering the oil content is provided.
本発明によれば、油分溶解用の炭化水素の使用量を抑えながら、且つ原油スラッジから回収した油分中に含まれる高分子炭化水素含有量を原油品質と同等まで少なくすることができる原油スラッジ中の油分の回収方法を提供することができる。そのため、本発明によれば、石油精製プロセス中に、原油スラッジから回収した油分を混合させても、石油精製プロセスにおける汚れが発生し難い原油スラッジ中の油分の回収方法を提供することができる。 According to the present invention, in the crude oil sludge that can reduce the amount of hydrocarbons used for dissolving oil components and reduce the polymer hydrocarbon content contained in the oil recovered from the crude oil sludge to the same level as the crude oil quality. It is possible to provide a method for recovering oil. Therefore, according to the present invention, it is possible to provide a method for recovering oil content in crude oil sludge that hardly causes contamination in the oil refining process even if the oil content recovered from the crude oil sludge is mixed during the oil refining process.
本発明の原油スラッジ中の油分の回収方法は、油分を含有する原油スラッジ（Ａ）から油分を回収する方法であって、該原油スラッジ（Ａ）に、芳香族性指数が２０以下の油分溶解用炭化水素（Ｂ）を混合し、原油スラッジ（Ａ）と該油分溶解用炭化水素（Ｂ）との混合物を６０〜９５℃で加熱攪拌し、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）との加熱攪拌処理物を得る第一工程と、該加熱攪拌処理物を遠心分離することにより、軽液と重分とを分離して、軽液を得る第二工程と、を有することを特徴とする原油スラッジ中の油分の回収方法である。 The method for recovering oil in crude sludge of the present invention is a method for recovering oil from crude oil sludge (A) containing oil, wherein the oil is dissolved in crude oil sludge (A) with an aromaticity index of 20 or less. Hydrocarbon sludge (A) and oil-dissolving hydrocarbon (B) are mixed by heating and stirring a mixture of crude oil sludge (A) and the oil-dissolving hydrocarbon (B) at 60 to 95 ° C. B) having a first step for obtaining a heat-stirred product and a second step for separating a light liquid and a heavy component by centrifuging the heat-stirred product to obtain a light liquid. This is a method for recovering oil content in crude oil sludge.
本発明の原油スラッジ中の油分の回収方法に係る第一工程は、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）とを混合し、次いで、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物を加熱撹拌して、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の加熱撹拌処理物を得る工程である。 The first step according to the method for recovering oil in the crude oil sludge of the present invention is to mix crude oil sludge (A) and oil-dissolving hydrocarbon (B), and then crude oil sludge (A) and oil-dissolving hydrocarbon. In this step, the mixture of (B) is heated and stirred to obtain a heated and stirred product of crude oil sludge (A) and oil-dissolving hydrocarbon (B).
第一工程に係る原油スラッジ（Ａ）は、原油が貯蔵されている原油中から発生し、原油タンクの底に堆積したスラッジである。原油スラッジ（Ａ）としては、原油採掘後に固形分や水分等が除去されて原油タンクに貯蔵され、製油所に出荷される前の原油タンク中の原油から発生し、原油タンクの底部に堆積した原油スラッジ；原油タンカーの原油タンクの底部に堆積した原油スラッジ；製油所で精製される前の貯蔵用の原油タンク中の原油から発生し、原油タンクの底部に堆積した原油スラッジ等が挙げられる。原油スラッジ（Ａ）は、１種類の原油から生成したものであってもよいし、複数種の原油から生成したものであってもよい。 Crude oil sludge (A) according to the first step is sludge generated from the crude oil in which the crude oil is stored and deposited on the bottom of the crude oil tank. Crude oil sludge (A) is removed from solids, moisture, etc. after crude oil extraction, stored in a crude oil tank, generated from crude oil in the crude oil tank before being shipped to a refinery, and deposited at the bottom of the crude oil tank Crude oil sludge; crude oil sludge accumulated at the bottom of a crude oil tank of a crude oil tanker; crude oil sludge generated from crude oil in a crude oil tank for storage before being refined at a refinery, and deposited at the bottom of the crude oil tank. Crude oil sludge (A) may be generated from one type of crude oil or may be generated from a plurality of types of crude oil.
原油スラッジ（Ａ）は、油分、アスファルテン、鉄分、砂、水等を含有している。原油スラッジ（Ａ）中の油分は、主に、炭素数４０以上のパラフィン及び芳香族炭化水素である。そして、この原油スラッジ（Ａ）中の油分が、本発明の原油スラッジ中の油分の回収方法により、原油スラッジ（Ａ）中から回収される成分である。 Crude oil sludge (A) contains oil, asphaltene, iron, sand, water and the like. The oil in the crude oil sludge (A) is mainly paraffins and aromatic hydrocarbons having 40 or more carbon atoms. And the oil content in this crude oil sludge (A) is a component collect | recovered from crude oil sludge (A) by the recovery method of the oil content in the crude oil sludge of this invention.
原油タンク内に堆積した原油スラッジ（Ａ）を、原油タンク外へ取り出す方法としては、特に制限されず、例えば、原油タンク内の原油を原油タンク外へ抜き出した後に、原油タンク内に堆積した原油スラッジ（Ａ）に高圧の原油を噴射し、破砕又は一部溶解した原油スラッジ（Ａ）を原油で原油タンク外へ押し出す方法（ＣＯＷ：Ｃｒｕｄｅ Ｏｉｌ Ｗａｓｈｉｎｇ）、原油タンク内の原油を原油タンク外へ抜き出した後に、人手により、原油タンク内に堆積した原油スラッジ（Ａ）を取り出す方法等が挙げられる。また、このようなＣＯＷ洗浄では、原油スラッジを原油タンク外へ押し出すために、原油に代えて、灯軽油が用いられることもある。 The method of taking out the crude oil sludge (A) deposited in the crude oil tank is not particularly limited. For example, the crude oil deposited in the crude oil tank after the crude oil in the crude oil tank is extracted out of the crude oil tank. A method of injecting high-pressure crude oil into sludge (A) and pushing crushed or partially dissolved crude oil sludge (A) out of the crude oil tank with crude oil (COW: Crude Oil Washing). Crude oil in the crude oil tank is taken out of the crude oil tank. Examples include a method of manually extracting the crude oil sludge (A) accumulated in the crude oil tank after the extraction. In such COW cleaning, kerosene oil may be used instead of crude oil in order to push crude sludge out of the crude oil tank.
油分溶解用炭化水素（Ｂ）は、芳香族性指数が２０以下、好ましくは０〜１５である。油分溶解用炭化水素（Ｂ）の芳香族性指数が、上記範囲にあることにより、原油スラッジから回収した油分中に含まれる高分子炭化水素含有量を原油品質と同等まで少なくすることができる。 The oil-dissolving hydrocarbon (B) has an aromaticity index of 20 or less, preferably 0 to 15. When the aromaticity index of the oil-dissolving hydrocarbon (B) is within the above range, the content of the high-molecular hydrocarbon contained in the oil recovered from the crude oil sludge can be reduced to the same level as the crude oil quality.
油分溶解用炭化水素（Ｂ）としては、例えば、芳香族指数が２０以下、好ましくは０〜１５のコンデンセート、灯軽油、パラフィン溶剤、原油等が挙げられる。芳香族指数が２０以下、好ましくは０〜１５であれば、原油も、油分溶解用炭化水素として用いることができる。 Examples of the oil-dissolving hydrocarbon (B) include condensate, kerosene oil, paraffin solvent, and crude oil having an aromatic index of 20 or less, preferably 0 to 15. If the aromatic index is 20 or less, preferably 0 to 15, crude oil can also be used as the oil-dissolving hydrocarbon.
原油スラッジ（Ａ）と混合する油分溶解用炭化水素（Ｂ）は、芳香族性指数が２０以下、好ましくは０〜１５であれば特に制限されない。例えば、油分溶解用炭化水素（Ｂ）として原油を用いる場合、油分溶解用炭化水素（Ｂ）として用いる原油としては、原油採掘後に固形分や水分等を除去し原油タンクに貯蔵する前の原油であってもよいし、原油採掘後に固形分や水分等を除去し原油タンクに貯蔵し間もない原油であり、原油スラッジが発生する前の原油であってもよいし、一定期間原油タンクに貯蔵することにより、原油タンクの底部に原油スラッジが発生した後の、原油タンク内の上澄みの原油であってもよい。 The oil-dissolving hydrocarbon (B) mixed with the crude oil sludge (A) is not particularly limited as long as the aromaticity index is 20 or less, preferably 0 to 15. For example, when crude oil is used as the oil-dissolving hydrocarbon (B), the crude oil used as the oil-dissolving hydrocarbon (B) is the crude oil before removing solids and moisture after the crude oil is mined and storing it in the crude oil tank. It may be a crude oil that has been solidly removed after being extracted and stored in a crude oil tank. It may be a crude oil before crude oil sludge is generated, or it may be stored in a crude oil tank for a certain period of time. Thus, the crude oil in the crude oil tank after the crude oil sludge is generated at the bottom of the crude oil tank may be used.
なお、原油スラッジ（Ａ）を原油タンクから取り出すときに、原油や灯軽油で原油スラッジ（Ａ）を原油タンク外へ押し出すこと（例えば、ＣＯＷ洗浄）により、原油スラッジ（Ａ）を取り出した場合、原油タンクから取り出されたものは、原油スラッジ（Ａ）と原油スラッジ（Ａ）の取り出しに用いられた原油又は灯軽油の混合物であるが、この場合、原油スラッジ（Ａ）の取り出しに用いられた原油又は灯軽油は、油分溶解用炭化水素（Ｂ）に含まれる。 When removing crude oil sludge (A) from the crude oil tank, the crude oil sludge (A) is taken out by pushing the crude oil sludge (A) out of the crude oil tank with crude oil or kerosene (for example, COW cleaning). What was taken out from the crude oil tank is a mixture of crude oil or kerosene used to take out crude oil sludge (A) and crude oil sludge (A). In this case, it was used to take out crude oil sludge (A). Crude oil or kerosene oil is included in the hydrocarbon for dissolving oil (B).
第一工程においては、先ず、原油スラッジ（Ａ）及び油分溶解用炭化水素（Ｂ）を混合する。その時、混合物に対する原油スラッジ（Ａ）の割合（（Ａ／（Ａ＋Ｂ））×１００）に制約はないが、好ましくは２０〜９０質量％、更に好ましくは２５〜７０質量％、となるように、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）とを混合する。原油スラッジ（Ａ）及び油分溶解用炭化水素（Ｂ）の合計に対する原油スラッジ（Ａ）の割合が、上記範囲未満だと、第二工程における処理量が増加し、経済性の低下を招き、また、上記範囲を超えると、原油スラッジからの油分の回収が不十分となる。 In the first step, first, crude oil sludge (A) and hydrocarbon for dissolving oil (B) are mixed. At that time, the ratio of crude oil sludge (A) to the mixture ((A / (A + B)) × 100) is not limited, but preferably 20 to 90% by mass, more preferably 25 to 70% by mass, Crude oil sludge (A) and oil-dissolving hydrocarbon (B) are mixed. If the ratio of crude oil sludge (A) to the total of crude oil sludge (A) and oil-dissolving hydrocarbon (B) is less than the above range, the throughput in the second step will increase, leading to a decrease in economic efficiency, If the above range is exceeded, recovery of oil from the crude oil sludge becomes insufficient.
なお、原油スラッジ（Ａ）を原油タンクから取り出すときに、原油や灯軽油で原油スラッジ（Ａ）を原油タンク外へ押し出すこと（例えば、ＣＯＷ洗浄）により、原油スラッジ（Ａ）を取り出した場合、原油スラッジ（Ａ）の取り出しに用いられた原油や灯軽油を、油分溶解用炭化水素（Ｂ）に含めて、原油スラッジ（Ａ）及び油分溶解用炭化水素（Ｂ）の合計に対する原油スラッジ（Ａ）の割合を算出する。そのため、この場合、原油タンクの底部に堆積している原油スラッジ（Ａ）及び原油スラッジ（Ａ）の取り出しに用いる油分溶解用炭化水素（Ｂ）の合計に対する原油スラッジ（Ａ）の割合が、所定の混合割合、すなわち、原油スラッジ（Ａ）及び油分溶解用炭化水素（Ｂ）の合計に対する原油スラッジ（Ａ）の割合が、好ましくは２０〜９０質量％、更に好ましくは２５〜７０質量％となる量の原油又は灯軽油（油分溶解用炭化水素（Ｂ））を用いて、原油スラッジ（Ａ）を原油タンク外へ取出し、取り出した原油スラッジ（Ａ）と原油スラッジの取り出しに用いた原油又は灯軽油の混合物を、そのまま撹拌に用いる原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物としてもよい。あるいは、原油タンクの底部に堆積している原油スラッジ（Ａ）を、少量の原油又は灯軽油（油分溶解用炭化水素（Ｂ））を用いて、原油タンク外へ取出し、取り出した原油スラッジ（Ａ）と原油スラッジの取り出しに用いた原油又は灯軽油の混合物に、更に、原油スラッジ（Ａ）の取り出しに用いた原油又は灯軽油と同じ種類の原油又は灯軽油、あるいは、異なる種類の原油又は灯軽油を混合して、所定の混
合割合、すなわち、原油スラッジ（Ａ）及び油分溶解用炭化水素（Ｂ）の合計に対する原油スラッジ（Ａ）の割合が、好ましくは２０〜９０質量％、更に好ましくは２５〜７０質量％にして、得られる混合物を、撹拌に用いる原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物としてもよい。
When removing crude oil sludge (A) from the crude oil tank, the crude oil sludge (A) is taken out by pushing the crude oil sludge (A) out of the crude oil tank with crude oil or kerosene (for example, COW cleaning). The crude oil and kerosene oil used to extract the crude oil sludge (A) is included in the oil-dissolving hydrocarbon (B), and the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) are added to the sum of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B). ) Is calculated. Therefore, in this case, the ratio of the crude oil sludge (A) to the total of the crude oil sludge (A) accumulated at the bottom of the crude oil tank and the oil-dissolving hydrocarbon (B) used for taking out the crude oil sludge (A) is predetermined. The ratio of the crude oil sludge (A) to the total of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) is preferably 20 to 90 mass%, more preferably 25 to 70 mass%. Crude oil or kerosene oil (hydrocarbon for oil dissolution (B)) is used to take crude oil sludge (A) out of the crude oil tank, and the extracted crude oil sludge (A) and the crude oil or light used to remove the crude oil sludge. A mixture of light oils may be a mixture of crude oil sludge (A) used for stirring as it is and oil-dissolving hydrocarbon (B). Alternatively, the crude oil sludge (A) deposited at the bottom of the crude oil tank is taken out of the crude oil tank using a small amount of crude oil or kerosene oil (oil-dissolving hydrocarbon (B)) and taken out. ) And crude oil or kerosene used for the removal of crude oil sludge, and further, the same type of crude oil or kerosene as the crude oil or kerosene used for removal of crude oil sludge (A), or a different type of crude oil or kerosene. Mixing light oil, the ratio of the crude sludge (A) to the predetermined mixing ratio, that is, the total of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) is preferably 20 to 90% by mass, more preferably It is good also considering it as 25-70 mass%, and making the mixture obtained the mixture of the crude oil sludge (A) used for stirring, and the hydrocarbon for oil-dissolving (B).
第一工程では、次いで、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）との混合物を、６０〜９５℃で加熱撹拌し、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）との加熱撹拌処理物を得る。原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）との混合物を加熱撹拌する際の加熱温度は、６０〜９５℃、好ましくは７０〜９０℃である。加熱撹拌の際の加熱温度が、上記範囲未満だと、原油スラッジ（Ａ）からの油分の回収が不十分となり、また、上記範囲を超えると、軽質留分の損失によるデメリットが発生する。原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物を加熱撹拌する方法としては、特に制限されず、例えば、原油タンクから取り出された原油スラッジ（Ａ）が貯留されるタンク内で、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物を加熱及び撹拌し、次いで、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物を、タンク外へ取出してから、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）を混合する方法が挙げられる。加熱撹拌時間は、特に制限されず、均一な混合状態となるよう、撹拌条件に応じて選択される。 Next, in the first step, a mixture of crude oil sludge (A) and oil-dissolving hydrocarbon (B) is heated and stirred at 60 to 95 ° C. to obtain crude oil sludge (A) and oil-dissolving hydrocarbon (B). To obtain a heated and stirred product. The heating temperature when heating and stirring the mixture of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) is 60 to 95 ° C, preferably 70 to 90 ° C. When the heating temperature at the time of heating and stirring is less than the above range, the recovery of oil from the crude oil sludge (A) becomes insufficient, and when it exceeds the above range, disadvantages due to loss of light fractions occur. The method for heating and stirring the mixture of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) is not particularly limited. For example, in the tank in which the crude oil sludge (A) taken out from the crude oil tank is stored, The mixture of crude oil sludge (A) and oil-dissolving hydrocarbon (B) is heated and stirred, and then the crude oil sludge (A) and oil-dissolving hydrocarbon (B) mixture is taken out of the tank, and then crude oil A method of mixing the sludge (A) and the oil-dissolving hydrocarbon (B) may be mentioned. The heating and stirring time is not particularly limited and is selected according to the stirring conditions so as to obtain a uniform mixed state.
原油スラッジ（Ａ）中の油分の含有量は、特に制限されないが、通常、３０〜８０質量％である。そして、この原油スラッジ（Ａ）中の油分は、第一工程において、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物を、６０〜９５℃、好ましくは７０〜９０℃で加熱撹拌することにより、油分溶解用炭化水素（Ｂ）に溶解する。 Although content in particular of oil content in crude oil sludge (A) is not restrict | limited, Usually, it is 30-80 mass%. In the first step, the oil in the crude oil sludge (A) is a mixture of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) at 60 to 95 ° C, preferably 70 to 90 ° C. As a result, the oil is dissolved in the hydrocarbon for dissolving oil (B).
本発明の原油スラッジ中の油分の回収方法に係る第二工程は、第一工程を行い得られた原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の加熱撹拌処理物を、６０〜９５℃で遠心分離することにより、軽液と重分とを分離して、軽液を得る工程である。 In the second step according to the method for recovering oil in the crude oil sludge of the present invention, the heated and stirred processed product of crude oil sludge (A) and oil-dissolving hydrocarbon (B) obtained by performing the first step is 60 to 95. This is a step of obtaining a light liquid by separating the light liquid and the heavy liquid by centrifugation at 0 ° C.
第二工程において、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の加熱撹拌処理物の遠心分離を行うときの温度は、６０〜９５℃、好ましくは７０〜９０℃である。遠心分離温度が、上記範囲未満だと、遠心分離中に、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の加熱撹拌処理物の一部が凝固したり、加熱撹拌処理物の流動性が大きく低下したりするため、遠心分離が行えなくなり、また、上記範囲を超えると、軽質留分の損失によるデメリットが発生する。また、第二工程において、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の加熱撹拌処理物の遠心分離を行うときの温度は、第一工程における、原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の混合物の加熱撹拌温度と同程度にする。 In the second step, the temperature at which the heated and stirred processed product of crude oil sludge (A) and oil-dissolving hydrocarbon (B) is centrifuged is 60 to 95 ° C, preferably 70 to 90 ° C. If the centrifugal separation temperature is less than the above range, during the centrifugal separation, a part of the heat-stirred treated product of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) is solidified or the fluidity of the heat-stirred treated product. Or the like, the centrifugal separation cannot be performed, and if it exceeds the above range, a demerit due to loss of the light fraction occurs. In the second step, the temperature at which the heated and stirred processed product of the crude oil sludge (A) and the oil-dissolving hydrocarbon (B) is centrifuged is the same as that used for the crude oil sludge (A) and oil-dissolving in the first step. The heating and stirring temperature of the hydrocarbon (B) mixture is set to the same level.
第一工程を行い得られる原油スラッジ（Ａ）と油分溶解用炭化水素（Ｂ）の加熱撹拌処理物は、比重が小さい軽液と軽液より比重が大きい重分の混合物であり、第二工程では、比重差により軽液と重分とを分離する。そして、軽液は、第一工程で原油スラッジ（Ａ）中の油分が油分溶解用炭化水素（Ｂ）に溶解することにより得られる液体である。つまり、軽液は、基本的に油分溶解用炭化水素（Ｂ）と油分溶解用炭化水素（Ｂ）に溶解した原油スラッジ（Ａ）中の油分とからなる。重分は、第一工程で油分溶解用炭化水素（Ｂ）には溶解しなかった原油スラッジ（Ａ）中の成分であり、主に、アスファルテン、ワックス、水分、鉄分、砂、及びこれら成分に抱き込まれて分離され難い状態にある油分などである。 The heat-stirred processed product of crude oil sludge (A) and oil-dissolving hydrocarbon (B) obtained by performing the first step is a mixture of a light liquid having a small specific gravity and a heavy component having a specific gravity larger than that of the light liquid. Then, the light liquid and the heavy component are separated by the specific gravity difference. The light liquid is a liquid obtained by dissolving the oil in the crude oil sludge (A) in the oil-dissolving hydrocarbon (B) in the first step. That is, the light liquid basically consists of the oil in the crude oil sludge (A) dissolved in the oil-dissolving hydrocarbon (B) and the oil-dissolving hydrocarbon (B). The heavy component is a component in the crude oil sludge (A) that was not dissolved in the oil-dissolving hydrocarbon (B) in the first step, and mainly contains asphaltene, wax, moisture, iron, sand, and these components. For example, oil that is embraced and difficult to separate.
第二工程において、加熱撹拌処理物を遠心分離するための遠心分離装置としては、特に制限されず、上記遠心分離温度を保ったまま、連続的に軽液と重分とを、比重の差により分離できるものであればよい。例えば、デカンター式遠心分離機、ディスクセパレータ式遠心分離機、又はこれらを組み合わせた遠心分離機が挙げられる。 In the second step, the centrifuge for centrifuging the heated and stirred product is not particularly limited, and the light liquid and the heavy component are continuously separated by the difference in specific gravity while maintaining the above-mentioned centrifugation temperature. Any material that can be separated is acceptable. For example, a decanter type centrifuge, a disk separator type centrifuge, or a combination of these is available.
第二工程を行い得られる軽液の物性は、特に制限されないが、密度は好ましくは０．８０〜０．９５ｇ／ｃｍ３、より好ましくは０．８０〜０．９０ｇ／ｃｍ３であり、融点は好ましくは４０〜１５０℃、より好ましくは４０〜１１０℃、さらに好ましくは４０〜９０℃であり、凝固点は好ましくは３０〜１４０℃、より好ましくは３０〜１００℃、さらに好ましくは３０〜８０℃であり、油分含有量は６０質量％以上である。 Although the physical properties of the light liquid obtained by performing the second step are not particularly limited, the density is preferably 0.80 to 0.95 g / cm 3 , more preferably 0.80 to 0.90 g / cm 3 , and the melting point Is preferably 40 to 150 ° C, more preferably 40 to 110 ° C, still more preferably 40 to 90 ° C, and the freezing point is preferably 30 to 140 ° C, more preferably 30 to 100 ° C, and further preferably 30 to 80 ° C. The oil content is 60% by mass or more.
そして、本発明の原油スラッジ中の油分の回収方法では、第二工程を行い得られる軽液を、原油（Ｃ）に混合することにより、原油スラッジ中の油分を再利用することができる。第二工程を行い得られる軽液を、原油（Ｃ）に混合する方法としては、特に制限されず、例えば、原油（Ｃ）の移送管中に、軽液を導入する方法や、原油（Ｃ）の原油タンクに軽液を供給する方法等が挙げられる。 And in the recovery method of the oil content in the crude oil sludge of this invention, the oil content in a crude oil sludge can be reused by mixing the light liquid obtained by performing a 2nd process with a crude oil (C). The method of mixing the light liquid obtained by performing the second step with the crude oil (C) is not particularly limited. For example, a method of introducing the light liquid into the crude oil (C) transfer pipe or the crude oil (C ) To supply light liquid to the crude oil tank.
第二工程を行い得られる軽液を混合する原油（Ｃ）は、特に制限されず、原油採掘後に固形分や水分等を除去し原油タンクに貯蔵する前の原油であってもよいし、原油採掘後に固形分や水分等を除去し原油タンクに貯蔵し間もない原油であり、原油スラッジが発生する前の原油であってもよいし、一定期間原油タンクに貯蔵することにより、原油タンクの底部に原油スラッジが発生した後の、原油タンク内の上澄みの原油であってもよい。原油（Ｃ）は、原油スラッジ（Ａ）の生成源の原油と同じ種類の原油であっても、異なる種類の原油であってもよく、また、油分溶解用炭化水素（Ｂ）として原油を用いた場合、その原油と同じ種類の原油であっても、異なる種類の原油であってもよい。 The crude oil (C) mixed with the light liquid obtained by performing the second step is not particularly limited, and may be crude oil before removing solids or moisture after storing the crude oil and storing it in the crude oil tank. It is crude oil that has been solidly removed after being mined and has been stored in a crude oil tank. It may be crude oil before crude oil sludge is generated, or it can be stored in a crude oil tank for a certain period of time. It may be the crude oil in the crude oil tank after the crude oil sludge is generated at the bottom. Crude oil (C) may be the same type of crude oil as the source of crude oil sludge (A) or a different type of crude oil, and crude oil is used as the oil-dissolving hydrocarbon (B). In this case, the crude oil may be the same type of crude oil or a different type of crude oil.
軽液を原油移送管内の原油（Ｃ）に導入する方法としては、ラインミキシング、スタティックミキサー、インジェクションノズル、ミキシングバルブ等による混合が挙げられる。 Examples of the method for introducing the light liquid into the crude oil (C) in the crude oil transfer pipe include mixing by line mixing, a static mixer, an injection nozzle, a mixing valve, and the like.
本発明の原油スラッジ中の油分の回収方法では、原油スラッジ中の油分を溶解させるものとして、芳香族性指数が２０以下、好ましくは０〜１５の油分溶解用炭化水素を用いて、原油スラッジ中の油分を該油分溶解用炭化水素に溶解させた後、遠心分離を行って軽液を得ることにより、油分溶解用の炭化水素の使用量を抑えながら、且つ、原油スラッジから回収した油分中に含まれる高分子炭化水素含有量を原油品質と同等まで少なくすることができる。そのため、本発明の原油スラッジ中の油分の回収方法によれば、石油精製プロセス中の原油に、原油スラッジから回収した油分を混合させても、言い換えると、石油精製プロセス中の原油に、油分溶解用炭化水素（Ｂ）に原油スラッジ（Ａ）中の油分を溶解させた後、遠心分離して得られる軽液を混合させても、石油精製プロセスにおける汚れを発生し難くすることができる。 In the method for recovering oil content in crude oil sludge according to the present invention, as the oil content in crude oil sludge is dissolved, an aromaticity index of 20 or less, preferably 0-15, is used to dissolve the oil content. In the oil recovered from the crude oil sludge, the amount of the oil is dissolved in the oil-dissolving hydrocarbon, and then centrifuged to obtain a light liquid. The polymer hydrocarbon content can be reduced to the same level as crude oil quality. Therefore, according to the method for recovering oil in crude oil sludge according to the present invention, even if the oil recovered from the crude oil sludge is mixed with the crude oil in the oil refining process, in other words, the oil is dissolved in the crude oil in the oil refining process. Even if the oil in the crude oil sludge (A) is dissolved in the hydrocarbon (B) for use, and then mixed with a light liquid obtained by centrifugation, it is possible to make it difficult to generate dirt in the petroleum refining process.
なお、本発明において、油分溶解用炭化水素（Ｂ）の芳香族性指数は、ＮＭＲ分析により確認される。具体的には、ピーク位置が０〜６０ｐｐｍのピークを脂肪族炭化水素のピークとして、１００〜１７０ｐｐｍのピークを芳香族性炭化水素のピークとして、それぞれの範囲に存在するピークのピーク面積を積算し、芳香族性炭化水素のピーク面積と脂肪族炭化水素のピーク面積の合計に対する、芳香族性炭化水素のピーク面積の百分率（（芳香族性炭化水素のピーク面積／（芳香族性炭化水素のピーク面積＋脂肪族炭化水素のピーク面積））×１００）を計算することにより、芳香族性指数を求めることが出来る。 In the present invention, the aromaticity index of the oil-dissolving hydrocarbon (B) is confirmed by NMR analysis. Specifically, the peak positions of 0 to 60 ppm are regarded as aliphatic hydrocarbon peaks, and the peak of 100 to 170 ppm is regarded as an aromatic hydrocarbon peak, and the peak areas of the peaks existing in the respective ranges are integrated. The percentage of the peak area of the aromatic hydrocarbon relative to the sum of the peak area of the aromatic hydrocarbon and the peak area of the aliphatic hydrocarbon ((peak area of the aromatic hydrocarbon / (peak of the aromatic hydrocarbon The aromaticity index can be obtained by calculating the area + the peak area of the aliphatic hydrocarbon)) × 100).
以下に実施例を示して本発明を更に具体的に説明するが、本発明はこれに制限されるものではない。 The present invention will be described more specifically with reference to the following examples, but the present invention is not limited thereto.
＜ＮＭＲ分析＞
装置：ＥＣＸ４００
測定ファイル：１３Ｃ ＮＭＲ ＮＮＥ．ｅｘ２
共鳴周波数：１００ＭＨｚ
観測範囲：２５ＫＨｚ（２５０ｐｐｍ）
データポイント：３２Ｋ
パルス幅：５．２３μ秒（４５°パルス）
パルス待ち時間：８秒
レシーバーゲイン：オートゲイン
積算回数：５０００
各試料を約２００ｍｇ採取した後、重クロロホルム（ＣＤＣｌ３）０．６ｍＬで溶解させ、５ｍｍφの試料管に採取した。原油スラッジ中の油分の溶解に用いた原油ｂと原油ｘのＮＭＲ分析の結果を図１及び図２に示す。
<NMR analysis>
Device: ECX400
Measurement file: 13C NMR NNE. ex2
Resonance frequency: 100 MHz
Observation range: 25 KHz (250 ppm)
Data point: 32K
Pulse width: 5.23 μs (45 ° pulse)
Pulse waiting time: 8 seconds Receiver gain: Auto gain integration count: 5000
About 200 mg of each sample was collected, dissolved in 0.6 mL of deuterated chloroform (CDCl 3 ), and collected in a 5 mmφ sample tube. The results of NMR analysis of crude oil b and crude oil x used for dissolving oil in the crude oil sludge are shown in FIGS.
＜原油スラッジ（Ａ）＞
原油タンクから回収された原油スラッジ
分析値：油分６４．３、質量％、アスファルテン１１．４質量％、水分２１．０質量％、セジメント分３．３質量％、芳香族性指数２２
＜スラッジ中の油分溶解用の原油（油分溶解用炭化水素（Ｂ））＞
ＮＭＲ分析結果が図１であり、以下の分析値を有する原油ｂ
ＡＰＩ ５２．２°、アスファルテン０．０２質量％、セジメント分０．０質量％、水分０．０質量％、芳香族性指数１２
＜スラッジ中の油分溶解用の原油＞
ＮＭＲ分析結果が図２であり、以下の分析値を有する原油ｘ
ＡＰＩ ３７．９°、アスファルテン１．５質量％ 、セジメント分０．０質量％、水分０．０質量％、芳香族性指数２２
<Crude oil sludge (A)>
Crude oil sludge recovered from crude oil tank
Analytical values: oil content 64.3, mass%, asphaltene 11.4 mass%, moisture 21.0 mass%, sediment content 3.3 mass%, aromaticity index 22
<Crude oil for dissolving oil in sludge (hydrocarbon for dissolving oil (B))>
The result of NMR analysis is FIG. 1 and crude oil b having the following analysis values
API 52.2 °, 0.02% by weight of asphaltene, 0.0% by weight of sediment, 0.0% by weight of moisture, aromaticity index 12
<Crude oil for dissolving oil in sludge>
FIG. 2 shows the NMR analysis result, and crude oil x having the following analysis values
API 37.9 °, asphaltene 1.5% by mass, sediment content 0.0% by mass, moisture 0.0% by mass, aromaticity index 22
(実施例１〜２)
原油スラッジａと原油ｂとを、その合計に対する原油スラッジａが表１に示す割合になるように撹拌容器に加え、混合物を８０℃で加熱撹拌した。
次いで、８０℃を保ったまま、加熱撹拌処理物を、８０℃に設定された遠心分離器に入れ、８０℃、１０００Ｇ、１分間の条件で、遠心分離を行った。
次いで、デカンテーションにより、軽液を分離し、軽液を得た。得られた軽液の分析値を表１に示す。表１の結果から、各スラッジ溶解用の原油や組成による影響を除いた軽液の算出値を表２に示す。なお、以下のように計算して、表２の値を算出した。表１に記載した軽液組成に、任意の混合割合における（原油スラッジａの各組成）／（原油スラッジａの各組成＋原油ｂ、原油ｘの各組成）を乗ずる。これら値の総和を百分率表記することで、原油スラッジａ由来の軽液組成である表２を算出する。
(Examples 1-2)
Crude oil sludge a and crude oil b were added to a stirring vessel so that the crude oil sludge a relative to the total amount was as shown in Table 1, and the mixture was heated and stirred at 80 ° C.
Next, while maintaining the temperature at 80 ° C., the heat-stirred product was put into a centrifuge set at 80 ° C. and centrifuged at 80 ° C., 1000 G for 1 minute.
Subsequently, the light liquid was separated by decantation to obtain a light liquid. The analysis values of the obtained light liquid are shown in Table 1. From the results in Table 1, Table 2 shows calculated values of light liquids excluding the influence of crude oil for dissolving each sludge and the composition. The values shown in Table 2 were calculated as follows. The light liquid composition shown in Table 1 is multiplied by (each composition of crude oil sludge a) / (each composition of crude oil sludge a + each composition of crude oil b, crude oil x) at an arbitrary mixing ratio. Table 2 which is a light liquid composition derived from crude oil sludge a is calculated by expressing the sum of these values as a percentage.
(比較例１〜２)
原油スラッジａと原油ｘとを、その合計に対する原油スラッジａが表１に示す割合になるように撹拌容器に加え、混合物を８０℃で加熱撹拌した。
次いで、８０℃を保ったまま、加熱撹拌処理物を、８０℃に設定された遠心分離器に入れ、８０℃、１０００Ｇ、１分間の条件で、遠心分離を行った。
次いで、デカンテーションにより、軽液を分離し、軽液を得た。得られた軽液の分析値を表１に示す。表１の結果から、各スラッジ溶解用の原油や組成による影響を除いた軽液の算出値を表２に示す。
(Comparative Examples 1-2)
Crude oil sludge a and crude oil x were added to a stirring vessel so that crude oil sludge a with respect to the total amount was as shown in Table 1, and the mixture was heated and stirred at 80 ° C.
Next, while maintaining the temperature at 80 ° C., the heat-stirred product was put into a centrifuge set at 80 ° C. and centrifuged at 80 ° C., 1000 G for 1 minute.
Subsequently, the light liquid was separated by decantation to obtain a light liquid. The analysis values of the obtained light liquid are shown in Table 1. From the results in Table 1, Table 2 shows calculated values of light liquids excluding the influence of crude oil for dissolving each sludge and the composition.
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