JP7464077B2 - Method and device for recovering oil from oil-containing waste liquid - Google Patents
Method and device for recovering oil from oil-containing waste liquid Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims description 141
- 239000002699 waste material Substances 0.000 title claims description 128
- 238000000034 method Methods 0.000 title claims description 38
- 239000003921 oil Substances 0.000 claims description 274
- 235000019198 oils Nutrition 0.000 claims description 274
- 239000002904 solvent Substances 0.000 claims description 81
- 238000000926 separation method Methods 0.000 claims description 43
- 238000000605 extraction Methods 0.000 claims description 42
- 238000011084 recovery Methods 0.000 claims description 31
- 239000002351 wastewater Substances 0.000 claims description 20
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- 238000009835 boiling Methods 0.000 claims description 11
- 235000013305 food Nutrition 0.000 claims description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- 238000004065 wastewater treatment Methods 0.000 claims description 8
- 239000002480 mineral oil Substances 0.000 claims description 7
- 239000001293 FEMA 3089 Substances 0.000 claims description 6
- 235000010446 mineral oil Nutrition 0.000 claims description 6
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 6
- 239000008158 vegetable oil Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000011144 upstream manufacturing Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000010775 animal oil Substances 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 239000012454 non-polar solvent Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 238000000998 batch distillation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001944 continuous distillation Methods 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002035 hexane extract Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- -1 sodium chloride Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
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- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
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Description
本発明は、油分含有廃液からの油分回収方法及び装置に係り、特に溶媒抽出を利用した油分含有廃液からの油分回収方法及び装置に関する。 The present invention relates to a method and device for recovering oil from oil-containing waste liquid, and in particular to a method and device for recovering oil from oil-containing waste liquid using solvent extraction.
石油プロセス、鉄鋼圧延工程、紙パルプ製造、金属切削工程、食品製造、皮革製造、厨房、下水等から発生する濃厚な有機廃水である含油廃水の処理方法としては、凝集処理（特許文献１）や、活性炭処理と凝集処理と膜分離処理とを組み合わせた処理（特許文献２）、生物処理（特許文献３）などが知られている。 Methods for treating oil-containing wastewater, which is thick organic wastewater generated from petroleum processes, steel rolling processes, paper and pulp manufacturing, metal cutting processes, food manufacturing, leather manufacturing, kitchens, sewage, etc., include coagulation treatment (Patent Document 1), a treatment that combines activated carbon treatment, coagulation treatment, and membrane separation treatment (Patent Document 2), and biological treatment (Patent Document 3).
油分の凝集分離処理では条件が複雑であり、原水濃度変化に対して処理水濃度が不安定である。膜処理では処理水油分濃度は安定するが、膜が閉塞し易いという問題がある。生物処理では油分の低減はなされるものの、排水中の主たるＢＯＤ成分処理の活性低下を招くなどの問題がある。 The conditions for oil coagulation and separation treatment are complex, and the treated water concentration is unstable in response to changes in the raw water concentration. With membrane treatment, the treated water oil concentration is stable, but there is the problem that the membrane is easily clogged. With biological treatment, the oil content is reduced, but there are problems such as a decrease in the activity of treating the main BOD components in the wastewater.
本発明は、油分含有廃液から油分を安定かつ効率的に分離して回収することができる油分含有廃液からの油分回収方法及び装置を提供することを課題とする。 The objective of the present invention is to provide a method and device for recovering oil from oil-containing waste liquid that can stably and efficiently separate and recover oil from the oil-containing waste liquid.
本発明者は、上記課題を解決すべく検討を重ねた結果、溶媒抽出を利用することにより、油分含有廃液から油分を安定かつ効率的に分離して回収することができることを見出した。
本発明は、次を要旨とするものである。
As a result of extensive investigations aimed at solving the above problems, the present inventors have discovered that by utilizing solvent extraction, oil can be stably and efficiently separated and recovered from oil-containing waste liquid.
The present invention relates to the following.
［１］ 油分含有廃液を溶媒で抽出処理することにより該油分含有廃液中の油分を該溶媒へ移行させる抽出工程と、該抽出した油分を含む溶媒と該廃液とを分離する分離工程と、分離された該油分を含む溶媒から油分を分離して回収する油分回収工程とを有し、該油分回収工程で油分が分離された溶媒を前記抽出工程で再利用することを特徴とする油分含有廃液からの油分回収方法。 [1] A method for recovering oil from oil-containing waste liquid, comprising an extraction step in which oil in the oil-containing waste liquid is transferred to a solvent by extracting the oil-containing waste liquid with the solvent, a separation step in which the solvent containing the extracted oil is separated from the waste liquid, and an oil recovery step in which the oil is separated and recovered from the separated oil-containing solvent, and the solvent from which the oil has been separated in the oil recovery step is reused in the extraction step.
［２］ 前記溶媒は回収対象油分より低い沸点を有しており、前記油分回収工程において、前記油分を含む溶媒から加温蒸留により前記油分を分離する［１］に記載の油分含有廃液からの油分回収方法。 [2] The method for recovering oil from an oil-containing waste liquid described in [1], in which the solvent has a boiling point lower than that of the oil to be recovered, and in the oil recovery process, the oil is separated from the solvent containing the oil by heated distillation.
［３］ 前記加温蒸留による分離において、分離された前記溶媒または前記油分の有する熱を、熱交換器またはヒートポンプを用いて前記油分を含む溶媒の加温に利用する［２］に記載の油分含有廃液からの油分回収方法。 [3] A method for recovering oil from an oil-containing waste liquid according to [2], in which the heat of the separated solvent or oil is used to heat the oil-containing solvent using a heat exchanger or a heat pump during the separation by heated distillation.
［４］ 前記抽出工程に先立ち、前記油分含有廃液を濃縮する濃縮工程をさらに有する［１］～［３］のいずれかに記載の油分含有廃液からの油分回収方法。 [4] The method for recovering oil from an oil-containing waste liquid according to any one of [1] to [3], further comprising a concentration step of concentrating the oil-containing waste liquid prior to the extraction step.
［５］ 前記分離工程で分離された廃液中に残存する溶媒を分解または分離する溶媒処理工程をさらに有する［１］～［４］のいずれかに記載の油分含有廃液からの油分回収方法。 [5] A method for recovering oil from an oil-containing waste liquid according to any one of [1] to [4], further comprising a solvent treatment step for decomposing or separating the solvent remaining in the waste liquid separated in the separation step.
［６］ 前記分離工程で分離された廃液を排水処理工程に供する［１］～［５］のいずれかに記載の油分含有廃液からの油分回収方法。 [6] A method for recovering oil from an oil-containing waste liquid according to any one of [1] to [5], in which the waste liquid separated in the separation step is subjected to a wastewater treatment step.
［７］ 前記抽出工程に先立ち、前記油分含有廃液に塩、アルカリ又は酸を添加する添加工程をさらに有する［１］～［６］のいずれかに記載の油分含有廃液からの油分回収方法。 [7] The method for recovering oil from an oil-containing waste liquid according to any one of [1] to [6], further comprising an addition step of adding a salt, an alkali or an acid to the oil-containing waste liquid prior to the extraction step.
［８］ 前記分離工程で分離された油分を含む溶媒中の油分濃度が１重量％以上である［１］～［７］のいずれかに記載の油分含有廃液からの油分回収方法。 [8] A method for recovering oil from an oil-containing waste liquid according to any one of [1] to [7], in which the oil concentration in the oil-containing solvent separated in the separation step is 1% by weight or more.
［９］ 前記油分含有廃液が、鉱物油を含有する自動車等の部品製造工場の廃液、ターペンチ油を含有する紙パ工場の廃液、動植物油を含有する製油工場、食品飲料工場又は飲食産業事業からの廃液のいずれかである［１］～［８］のいずれかに記載の油分含有廃液からの油分回収方法。 [9] A method for recovering oil from oil-containing waste liquid according to any one of [1] to [8], wherein the oil-containing waste liquid is any one of waste liquids from a manufacturing plant for automobile parts or the like that contains mineral oil, waste liquids from a paper and pulp factory that contains turpentine oil, waste liquids from an oil refinery that contains animal and vegetable oils, food and beverage factories, and waste liquids from the food and beverage industry.
［１０］ 前記油分含有廃液が、非極性溶媒に抽出された有機物含有廃液である［１］～［８］のいずれかに記載の油分含有廃液からの油分回収方法。 [10] A method for recovering oil from an oil-containing waste liquid according to any one of [1] to [8], wherein the oil-containing waste liquid is an organic matter-containing waste liquid extracted into a non-polar solvent.
［１１］ 前記油分回収工程で回収された油分を、前記油分含有廃液排出場所のエネルギー源として使用する［１］～［１０］のいずれかに記載の油分含有廃液からの油分回収方法。 [11] A method for recovering oil from oil-containing waste liquid described in any one of [1] to [10], in which the oil recovered in the oil recovery process is used as an energy source for the site where the oil-containing waste liquid is discharged.
［１２］ 油分含有廃液を溶媒で抽出処理することにより該油分含有廃液中の油分を該溶媒へ移行させる抽出手段と、該抽出した油分を含む溶媒と該廃液とを分離する分離手段と、分離された該油分を含む溶媒から油分を分離して回収する油分回収手段と、該油分回収手段で油分が分離された溶媒を前記抽出手段へ送給する給液手段とを有することを特徴とする油分含有廃液からの油分回収装置。 [12] An apparatus for recovering oil from oil-containing waste liquid, comprising: an extraction means for transferring oil in the oil-containing waste liquid to a solvent by extracting the oil-containing waste liquid with the solvent; a separation means for separating the extracted oil-containing solvent from the waste liquid; an oil recovery means for separating and recovering oil from the separated oil-containing solvent; and a liquid supply means for supplying the solvent from which the oil has been separated by the oil recovery means to the extraction means.
［１３］ 前記溶媒は回収対象油分より低い沸点を有しており、前記油分回収手段は、前記油分を含む溶媒から加温蒸留により前記油分を分離する手段である［１２］に記載の油分含有廃液からの油分回収装置。 [13] The apparatus for recovering oil from oil-containing waste liquid described in [12], in which the solvent has a boiling point lower than that of the oil to be recovered, and the oil recovery means is a means for separating the oil from the solvent containing the oil by heated distillation.
［１４］ 前記加温蒸留により分離された前記溶媒または前記油分の有する熱を用いて、前記油分を含む溶媒を加温するための熱交換器またはヒートポンプを有する［１３］に記載の油分含有廃液からの油分回収装置。 [14] An oil recovery device from an oil-containing waste liquid as described in [13], which has a heat exchanger or heat pump for heating the oil-containing solvent using the heat of the solvent or the oil separated by the heating distillation.
［１５］ 前記抽出手段の前段に、前記油分含有廃液を濃縮する濃縮手段をさらに有する［１２］～［１４］のいずれかに記載の油分含有廃液からの油分回収装置。 [15] An apparatus for recovering oil from an oil-containing waste liquid according to any one of [12] to [14], further comprising a concentrating means for concentrating the oil-containing waste liquid, located upstream of the extraction means.
［１６］ 前記分離手段で分離された廃液中に残存する溶媒を分解または分離する溶媒処理手段をさらに有する［１２］～［１５］のいずれかに記載の油分含有廃液からの油分回収装置。 [16] An oil recovery device from an oil-containing waste liquid described in any one of [12] to [15], further comprising a solvent treatment means for decomposing or separating the solvent remaining in the waste liquid separated by the separation means.
［１７］ 前記分離手段で分離された廃液を排水処理手段に供する送液手段を更に有する［１２］～［１６］のいずれかに記載の油分含有廃液からの油分回収装置。 [17] An oil recovery device from an oil-containing waste liquid described in any one of [12] to [16], further comprising a liquid delivery means for supplying the waste liquid separated by the separation means to a wastewater treatment means.
［１８］ 前記抽出手段の前段に、前記油分含有廃液に塩、アルカリ又は酸を添加する添加手段をさらに有する［１２］～［１７］のいずれかに記載の油分含有廃液からの油分回収装置。 [18] An apparatus for recovering oil from an oil-containing waste liquid according to any one of [12] to [17], further comprising an addition means for adding a salt, an alkali or an acid to the oil-containing waste liquid, prior to the extraction means.
［１９］ 前記分離手段で分離された油分を含む溶媒中の油分濃度が１重量％以上である［１２］～［１８］のいずれかに記載の油分含有廃液からの油分回収装置。 [19] An oil recovery device from an oil-containing waste liquid according to any one of [12] to [18], in which the oil concentration in the oil-containing solvent separated by the separation means is 1% by weight or more.
［２０］ 前記油分含有廃液が、鉱物油を含有する自動車等の部品製造工場の廃液、ターペンチ油を含有する紙パ工場の廃液、動植物油を含有する製油工場、食品飲料工場又は飲食産業事業からの廃液のいずれかである［１２］～［１９］のいずれかに記載の油分含有廃液からの油分回収装置。 [20] An oil recovery device from oil-containing waste liquid described in any one of [12] to [19], wherein the oil-containing waste liquid is any one of waste liquids from a manufacturing plant for automobile parts or the like that contains mineral oil, waste liquids from a paper and pulp factory that contains turpentine oil, waste liquids from an oil refinery that contains animal and vegetable oils, waste liquids from a food and beverage factory, or waste liquids from the food and beverage industry.
［２１］ 前記油分含有廃液が、非極性溶媒に抽出された有機物含有廃液である［１２］～［１９］のいずれかに記載の油分含有廃液からの油分回収装置。 [21] An apparatus for recovering oil from an oil-containing waste liquid according to any one of [12] to [19], wherein the oil-containing waste liquid is an organic matter-containing waste liquid extracted into a non-polar solvent.
［２２］ 前記油分回収手段で回収された油分を、前記油分含有廃液排出場所へエネルギー源として供給する手段を更に有する［１２］～［２１］のいずれかに記載の油分含有廃液からの油分回収装置。 [22] An oil recovery device from oil-containing waste liquid described in any one of [12] to [21], further comprising a means for supplying the oil recovered by the oil recovery means to the oil-containing waste liquid discharge location as an energy source.
本発明によると、溶媒抽出を利用することにより、油分含有廃液から油分を安定かつ効率的に分離して回収することができる。また、本発明では、抽出に用いた溶媒を再利用するので、処理コストも安価である。
本発明によれば、排水処理を阻害する油分含有廃液中の油分を大幅に低減すると共に、高純度の油分を回収してこれを再利用することができると共に、従来、産業廃棄物として処分されていた油分含有廃液を排水処理に適用することが可能となり、その工業上の利用価値は極めて大きい。
According to the present invention, by utilizing solvent extraction, oil can be stably and efficiently separated and recovered from oil-containing waste liquid. In addition, since the solvent used in the extraction is reused in the present invention, the processing cost is low.
According to the present invention, the oil content in oil-containing wastewater that inhibits wastewater treatment can be significantly reduced, high-purity oil can be recovered and reused, and oil-containing wastewater that was previously disposed of as industrial waste can be applied to wastewater treatment, making the industrial utility of the present invention extremely high.
以下に本発明の油分含有廃液からの油分回収方法及び装置の実施の形態を図１を参照して説明するが、本発明は何ら以下のものに限定されるものではなく、本発明の要旨の範囲内で種々に変更して実施することができる。 The embodiment of the method and device for recovering oil from oil-containing waste liquid according to the present invention will be described below with reference to FIG. 1. However, the present invention is not limited to the following and can be modified in various ways within the scope of the present invention.
図１は、本発明の実施の形態に係る油分含有廃液からの油分回収方法及び装置を示すフロー図である。
なお、本発明において処理対象となる油分含有廃液としては、石油プロセス、鉄鋼圧延工程、紙パルプ製造、金属切削工程、食品製造、皮革製造、厨房、下水等から発生する濃厚な油分含有廃液、具体的には、水性切削液廃液、製紙やパルプ工場から排出されるターペンチ油含有排水、食品排水が挙げられるが、何らこれらに限定されない。また、油分含有廃液中の油分についても鉱物油、植物油のいずれでもよい。これらの油分含有廃液の油分濃度は、通常０．０５～１重量％程度である。
油分含有廃液としては、より具体的には、鉱物油を含有する自動車等の部品製造工場の廃液、ターペンチ油を含有する紙パ工場の廃液、動植物油を含有する製油工場、食品飲料工場又は飲食産業事業からの廃液が挙げられる。
また、油分含有廃液は、非極性溶媒に抽出された有機物含有廃液であってもよい。
FIG. 1 is a flow diagram showing a method and apparatus for recovering oil from an oil-containing waste liquid according to an embodiment of the present invention.
In addition, the oil-containing waste liquid to be treated in the present invention includes, but is not limited to, thick oil-containing waste liquid generated from petroleum processes, steel rolling processes, paper and pulp manufacturing, metal cutting processes, food manufacturing, leather manufacturing, kitchens, sewage, etc., specifically, aqueous cutting fluid waste liquid, turpentine oil-containing wastewater discharged from paper and pulp factories, and food wastewater. In addition, the oil in the oil-containing waste liquid may be either mineral oil or vegetable oil. The oil concentration of these oil-containing waste liquids is usually about 0.05 to 1% by weight.
More specifically, examples of oil-containing waste liquids include waste liquids from automobile part manufacturing factories that contain mineral oils, waste liquids from paper and pulp factories that contain turpentine oil, and waste liquids from oil refineries, food and beverage factories, or food and beverage industries that contain animal and vegetable oils.
The oil-containing waste liquid may also be an organic matter-containing waste liquid extracted into a non-polar solvent.
図１において、油分含有廃液は、配管１を介して膜分離装置２に導入され、膜分離により濃縮される。膜を透過した透過水の一部は、配管４Ａから膜分離装置２に返送される。透過水の残部は、配管４Ｂを介して排水処理設備（図示せず）へ送水され、処理される。
In FIG. 1, oil-containing waste liquid is introduced into
膜分離装置２の濃縮水及び抽出用溶媒は、それぞれ配管５及び配管７を介して抽出装置６の混合部６ａに供給される。
The concentrated water and extraction solvent from the
混合部６ａに供給された濃縮水と抽出用溶媒は、混合部６ａにて混合され、濃縮水中の油分を溶媒中に取り込む。即ち、濃縮水中の油分が抽出用溶媒に溶解する。油分が溶解した溶媒と油分が抽出された濃縮水（残液）は、分離部６ｂで分離され、油分が溶解した溶媒が配管８を介して熱交換器９の冷熱源流路に供給され、被冷却流体流路を流れる溶媒蒸気と熱交換し、昇温して配管１０より蒸留塔１１に導入される。蒸留塔１１では低沸点成分である溶媒が塔頂側へ流れ、高沸点成分である油分が塔底側へ流れる。溶媒蒸気は、蒸留塔１１から配管１２を介して熱交換器９の被冷却流体流路に供給され、冷熱源流路を流れる抽出装置流出液（低温液）と熱交換して冷却され、液状溶媒となる。この液状溶媒が配管７によって抽出装置６の混合部６ａに送液され、抽出用溶媒として再利用される。
The concentrated water and the extraction solvent supplied to the
蒸留塔１１の塔底からは、分離された油分が配管１４を介して取り出される。この油分は、回収油として液体燃料又は助燃剤などとして、発電、その他の各種用途に利用される。なお、必要に応じ、回収油に対して更に他の処理が施されてもよい。
The separated oil is taken out from the bottom of the
前記抽出装置６の分離部６ｂからは、油分が抽出された残液が配管２０を介して取り出され、膜分離装置２１に送液され、膜分離により、該残液中の溶媒成分（残存溶媒）の濃縮が行われる。
The residual liquid from which the oil has been extracted is taken out from the
膜分離装置２１の膜２１ａを透過した透過水は、配管２２を介して処理水として取り出される。膜分離装置２１の濃縮水は、配管２３を介して排出され、廃液処理工程（図示せず）へ送られて、濃縮処理又は排水処理等に供される。
The permeate that permeates the
上記実施の形態では、油分含有廃液を膜分離装置２で膜分離処理して油分濃度を高めるようにしているが、容易に油分と水分が分離する油成分については比重差やマイクロエアーを利用した油水分離機で分離処理を施し、その後、直ちに又は必要に応じ膜分離処理などの分離処理を行ってから、抽出装置６に送液してもよい。
抽出装置６などの抽出装置は連続式、バッチ式のいずれでもよい。工業的規模で用いられる連続液液抽出装置としては、ミキサーセトラ型、スプレー塔、多孔板塔（目皿塔）などがあるが、これら又はそれ以外のいずれでもよい。
In the above embodiment, the oil-containing waste liquid is subjected to membrane separation processing in the
The extraction apparatus such as the extraction apparatus 6 may be of either a continuous type or a batch type. Continuous liquid-liquid extraction apparatuses used on an industrial scale include mixer-settler type, spray towers, perforated plate towers (perforated plate towers), and the like, and any of these or other types may be used.
抽出に用いる溶媒は、抽出対象油との相性および溶媒再生の総合的観点から決定するのが好ましい。 The solvent used for extraction should be determined based on a comprehensive consideration of compatibility with the oil to be extracted and solvent regeneration.
抽出により油分を含む溶媒から加温蒸留により油分を分離する場合は、該油分よりも沸点の低い溶媒が用いられる。この場合、抽出溶媒は分離対象油分の沸点（２５０～６００℃程度）よりも沸点が低いものを用いることが必要であり、排水を直接蒸留するよりエネルギー的に低い必要があるため、１００℃以下である必要がある。したがって、抽出に用いる溶媒の沸点は４０～９０℃程度であることが好ましい。 When separating oil from a solvent that contains oil by extraction using heated distillation, a solvent with a lower boiling point than the oil is used. In this case, it is necessary to use an extraction solvent with a lower boiling point than the boiling point of the oil to be separated (approximately 250 to 600°C), and since this requires less energy than directly distilling wastewater, it needs to be below 100°C. Therefore, it is preferable for the boiling point of the solvent used for extraction to be around 40 to 90°C.
抽出に用いる溶媒としては、具体的にはノルマルヘキサン、ヘプタン、ペンタン、オクタン、ジエチルエーテル、メチルｔｅｒｔ－ブチルエーテル、１－オクタノール、クロロホルム、四塩化炭素、ベンゼン、トルエン、酢酸エチル、アセトン、ジクロロメタン、アセトニトリルなどが挙げられるが、何らこれらの溶媒に限定されるものではない。 Specific examples of solvents used for extraction include normal hexane, heptane, pentane, octane, diethyl ether, methyl tert-butyl ether, 1-octanol, chloroform, carbon tetrachloride, benzene, toluene, ethyl acetate, acetone, dichloromethane, and acetonitrile, but are not limited to these solvents.
図１では、加温蒸留により、油分を含む溶媒から油分を分離することで、溶媒を再生している。溶媒の再生には、このように油分と溶媒との沸点差を利用した加温蒸留が好適である。加温蒸留の方式としては、回分式蒸留と連続式蒸留のいずれも適用可能であり、フラッシュ蒸留、棚段塔、充填塔などの方式が適用可能である。 In Figure 1, oil is separated from a solvent containing oil by heated distillation, and the solvent is regenerated. Heat distillation, which takes advantage of the difference in boiling points between the oil and the solvent, is suitable for regenerating the solvent. Both batch and continuous distillation methods can be used for heated distillation, and methods such as flash distillation, plate columns, and packed columns can be used.
本発明において、抽出に供する油分含有廃液中の油分濃度としては、０．０５～５重量％程度（例えば０．１重量％以上）であることが、抽出効率の観点から好ましい。従って、油分含有廃液の油分濃度が上記範囲よりも低い場合には、抽出処理に先立ち、重力分離、加圧浮上や膜分離装置、その他の濃縮手段により濃縮するのが好ましい。なお、油分含有廃液の油分濃度が上記範囲を超える場合でも同法の適用は可能である。 In the present invention, the oil concentration in the oil-containing waste liquid to be extracted is preferably about 0.05 to 5% by weight (e.g., 0.1% by weight or more) from the viewpoint of extraction efficiency. Therefore, if the oil concentration of the oil-containing waste liquid is lower than the above range, it is preferable to concentrate it by gravity separation, pressure flotation, membrane separation equipment, or other concentrating means prior to the extraction treatment. Note that this method can be applied even if the oil concentration of the oil-containing waste liquid exceeds the above range.
また、油分含有廃液からの油分の分離を促進するために、抽出処理に先立ち、油分含有廃液に塩化ナトリウムなどの塩や、アルカリ又は酸を添加してもよい。
たとえば、塩化ナトリウムであれば、０．０５～１重量％程度の油分を含む油分含有廃液に０．１～３０重量％程度添加、またはｐＨを２程度まで低下させることで、油分の分離効率を高めることができる。
In order to promote the separation of oil from the oil-containing waste liquid, a salt such as sodium chloride, an alkali or an acid may be added to the oil-containing waste liquid prior to the extraction treatment.
For example, in the case of sodium chloride, the oil separation efficiency can be improved by adding about 0.1 to 30% by weight to an oil-containing waste liquid containing about 0.05 to 1% by weight of oil, or by lowering the pH to about 2.
本発明においては、このようにして油分含有廃液から油分を抽出した後の溶媒の油分濃度としては、１重量％以上、特に４重量％以上であることが好ましい。例えば、ノルマルヘキサンを用いて抽出を行った場合、抽出後のノルマルヘキサンの油分濃度は２～１０重量％程度であることが、油分分離効率、溶媒再生における熱エネルギー効率の観点から好ましい。 In the present invention, the oil concentration of the solvent after the oil has been extracted from the oil-containing waste liquid in this manner is preferably 1% by weight or more, and particularly 4% by weight or more. For example, when extraction is performed using normal hexane, it is preferable that the oil concentration of the normal hexane after extraction is about 2 to 10% by weight from the standpoint of oil separation efficiency and thermal energy efficiency in solvent regeneration.
図１では、膜分離装置２１により、油分分離後の廃液（残液）中の残存物質を逆浸透膜処理を適用して分離しているが、そのうち溶媒成分の分離には活性炭などの吸着処理を適用してもよい。また、残存溶媒は、酸化剤添加により分解処理してもよい。
In FIG. 1, the
以下に実施例に代わる実験例を挙げて本発明による効果を示す。 The following experimental examples are presented in place of the working examples to demonstrate the effects of the present invention.
［実験例１］
油分濃度：３ｇ／Ｌ（ノルマルヘキサン抽出物濃度）の鉱物油含有廃水から油分をノルマルヘキサンで抽出した。なお、抽出処理に先立ち、廃液に食塩を３０重量％添加した場合と、添加しない場合との２例について試験した。
抽出には試験管を用い、条件は次の通りとした。
Ａ：廃液への食塩添加なし
Ｂ：廃液への食塩添加あり（ＮａＣｌ濃度：３０重量％）
廃液：ノルマルヘキサン容積比＝１０：１（Ａ、Ｂ共通）
操作方法（Ａ，Ｂ共通）：
試験管攪拌混合（１００回縦往復）→静置分離（３０分）→上澄み採取
採取した上澄み（油分含有ノルマルヘキサン）中の油分濃度は、以下の通りであった。
Ａ＝０．５重量％
Ｂ＝４．５重量％
この試験より、油分含有廃液より、溶媒抽出により油分を十分に分離回収できること、及び油分含有廃液に食塩を添加することにより、回収効率が向上することが認められた。
[Experimental Example 1]
Oil was extracted from mineral oil-containing wastewater with normal hexane, with an oil concentration of 3 g/L (normal hexane extract concentration). Prior to the extraction process, two tests were conducted: one in which 30% by weight of salt was added to the wastewater, and the other in which salt was not added.
A test tube was used for extraction under the following conditions:
A: No salt added to waste liquid B: Salt added to waste liquid (NaCl concentration: 30% by weight)
Waste liquid: normal hexane volume ratio = 10:1 (common to A and B)
Operation method (common to A and B):
Test tube agitation mixing (100 vertical reciprocations) → standing to separate (30 minutes) → supernatant collection The oil concentrations in the collected supernatants (oil-containing normal hexane) were as follows:
A=0.5% by weight
B=4.5% by weight
This test confirmed that oil can be sufficiently separated and recovered from oil-containing waste liquid by solvent extraction, and that the recovery efficiency can be improved by adding salt to the oil-containing waste liquid.
［実験例２］
実験例１のＢの抽出実験で得られた油分濃度４．５重量％のノルマルヘキサンを開放容器に１０ｇ入れホットプレートにて、８０℃で１時間加温後に乾燥させたところ、残留油分として０．４５ｇを得ることができ、加温蒸留により、油分を含む溶媒から油分を効率的に分離することができることが確認された。
[Experimental Example 2]
10 g of normal hexane with an oil concentration of 4.5% by weight obtained in the extraction experiment of Experimental Example 1, B, was placed in an open container and heated on a hot plate at 80°C for 1 hour and then dried. As a result, 0.45 g of residual oil was obtained. It was confirmed that oil can be efficiently separated from a solvent containing oil by heated distillation.
２，２１ 膜分離装置
６ 抽出装置
１１ 蒸留塔
2, 21 Membrane separation device 6
Claims (18)
前記油分含有廃液が、水性切削廃液、製紙又はパルプ工場から排出されるターペンチン油含有排水、食品排水のいずれかであり、かつ
該油分含有廃液は、鉱物油、植物油のいずれかである油分を０．０５～１重量％含有する油分含有廃液であり、
前記溶媒が、ノルマルヘキサンであることを特徴とする油分含有廃液からの油分回収方法。 A method for recovering oil from an oil-containing waste liquid, comprising: an extraction step of extracting an oil-containing waste liquid with a solvent to transfer oil in the oil-containing waste liquid to the solvent; a separation step of separating the extracted oil-containing solvent from the waste liquid; and an oil recovery step of separating and recovering the oil from the separated oil-containing solvent, wherein the solvent from which the oil has been separated in the oil recovery step is reused in the extraction step,
The oil-containing wastewater is any one of an aqueous cutting wastewater, a turpentine oil-containing wastewater discharged from a paper or pulp mill, and a food wastewater; and
The oil-containing waste liquid is an oil-containing waste liquid containing 0.05 to 1% by weight of an oil component which is either a mineral oil or a vegetable oil,
A method for recovering oil from an oil-containing waste liquid, characterized in that the solvent is normal hexane.
前記油分含有廃液が、水性切削廃液、製紙又はパルプ工場から排出されるターペンチン油含有排水、食品排水のいずれかであり、かつ
該油分含有廃液は、鉱物油、植物油のいずれかである油分を０．０５～１重量％含有する油分含有廃液であり、
前記溶媒がノルマルヘキサンであることを特徴とする油分含有廃液からの油分回収装置。 An apparatus for recovering oil from an oil-containing waste liquid, comprising: an extraction means for transferring oil in the oil-containing waste liquid to a solvent by extracting the oil-containing waste liquid with the solvent; a separation means for separating the extracted oil-containing solvent from the waste liquid; an oil recovery means for separating and recovering the oil from the separated oil-containing solvent; and a liquid supply means for supplying the solvent from which the oil has been separated by the oil recovery means to the extraction means,
The oil-containing wastewater is any one of an aqueous cutting wastewater, a turpentine oil-containing wastewater discharged from a paper or pulp mill, and a food wastewater; and
The oil-containing waste liquid is an oil-containing waste liquid containing 0.05 to 1% by weight of an oil component which is either a mineral oil or a vegetable oil,
1. An apparatus for recovering oil from an oil-containing waste liquid, wherein the solvent is normal hexane.
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| JP2018062512A (en) | 2016-10-12 | 2018-04-19 | 三菱ケミカル株式会社 | Method and apparatus for producing aqueous organic carboxylic acid solution |
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