JP2017154092A - Demulsification apparatus and demulsification method - Google Patents
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Abstract
Description
本発明は、解乳化装置及び解乳化方法に関する。 The present invention relates to a demulsification apparatus and a demulsification method.
近年、連続相となる液体の中に微小液滴（分散相）が分散しているエマルションが様々な分野で利用されている。例えば、工業用化学薬品、化粧品、食品添加物、医薬材料などとしてエマルションは利用されている。エマルションの基本成分は水・油・界面活性剤であるが、実際に利用されているエマルションは複雑な多成分系である。また、エマルションは、通常、分散相が油相である水中油型エマルション（Ｏ／Ｗエマルション）と、分散相が水相である油中水型エマルション（Ｗ／Ｏエマルション）とに分類される。
一方、食品、農薬、薬剤、塗料、インク、接着剤などの製造工程で排出される廃水、製造装置の洗浄で排出される洗浄廃水、切削油などを用いて金属加工することにより生じる廃水などがエマルションとなっている場合がある。エマルションは安定であるため、廃水を水分と油分とに自然分離することは難しく、その多くが産業廃棄物として焼却処理されている。そこでエマルションを解乳化し水と油に分離することにより、廃液処理費用の削減すること、廃液を再利用することなどが望まれている。なお、解乳化とは、エマルションとして安定している系を積極的に破壊して相分離系へ移行させるプロセスをいう。
解乳化方法としては、遠心力・せん断力をエマルションに付与する方法、エマルションに電場を印加する方法（例えば、特許文献１参照）、酸性物質又は塩基性物質をエマルションに添加する方法、凝集剤をエマルションに添加する方法などが挙げられる。
エマルションに電場を印加する方法は、エマルションを連続的に解乳化することができること、凝集剤を必要としないこと、分離した液の品質が落ちにくいことなどの利点がある。
In recent years, emulsions in which fine droplets (dispersed phase) are dispersed in a liquid that is a continuous phase have been used in various fields. For example, emulsions are used as industrial chemicals, cosmetics, food additives, pharmaceutical materials and the like. The basic components of an emulsion are water, oil, and a surfactant, but the emulsion actually used is a complex multi-component system. Emulsions are usually classified into an oil-in-water emulsion (O / W emulsion) in which the dispersed phase is an oil phase and a water-in-oil emulsion (W / O emulsion) in which the dispersed phase is an aqueous phase.
On the other hand, wastewater discharged from manufacturing processes such as food, agricultural chemicals, chemicals, paints, inks, adhesives, cleaning wastewater discharged by cleaning of manufacturing equipment, wastewater generated by metal processing using cutting oil, etc. May be an emulsion. Since emulsions are stable, it is difficult to naturally separate wastewater into moisture and oil, and many of them are incinerated as industrial waste. Therefore, it is desired to reduce the waste liquid treatment cost and reuse the waste liquid by demulsifying the emulsion and separating it into water and oil. Note that demulsification refers to a process in which a system that is stable as an emulsion is actively destroyed and transferred to a phase separation system.
As a demulsification method, a method of imparting centrifugal force / shear force to the emulsion, a method of applying an electric field to the emulsion (for example, see Patent Document 1), a method of adding an acidic substance or a basic substance to the emulsion, and a flocculant The method of adding to an emulsion is mentioned.
The method of applying an electric field to the emulsion has advantages such that the emulsion can be continuously demulsified, a flocculant is not required, and the quality of the separated liquid is difficult to deteriorate.
上記のようなエマルションに電場を印加する解乳化方法について、本発明者はさらに詳しく検討した結果、油の含有量が多いW/Oエマルションの解乳化には有効であるが、油の含有量が少ないO/Wエマルションの解乳化にはあまり有効でないことを見出した。
本発明は、このような事情に鑑みてなされたものであり、油の含有量が少ないO/Wエマルションを解乳化するのに適した解乳化装置及び解乳化方法を提供する。
As for the demulsification method in which an electric field is applied to the emulsion as described above, the present inventors have further studied in detail, and as a result, the present invention is effective for demulsification of a W / O emulsion having a large oil content. It was found that it was not very effective for demulsification of few O / W emulsions.
The present invention has been made in view of such circumstances, and provides a demulsification apparatus and a demulsification method suitable for demulsifying an O / W emulsion having a low oil content.
本発明は、エマルションの流れと有機溶剤の流れとを合流させスラグ流、平行二相流又はこれらの流れの混合流を形成する合流部と、第１電極と第２電極とを有する電極対と、前記電極対に挟まれかつ前記スラグ流、前記平行二相流又は前記混合流が流れる細長い流路と、前記電極対に電圧を印加する電源回路とを備えることを特徴とする解乳化装置を提供する。
また、本発明は、エマルション相と有機溶剤相からなるスラグ流、平行二相流又はこれらの流れの混合流に交流電場を印加する工程を含む解乳化方法を提供する。
なお、スラグ流とは細長い流路をエマルション相と有機溶剤相とが交互に流れる流れであり、平行二相流とは細長い流路をエマルション相と有機溶剤相とが平行に流れる流れである。混合流とは、スラグ流と平行二相流とが混ざり合った流れである。
The present invention relates to an electrode pair having a first electrode and a second electrode, a merging portion that combines a flow of an emulsion and a flow of an organic solvent to form a slag flow, a parallel two-phase flow, or a mixed flow of these flows, and A demulsifying device comprising: an elongated channel sandwiched between the electrode pair and through which the slug flow, the parallel two-phase flow or the mixed flow flows; and a power supply circuit for applying a voltage to the electrode pair. provide.
Moreover, this invention provides the demulsification method including the process of applying an alternating current electric field to the slag flow which consists of an emulsion phase and an organic solvent phase, a parallel two-phase flow, or the mixed flow of these flows.
The slag flow is a flow in which the emulsion phase and the organic solvent phase alternately flow in the elongated flow path, and the parallel two-phase flow is a flow in which the emulsion phase and the organic solvent phase flow in parallel in the elongated flow path. The mixed flow is a flow in which a slag flow and a parallel two-phase flow are mixed.
本発明の解乳化装置は、エマルションの流れと有機溶剤の流れとを合流させスラグ流、平行二相流又はこれらの流れの混合流を形成する合流部と、前記スラグ流、前記平行二相流又は前記混合流が流れる細長い流路とを備えるため、被処理液体であるエマルションを有機溶剤と共にスラグ流、平行二相流又は混合流として細長い流路に流すことができる。
本発明の解乳化装置は、第１電極と第２電極とを有する電極対と、前記電極対に電圧を印加する電源回路とを備えるため、電源回路により電極対間に交流電圧を印加することができ、第１電極と第２電極との間に交流電場を発生させることができる。
前記細長い流路は前記電極対に挟まれるため、細長い流路を流れるエマルション相と有機溶剤相とからなるスラグ流、平行二相流又は混合流に電極対により交流電場を長時間印加することができる。このことにより、エマルションを解乳化することができる。このことは、本発明者が行った実験により実証された。
解乳化のメカニズムは明らかではないが、次のように考えられる。交流電場により微小空間のエマルション相に循環流が生じ、この循環流によりエマルション相に含まれる油相が有機溶剤相に合一化されると考えられる。このため、エマルション相に含まれる水相と油相とが分離し、エマルションが解乳化されると考えられる。
The demulsifying device of the present invention includes a slag flow, a parallel two-phase flow or a merged portion that forms a mixed flow of these flows by combining the emulsion flow and the organic solvent flow, the slag flow, and the parallel two-phase flow. Alternatively, an emulsion that is a liquid to be treated can be flowed together with an organic solvent into the elongated channel as a slag stream, a parallel two-phase flow, or a mixed stream.
The demulsification apparatus of the present invention includes an electrode pair having a first electrode and a second electrode, and a power supply circuit for applying a voltage to the electrode pair, so that an AC voltage is applied between the electrode pair by the power supply circuit. An AC electric field can be generated between the first electrode and the second electrode.
Since the elongate channel is sandwiched between the electrode pairs, an AC electric field can be applied for a long time to the slag flow, parallel two-phase flow, or mixed flow composed of an emulsion phase and an organic solvent phase flowing through the elongate channel. it can. This makes it possible to demulsify the emulsion. This was verified by experiments conducted by the present inventors.
The mechanism of demulsification is not clear, but is considered as follows. It is considered that a circulating flow is generated in the emulsion phase in a minute space by the alternating electric field, and the oil phase contained in the emulsion phase is united with the organic solvent phase by this circulating flow. For this reason, it is considered that the water phase and the oil phase contained in the emulsion phase are separated, and the emulsion is de-emulsified.
本発明の解乳化装置は、エマルションの流れと有機溶剤の流れとを合流させスラグ流、平行二相流又はこれらの流れの混合流を形成する合流部と、第１電極と第２電極とを有する電極対と、前記電極対に挟まれかつ前記スラグ流、前記平行二相流又は前記混合流が流れる細長い流路と、前記電極対に電圧を印加する電源回路とを備えることを特徴とする。
本発明の解乳化方法は、エマルション相と有機溶剤相からなるスラグ流、平行二相流又はこれらの流れの混合流に交流電場を印加する工程を含むことを特徴とする。
The demulsifying device of the present invention includes a merging portion that merges a flow of an emulsion and a flow of an organic solvent to form a slag flow, a parallel two-phase flow, or a mixed flow of these flows, and a first electrode and a second electrode. An electrode pair having an elongated flow path sandwiched between the electrode pair and through which the slag flow, the parallel two-phase flow or the mixed flow flows, and a power supply circuit for applying a voltage to the electrode pair. .
The demulsification method of the present invention is characterized in that it includes a step of applying an alternating electric field to a slag flow comprising an emulsion phase and an organic solvent phase, a parallel two-phase flow, or a mixed flow of these flows.
本発明の解乳化装置に含まれる合流部は、水中油型エマルションの流れと有機溶剤の流れとを合流させスラグ流、平行二相流又は混合流を形成するように設けられたことが好ましい。このことにより、本発明の解乳化装置により水中油型エマルションを解乳化することができる。
本発明の解乳化装置に含まれる細長い流路は、絶縁性の流路部材により形成されたことが好ましい。このことにより、細長い流路を流れるスラグ流、平行二相流又は混合流に大きな電場を印加することができ、エマルションを効率よく解乳化することができる。
It is preferable that the confluence | merging part contained in the demulsification apparatus of this invention is provided so that the flow of an oil-in-water emulsion and the flow of an organic solvent may be merged, and a slag flow, a parallel two-phase flow, or a mixed flow may be formed. Thereby, the oil-in-water emulsion can be demulsified by the demulsifying device of the present invention.
The elongated channel included in the demulsifying device of the present invention is preferably formed by an insulating channel member. As a result, a large electric field can be applied to the slag flow, parallel two-phase flow or mixed flow flowing through the elongated channel, and the emulsion can be efficiently demulsified.
本発明の解乳化装置は、前記細長い流路を流れた液体が流入する貯留槽を備えることが好ましい。このことにより、電場処理により解乳化された液体を貯留槽において水層と油層とに分離することができ、エマルションを水と油に分離して処理することが可能になる。
本発明の解乳化装置は、エマルションに添加剤を加える添加部を備えることが好ましい。エマルションに添加剤を加えることにより、解乳化することが難しいエマルションを解乳化しやすいエマルションに改質することが可能になる。
The demulsifying device of the present invention preferably includes a storage tank into which the liquid flowing through the elongated channel flows. As a result, the liquid demulsified by the electric field treatment can be separated into the water layer and the oil layer in the storage tank, and the emulsion can be separated into water and oil for processing.
The demulsifying device of the present invention preferably includes an adding section for adding an additive to the emulsion. By adding an additive to the emulsion, it is possible to modify an emulsion that is difficult to demulsify into an emulsion that is easy to demulsify.
本発明の解乳化方法は、エマルションの流れと有機溶剤の流れとを合流させ前記スラグ流、前記平行二相流又は前記混合流を形成する工程を含むことが好ましい。このことにより、電場処理の対象となるスラグ流、平行二相流又は混合流を形成することができる。
本発明の解乳化方法は、水中油型エマルション相と有機溶剤相からなるスラグ流、平行二相流又は混合流に交流電場を印加する工程を含むことが好ましい。このことにより、水中油型エマルションを解乳化することができる。
本発明の解乳化方法は、交流電場印加後の前記スラグ流、前記平行二相流又は前記混合流を貯留槽に流入させる工程をさらに含むことが好ましい。このことにより、電場処理により解乳化された液体を水層と油層とに分離することができ、エマルションを水と油に分離して処理することが可能になる。
The demulsification method of the present invention preferably includes a step of joining the flow of the emulsion and the flow of the organic solvent to form the slag flow, the parallel two-phase flow or the mixed flow. This makes it possible to form a slag flow, a parallel two-phase flow, or a mixed flow that is subject to electric field treatment.
The demulsification method of the present invention preferably includes a step of applying an alternating electric field to a slag flow, a parallel two-phase flow or a mixed flow comprising an oil-in-water emulsion phase and an organic solvent phase. This makes it possible to demulsify the oil-in-water emulsion.
The demulsification method of the present invention preferably further includes a step of allowing the slag flow, the parallel two-phase flow or the mixed flow after application of an alternating electric field to flow into a storage tank. As a result, the liquid demulsified by the electric field treatment can be separated into an aqueous layer and an oil layer, and the emulsion can be separated into water and oil for treatment.
以下、図面を用いて本発明の一実施形態を説明する。図面や以下の記述中で示す構成は、例示であって、本発明の範囲は、図面や以下の記述中で示すものに限定されない。 Hereinafter, an embodiment of the present invention will be described with reference to the drawings. The configurations shown in the drawings and the following description are merely examples, and the scope of the present invention is not limited to those shown in the drawings and the following description.
図１は本実施形態の解乳化装置の概略構成図であり、図２は図１の破線Ａ−Ａにおける電場形成部の概略断面図であり、図３は図２の破線Ｂ−Ｂにおける電場形成部の概略断面図である。図４は、本実施形態の解乳化装置の概念図であり、図５（ａ）はスラグ流におけるエマルション相の解乳化の概念図であり、図５（ｂ）は平行二相流におけるエマルションの解乳化の概念図である。 FIG. 1 is a schematic configuration diagram of a demulsification apparatus according to the present embodiment, FIG. 2 is a schematic cross-sectional view of an electric field forming unit along broken line AA in FIG. 1, and FIG. 3 is an electric field along broken line BB in FIG. It is a schematic sectional drawing of a formation part. FIG. 4 is a conceptual diagram of the demulsification apparatus of the present embodiment, FIG. 5 (a) is a conceptual diagram of demulsification of the emulsion phase in the slag flow, and FIG. 5 (b) is a diagram of the emulsion in the parallel two-phase flow. It is a conceptual diagram of demulsification.
本実施形態の解乳化装置３０は、エマルション１２の流れと有機溶剤２２の流れとを合流させスラグ流３３、平行二相流３４又はこれらの流れの混合流を形成する合流部７と、第１電極１と第２電極２とを有する電極対４と、電極対４に挟まれかつスラグ流３３、平行二相流３４又は混合流が流れる細長い流路６と、電極対４に電圧を印加する電源回路１０とを備えることを特徴とする。
本実施形態の解乳化方法は、エマルション相１３と有機溶剤相２３からなるスラグ流３３、平行二相流３４又はこれらの流れの混合流に交流電場を印加する工程を含むことを特徴とする。
以下、本実施形態の解乳化装置及び解乳化方法について説明する。
The demulsifying device 30 of this embodiment includes a slag flow 33, a parallel two-phase flow 34, or a combined portion 7 that forms a mixed flow of these flows by combining the flow of the emulsion 12 and the flow of the organic solvent 22, and the first A voltage is applied to the electrode pair 4 having the electrode 1 and the second electrode 2, the elongated channel 6 sandwiched between the electrode pair 4 and through which the slag flow 33, parallel two-phase flow 34 or mixed flow flows, and the electrode pair 4. And a power supply circuit 10.
The demulsification method of the present embodiment includes a step of applying an alternating electric field to a slag flow 33, a parallel two-phase flow 34, or a mixed flow of these flows composed of the emulsion phase 13 and the organic solvent phase 23.
Hereinafter, the demulsification apparatus and the demulsification method of this embodiment will be described.
１．スラグ流又は平行二相流の形成
本実施形態の解乳化装置３０及び解乳化方法による解乳化の被処理液は、エマルション１２である。被処理液は、水中油型エマルションであってもよく、油中水型エマルションであってもよい。水中油型エマルションは、連続相である水相３１中に分散相である油相３２が分散したエマルションである。油中水型エマルションは、連続相である油相３２中に分散相である水相３１が分散したエマルションである。
エマルション１２は、例えば、食品、農薬、薬剤、塗料、インク、接着剤などの製造工程で排出される廃水、製造装置の洗浄で排出される洗浄廃水、切削油などを用いて金属加工することにより生じる廃水などである。また、エマルション１２は、水に可溶な塩化物を含んでもよい。
1. Formation of slug flow or parallel two-phase flow The liquid to be treated for demulsification by the demulsification apparatus 30 and the demulsification method of this embodiment is an emulsion 12. The liquid to be treated may be an oil-in-water emulsion or a water-in-oil emulsion. The oil-in-water emulsion is an emulsion in which an oil phase 32 that is a dispersed phase is dispersed in an aqueous phase 31 that is a continuous phase. The water-in-oil emulsion is an emulsion in which an aqueous phase 31 that is a dispersed phase is dispersed in an oil phase 32 that is a continuous phase.
The emulsion 12 is processed by metal processing using, for example, waste water discharged in the manufacturing process of food, agricultural chemicals, drugs, paints, inks, adhesives, cleaning waste water discharged by cleaning of the manufacturing apparatus, cutting oil, and the like. This is the wastewater that is generated. Moreover, the emulsion 12 may contain a chloride soluble in water.
エマルション１２は、実質的に一定流量で合流部７に供給される。このことにより、合流部７でスラグ流３３、平行二相流３４又は混合流を形成することができる。例えば、図１に示した解乳化装置３０のように、エマルション槽１４にエマルション１２を貯留し、ポンプ１６ａによりエマルション１２を合流部７に供給することができる。また、図４に示した解乳化装置３０のように、シリンジポンプ１７ａによりエマルション１２を合流部７に供給してもよい。 The emulsion 12 is supplied to the junction 7 at a substantially constant flow rate. As a result, the slag flow 33, the parallel two-phase flow 34, or the mixed flow can be formed at the junction 7. For example, like the demulsification apparatus 30 shown in FIG. 1, the emulsion 12 can be stored in the emulsion tank 14, and the emulsion 12 can be supplied to the merge part 7 with the pump 16a. Moreover, you may supply the emulsion 12 to the confluence | merging part 7 with the syringe pump 17a like the demulsification apparatus 30 shown in FIG.
エマルション１２を合流部７に供給する前にエマルション１２を通過させるろ過部１５を設けてもよい。このことにより、エマルション１２に含まれる固形物を除去することができる。
本実施形態の解乳化装置３０は、エマルション１２に添加剤を加える添加部２５を備えてもよい。添加剤を加えることによりエマルション１２が解乳化されやすくなる。添加剤は、例えば、塩化ナトリウム、塩化カルシウム、塩化ランタンなどの水に可溶な塩化物である。
Before supplying the emulsion 12 to the merging unit 7, a filtration unit 15 that allows the emulsion 12 to pass therethrough may be provided. By this, the solid substance contained in the emulsion 12 can be removed.
The demulsification apparatus 30 according to the present embodiment may include an addition unit 25 that adds an additive to the emulsion 12. By adding the additive, the emulsion 12 is easily demulsified. Additives are water-soluble chlorides, such as sodium chloride, calcium chloride, lanthanum chloride, for example.
有機溶剤２２は、エマルション１２に含まれる油相を吸収する溶剤である。有機溶剤２２は、エマルション１２に含まれる油相を溶解可能であり水に不溶な有機溶剤であれば特に限定されないが、例えば、ｐ−キシレン、トルエン、ケロシンなどである。
有機溶剤２２は、実質的に一定流量で合流部７に供給される。このことにより、合流部７でスラグ流３３、平行二相流３４又は混合流を形成することができる。例えば、図１に示した解乳化装置３０のように、有機溶剤槽２４に有機溶剤２２を貯留し、ポンプ１６ｂにより有機溶剤２２を合流部７に供給することができる。また、図４に示した解乳化装置３０のように、シリンジポンプ１７ｂにより有機溶剤２２を合流部７に供給してもよい。
The organic solvent 22 is a solvent that absorbs the oil phase contained in the emulsion 12. The organic solvent 22 is not particularly limited as long as it can dissolve the oil phase contained in the emulsion 12 and is insoluble in water. Examples thereof include p-xylene, toluene, and kerosene.
The organic solvent 22 is supplied to the merging unit 7 at a substantially constant flow rate. As a result, the slag flow 33, the parallel two-phase flow 34, or the mixed flow can be formed at the junction 7. For example, like the demulsification apparatus 30 shown in FIG. 1, the organic solvent 22 can be stored in the organic solvent tank 24, and the organic solvent 22 can be supplied to the junction part 7 by the pump 16b. Moreover, you may supply the organic solvent 22 to the junction part 7 with the syringe pump 17b like the demulsification apparatus 30 shown in FIG.
合流部７は、エマルション１２の流れと有機溶剤２２の流れとを合流させスラグ流３３、平行二相流３４又は混合流を形成する部分である。合流部７は、細長い流路６の少なくとも一部にスラグ流３３が流れるように設けることができる。
合流部７には、エマルション１２が合流部７に流入するエマルション流路３６と、有機溶剤２２が合流部７に流入する有機溶剤流路３７と、合流部７で形成したスラグ流３３、平行二相流３４又は混合流が流れる細長い流路６とが接続される。
この細長い流路６は、第１電極１と第２電極２とに挟まれ、スラグ流３３、平行二相流３４又は混合流に交流電場が印加されるが、このことは後述する。
The merge portion 7 is a portion that merges the flow of the emulsion 12 and the flow of the organic solvent 22 to form a slag flow 33, a parallel two-phase flow 34, or a mixed flow. The merge portion 7 can be provided so that the slag flow 33 flows in at least a part of the elongated channel 6.
The merging section 7 includes an emulsion flow path 36 in which the emulsion 12 flows into the merging section 7, an organic solvent flow path 37 in which the organic solvent 22 flows into the merging section 7, a slag flow 33 formed in the merging section 7, The long flow path 6 through which the phase flow 34 or the mixed flow flows is connected.
The elongated channel 6 is sandwiched between the first electrode 1 and the second electrode 2, and an alternating electric field is applied to the slag flow 33, the parallel two-phase flow 34, or the mixed flow, which will be described later.
スラグ流３３とは、細長い流路６をエマルション相１３と有機溶剤相２３とが交互に流れる流れである。合流部７によりスラグ流３３を形成すると、細長い流路６中において、エマルション相１３を隣接する２つの有機溶剤相２３の間に閉じ込めることができる。また、エマルション相１３と有機溶剤相２３との界面を多く形成することができる。例えば、図４、図５（ａ）のように、流路部材８中の流路６にスラグ流を流すことができる。また、細長い流路６では、流動形態がスラグ流から平行二相流に変化してもよい。この場合、流動形態はスラグ流３３と平行二相流３４とが混ざり合った混合流となる。 The slag flow 33 is a flow in which the emulsion phase 13 and the organic solvent phase 23 alternately flow through the elongated channel 6. When the slag flow 33 is formed by the joining portion 7, the emulsion phase 13 can be confined between the two adjacent organic solvent phases 23 in the elongated channel 6. In addition, many interfaces between the emulsion phase 13 and the organic solvent phase 23 can be formed. For example, as shown in FIG. 4 and FIG. 5A, a slag flow can be caused to flow through the flow path 6 in the flow path member 8. Moreover, in the elongate flow path 6, a flow form may change from a slag flow to a parallel two-phase flow. In this case, the flow form is a mixed flow in which the slag flow 33 and the parallel two-phase flow 34 are mixed.
平行二相流３４とは細長い流路６中をエマルション相１３と有機溶剤相２３とが平行に流れる流れである。合流部７により平行二相流３４を形成することにより、エマルション相１３と有機溶剤相２３との界面を広くすることができる。例えば、図５（ｂ）のように、流路部材８中の流路６に平行二相流３４を流すことができる。また、細長い流路６では、流動形態が平行二相流からスラグ流に変化してもよい。この場合、流動形態はスラグ流３３と平行二相流３４とが混ざり合った混合流となる。 The parallel two-phase flow 34 is a flow in which the emulsion phase 13 and the organic solvent phase 23 flow in parallel in the elongated channel 6. By forming the parallel two-phase flow 34 by the merge part 7, the interface between the emulsion phase 13 and the organic solvent phase 23 can be widened. For example, as shown in FIG. 5B, a parallel two-phase flow 34 can flow through the flow path 6 in the flow path member 8. Moreover, in the elongate flow path 6, the flow form may change from a parallel two-phase flow to a slag flow. In this case, the flow form is a mixed flow in which the slag flow 33 and the parallel two-phase flow 34 are mixed.
合流部７は、２つの流入流路と１つの流出流路からなるＴ字流路又はＹ字流路を有することができる。また、合流部７は、流出流路に内挿されたビーズを有することができる。それによってスラグ流を容易に形成できる。
合流部７は、例えばＴ字管であってもよく、Ｙ字管であってもよい。この場合、細長い流路６にスラグ流３３、平行二相流３４又は混合流を流すことができる。また、細長い流路６の流動形態が混合流の場合、流動形態がスラグ流３３から平行二相流３４に変化する場合や流動形態が平行二相流３４からスラグ流３３に変化する場合がある。
また、合流部７は、ビーズ内挿型マイクロリアクタであってもよい。この場合、細長い流路６の流動形態は、約１ｍｍのスラグ流３３とすることができる。
The merging portion 7 can have a T-shaped channel or a Y-shaped channel including two inflow channels and one outflow channel. Moreover, the junction part 7 can have a bead inserted in the outflow channel. Thereby, a slag flow can be easily formed.
The junction 7 may be, for example, a T-shaped tube or a Y-shaped tube. In this case, the slug flow 33, the parallel two-phase flow 34, or the mixed flow can flow through the elongated flow path 6. Further, when the flow form of the elongated channel 6 is a mixed flow, the flow form may change from the slag flow 33 to the parallel two-phase flow 34 or the flow form may change from the parallel two-phase flow 34 to the slag flow 33. .
Further, the junction 7 may be a bead-inserted microreactor. In this case, the flow form of the elongated channel 6 can be a slug flow 33 of about 1 mm.
２．電場の形成
本実施形態の解乳化装置３０は、第１電極１と第２電極２とを有する電極対４と、電極対４に電圧を印加する電源回路１０とを備える。第１電極１と第２電極２は、その間に交流電場が発生するように設けられる。例えば、板状の第１電極１と板状の第２電極２とを流路部材８を挟んで重ねて配置することができる。また、第１電極１と第２電極２とは平行に配置することができる。また、第１電極１または第２電極２は、平板状とすることができる。このような構成において、電源回路１０により第１電極１と第２電極２との間に交流電圧を印加すると、第１電極１と第２電極２との間に交流電場を生じさせることができる。
また、第１電極１または第２電極２は、方形の金属板であってもよく、正方形の金属板であってもよい。第１電極１の材料または第２電極２の材料は、導電性材料であれば特に限定されないが、例えば金属銅、金属銀、金属アルミニウムなどである。
また、第１電極１または第２電極２は、電極端子を有してもよい。このことにより、電極端子を介して電源回路１０と接続することができる。
2. Formation of Electric Field The demulsification device 30 of this embodiment includes an electrode pair 4 having a first electrode 1 and a second electrode 2, and a power supply circuit 10 that applies a voltage to the electrode pair 4. The first electrode 1 and the second electrode 2 are provided so that an alternating electric field is generated therebetween. For example, the plate-like first electrode 1 and the plate-like second electrode 2 can be arranged so as to overlap each other with the flow path member 8 interposed therebetween. Moreover, the 1st electrode 1 and the 2nd electrode 2 can be arrange | positioned in parallel. Moreover, the 1st electrode 1 or the 2nd electrode 2 can be made into flat form. In such a configuration, when an AC voltage is applied between the first electrode 1 and the second electrode 2 by the power supply circuit 10, an AC electric field can be generated between the first electrode 1 and the second electrode 2. .
The first electrode 1 or the second electrode 2 may be a square metal plate or a square metal plate. Although the material of the 1st electrode 1 or the material of the 2nd electrode 2 will not be specifically limited if it is an electroconductive material, For example, they are metal copper, metal silver, metal aluminum, etc.
Moreover, the 1st electrode 1 or the 2nd electrode 2 may have an electrode terminal. Thus, the power supply circuit 10 can be connected via the electrode terminal.
電源回路１０は、第１電極１と第２電極２との間に交流電圧を印加することができれば特に限定されないが、例えば、高電圧発生装置１８を備えることができる。このことにより、第１電極１と第２電極２との間に強い電場を発生させることができる。また、電源回路１０は、高電圧発生装置１８とファンクションジェネレータ１９の両方を備えることもできる。このことにより、第１電極１と第２電極２との間に、任意の周波数と波形を持った交流電圧を印加することができる。
また、電源回路１０は、第１電極１と第２電極２との間に１０×１０4Ｖ／ｍ以上５００×１０4Ｖ／ｍ以下の電場が生じるように電極対４に電圧を印加することができる。さらに、電源回路１０は、第１電極１と第２電極２との間に１０Ｈｚ以上５００Ｈｚ以下の交流電圧を印加することができる。電源回路１０により、第１電極１と第２電極２との間に交流電圧を印加する場合、交流電圧の波形は、正弦波であってもよく、矩形波であってもよく、三角波であってもよい。
Although the power supply circuit 10 will not be specifically limited if an alternating voltage can be applied between the 1st electrode 1 and the 2nd electrode 2, For example, the high voltage generator 18 can be provided. Thereby, a strong electric field can be generated between the first electrode 1 and the second electrode 2. The power supply circuit 10 can also include both the high voltage generator 18 and the function generator 19. Thereby, an alternating voltage having an arbitrary frequency and waveform can be applied between the first electrode 1 and the second electrode 2.
The power supply circuit 10 applies a voltage to the electrode pair 4 so that an electric field of 10 × 10 4 V / m or more and 500 × 10 4 V / m or less is generated between the first electrode 1 and the second electrode 2. be able to. Furthermore, the power supply circuit 10 can apply an AC voltage of 10 Hz to 500 Hz between the first electrode 1 and the second electrode 2. When an AC voltage is applied between the first electrode 1 and the second electrode 2 by the power supply circuit 10, the waveform of the AC voltage may be a sine wave, a rectangular wave, or a triangular wave. May be.
第１電極１と第２電極２との間に生じさせる電場の電界強度（Ｖ／ｍ）は、第１電極１と第２電極２との間に印加する電圧を第１電極１と第２電極２との間隔Ｄで割った値で表すことができる。第１電極１と第２電極２との間隔Ｄは、例えば、０．２ｍｍ以上４０ｍｍ以下とすることができる。このことにより、比較的低い印加電圧で第１電極１と第２電極２との間に高い電界強度の電場を発生させることができる。
第１電極１と第２電極２との間隔Ｄは、第１電極１と第２電極２との間に一定の厚みを有するスペーサ２６を設けることにより、一定の間隔とすることができる。また、第１電極１と第２電極２との間隔Ｄは、流路部材８の厚さを一定にすることにより、一定の間隔とすることもできる。
なお、スペーサ２６の材料は、絶縁性材料とすることができ、例えば、良好な電気絶縁性を有するプラスチックとすることができる。また、スペーサ２６の材料は、例えば、アセタール樹脂とすることができる。
The electric field strength (V / m) of the electric field generated between the first electrode 1 and the second electrode 2 is a voltage applied between the first electrode 1 and the second electrode 2. It can be represented by a value divided by the distance D from the electrode 2. The distance D between the first electrode 1 and the second electrode 2 can be set to, for example, 0.2 mm or more and 40 mm or less. Thereby, an electric field having a high electric field strength can be generated between the first electrode 1 and the second electrode 2 with a relatively low applied voltage.
The distance D between the first electrode 1 and the second electrode 2 can be made constant by providing a spacer 26 having a constant thickness between the first electrode 1 and the second electrode 2. Further, the distance D between the first electrode 1 and the second electrode 2 can be made constant by making the thickness of the flow path member 8 constant.
The material of the spacer 26 can be an insulating material, for example, a plastic having good electrical insulation. The material of the spacer 26 can be, for example, an acetal resin.
３．電場による解乳化
合流部７で形成したスラグ流３３、平行二相流３４又は混合流が流れる細長い流路６は、第１電極１と第２電極２とに挟まれる。このため、細長い流路６を流れるエマルション相１３と有機溶剤相２３とからなるスラグ流３３、平行二相流３４又は混合流に電極対４により交流電場を長時間印加することができる。このことにより、エマルション１２を解乳化することができる。このことは、本発明者が行った実験により実証された。
解乳化のメカニズムは明らかではないが、次のように考えられる。交流電場により微小空間のエマルション相１３に循環流が生じ、この循環流によりエマルション相１３に含まれる油相が有機溶剤相に合一化されると考えられる。このため、エマルション相１３に含まれる水相３１と油相３２とが分離し、エマルションが解乳化されると考えられる。
例えば、図５（ａ）（ｂ）のように、交流電場下では、エマルション相１３に含まれる油相３２は、有機溶剤相２３に吸収されていくと考えられる。
3. Demulsification by an electric field A slender flow path 6 in which a slag flow 33, a parallel two-phase flow 34 or a mixed flow formed in the merge section 7 flows is sandwiched between the first electrode 1 and the second electrode 2. Therefore, an alternating electric field can be applied for a long time by the electrode pair 4 to the slag flow 33, the parallel two-phase flow 34, or the mixed flow composed of the emulsion phase 13 and the organic solvent phase 23 flowing through the elongated flow path 6. Thereby, the emulsion 12 can be de-emulsified. This was verified by experiments conducted by the present inventors.
The mechanism of demulsification is not clear, but is considered as follows. It is considered that a circulating flow is generated in the emulsion phase 13 in a minute space by the alternating electric field, and the oil phase contained in the emulsion phase 13 is united with the organic solvent phase by this circulating flow. For this reason, it is thought that the water phase 31 and the oil phase 32 contained in the emulsion phase 13 are separated, and the emulsion is demulsified.
For example, as shown in FIGS. 5A and 5B, the oil phase 32 contained in the emulsion phase 13 is considered to be absorbed by the organic solvent phase 23 under an alternating electric field.
細長い流路６を形成する流路部材８は、内部に流路６を有するチューブ状であってもよく、内部に細長い流路６を有する板状であってもよい。また、流路部材８は、少なくとも一部が第１電極１と第２電極２とに挟まれる。このことにより、細長い流路６のスラグ流３３、平行二相流３４又は混合流に電極対４間の交流電場を印加することができ、スラグ流３３、平行二相流３４又は混合流を電場処理することができる。また、このことにより、流路６のスラグ流３３、平行二相流３４又は混合流を連続して電場処理することが可能になる。また、第１電極１と第２電極２と流路部材８とは、電場形成部１１を構成してもよい。 The channel member 8 forming the elongated channel 6 may be a tube having the channel 6 inside, or may be a plate having the elongated channel 6 inside. In addition, at least a part of the flow path member 8 is sandwiched between the first electrode 1 and the second electrode 2. Thus, an alternating electric field between the electrode pair 4 can be applied to the slug flow 33, the parallel two-phase flow 34, or the mixed flow of the elongated channel 6, and the slug flow 33, the parallel two-phase flow 34, or the mixed flow can be applied to the electric field. Can be processed. In addition, this makes it possible to continuously treat the slag flow 33, the parallel two-phase flow 34, or the mixed flow in the flow path 6 with an electric field. Further, the first electrode 1, the second electrode 2, and the flow path member 8 may constitute an electric field forming unit 11.
細長い流路６は、直線状に設けられてもよく、屈曲部を有するように設けられてもよく、蛇行するように設けられてもよい。例えば、図１〜３に示したように、流路部材８は、チューブ状であり、流路６が蛇行するように設けることができる。このように流路６を蛇行するように設けることにより、流路６の距離を長くしても解乳化装置３０が大型化することを抑制することができる。
流路部材８（細長い流路６）の一方の端は合流部７に接続することができ、他方の端は貯留槽２１に接続することができる。このことにより、合流部７で形成したスラグ流３３、平行二相流３４又は混合流を細長い流路６に流し電場処理することができ、電場処理後の液体を貯留槽２１に流入させることができる。
電極対４の間において、細長い流路６の長さは、例えば１０ｃｍ以上５０ｍ以下とすることができ、好ましくは１０ｃｍ以上１０ｍ以下とすることができる。なお、細長い流路６の一部が電極対４からはみ出している場合には、細長い流路６の電極対４に挟まれた部分の長さの合計が１０ｃｍ以上５０ｍ以下とすることができ、好ましくは１０ｃｍ以上１０ｍ以下とすることができる。また、細長い流路６の長さ、スラグ流などの流量、又はその両方を変更することにより、スラグ流３３又は平行二相流３４を電場処理する時間を変更することができる。
また、流路部材８が柔軟性を有するチューブである場合、図１〜３に示したように、流路部材８を配置する位置が定まるようにスペーサ２６を設けてもよい。このことにより、流路部材８を第１電極１と第２電極２との間に安定して配置することができる。なお、図１〜３に示した電場形成部１１では、第１電極１と第２電極２との間に流路部材８が蛇行して配置されるスペースを空けて配置されたスペーサ２６が設けられている。
The elongated channel 6 may be provided in a straight line, may be provided with a bent portion, or may be provided so as to meander. For example, as illustrated in FIGS. 1 to 3, the flow path member 8 has a tubular shape and can be provided so that the flow path 6 meanders. Thus, by providing the flow path 6 so as to meander, it is possible to prevent the demulsification apparatus 30 from increasing in size even if the distance of the flow path 6 is increased.
One end of the flow path member 8 (elongated flow path 6) can be connected to the junction 7, and the other end can be connected to the storage tank 21. As a result, the slag flow 33, the parallel two-phase flow 34 or the mixed flow formed at the merging portion 7 can be flowed into the elongated channel 6 to be subjected to the electric field treatment, and the liquid after the electric field treatment can be caused to flow into the storage tank 21. it can.
Between the electrode pair 4, the length of the elongate flow path 6 can be 10 cm or more and 50 m or less, for example, Preferably it can be 10 cm or more and 10 m or less. When a part of the elongated channel 6 protrudes from the electrode pair 4, the total length of the portions sandwiched between the electrode pair 4 of the elongated channel 6 can be 10 cm or more and 50 m or less, Preferably, it can be 10 cm or more and 10 m or less. Moreover, the electric field process time of the slag flow 33 or the parallel two-phase flow 34 can be changed by changing the length of the elongated channel 6, the flow rate of the slag flow, or both.
In addition, when the flow path member 8 is a flexible tube, as shown in FIGS. 1 to 3, the spacer 26 may be provided so that the position where the flow path member 8 is arranged is determined. Thus, the flow path member 8 can be stably disposed between the first electrode 1 and the second electrode 2. In the electric field forming unit 11 shown in FIGS. 1 to 3, a spacer 26 is provided between the first electrode 1 and the second electrode 2 so as to provide a space in which the flow path member 8 meanders. It has been.
細長い流路６は、電極対４間において同一平面上に設けられてもよい。このことにより、流路６の長さが長い場合でも、第１電極１と第２電極２との間隔を狭くすることができ、第１電極１と第２電極２との間に強い電場を発生させることができる。細長い流路６は、例えば、図２、３に示した電場形成部１１のように破線Ｂ−Ｂを含む平面上に設けることができる。
また、流路部材８は、第１電極１及び第２電極２の両方に接触するように設けることができる。このことにより、第１電極１と第２電極２との間隔を狭くすることができ、流路６に流れるスラグ流３３、平行二相流３４又は混合流に大きい電場をかけることができる。
The elongate channel 6 may be provided on the same plane between the electrode pair 4. Thereby, even when the length of the flow path 6 is long, the distance between the first electrode 1 and the second electrode 2 can be reduced, and a strong electric field is generated between the first electrode 1 and the second electrode 2. Can be generated. The elongate channel 6 can be provided on a plane including a broken line BB like the electric field forming unit 11 shown in FIGS.
Further, the flow path member 8 can be provided so as to contact both the first electrode 1 and the second electrode 2. Thereby, the space | interval of the 1st electrode 1 and the 2nd electrode 2 can be narrowed, and a big electric field can be applied to the slag flow 33, the parallel two-phase flow 34, or mixed flow which flows into the flow path 6.
流路部材８が有する細長い流路６の断面の形状は、特に限定されないが、例えば、円形、方形とすることができる。また、細長い流路６は、対向する内壁間の最短距離ｄが０．１ｍｍ以上３０ｍｍ以下となるように設けることができる。また、細長い流路６の断面が円形の場合、細長い流路６の直径ｄは、０．１ｍｍ以上３０ｍｍ以下とすることができる。また、流路６が電極対４間において同一平面上に設けられた場合、この平面に垂直な方向の流路６の対向する内壁間の距離ｄが０．１ｍｍ以上３０ｍｍ以下となるように流路６を設けることができる。例えば、流路部材８には、内径１ｍｍ、外径３ｍｍのフッ素ゴムチューブを用いることができる。
このような構成にすることにより、微小空間を流れるスラグ流３３、平行二相流３４又は混合流に強い交流電場を印加することができる。
The shape of the cross section of the elongated channel 6 included in the channel member 8 is not particularly limited, but may be, for example, a circle or a rectangle. Moreover, the elongate flow path 6 can be provided so that the shortest distance d between the opposing inner walls may be 0.1 mm or more and 30 mm or less. Moreover, when the cross section of the elongate flow path 6 is circular, the diameter d of the elongate flow path 6 can be 0.1 mm or more and 30 mm or less. Further, when the flow path 6 is provided on the same plane between the electrode pair 4, the distance d between the opposing inner walls of the flow path 6 in the direction perpendicular to the plane is 0.1 mm or more and 30 mm or less. A path 6 can be provided. For example, the flow path member 8 can be a fluororubber tube having an inner diameter of 1 mm and an outer diameter of 3 mm.
With such a configuration, a strong alternating electric field can be applied to the slag flow 33, the parallel two-phase flow 34, or the mixed flow that flows through the minute space.
流路部材８の材料は、絶縁性材料とすることができる。このことにより、電極対４の間隔を狭くしても電極対４間にリーク電流が流れることを抑制することができる。また、第１電極１と第２電極２との間隔を狭くすることができ、流路６のスラグ流３３、平行二相流３４又は混合流に大きい交流電場を印加することができる。
また、流路部材８の材料は、エマルション１２及び有機溶剤２２に対する耐食性を有する材料とすることができる。流路部材８の材料は、例えば、ガラス、シリコン樹脂、フッ素樹脂などである。
The material of the flow path member 8 can be an insulating material. As a result, it is possible to suppress the leakage current from flowing between the electrode pair 4 even if the distance between the electrode pair 4 is narrowed. Moreover, the space | interval of the 1st electrode 1 and the 2nd electrode 2 can be narrowed, and a big alternating electric field can be applied to the slag flow 33 of the flow path 6, the parallel two-phase flow 34, or a mixed flow.
Further, the material of the flow path member 8 can be a material having corrosion resistance to the emulsion 12 and the organic solvent 22. The material of the flow path member 8 is, for example, glass, silicon resin, fluorine resin, or the like.
４．油水分離
本実施形態の解乳化装置３０は、細長い流路６を流れた液体が流入する貯留槽２１を備えることができる。電極対４により電場処理されたスラグ流３３、平行二相流３４又は混合流は、貯留槽２１に流入する。
スラグ流３３、平行二相流３４又は混合流に含まれるエマルション相１３は電場処理により解乳化されているため、貯留槽２１には、エマルションの油相が溶解した有機溶剤相と実質的に油相を含まない水相とのスラグ流３３、平行二相流３４又は混合流が流入する。この流入した液体を貯留槽２１に貯留することにより、水と有機溶剤の比重の差により、水が下層となり、有機溶剤が上層となるように分離する。このため、水と有機溶剤とを分離して処理することが可能になる。また、分離された有機溶剤は、エマルション２２を解乳化する有機溶剤２２として再利用することができる。なお、エマルション２２に含まれる界面活性剤は、上層の有機溶剤層と下層の水層との間の界面活性剤含有物２９として分離される。
4). Oil / Water Separation The demulsification apparatus 30 of the present embodiment can include a storage tank 21 into which the liquid that has flowed through the elongated channel 6 flows. The slag flow 33, the parallel two-phase flow 34 or the mixed flow that has been subjected to the electric field treatment by the electrode pair 4 flows into the storage tank 21.
Since the emulsion phase 13 contained in the slag flow 33, the parallel two-phase flow 34 or the mixed flow is demulsified by electric field treatment, the storage tank 21 has substantially the same organic solvent phase as the oil phase of the emulsion and the oil. A slag flow 33, a parallel two-phase flow 34 or a mixed flow with an aqueous phase not containing a phase flows in. By storing this inflowing liquid in the storage tank 21, it separates so that water becomes a lower layer and an organic solvent becomes an upper layer due to the difference in specific gravity between water and the organic solvent. For this reason, it becomes possible to separate and process water and the organic solvent. Further, the separated organic solvent can be reused as the organic solvent 22 for demulsifying the emulsion 22. The surfactant contained in the emulsion 22 is separated as a surfactant-containing material 29 between the upper organic solvent layer and the lower aqueous layer.
解乳化実験１
図１〜３に示したような解乳化装置３０を用いて解乳化実験を行った。ただし、合流部７へのエマルション１２及び有機溶剤２２の供給は、図４に示したようなシリンジポンプ１７ａ、１７ｂを用いた。
合流部７には、ビーズ内挿型マイクロリアクタ又はＹ字管とした。合流部７にビーズ内挿型マイクロリアクタを用いると細長い流路６の流動形態は約１ｍｍのスラグ流となる。
合流部７にＹ字管を用いると細長い流路６の流動形態は、スラグ流、平行二相流又は混合流となる。流動形態が混合流の場合、流動形態がスラグ流から平行二相流に変化する場合や平行二相流からスラグ流に変化する場合がある。流動形態がスラグ流の場合、ビーズ内挿型マイクロリアクタを用いる場合に比べ、スラグ流の各相の長さは長くなる。
Demulsification experiment 1
The demulsification experiment was performed using the demulsification apparatus 30 as shown in FIGS. However, the syringe pumps 17a and 17b as shown in FIG. 4 were used to supply the emulsion 12 and the organic solvent 22 to the merging section 7.
The junction 7 is a bead-inserted microreactor or a Y-shaped tube. When a bead-inserted microreactor is used for the merging section 7, the flow form of the elongated channel 6 becomes a slag flow of about 1 mm.
If a Y-shaped tube is used for the junction 7, the flow form of the elongated channel 6 is a slag flow, a parallel two-phase flow, or a mixed flow. When the flow form is a mixed flow, the flow form may change from a slag flow to a parallel two-phase flow or may change from a parallel two-phase flow to a slag flow. When the flow form is a slag flow, the length of each phase of the slag flow becomes longer than when a bead-inserted microreactor is used.
電場形成部１１では、第１電極１及び第２電極２にそれぞれ１００ｍｍ×１００ｍｍの銅板を用い、アセタール樹脂製のスペーサ２６を第１電極１と第２電極２との間に設け、流路部材８が蛇行して配置されるように第１電極１と第２電極２との間に空間を設けた。また、第１電極１と第２電極２との間隔は３ｍｍとした。また、リーク電流の抑制および安全性の向上のために、第１電極１と第２電極２とを挟むようにアセタール樹脂製のカバーを設けた。流路部材８には、フッ素樹脂製のチューブ（外径３ｍｍ、内径１ｍｍ）を用い、スペーサ２６により形成された空間に流路部材８を配置した。なお、第１電極１と第２電極２との間に位置するチューブの長さは、約７６０ｍｍである。また、流路部材８の一方の端は、合流部７に接続し、流路部材８の他方の端は、貯留槽２１であるメスシリンダー内に配置した。 In the electric field forming unit 11, a copper plate of 100 mm × 100 mm is used for each of the first electrode 1 and the second electrode 2, an acetal resin spacer 26 is provided between the first electrode 1 and the second electrode 2, and a flow path member A space was provided between the first electrode 1 and the second electrode 2 so that 8 was meandered. The distance between the first electrode 1 and the second electrode 2 was 3 mm. Further, an acetal resin cover was provided so as to sandwich the first electrode 1 and the second electrode 2 in order to suppress leakage current and improve safety. As the flow path member 8, a fluororesin tube (outer diameter 3 mm, inner diameter 1 mm) was used, and the flow path member 8 was disposed in a space formed by the spacer 26. In addition, the length of the tube located between the 1st electrode 1 and the 2nd electrode 2 is about 760 mm. Further, one end of the flow path member 8 was connected to the merging portion 7, and the other end of the flow path member 8 was disposed in the graduated cylinder that is the storage tank 21.
水相と油相とを１０：１の体積比で混合し、界面活性剤を所定量添加し、ホモジナイザを用いて24000rpmで６０秒攪拌して表１に示した試料１〜２４のエマルションを調製した（エマルションの油含有量：約９％）。水相には、純水、ＮａＣｌ水溶液、ＣａＣｌ2水溶液又はＬａＣｌ3水溶液を用いた。各水溶液のイオン強度は０．２７mol・L-1とした。油相には、ｐ−キシレン又はトルエンを用いた。界面活性剤には、ソルビタンモノオレエート（Span80）、ポリオキシエチレンソルビタンモノラウラート（Tween20）又は直鎖アルキルベンゼンスルホン酸ナトリウム（LAS）を用いた。調製したエマルションは、水中油型エマルションになっていると考えられる。 A water phase and an oil phase are mixed at a volume ratio of 10: 1, a predetermined amount of a surfactant is added, and the mixture is stirred for 60 seconds at 24000 rpm using a homogenizer to prepare emulsions of samples 1 to 24 shown in Table 1. (Oil content of emulsion: about 9%). For the aqueous phase, pure water, NaCl aqueous solution, CaCl 2 aqueous solution or LaCl 3 aqueous solution was used. The ionic strength of each aqueous solution was 0.27 mol·L −1 . In the oil phase, p-xylene or toluene was used. As the surfactant, sorbitan monooleate (Span 80), polyoxyethylene sorbitan monolaurate (Tween 20), or sodium linear alkylbenzene sulfonate (LAS) was used. The prepared emulsion is considered to be an oil-in-water emulsion.
図４に示したようなシリンジポンプ１７ａに調製したエマルションを入れ、シリンジポンプ１７ｂに表１に示した有機溶剤を入れた。なお、有機溶剤には、エマルションの油相と同じ溶剤を用いた。
第１及び第２電極間の電界強度が１０００ｋＶ・ｍ-1となるように周波数１００Ｈｚの交流電圧を第１及び第２電極間に印加した状態で、シリンジポンプ１７ａ、１７ｂによりエマルション及び有機溶剤を５０：５０で合流部７に供給し、合流部７で形成されたスラグ流、平行二相流又は混合流を第１及び第２電極間の細長い流路６に流した。そして、細長い流路６を流れるスラグ流、平行二相流又は混合流に交流電場を印加した後、スラグ流、平行二相流又は混合流をメスシリンダーに流し込んだ。メスシリンダーに回収した液体は、自然分離させ、解乳化の成否を目視で判断した。なお、合流部７へのエマルション及び有機溶剤の供給流量は、スラグ流、平行二相流又は混合流が細長い流路を流れる間に約２１５秒間交流電場が印加されるように調節した。
The prepared emulsion was put into the syringe pump 17a as shown in FIG. 4, and the organic solvent shown in Table 1 was put into the syringe pump 17b. As the organic solvent, the same solvent as the oil phase of the emulsion was used.
In a state where an alternating voltage of a frequency of 100 Hz is applied between the first and second electrodes so that the electric field strength between the first and second electrodes is 1000 kV · m −1 , the emulsion and the organic solvent are removed by the syringe pumps 17a and 17b. The slag flow, the parallel two-phase flow, or the mixed flow formed at the merging portion 7 was supplied to the elongated flow path 6 between the first and second electrodes at 50:50. Then, an AC electric field was applied to the slag flow, parallel two-phase flow, or mixed flow flowing through the elongated channel 6, and then the slag flow, parallel two-phase flow, or mixed flow was flowed into the graduated cylinder. The liquid collected in the graduated cylinder was naturally separated, and the success or failure of the demulsification was judged visually. In addition, the supply flow rates of the emulsion and the organic solvent to the junction 7 were adjusted so that an alternating electric field was applied for about 215 seconds while the slag flow, the parallel two-phase flow, or the mixed flow flowed through the elongated channel.
表１に解乳化実験における解乳化の成否を示した。解乳化実験において、表１において○を記したものは解乳化成功、一方、表１において×を記したものは解乳化不成功と判定されたものである。なお、横線で示した実験は行っていない。また、図６（ａ）は、解乳化に成功した試料３のメスシリンダーに回収した液体の写真であり（合流部７にビーズ内挿型マイクロリアクタを使用）、図６（ｂ）は解乳化に失敗した試料１０のメスシリンダーに回収した液体の写真である（合流部７にビーズ内挿型マイクロリアクタを使用）。
解乳化に成功した試料では、図６（ａ）に示した写真のように、下層の透明な水と、上層の透明なｐ−キシレンとが界面活性剤含有物を挟んで分離した。解乳化に失敗した試料では、図６（ｂ）に示した写真のように、下層の白濁したエマルションと上層の透明なｐ−キシレンとに分離した。
Table 1 shows the success or failure of the demulsification in the demulsification experiment. In the demulsification experiment, those marked with ◯ in Table 1 were judged as successful demulsification, while those marked with x in Table 1 were judged as unsuccessful demulsification. The experiment indicated by the horizontal line was not performed. FIG. 6 (a) is a photograph of the liquid collected in the graduated cylinder of Sample 3 that has been successfully demulsified (using a bead-inserted microreactor at the junction 7), and FIG. 6 (b) is for demulsification. It is the photograph of the liquid collect | recovered to the measuring cylinder of the sample 10 which failed (bead insertion type | mold microreactor is used for the confluence | merging part 7).
In the sample that succeeded in demulsification, as shown in the photograph shown in FIG. 6A, the transparent water in the lower layer and the transparent p-xylene in the upper layer were separated with the surfactant-containing material in between. In the sample that failed in demulsification, as shown in the photograph shown in FIG. 6 (b), it was separated into a white turbid emulsion in the lower layer and transparent p-xylene in the upper layer.
有機溶剤及びエマルションの油相にｐ−キシレンを用いた試料では、試料３、７、１１で解乳化に成功した。これらの試料では水相にCaCl2水溶液を用いている。
これらの解乳化に成功した試料３、７、１１では、合流部７にビーズ内挿型マイクロリアクタを用いた場合でも、Ｙ字管を用いた場合でも解乳化に成功した。一方、解乳化に失敗した試料１、２、４〜６、８〜１０、１２では、合流部７にビーズ内挿型マイクロリアクタを用いた場合でも、Ｙ字管を用いた場合でも解乳化に失敗した。従って、解乳化の成否は、その流動形態に依存しないと考えられる。
有機溶剤及びエマルションの油相にトルエンを用いた試料では、試料１４、１５、１６、２０、２４で解乳化に成功した。試料１４、１５、１６では界面活性剤にSpan80を用いており、試料２０、２４では水相にLaCl3水溶液を用いている。
従って、表１の結果からすると、エマルションの種類、有機溶剤の種類により、解乳化できる場合とできない場合があるけれども、エマルションを有機溶剤とともにスラグ流、平行二相流又は混合流を細長い流路に流しながら交流電場を印加することは、エマルションの解乳化に有効であることがわかる。
また表１に示す結果から、エマルションに添加剤を添加することや適切な有機溶剤を選択することにより、エマルションを解乳化できるとも考えられる。
Samples using p-xylene for the organic solvent and the oil phase of the emulsion were successfully demulsified in Samples 3, 7, and 11. In these samples, an aqueous CaCl 2 solution is used for the aqueous phase.
Samples 3, 7, and 11 that succeeded in demulsification succeeded in demulsification regardless of whether a bead-inserted microreactor or a Y-shaped tube was used for the junction 7. On the other hand, samples 1, 2, 4-6, 8-10, and 12 that failed in demulsification failed in demulsification regardless of whether a bead-inserted microreactor was used for the junction 7 or a Y-shaped tube was used. did. Therefore, it is considered that the success or failure of the demulsification does not depend on the flow form.
Samples using toluene for the organic solvent and the oil phase of the emulsion were successfully demulsified with Samples 14, 15, 16, 20, and 24. Samples 14, 15, and 16 use Span 80 as the surfactant, and Samples 20 and 24 use an aqueous LaCl 3 solution in the aqueous phase.
Therefore, according to the results in Table 1, depending on the type of emulsion and the type of organic solvent, demulsification may or may not be possible. It can be seen that applying an alternating electric field while flowing is effective for demulsification of the emulsion.
From the results shown in Table 1, it is also considered that the emulsion can be de-emulsified by adding an additive to the emulsion or selecting an appropriate organic solvent.
解乳化実験２（比較例）
スラグ流、平行二相流又は混合流を形成せずに、エマルションを細長い流路に流し交流電場を印加する解乳化実験を行った。この実験では、合流部７は使わずにシリンジポンプからエマルションを直接細長い流路６に供給して、エマルションに交流電場を印加した。エマルションの水相には純水を用い油相にはｐ−キシレンを用い界面活性剤にはSpan80を用いた。また、４種類の油含有量の異なるエマルションについて解乳化実験を行った。他の条件は解乳化実験１と同じにした。
図７に実験結果を示す。図７は、実験に用いたエマルションの油含有量と、解乳化率との関係を示すグラフである。解乳化率（％）は、式（電場印加処理により解乳化した油相の体積（ｍｌ））÷（実験に用いたエマルション中の油相の全体積（ｍｌ））×１００を用いて計算した。
油含有量が２０vol％を超えると高い解乳化率でエマルションを解乳化することができたが、油含有量が１７vol％以下であるとエマルションを解乳化できないことがわかった。
Demulsification experiment 2 (comparative example)
A demulsification experiment was conducted in which an emulsion was applied to an elongated channel and an alternating electric field was applied without forming a slag flow, a parallel two-phase flow or a mixed flow. In this experiment, the emulsion was directly supplied from the syringe pump to the elongate flow path 6 without using the merging portion 7, and an alternating electric field was applied to the emulsion. Pure water was used for the water phase of the emulsion, p-xylene was used for the oil phase, and Span 80 was used for the surfactant. In addition, demulsification experiments were performed on four types of emulsions having different oil contents. Other conditions were the same as in Demulsification Experiment 1.
FIG. 7 shows the experimental results. FIG. 7 is a graph showing the relationship between the oil content of the emulsion used in the experiment and the demulsification rate. The demulsification rate (%) was calculated using the formula (volume of oil phase demulsified by electric field application treatment (ml)) / (total volume of oil phase in emulsion used in experiment (ml)) × 100. .
When the oil content exceeded 20 vol%, the emulsion could be demulsified at a high demulsification rate, but when the oil content was 17 vol% or less, it was found that the emulsion could not be demulsified.
一方、スラグ流、平行二相流又は混合流に交流電場を印加した解乳化実験１では、油含有量が約９％のエマルションを解乳化することができた。従って、スラグ流、平行二相流又は混合流に交流電場を印加する解乳化方法は、油含有量の低いエマルションの解乳化に有効であることがわかった。 On the other hand, in the demulsification experiment 1 in which an alternating electric field was applied to a slag flow, a parallel two-phase flow, or a mixed flow, an emulsion having an oil content of about 9% could be demulsified. Therefore, it was found that the demulsification method in which an alternating electric field is applied to a slag flow, a parallel two-phase flow or a mixed flow is effective for demulsification of an emulsion having a low oil content.
１：第１電極 ２：第２電極 ４：電極対 ６：細長い流路 ７：合流部 ８：流路部材 １０：電源回路 １１：電場形成部 １２：エマルション １３：エマルション相 １４：エマルション槽 １５：ろ過部 １６ａ、１６ｂ：ポンプ １７ａ、１７ｂ：シリンジポンプ １８：高電圧発生装置 １９：ファンクションジェネレータ ２０：電線 ２１：貯留槽 ２２：有機溶剤 ２３：有機溶剤相 ２４：有機溶剤槽 ２５：添加部 ２６：スペーサ ２７：水相 ２８：有機溶剤相 ２９：界面活性剤含有物 ３０：解乳化装置 ３１：水相 ３２：油相 ３３：スラグ流 ３４：平行二相流 ３６：エマルション流路 ３７：有機溶剤流路 1: 1st electrode 2: 2nd electrode 4: Electrode pair 6: Elongated flow path 7: Merge part 8: Flow path member 10: Power supply circuit 11: Electric field forming part 12: Emulsion 13: Emulsion phase 14: Emulsion tank 15: Filtration part 16a, 16b: Pump 17a, 17b: Syringe pump 18: High voltage generator 19: Function generator 20: Electric wire 21: Storage tank 22: Organic solvent 23: Organic solvent phase 24: Organic solvent tank 25: Addition part 26: Spacer 27: Water phase 28: Organic solvent phase 29: Surfactant-containing material 30: Demulsifier 31: Water phase 32: Oil phase 33: Slag flow 34: Parallel two-phase flow 36: Emulsion channel 37: Organic solvent flow Road
Claims (8)
前記エマルションは、水中油型エマルションである請求項６に記載の解乳化方法。 Further comprising the step of combining the flow of the emulsion and the flow of the organic solvent to form the slag flow, the parallel two-phase flow or the mixed flow,
The demulsification method according to claim 6, wherein the emulsion is an oil-in-water emulsion.
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