JP7295554B2 - Supercritical fluid dispersion method - Google Patents

Supercritical fluid dispersion method Download PDF

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JP7295554B2
JP7295554B2 JP2019053466A JP2019053466A JP7295554B2 JP 7295554 B2 JP7295554 B2 JP 7295554B2 JP 2019053466 A JP2019053466 A JP 2019053466A JP 2019053466 A JP2019053466 A JP 2019053466A JP 7295554 B2 JP7295554 B2 JP 7295554B2
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恵一 佐野
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Jokoh Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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本発明は、超臨界流体分散方法に関し、特に被処理物を超臨界流体中に分散させて微小化する方法に関する。 TECHNICAL FIELD The present invention relates to a supercritical fluid dispersion method, and more particularly to a method of dispersing an object to be processed in a supercritical fluid and miniaturizing the object.

被処理物の微小化方法としては、従前、乾式または湿式の粉砕機が使用されている従前の乾式または湿式の粉砕機では、少量の微小化には不向きであった。発明者は、以前より被処理物と流体を混合した混合物を細管内に加圧しながら流動させることにより、効率的な少量の被処理物の微小化を実現してきた（例えば、特許文献１参照）。 Conventionally, dry or wet pulverizers have been used as a method for miniaturizing an object to be treated, but conventional dry or wet pulverizers were not suitable for miniaturization of a small amount. The inventor has realized efficient miniaturization of a small amount of the object to be processed by flowing a mixture of the object to be processed and a fluid while pressurizing it in a narrow tube (see, for example, Patent Document 1). .

混合物の細管内の流動に際し、処理効率の点から高速で流動させる必要があり、混合物は非常に高圧にして流動されていた。特に、水、有機溶媒の場合、被処理物と流体を混合した混合物の状態では高粘度となり流動性の低下が生じやすい。そのため、圧送用のポンプには高出力が要求され、装置自体の規模は大きくなりやすい。また配管は混合物の流動時の圧力負荷を受けるため、耐圧施工等が必要である。そこで、微小化のための設備負担は大きい。 When the mixture flows in the narrow tube, it is necessary to make it flow at a high speed from the viewpoint of processing efficiency, and the mixture is flowed under a very high pressure. In particular, in the case of water or an organic solvent, the mixture of the material to be treated and the fluid is highly viscous, and the fluidity tends to decrease. Therefore, a pump for pressure feeding is required to have a high output, and the scale of the device itself tends to be large. In addition, since the piping receives a pressure load when the mixture flows, it is necessary to perform pressure-resistant construction. Therefore, the equipment burden for miniaturization is large.

さらに、微小化の処理を終えて微小化された被処理物と溶媒となる流体の混合物から、目的の微小化された被処理物を分離する必要がある。水、有機溶媒の使用では、蒸発等の事後的な分離の処理が必要な場合もある。 Furthermore, it is necessary to separate the target micronized object to be processed from the mixture of the micronized object to be processed and the fluid serving as the solvent after finishing the micronization process. When water or an organic solvent is used, it may be necessary to perform post-separation such as evaporation.

特開２０１８－１００４７４号公報JP 2018-100474 A

そこで、発明者は、被処理物と混合した流体の良好な流動性を維持しつつ、処理後の分離の容易な被処理物の微小化の方法が望まれていた。本発明は前記の点に鑑みなされたものであり、被処理物と混合する流体に超臨界流体を用いることにより、処理時の良好な流動性と処理後の分離の容易さを兼ね備える超臨界流体分散方法を提供する。 Therefore, the inventors desired a method for miniaturizing an object to be processed that can be easily separated after processing while maintaining good fluidity of the fluid mixed with the object to be processed. The present invention has been made in view of the above points, and by using a supercritical fluid as the fluid to be mixed with the object to be processed, the supercritical fluid has both good fluidity during processing and easy separation after processing. Provide a distribution method.

すなわち、第１の形態は、被処理物を超臨界流体中に分散させて第１分散物を得る第１超臨界流体分散工程と、第１分散物を、小径流路部を備えてなるオリフィスホモジナイザ部へ加圧供給し第１分散物中の被処理物を微小化して第２分散物を得る第２超臨界流体分散工程と、を備えることを特徴とする。 That is, the first mode includes a first supercritical fluid dispersing step of dispersing an object to be processed in a supercritical fluid to obtain a first dispersion; and a second supercritical fluid dispersing step of pressurizing and supplying the material to the homogenizer to micronize the material to be processed in the first dispersion to obtain a second dispersion.

第２の形態は、第２超臨界流体分散工程において、第１分散物がオリフィスホモジナイザ部を通過後、通過後の第１分散物が再度オリフィスホモジナイザ部を通過することを繰り返して第２分散物が調製されることを特徴とする。 In the second form, in the second supercritical fluid dispersion step, after the first dispersion passes through the orifice homogenizer unit, the first dispersion after passing repeats passing through the orifice homogenizer unit again to obtain the second dispersion. is prepared.

第３の形態は、第２超臨界流体分散工程の後、第２分散物から超臨界流体を除去し被処理物の微小化物を単離する単離工程が加えられることを特徴とする。 A third embodiment is characterized in that an isolation step of removing the supercritical fluid from the second dispersion and isolating the micronized material to be processed is added after the second supercritical fluid dispersing step.

第４の形態は、超臨界流体が、二酸化炭素の超臨界流体であることを特徴とする。 A fourth aspect is characterized in that the supercritical fluid is a carbon dioxide supercritical fluid.

第５の形態は、オリフィスホモジナイザ部は、複数の流入側流路部と、複数の流出側流路部と、複数の流入側流路部を単一に集合させる集合部と、集合部の下流に接続されたオリフィス流路部と、オリフィス流路部の下流に接続されオリフィス流路部を分岐させ複数の流出側流路部と接続する分岐部と、を備えることを特徴とする。 In a fifth aspect, the orifice homogenizer section includes a plurality of inflow-side flow passages, a plurality of outflow-side flow passages, a collecting portion for collecting the plurality of inflow-side flow passages into a single unit, and a downstream of the collecting portion. and a branching portion connected downstream of the orifice flow path and branching the orifice flow path to connect with a plurality of outflow side flow paths.

本発明の超臨界流体分散方法によると、被処理物を超臨界流体中に分散させて第１分散物を得る第１超臨界流体分散工程と、第１分散物を、小径流路部を備えてなるオリフィスホモジナイザ部へ加圧供給し第１分散物中の被処理物を微小化して第２分散物を得る第２超臨界流体分散工程と、を備えるため、被処理物を微小化する処理時の良好な流動性と処理後の溶媒となる流体の分離の容易さを兼ね備えことができる。 According to the supercritical fluid dispersing method of the present invention, the first supercritical fluid dispersing step of dispersing the object to be processed in the supercritical fluid to obtain the first dispersion; and a second supercritical fluid dispersing step of pressurizing and supplying to an orifice homogenizer unit consisting of a second supercritical fluid to obtain a second dispersion by miniaturizing the object to be processed in the first dispersion. It is possible to combine good fluidity and ease of separation of the fluid that becomes the solvent after treatment.

超臨界流体分散方法を実施する第１実施形態の超臨界流体分散装置の全体構成図である。1 is an overall configuration diagram of a supercritical fluid dispersion apparatus of a first embodiment that implements a supercritical fluid dispersion method; FIG. オリフィスホモジナイザ部の主要部縦断面図である。FIG. 4 is a vertical cross-sectional view of main parts of an orifice homogenizer section; オリフィスホモジナイザ部の主要部横断面図である。FIG. 4 is a cross-sectional view of main parts of an orifice homogenizer section; 第１実施形態の超臨界流体分散装置の可動時の第１概略説明図である。FIG. 4 is a first schematic explanatory view of the supercritical fluid dispersion device of the first embodiment when it is movable. 第１実施形態の超臨界流体分散装置の可動時の第２概略説明図である。FIG. 4 is a second schematic explanatory view of the supercritical fluid dispersion device of the first embodiment when it is movable. 第２実施形態の超臨界流体分散装置の可動時の第１概略説明図である。FIG. 11 is a first schematic explanatory view of the supercritical fluid dispersion device of the second embodiment when it is movable. 第２実施形態の超臨界流体分散装置の可動時の第２概略説明図である。FIG. 11 is a second schematic explanatory view of the supercritical fluid dispersion device of the second embodiment when it is movable. 第２実施形態の超臨界流体分散装置の可動時の第３概略説明図である。FIG. 11 is a third schematic explanatory diagram of the supercritical fluid dispersion device of the second embodiment when it is movable.

本発明の超臨界流体分散方法を説明するに際し、図１の超臨界流体分散装置１（第１実施形態）の全体構成図を用いながら説明する。むろん、図示の装置はひとつの実施形態の開示であるため、本発明の超臨界流体分散方法を実現する構成は図示の形態に限定されない。 When explaining the supercritical fluid dispersion method of the present invention, it will be explained with reference to the overall configuration diagram of the supercritical fluid dispersion apparatus 1 (first embodiment) of FIG. Of course, since the illustrated apparatus is disclosed as one embodiment, the configuration for realizing the supercritical fluid dispersion method of the present invention is not limited to the illustrated form.

図示の超臨界流体分散装置１では、原料タンク３０、分岐ブロック４０、オリフィスホモジナイザ部１０、ポンプ部５０を備え、原料タンク３０に流体貯留タンク６０が接続される。そして、最終的に処理を終えた被処理物はドレイン部９０から回収される。 The illustrated supercritical fluid dispersion apparatus 1 includes a raw material tank 30 , a branch block 40 , an orifice homogenizer section 10 and a pump section 50 , and a fluid storage tank 60 is connected to the raw material tank 30 . Then, the object to be processed that has finally been processed is collected from the drain section 90 .

被処理物を貯留する原料タンク３０と、その下流の分岐ブロック４０は配管部８１を介して設置される。原料タンク３０は被処理物を貯留する耐圧容器であり、後出の超臨界流体の流通時の温度、圧力を維持可能な容器である。さらに、原料タンク３０には、攪拌機３１が設けられ、被処理物と超臨界流体は混合されて分散物となる。 A raw material tank 30 for storing a material to be processed and a branch block 40 downstream thereof are installed via a pipe portion 81 . The raw material tank 30 is a pressure-resistant container for storing the object to be processed, and is a container capable of maintaining the temperature and pressure during the flow of the supercritical fluid, which will be described later. Furthermore, the raw material tank 30 is provided with a stirrer 31, and the material to be processed and the supercritical fluid are mixed to form a dispersion.

図示の実施形態の超臨界流体分散装置１では、原料タンク３０が超臨界流体の温度及び圧力条件を維持する。原料タンク３０には加温器（ヒータ）等が設置される。なお、分散物の流動時の圧力は、流体貯留タンク６０から圧送ポンプ６１により供給される超臨界流体の供給圧力を通じて制御される。配管部８１には逆止弁７０と切替弁７１が設置される。分岐ブロック４０側から原料タンク３０側への逆流は逆止弁７０と切替弁７１により規制される。 In the supercritical fluid dispersion apparatus 1 of the illustrated embodiment, the raw material tank 30 maintains the temperature and pressure conditions of the supercritical fluid. A heater or the like is installed in the raw material tank 30 . The pressure during flow of the dispersion is controlled by the supply pressure of the supercritical fluid supplied from the fluid storage tank 60 by the pressure pump 61 . A check valve 70 and a switching valve 71 are installed in the piping portion 81 . Backflow from the branch block 40 side to the raw material tank 30 side is regulated by the check valve 70 and the switching valve 71 .

ポンプ部５０は分岐ブロック４０と配管部８２により接続される。また、オリフィスホモジナイザ部１０は配管部８３により分岐ブロック４０と接続される。さらに、オリフィスホモジナイザ部１０は配管部８４により原料タンク３０と接続される。ドレイン部９０側には配管部８６が設けられる。また、図示のとおり、各配管部には切替弁７２，７３，７４が接続される。各切替弁はポンプ部５０の動作時の流体の流路を規制する。各切替弁は電磁弁、手動弁の適宜である。配管部８１，８２，８３，８４，８５，８６は、保温性、耐圧性に優れた中空管体であり、被処理物と超臨界流体の混合により生じた分散物が温度及び圧力を維持しながら流動する。 The pump section 50 is connected to the branch block 40 by a piping section 82 . Also, the orifice homogenizer section 10 is connected to the branch block 40 by a pipe section 83 . Furthermore, the orifice homogenizer section 10 is connected to the raw material tank 30 by a piping section 84 . A piping portion 86 is provided on the drain portion 90 side. Also, as shown in the figure, switching valves 72, 73, and 74 are connected to the respective piping portions. Each switching valve regulates the flow path of the fluid during operation of the pump section 50 . Each switching valve may be an electromagnetic valve or a manual valve. The pipe parts 81, 82, 83, 84, 85, 86 are hollow pipe bodies with excellent heat insulation and pressure resistance, and the dispersion generated by mixing the object to be processed and the supercritical fluid maintains the temperature and pressure. flow while

分岐ブロック４０の構造は特段限定されないものの、金属等の耐圧材料から形成され、内部にＴ字状の流路が形成された部材である。または、分岐ブロック４０は公知の三方弁等でも良い。 Although the structure of the branch block 40 is not particularly limited, it is a member formed of a pressure-resistant material such as metal and having a T-shaped flow path formed therein. Alternatively, the branch block 40 may be a known three-way valve or the like.

ポンプ部５０は構造体内にピストン５１を備えており、一般にピストンポンプと称される。ピストン５１の後退時（後出の図３参照）、ポンプ部５０のハウジング５２内に被処理物と超臨界流体との混合により生じた分散物が流入する。ピストン５１の前進時（後出の図４参照）、被処理物と超臨界流体の分散物はポンプ部５０から吐出されてオリフィスホモジナイザ部１０に流入する。ピストン５１の前進及び後退は、油圧駆動またはサーボモータ等により制御される。被処理物と超臨界流体の分散物はオリフィスホモジナイザ部１０を通過後、原料タンク３０に流入する。 Pump section 50 includes a piston 51 within its structure and is commonly referred to as a piston pump. When the piston 51 is retracted (see FIG. 3 which will be described later), the dispersion produced by mixing the material to be treated and the supercritical fluid flows into the housing 52 of the pump section 50 . When the piston 51 advances (see FIG. 4 described later), the dispersion of the material to be processed and the supercritical fluid is discharged from the pump section 50 and flows into the orifice homogenizer section 10 . Advancement and retreat of the piston 51 are controlled by a hydraulic drive, a servomotor, or the like. After passing through the orifice homogenizer section 10 , the material to be processed and the supercritical fluid dispersion flow into the raw material tank 30 .

原料タンク３０の上流に超臨界流体を貯留する流体貯留タンク６０が設置され、配管部８５により接続される。超臨界流体を圧送する圧送ポンプ６１は配管部８５に設置され、超臨界流体は流体貯留タンク６０から原料タンク３０へ供給される。 A fluid storage tank 60 for storing a supercritical fluid is installed upstream of the raw material tank 30 and connected by a pipe section 85 . A pumping pump 61 for pumping the supercritical fluid is installed in the piping section 85 , and the supercritical fluid is supplied from the fluid storage tank 60 to the raw material tank 30 .

オリフィスホモジナイザ部１０を通過して微小化（粉砕）が進行した被処理物と超臨界流体の分散物は、最終的にドレイン部９０から超臨界流体分散装置１の外部に流出する。 The dispersion of the object to be processed and the supercritical fluid, which has passed through the orifice homogenizer section 10 and has been miniaturized (pulverized), finally flows out of the supercritical fluid dispersion apparatus 1 from the drain section 90 .

オリフィスホモジナイザ部１０について、図２の主要部縦断面図及び図３の主要部横断面図を用いてその構造を説明する。図２のＡ－Ａ線における横断面が図３（ａ）であり、図２のＢ－Ｂ線における横断面が図３（ｂ）であり、図２のＣ－Ｃ線における横断面が図３（ｃ）である。 The structure of the orifice homogenizer section 10 will be described with reference to the vertical cross-sectional view of the main part in FIG. 2 and the cross-sectional view of the main part in FIG. The cross section taken along line AA in FIG. 2 is shown in FIG. 3A, the cross section taken along line BB in FIG. 2 is shown in FIG. 3B, and the cross section taken along line CC in FIG. 3(c).

オリフィスホモジナイザ部１０は、第１ブロック２１と第２ブロック２２、そして第１ブロック２１と第２ブロック２２の間に介装される第３ブロック２３により形成される。第１ブロック２１において、複数の流入側流路部１１，１２が形成される（図２及び図３（ａ）参照）。また、第２ブロック２２においても、複数の流出側流路部１８，１９が形成される。 The orifice homogenizer section 10 is formed by a first block 21 , a second block 22 , and a third block 23 interposed between the first block 21 and the second block 22 . In the first block 21, a plurality of inflow-side channel portions 11 and 12 are formed (see FIGS. 2 and 3(a)). Also, in the second block 22, a plurality of outflow-side channel portions 18 and 19 are formed.

第１ブロック２１と第３ブロック２３との接合面に意図的に第１空隙部１４が形成される。この第１空隙部１４が複数の流入側流路部１１，１２を単一に集合させる集合部１３となる（図２及び図３（ｂ）参照）。集合部１３（第１空隙部１４）の下流側は第３ブロック２３となり、同第３ブロック２３内にオリフィス流路部１５が形成される（図２及び図３（ｃ）参照）。 A first gap 14 is intentionally formed in the joint surface between the first block 21 and the third block 23 . The first gap portion 14 becomes a gathering portion 13 that aggregates the plurality of inflow-side channel portions 11 and 12 into a single unit (see FIGS. 2 and 3(b)). A third block 23 is provided on the downstream side of the collecting portion 13 (first gap portion 14), and the orifice passage portion 15 is formed in the third block 23 (see FIGS. 2 and 3(c)).

オリフィス流路部１５の下流側においても、第３ブロック２３と第２ブロック２２との接合面にも意図的に第２空隙部１６が形成される。この第２空隙部１６がオリフィス流路部１５を分岐させて複数の流出側流路部１８，１９と接続する分岐部１７となる。 A second gap 16 is also intentionally formed on the joint surface between the third block 23 and the second block 22 on the downstream side of the orifice channel portion 15 . The second gap 16 branches the orifice channel portion 15 to form a branch portion 17 that connects to a plurality of outflow channel portions 18 and 19 .

流入側流路部１１，１２及び流出側流路部１８，１９の内直径（Ｄ１）は相互に同一であり、オリフィス流路部１５の内直径（Ｄ２）よりも大きく形成される。具体的には、内直径（Ｄ１）は、内直径（Ｄ２）の５ないし７倍である。また、第１空隙部１４の距離（Ｄ３）は内直径（Ｄ１）と同等に規定される。従って、オリフィス流路部１５は小径流路部である。 The inner diameters (D1) of the inflow-side channel portions 11 and 12 and the outflow-side channel portions 18 and 19 are the same and are formed larger than the inner diameter (D2) of the orifice channel portion 15 . Specifically, the inner diameter (D1) is 5 to 7 times the inner diameter (D2). Also, the distance (D3) of the first gap 14 is defined to be the same as the inner diameter (D1). Therefore, the orifice channel portion 15 is a small diameter channel portion.

次に、オリフィスホモジナイザ部１０を用いた際の作用を説明する。被処理物を超臨界流体中に分散させた分散物（圧送流体）は流入側流路部１１，１２を経由して集合部１３（第１空隙部１４）に侵入する。ここで、オリフィス流路部１５は流入側流路部１１，１２よりも狭小であるため、分散物の流量は低下する。そして、分散物（圧送流体）の圧力変化が生じ、それぞれの流入側流路部から流入した分散物は集合部１３において衝突する。このときの分散物中の被処理物同士は衝突時のエネルギーにより破砕される。このように、分散物が流入側流路部１１，１２からオリフィス流路部１５へ流動するごとに、分散物中の被処理物同士の衝突が進み、結果として分散物は粉砕される。 Next, the operation when the orifice homogenizer section 10 is used will be described. A dispersion (pressure-fed fluid) obtained by dispersing the object to be processed in the supercritical fluid enters the collecting portion 13 (first gap portion 14) via the inflow-side passage portions 11 and 12 . Here, since the orifice channel portion 15 is narrower than the inflow channel portions 11 and 12, the flow rate of the dispersed matter is reduced. Then, a pressure change occurs in the dispersed matter (pumped fluid), and the dispersed matter that has flowed in from each of the inflow-side channel portions collides at the gathering portion 13 . The objects to be treated in the dispersion at this time are crushed by the energy of collision. In this manner, each time the dispersed material flows from the inflow-side channel portions 11 and 12 to the orifice channel portion 15, the objects to be treated in the dispersed material collide with each other, and as a result, the dispersed material is pulverized.

図示の流入側流路部及び流入側流路部はともに２つである。むろん、流入側流路部及び流入側流路部の形成数は１以上である。ただし、分散物中の被処理物の衝突を促すため、流入側流路部及び流入側流路部の形成数は２以上であることがさらに望ましい。図示のオリフィスホモジナイザ部１０は、流入側及び流出側はともに対称形である。そこで、説明の便宜状流入側及び流出側としている。流入側と流出側が対称形であるため、オリフィスホモジナイザ部１０はいずれの向きからの流入においても機能し得る。従って、分散物が流出側流路部１８，１９から流入してオリフィス流路部１５通過し流入側流路部１１，１２より流出する場合もある。 There are two inflow-side channel portions and two inflow-side channel portions in the drawing. Of course, the number of inflow-side channel portions and inflow-side channel portions to be formed is one or more. However, in order to promote the collision of the material to be processed in the dispersed matter, it is more desirable that the number of the inflow-side channel portions and the number of the inflow-side channel portions formed is two or more. The illustrated orifice homogenizer section 10 is symmetrical on both the inlet and outlet sides. Therefore, for convenience of explanation, they are referred to as an inflow side and an outflow side. Since the inflow side and the outflow side are symmetrical, the orifice homogenizer section 10 can function with inflow from either direction. Therefore, there are cases where the dispersed material flows in from the outflow side passage portions 18 and 19, passes through the orifice passage portion 15, and flows out from the inflow side passage portions 11 and 12. FIG.

これより、第１実施形態の超臨界流体分散装置１を用い、本発明の超臨界流体分散方法を説明する。はじめに、被処理物は超臨界流体中に分散されて「第１分散物」となる（「第１超臨界流体分散工程」）。分散は原料タンク３０で行われる。 The supercritical fluid dispersion method of the present invention will now be described using the supercritical fluid dispersion apparatus 1 of the first embodiment. First, the object to be processed is dispersed in the supercritical fluid to form a "first dispersion" ("first supercritical fluid dispersion step"). Dispersion takes place in raw material tank 30 .

微小化の対象である被処理物は、例えば、セルロース、グラファイト、グラフェン、カーボンナノチューブ、複合金属酸化物（スピネル、ペロブスカイト等の結晶質）等の多岐にわたる物質である。被処理物同士の衝突を通じて微小化することにより、事後的に樹脂等に混合する際の均一な分散性が高まる。そのため、素材の性能向上が見込まれる。 Objects to be processed, which are targets for miniaturization, include a wide variety of substances such as cellulose, graphite, graphene, carbon nanotubes, and composite metal oxides (crystalline materials such as spinel and perovskite). By miniaturizing the objects to be treated through collision with each other, uniform dispersibility is enhanced when mixed with resin or the like afterwards. Therefore, performance improvement of the material is expected.

この分散方法において使用される超臨界流体は二酸化炭素または水である。特に、二酸化炭素は、常温、常圧下において気化するため超臨界流体として好ましい。また、極性を有する分子ではあるものの、水と比較して極性に伴う反応性は弱い。超臨界流体が二酸化炭素の場合、ドレイン部９０からの放出後、二酸化炭素のみが常温、常圧下において気化する。このため、分散後の分離は極めて容易である。 The supercritical fluid used in this dispersion method is carbon dioxide or water. In particular, carbon dioxide is preferred as a supercritical fluid because it evaporates under normal temperature and normal pressure. Also, although it is a polar molecule, its reactivity associated with polarity is weaker than that of water. When the supercritical fluid is carbon dioxide, only the carbon dioxide vaporizes under normal temperature and normal pressure after being discharged from the drain part 90 . Therefore, separation after dispersion is extremely easy.

ここで、超臨界流体は、各物質に特有の温度、圧力条件により液体と気体の区別がつかない状態となった流体である。具体的に、二酸化炭素の臨界温度は３０４．１Ｋ、臨界圧力は７．３８ＭＰａであり、水の臨界温度は６４７．３Ｋ、臨界圧力は２２．１２ＭＰａであり、エタンの臨界温度は３０５．３Ｋ、臨界圧力は４．８７ＭＰａであり、プロパンの臨界温度は３６９．８Ｋ、臨界圧力は４．２５ＭＰａである。 Here, a supercritical fluid is a fluid in which liquid and gas are indistinguishable due to temperature and pressure conditions specific to each substance. Specifically, carbon dioxide has a critical temperature of 304.1 K and a critical pressure of 7.38 MPa, water has a critical temperature of 647.3 K and a critical pressure of 22.12 MPa, and ethane has a critical temperature of 305.3 K, The critical pressure is 4.87 MPa, the critical temperature of propane is 369.8 K, and the critical pressure is 4.25 MPa.

超臨界流体は、通常状態の水、有機溶媒等と比較して高い流動性を備える。このことから被処理物を混合後の第１分散物の粘度低下が予想される。従って、配管部内、特には小径流路部を有するオリフィスホモジナイザ部１０へ加圧供給時の圧送時の抵抗軽減が期待される。 A supercritical fluid has higher fluidity than water, an organic solvent, or the like in a normal state. From this, it is expected that the viscosity of the first dispersion after mixing the material to be treated will decrease. Therefore, it is expected to reduce the resistance during pressurized supply to the orifice homogenizer 10 having a small-diameter flow path in the piping section, in particular.

超臨界流体には、二酸化炭素、水の他に、エタン、プロパン、エチレン等の有機分子を使用することも可能である。二酸化炭素と水は極性を有する分子である。そのため、超臨界流体分散装置１において処理を続ける間に、超臨界の条件により被処理物が極性分子により攻撃（反応）を受ける可能性もある。これに対し、エタン、プロパン、エチレンは、非極性の分子である。そのため、超臨界の条件が持続するとしても被処理物との反応性は乏しい。そこで、被処理物の性質を考慮して超臨界流体の種類は選択される。 In addition to carbon dioxide and water, organic molecules such as ethane, propane, and ethylene can also be used as supercritical fluids. Carbon dioxide and water are polar molecules. Therefore, while the processing is continued in the supercritical fluid dispersion apparatus 1, the object to be processed may be attacked (reacted) by polar molecules under supercritical conditions. In contrast, ethane, propane, and ethylene are non-polar molecules. Therefore, even if supercritical conditions persist, reactivity with the object to be treated is poor. Therefore, the type of supercritical fluid is selected in consideration of the properties of the object to be processed.

第１分散物は、小径流路部を有するオリフィスホモジナイザ部１０へ加圧供給される。加圧供給は、ポンプ部５０内のピストン５１の押圧力により行われる。第１分散物がオリフィスホモジナイザ部１０に流入して当該オリフィスホモジナイザ部１０を通過する。ここで、前述の説明のとおり、第１分散物中の被処理物は、オリフィスホモジナイザ部１０の流路内において衝突した際の衝撃エネルギーにより、当初よりも微小化が促進する。こうして第１分散物がオリフィスホモジナイザ部１０を通過することにより「第２分散物」が得られる（「第２超臨界流体分散工程」）。第２分散物は、第１分散物と比較して分子鎖長の縮小、結晶構造の崩壊等により、被処理物の微小化が進行した状態の分散物である。 The first dispersion is pressurized and supplied to an orifice homogenizer section 10 having a small diameter channel section. The pressurized supply is performed by the pressing force of the piston 51 inside the pump section 50 . The first dispersion flows into the orifice homogenizer section 10 and passes through the orifice homogenizer section 10 . Here, as described above, the material to be processed in the first dispersion is further miniaturized by the impact energy when it collides in the flow path of the orifice homogenizer section 10 . In this way, the first dispersion passes through the orifice homogenizer section 10 to obtain a "second dispersion" ("second supercritical fluid dispersion step"). The second dispersion is a dispersion in which the object to be processed is in a state of being microminiaturized due to reduction in molecular chain length, collapse of the crystal structure, etc. compared to the first dispersion.

第２超臨界流体分散工程の後、第２分散物は配管部８６を経由してドレイン部９０から放出される。超臨界流体に二酸化炭素を使用した場合、二酸化炭素の超臨界流体はドレイン部９０へ放出された第２分散物から蒸発により容易に除去される。結果、被処理物の微小化物は単離される（「単離工程」）。超臨界流体に水を使用した場合、被処理物の微小化物の単離のため、蒸発器（図示せず）等が別途ドレイン部９０に装備される。エタン、プロパン、エチレン等が超臨界流体である場合、これらは常温、常圧下では可燃性の気体であるため専用の回収器（図示せず）等が別途ドレイン部９０に装備される。 After the second supercritical fluid dispersion step, the second dispersion is discharged from drain section 90 via piping section 86 . If carbon dioxide is used as the supercritical fluid, the carbon dioxide supercritical fluid is easily removed from the second dispersion discharged to the drain portion 90 by evaporation. As a result, micronized substances of the object to be processed are isolated (“isolation step”). When water is used as the supercritical fluid, the drain section 90 is separately equipped with an evaporator (not shown) or the like for isolating minute particles of the object to be processed. When ethane, propane, ethylene, etc. are supercritical fluids, they are combustible gases under normal temperature and normal pressure, so a dedicated collector (not shown) or the like is separately installed in the drain part 90 .

単離工程は、超臨界流体の溶媒から微小化された被処理物（微小化物）を分離する際に加えられる工程である。例えば、セルロースの被処理物と超臨界流体の水が混合された状態において、微小化後においても微小化物を分離する必要が無い場合、つまり、湿潤な混合状態が所望されているときには、単離工程は省略される。 The isolation step is a step added when the miniaturized object to be processed (miniaturized object) is separated from the solvent of the supercritical fluid. For example, in a state in which the cellulose material to be processed and the water of the supercritical fluid are mixed, if there is no need to separate the micronized matter even after micronization, that is, when a wet mixed state is desired, isolation steps are omitted.

図４及び図５の概略説明図を用い、第１実施形態の超臨界流体分散装置１における流体の経路を説明する。はじめに、ポンプ部５０のピストン５１が後退し（図４の白抜き矢印方向）、ハウジング５２内が減圧する。そこで、原料タンク３０内の第１分散物は配管部８１、分岐ブロック４０、配管部８２を通じてポンプ部５０のハウジング５２内に流入する（図４参照）。このとき、第１分散物の流動する方向は原料タンク３０から分岐ブロック４０へ向かう正流方向であるため、逆止弁７０と弁開放状態の切替弁７１を通過可能である。 The fluid path in the supercritical fluid dispersion device 1 of the first embodiment will be described with reference to schematic explanatory diagrams of FIGS. 4 and 5. FIG. First, the piston 51 of the pump portion 50 retreats (in the direction of the white arrow in FIG. 4), and the pressure inside the housing 52 is reduced. Therefore, the first dispersion in the raw material tank 30 flows into the housing 52 of the pump section 50 through the piping section 81, the branch block 40, and the piping section 82 (see FIG. 4). At this time, since the flow direction of the first dispersion is the forward flow direction from the raw material tank 30 to the branch block 40, it can pass through the check valve 70 and the switching valve 71 in the open state.

次に、ポンプ部５０のピストン５１が前進し（図５の白抜き矢印方向）、ハウジング５２内の第１分散物はポンプ部５０から押出される。そして、第１分散物は配管部８２、分岐ブロック４０、配管部８３を通過してオリフィスホモジナイザ部１０に流入する。ポンプ部５０の押出力により、第１分散物は小径流路部を備えたオリフィスホモジナイザ部１０を通過することができる（図５参照）。 Next, the piston 51 of the pump portion 50 advances (in the direction of the white arrow in FIG. 5), and the first dispersion in the housing 52 is extruded from the pump portion 50 . Then, the first dispersion passes through the piping section 82 , the branch block 40 and the piping section 83 and flows into the orifice homogenizer section 10 . The pushing force of the pump section 50 allows the first dispersion to pass through the orifice homogenizer section 10 having a small diameter channel section (see FIG. 5).

第１分散物はオリフィスホモジナイザ部１０を通過することにより微小化が進み第２分散物となる。そして、第２分散物は配管部８４、切替弁７３を経由して原料タンク３０へ流入する。続いて、再度、原料タンク３０内の第１分散物（混入後の第２分散物）はポンプ部５０のハウジング５２内に流入し（図４参照）、ポンプ部５０の押出力により、第１分散物（混入後の第２分散物）はオリフィスホモジナイザ部１０を通過する（図５参照）。 As the first dispersion passes through the orifice homogenizer section 10, the miniaturization progresses to become the second dispersion. Then, the second dispersion flows into the raw material tank 30 via the piping section 84 and the switching valve 73 . Subsequently, the first dispersion (the second dispersion after mixing) in the raw material tank 30 again flows into the housing 52 of the pump section 50 (see FIG. 4), and the pushing force of the pump section 50 pushes the first dispersion. The dispersion (second dispersion after mixing) passes through the orifice homogenizer section 10 (see FIG. 5).

こうして、第１分散物はオリフィスホモジナイザ部１０を通過後、第１分散物が再度オリフィスホモジナイザ部１０を通過することを繰り返して第２分散物が調製される。即ち、オリフィスホモジナイザ部１０における被処理物の相互の衝突回数が増加して、より微小化が促進する。被処理物の微小化が十分に進行した時点において、第２分散物は配管部８６の先のドレイン部９０から放出される（図５中の破線矢印を参照。）。 Thus, after the first dispersion passes through the orifice homogenizer section 10, the first dispersion is repeatedly passed through the orifice homogenizer section 10 again to prepare a second dispersion. That is, the number of mutual collisions of the objects to be processed in the orifice homogenizer unit 10 increases, further promoting miniaturization. When the miniaturization of the object to be processed has sufficiently progressed, the second dispersion is discharged from the drain section 90 ahead of the piping section 86 (see the broken line arrow in FIG. 5).

さらに、図６，図７，図８の概略説明図を用い、第２実施形態の超臨界流体分散装置２における流体の経路を説明する。第２実施形態の超臨界流体分散装置２は、配管部８４に中間タンク３５を設置している。その他の構成は第１実施形態の超臨界流体分散装置１と同様であるため、説明を省略する。 Further, the fluid paths in the supercritical fluid dispersion device 2 of the second embodiment will be described with reference to schematic explanatory diagrams of FIGS. The supercritical fluid dispersion device 2 of the second embodiment has the intermediate tank 35 installed in the piping section 84 . Since other configurations are the same as those of the supercritical fluid dispersion device 1 of the first embodiment, description thereof is omitted.

はじめに、ポンプ部５０のピストン５１が後退しハウジング５２内が減圧する。そこで、原料タンク３０内の第１分散物は配管部８１、分岐ブロック４０、配管部８２を通じてポンプ部５０のハウジング５２内に流入する（図６参照）。このとき、第１分散物の流動する方向は正流方向であるため、逆止弁７０と弁開放状態の切替弁７１を通過可能である。 First, the piston 51 of the pump portion 50 retreats and the pressure inside the housing 52 is reduced. Therefore, the first dispersion in the raw material tank 30 flows into the housing 52 of the pump section 50 through the piping section 81, the branch block 40, and the piping section 82 (see FIG. 6). At this time, since the direction in which the first dispersion flows is the forward flow direction, it can pass through the check valve 70 and the switching valve 71 in the open state.

次に、ポンプ部５０のピストン５１が前進してハウジング５２内の第１分散物はポンプ部５０から押出される。そして、第１分散物は配管部８２、分岐ブロック４０、配管部８３を通過してオリフィスホモジナイザ部１０に流入する。ポンプ部５０の押出力により、第１分散物は小径流路部を備えたオリフィスホモジナイザ部１０を通過することができる（図６参照）。第２分散物はオリフィスホモジナイザ部１０通過することにより微小化が進み第２分散物となる。そして、第２実施形態の超臨界流体分散装置２においては、第２分散物は中間タンク３５へ流入する。 The piston 51 of the pump portion 50 is then advanced to push the first dispersion in the housing 52 out of the pump portion 50 . Then, the first dispersion passes through the piping section 82 , the branch block 40 and the piping section 83 and flows into the orifice homogenizer section 10 . The pushing force of the pump section 50 allows the first dispersion to pass through the orifice homogenizer section 10 having a small diameter channel section (see FIG. 6). As the second dispersion passes through the orifice homogenizer section 10, the miniaturization progresses to become the second dispersion. Then, in the supercritical fluid dispersion device 2 of the second embodiment, the second dispersion flows into the intermediate tank 35 .

中間タンク３５が原料タンク３０と別に備えられているため、微小化の進んだ第２分散物と原料タンク３０内の処理前の被処理物との混合は回避される。第２実施形態の超臨界流体分散装置２の場合、バッチ処理による方式が好適である。中間タンク３５には、超臨界流体の臨界温度及び臨界圧力を維持するための加温器、加圧器等が適宜備えられる（図示せず）。 Since the intermediate tank 35 is provided separately from the raw material tank 30 , mixing of the second dispersion, which is highly miniaturized, and the material to be processed in the raw material tank 30 before processing is avoided. In the case of the supercritical fluid dispersion device 2 of the second embodiment, batch processing is suitable. The intermediate tank 35 is appropriately provided with a heater, a pressurizer, etc. (not shown) for maintaining the critical temperature and critical pressure of the supercritical fluid.

続いて、ポンプ部５０におけるピストン５１の後退により、ハウジング５２内は負圧になる。そこで、中間タンク３５内の第２分散物は、図７とは逆にオリフィスホモジナイザ部１０の流出側流路部１８，１９から流入し、流入側流路部１１，１２から流出する。そして、配管部８３、分岐ブロック４０、配管部８２を通過してポンプ部５０のハウジング５２内に流入する（図８参照）。この後、ポンプ部５０のピストン５１の押出力により、第２分散物は再びオリフィスホモジナイザ部１０を通過する（図６参照）。 Subsequently, due to the retraction of the piston 51 in the pump section 50, the pressure inside the housing 52 becomes negative. Therefore, the second dispersion in the intermediate tank 35 flows in from the outflow side channel portions 18 and 19 of the orifice homogenizer portion 10 and flows out from the inflow side channel portions 11 and 12 in the opposite direction to FIG. Then, it flows into the housing 52 of the pump section 50 through the piping section 83, the branch block 40, and the piping section 82 (see FIG. 8). Thereafter, the second dispersion passes through the orifice homogenizer section 10 again due to the pushing force of the piston 51 of the pump section 50 (see FIG. 6).

第２実施形態の超臨界流体分散装置２では、第１分散物がオリフィスホモジナイザ部１０を通過後、いったん中間タンク３５に貯留され、再度オリフィスホモジナイザ部１０を逆向きに通過することを繰り返して第２分散物が調製される。特に、オリフィスホモジナイザ部１０は上流側及び下流側が共通構造であるため、このような流動の向きを逆転させる使い方が可能となる。むろん、配管部の構成から、中間タンク３５に貯留された第２分散物を原料タンク３０に戻し入れることも可能である。 In the supercritical fluid dispersion apparatus 2 of the second embodiment, after the first dispersion passes through the orifice homogenizer section 10, it is temporarily stored in the intermediate tank 35, and is repeatedly passed through the orifice homogenizer section 10 in the opposite direction. Two dispersions are prepared. In particular, since the orifice homogenizer part 10 has a common structure on the upstream side and the downstream side, it is possible to use such a method of reversing the flow direction. Of course, it is also possible to return the second dispersion stored in the intermediate tank 35 to the raw material tank 30 due to the configuration of the piping section.

本発明の超臨界流体分散方法は、溶媒に超臨界流体を用いることにより高い流動性を確保して被処理物を分散させて流動、粉砕できる。このため、流路中の流動性は良好となり、従前の圧送時の負荷を軽減することができて有望である。 The supercritical fluid dispersing method of the present invention uses a supercritical fluid as a solvent to ensure high fluidity and disperse, flow, and pulverize the object to be treated. For this reason, the fluidity in the flow path is improved, and it is promising that the load during the conventional pumping can be reduced.

１，２ 超臨界流体分散装置
１０ オリフィスホモジナイザ部
１１，１２ 流入側流路部
１３ 集合部
１４ 第１空隙部
１５ オリフィス流路部
１６ 第２空隙部
１７ 分岐部
１８，１９ 流出側流路部
２１ 第１ブロック
２２ 第２ブロック
２３ 第３ブロック
３０ 原料タンク
３５ 中間タンク
４０ 分岐ブロック
５０ ポンプ部
５１ ピストン
５２ ハウジング
６０ 流体貯留タンク
６１ 圧送ポンプ
７０ 逆止弁
７１，７２，７３，７４ 切替弁
８１，８２，８３，８４，８５ 配管部
９０ ドレイン部 Reference Signs List 1, 2 Supercritical Fluid Dispersing Device 10 Orifice Homogenizer 11, 12 Inflow Channel 13 Collecting Portion 14 First Gap 15 Orifice Channel 16 Second Gap 17 Branching 18, 19 Outflow Channel 21 1st block 22 2nd block 23 3rd block 30 raw material tank 35 intermediate tank 40 branch block 50 pump section 51 piston 52 housing 60 fluid storage tank 61 force pump 70 check valve 71, 72, 73, 74 switching valve 81, 82 , 83, 84, 85 piping section 90 drain section

Claims (5)

超臨界流体を貯留する流体貯留タンクと、
前記流体貯留タンクの下流に設置され前記流体貯留タンクから供給される超臨界流体中に被処理物を分散させる原料タンクと、
前記原料タンクの下流に設置される分岐ブロックと、
前記分岐ブロックの下流の一方側に設置されるポンプ部と、
前記分岐ブロックの下流の他方側に設置されるオリフィスホモジナイザ部と、
前記オリフィスホモジナイザ部の下流に設置され、前記オリフィスホモジナイザ部と前記原料タンクと接続する配管部に設置される中間タンクと、を備える超臨界流体分散装置における超臨界流体分散方法であって、
前記原料タンクにおいて被処理物を超臨界流体中に分散させて第１分散物を得る第１超臨界流体分散工程と、
前記第１分散物を前記ポンプ部に流入させた後に前記ポンプ部から押出して小径流路部を備えてなる前記オリフィスホモジナイザ部へ加圧供給し前記第１分散物中の被処理物を微小化して第２分散物を得る第２超臨界流体分散工程と、
前記第２分散物を前記中間タンクに流入させる工程と、
前記中間タンクに流入した前記第２分散物を前記オリフィスホモジナイザ部と、前記分岐ブロックとを経由して前記ポンプ部に流入させる工程と、
を備えることを特徴とする超臨界流体分散方法。 a fluid storage tank that stores a supercritical fluid;
a raw material tank installed downstream of the fluid storage tank for dispersing the material to be processed in the supercritical fluid supplied from the fluid storage tank;
a branch block installed downstream of the raw material tank;
a pump unit installed on one side downstream of the branch block;
an orifice homogenizer unit installed on the other downstream side of the branch block;
A supercritical fluid dispersing method in a supercritical fluid dispersing apparatus comprising an intermediate tank installed downstream of the orifice homogenizer unit and installed in a piping unit connecting the orifice homogenizer unit and the raw material tank,
a first supercritical fluid dispersing step of dispersing the object to be processed in the supercritical fluid in the raw material tank to obtain a first dispersion;
After the first dispersion is made to flow into the pump section, it is pushed out from the pump section and pressurized and supplied to the orifice homogenizer section having a small-diameter flow path section, thereby miniaturizing the material to be processed in the first dispersion. a second supercritical fluid dispersing step of obtaining a second dispersion by
flowing the second dispersion into the intermediate tank;
a step of causing the second dispersion that has flowed into the intermediate tank to flow into the pump section via the orifice homogenizer section and the branch block;
A supercritical fluid dispersion method, comprising: 前記第２超臨界流体分散工程において、前記第１分散物が前記オリフィスホモジナイザ部を通過後、通過後の前記第１分散物が再度前記オリフィスホモジナイザ部を通過することを繰り返して前記第２分散物が調製される請求項１に記載の超臨界流体分散方法。 In the second supercritical fluid dispersing step, after the first dispersion passes through the orifice homogenizer section, the first dispersion after passing through the orifice homogenizer section is repeated to repeat the second dispersion. The supercritical fluid dispersion method of claim 1, wherein is prepared. 前記第２超臨界流体分散工程の後、前記第２分散物から前記超臨界流体を除去し被処理物の微小化物を単離する単離工程が加えられる請求項１または２に記載の超臨界流体分散方法。 3. The supercritical fluid according to claim 1 or 2, wherein after the second supercritical fluid dispersing step, an isolating step is added to remove the supercritical fluid from the second dispersion and isolate the micronized material to be processed. Fluid dispersion method. 前記超臨界流体が、二酸化炭素の超臨界流体である請求項１ないし３のいずれか１項に記載の超臨界流体分散方法。 4. The supercritical fluid dispersion method according to any one of claims 1 to 3, wherein the supercritical fluid is a carbon dioxide supercritical fluid. 前記オリフィスホモジナイザ部は、
複数の流入側流路部と、
複数の流出側流路部と、
前記複数の流入側流路部を単一に集合させる集合部と、
前記集合部の下流に接続されたオリフィス流路部と、
前記オリフィス流路部の下流に接続され前記オリフィス流路部を分岐させ前記複数の流出側流路部と接続する分岐部と、
を備える請求項１ないし４のいずれか１項に記載の超臨界流体分散方法。
The orifice homogenizer section includes:
a plurality of inflow-side channel portions;
a plurality of outflow-side channel portions;
a collecting portion for collecting the plurality of inflow-side channel portions into a single unit;
an orifice channel portion connected downstream of the collecting portion;
a branching portion that is connected downstream of the orifice channel portion and branches the orifice channel portion to connect to the plurality of outflow side channel portions;
The supercritical fluid dispersion method according to any one of claims 1 to 4, comprising:
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