JP7281128B1 - Ionic liquid spraying device and ionic liquid spraying method - Google Patents

Abstract

Kind Code: A1 An ionic liquid spraying device capable of suppressing deterioration of an ionic liquid, suppressing an increase in cost, and spraying the ionic liquid into droplets having a minute diameter similar to vaporization, which cannot be easily seen with the naked eye, and an ionic liquid. A spraying method is provided. Kind Code: A1 An ionic liquid spraying device includes a liquid collecting section, a discharging section, a liquid feeding means, a power supply section, and a vacuum vessel. The liquid collection part 10 has an opening 10 a and contains the ionic liquid 3 . The ejection part 20 includes a nozzle 21 and a counter electrode 22 and ejects droplets of the ionic liquid 3 . The nozzle 21 ejects the ionic liquid 3 . The counter electrode 22 is arranged to face the nozzle 21 . The liquid sending means 30 can open and close the opening 10 a of the liquid collecting part 10 and sends the ionic liquid 3 from the liquid collecting part 10 to the discharging part 20 . The power supply section 40 applies a voltage between the nozzle 21 and the counter electrode 22 of the discharge section 20 . The vacuum vessel 50 accommodates the liquid collecting section 10 . [Selection drawing] Fig. 1

Description

TECHNICAL FIELD The present invention relates to an ionic liquid spraying apparatus and an ionic liquid spraying method, and in particular, an ionic liquid for spraying an ionic liquid used for purification of various organic compounds, etc., in the form of droplets having a very small diameter that cannot be easily seen with the naked eye. The present invention relates to a spraying device and an ionic liquid spraying method.

Organic EL devices using organic electroluminescence (hereinafter referred to as organic EL) have attracted attention as devices used for next-generation displays, next-generation lighting, and the like. As for organic compounds (hereinafter referred to as organic EL chemical materials), which are the main materials of organic EL devices, there is a demand for mass production due to an increase in demand, as well as for high purity in order to obtain high characteristics.

A sublimation purification method is conventionally used for the purification of organic EL chemical materials. However, according to the current sublimation purification method, in order to sufficiently purify the organic EL chemical material, it is necessary to repeat the purification multiple times, and the yield is often 50% or less. Therefore, it has been pointed out that it is difficult to mass-produce high-purity organic EL chemical materials at low cost using the current sublimation refining method. It has been demanded.

Regarding a technique for purifying an organic compound such as an organic EL chemical material at a high yield, Patent Document 1 describes a purification method for purifying an organic compound using a vaporized ionic liquid. According to the purification method described in Patent Document 1, after the ionic liquid vaporized by heating and the organic compound vaporized by heating are brought into contact with each other, the mixture is cooled, the organic compound is precipitated as a solid, and the organic compound is purified.

According to the purification method described in Patent Document 1, by vaporizing the organic compound and the ionic liquid, the contact area between the two per unit volume increases, and there is no need to repeat purification many times, resulting in a high yield. can be used to purify organic compounds, and the cost of refining organic EL chemical materials can be expected to be low.

JP 2019-163243 A

However, in the ionic liquid microparticulation and micronization means under reduced pressure disclosed in Patent Document 1, the first container, the second container, and the capture container are respectively connected and integrated by the decompressor. The pressure of is adjusted to 5 × 10 ^-3 Pa, but since it is necessary to keep the second container storing the ionic liquid at about 200 ° C., the ionic liquid is denatured by discoloration and thermal decomposition due to heating. There was a problem that it was difficult to reuse by doing. Moreover, if the reuse of the ionic liquid, which is relatively expensive, is restricted, it may lead to an increase in cost. In addition, the ionic liquid has an extremely low vapor pressure and is difficult to evaporate even in a vacuum, requiring a large amount of heat to evaporate the ionic liquid, which increases the cost required for heating.

Furthermore, when various ionic liquids are used, for example, when ionic liquids are used to purify various chemical substances, ionic liquids that are colored or decomposed due to excessive heating to vaporize as small-diameter droplets are not suitable. It is difficult to use in the purification method described in Patent Document 1, no matter how excellent the other chemical properties are.

The present invention has been made in view of the above problems, and an object of the present invention is to discolor an ionic liquid even under a reduced pressure of about 1×10 ⁻⁷ to 1×10 ⁻¹ Pa, which is an ultra-high vacuum or a high vacuum. To provide an ionic liquid spraying device and an ionic liquid spraying method that can prevent the occurrence of thermal decomposition and can spray the ionic liquid as droplets with a small diameter that cannot be easily seen with the naked eye. be.

An ionic liquid spraying device disclosed in the present application includes a liquid collection section, a discharge section, liquid transfer means, a power supply section, and a vacuum vessel. The liquid collection part has an opening and contains an ionic liquid. The ejection unit includes a nozzle and a counter electrode, and ejects droplets of the ionic liquid. The nozzle is made of a conductor and ejects the ionic liquid. The counter electrode is arranged to face the nozzle. The liquid sending means is capable of opening and closing the opening of the liquid collecting section, includes an infusion tube, and sends the ionic liquid from the liquid collecting section to the discharging section. The infusion tube is formed from a conductor and electrically connected to the nozzle. The power supply section applies a voltage between the nozzle of the discharge section and the counter electrode. The vacuum container accommodates the liquid collecting part.

In the ionic liquid spraying device disclosed in the present application, the liquid sending means includes a piston and moving means. The piston is made of a conductor and housed in the vacuum vessel, fitted with the liquid collection part through the opening, and pushes out the ionic liquid from the liquid collection part . The moving means has a function of moving the liquid collecting part between an open state and a closed state , and a constant movement of the liquid collecting part so as to push out the ionic liquid from the liquid collecting part in the closed state. It has the ability to move at speed . The open state is a state in which the opening of the liquid collecting portion is opened. The closed state is a state in which the opening of the liquid collecting portion is closed. The liquid collection part includes a fitted part that is fitted with the piston and into which the ionic liquid is injected. The piston has a liquid guide hole that extends through itself in the longitudinal direction and communicates the inside of the fitted portion with the infusion tube, and is electrically connected to the liquid guide tube.

Moreover, in the ionic liquid spraying device disclosed in the present application, the liquid collection part includes a plurality of the fitted parts. The liquid sending means includes a plurality of the pistons. The plurality of pistons are fitted with the plurality of fitted portions.

Furthermore, in the ionic liquid spraying device disclosed in the present application, the power supply section is electrically connected to the nozzle via the piston and the infusion tube .

Further , the ionic liquid spraying device disclosed in the present application includes a liquid collecting section, a discharging section, liquid feeding means, a power source section, and a vacuum vessel. The liquid collection part has an opening and contains an ionic liquid. The ejection part includes a nozzle and a counter electrode, and ejects droplets of the ionic liquid. The nozzle ejects the ionic liquid. The counter electrode is arranged to face the nozzle. The liquid sending means is capable of opening and closing the opening of the liquid collecting section, and sends the ionic liquid from the liquid collecting section to the discharging section. The power supply section applies a voltage between the nozzle of the discharge section and the counter electrode. The vacuum container accommodates the liquid collecting part. The power supply unit includes a first power supply and a second power supply. The first power supply applies a constant voltage between the nozzle and the counter electrode. The second power supply is a bipolar power supply, and applies a voltage in a voltage range whose absolute value is smaller than that of the first power supply between the nozzle and the counter electrode.

Further, the ionic liquid spraying method disclosed in the present application is a method of spraying an ionic liquid using the above-described ionic liquid spraying device, and includes a deaeration step, a liquid transfer step, a voltage application step, and a release step. Equipped with The degassing step is a step of degassing the ionic liquid by depressurizing the vacuum vessel in an open state in which the opening of the liquid collecting portion is open. In the liquid feeding step, after the degassing step, the liquid feeding means feeds the ionic liquid from the liquid collecting portion to the discharging portion in a closed state in which the opening of the liquid collecting portion is closed. is. The voltage applying step is a step in which the power supply section applies a voltage between the nozzle of the discharge section and the counter electrode. The ejection step is a step in which the ejection section ejects droplets of the ionic liquid by a potential difference between the nozzle and the counter electrode.

According to the ionic liquid spraying apparatus according to the present invention, the ionic liquid is prevented from discoloration and thermal decomposition even under a reduced pressure of about 1×10 ⁻⁷ to 1×10 ⁻¹ Pa, which is an ultra-high vacuum or a high vacuum. In addition, the ionic liquid can be sprayed as fine droplets that cannot be easily seen with the naked eye.

1 is a front view showing an ionic liquid spraying device according to an embodiment of the present invention; FIG. 2 is a front view showing the ionic liquid spraying device of FIG. 1 in an open state; FIG. It is a front view which shows an example of the external device connected with the ionic liquid spraying apparatus which concerns on embodiment of this invention. It is a partially enlarged view showing an ionic liquid spraying device according to another embodiment of the present invention. It is a front view which shows the ionic liquid spraying apparatus which concerns on other embodiment of this invention.

DETAILED DESCRIPTION OF THE INVENTION An ionic liquid spraying device and an ionic liquid spraying method according to embodiments of the present invention will be described in detail below with reference to the drawings. It should be noted that the embodiments described below are preferred specific examples for carrying out the present invention, and thus are subject to various technical limitations. is not limited to this embodiment unless specified.

<Embodiment>
An ionic liquid spraying device according to an embodiment of the present invention will be described below with reference to FIGS. 1 to 3. FIG. FIG. 1 is a front view showing an ionic liquid spraying device according to an embodiment. FIG. 2 is a front view showing the ionic liquid spraying device of FIG. 1 in an open state. FIG. 3 is a front view showing an example of an external device connected to the ionic liquid spraying device according to the embodiment.

As shown in FIGS. 1 to 3, the ionic liquid spraying device according to the embodiment has a connection part 2 that connects to an external device 1, and electrosprays the ionic liquid 3 at normal temperature and under vacuum to the naked eye. This is a device for supplying an external device 1 with droplets 3a having a nano-sized minute diameter that is not easily visible and similar to vaporization, and is sprayed from a connecting portion 2 toward the outside.

The external device 1 of the embodiment uses fine-diameter droplets 3a of the ionic liquid 3 supplied from the ionic liquid spray device to purify the organic EL chemical material, as will be described in detail later with reference to FIG. It is a device that However, organic EL chemistries, as used herein, refer to organic compounds as primary materials in devices utilizing organic electro-luminescence (organic EL devices).

Organic EL chemistries include hole-injecting materials, hole-transporting materials, electron-transporting materials, and charge-generating materials. In this specification, an organic EL chemical material refining device is given as an example of an external device connected to the ionic liquid spraying device of the embodiment. However, the ionic liquid spraying device of the embodiment may be connected to any external device as long as it uses the micro-diameter droplets 3a of the ionic liquid 3 for some purpose. For example, when connecting a chemical refining device to the ionic liquid spraying device of the embodiment, not only organic EL chemical materials, but also chemical substances that have physical properties that change from solid to gas can be used for other electronic applications. The ionic liquid spraying device of the embodiment can be preferably connected to the purification device for materials or pharmaceuticals.

Therefore, the ionic liquid spraying device according to the embodiment can be used not only in the industrial field such as the purification of organic compounds such as the organic EL chemical materials described above, but also in the academic field such as basic research and development at universities and various research institutes. is also expected. In the academic field, in the basic research field of nanomaterials that requires vacuum deposition of ionic liquids, it is possible to replace the conventional laser heating or resistance heating method and control the amount of evaporation from the nanoscale to the macroscale with high efficiency. As an apparatus, the ionic liquid spraying apparatus of the present invention can be expected.

In the embodiment, the connecting portion 2 is a circular metal plate or resin plate, and is provided with a through hole (not shown) into which a nozzle 21 described below is airtightly inserted, a bolt hole for connecting the external device 1, and the like. .

Ionic liquids are molten salts composed only of cations and anions. Compared to ordinary salts, ionic liquids have a significantly lower melting point, excellent chemical stability, and high ionic conductivity. It has characteristics such as flame retardancy and special solubility. An ionic liquid consists only of ions, has a relatively large long-range attractive force (Coulombic force) between particles, and has an extremely low vapor pressure. Therefore, it does not evaporate even under vacuum, and the ionic liquid can be sprayed under vacuum.

In addition, since the mean free path of particles is short under vacuum unlike under atmospheric pressure, the droplets are less likely to coalesce, and the droplets 3a of the nano-sized ionic liquid 3 can be stabilized relatively easily. For example, under a high vacuum of the order of 1×10 ⁻² Pa or less, discharge is less likely to occur than under atmospheric pressure, and a higher voltage power source can be used to spray droplets 3 a of the ionic liquid 3 as high-speed particle beams. .

Further, specific components of the ionic liquid are selected according to the purpose of use. The component is not particularly limited as long as it has absorbency to absorb impurities contained in the object to be purified, such as the EL chemical material. As the ionic liquid 3, a known or commercially available one can be used. For example, the ionic liquid 3 consists of the anions and cations shown below.

Examples of anions include chloride ion (Cl ^- ), bromide ion (Br ^- ), iodide ion (I ^- ), hexafluorophosphate (PF ₆ ^- ), tetrafluoroborate (BF ₄ ^- ), p-toluenesulfonate. (p-CH ₃ —C ₆ H ₄ SO ₃ ⁻ ), trifluoromethanesulfonate (CF ₃ SO ₃ ⁻ ), bis(trifluoromethanesulfonyl)imide [(CF ₃ SO ₂ ) ₂ N ⁻ ], dicyanamide [(NC ) ₂ N ⁻ ], tris(trifluoromethylsulfonyl)methide [(CF ₃ SO ₂ ) ₃ C ⁻ ], acetate ion (CH ₃ COO ⁻ ), trifluoroacetate ion (CF ₃ COO ⁻ ), etc. is selected.

Examples of cations include nitrogen-containing cyclic cation compounds such as pyridinium, pyrimidinium, pyrazolium, pyrrolidinium, piperidinium, imidazolium, and derivatives thereof; amine-based cations of tetraalkylammonium and derivatives thereof; phosphonium, trialkylsulfonium, tetraalkylphosphonium, etc. phosphine-based cations and derivatives thereof; lithium cations and derivatives thereof;

The ionic liquid spraying device according to the embodiment includes a liquid collecting section 10 , a discharging section 20 , a liquid feeding means 30 , a first power source 41 as a power source section 40 , and a vacuum vessel 50 .

As shown in FIG. 2, the liquid collecting part 10 has a cylindrical shape as a whole, and has an opening 10a, a fitted part 10b, and a tapered part 10c. Accommodates 3. The material of the liquid collecting part 10 is not particularly limited, and may be metal or resin. The liquid part 10 is made of resin.

The opening 10a is located at one end of the fitted portion 10b, in the embodiment, at the upper end of the fitted portion 10b. The fitted portion 10b is a columnar space formed inside the liquid collecting portion 10, into which the ionic liquid 3 is injected through the opening 10a, and is fitted with a piston 31, which will be described later, through the opening 10a. . The other end of the fitted portion 10b, which is the lower end in the embodiment, is a completely closed bottom, and the ionic liquid 3 is sent outside from the fitted portion 10b through the opening 10a. The tapered portion 10c is continuous with the fitted portion 10b, and is formed of a mortar-shaped slope whose diameter increases from the opening 10a toward one end of the liquid collecting portion 10, or the upper end in the embodiment.

The ejection part 20 includes a nozzle 21 and a counter electrode 22, and ejects droplets 3a of the ionic liquid 3. FIG. Hereinafter, the principle that the discharge unit 20 discharges the ionic liquid 3 as nano-sized droplets 3a will be described.

When a voltage is applied between the nozzle 21 and the counter electrode 22 , when the electrostatic force acting on the interface exceeds the surface tension of the ionic liquid 3 at the end of the nozzle 21 , Taylor A cone is formed and electrospray occurs. This electrospray is a phenomenon in which an electrostatic force generated by an electric field generates liquid threads from the tip of a Taylor cone, and the liquid threads split to spray and discharge the ionic liquid 3 in the form of fine droplets. When the Coulomb force acting between ions in the ejected droplet becomes larger than the surface tension of the droplet, Rayleigh splitting occurs, and the droplet splits to promote further miniaturization. In other words, at the tip of the nozzle 21, the charged ionic liquid 3 becomes charged microparticles that have been miniaturized to nano-size, that is, microdroplets, and is attracted by the Coulomb force from the counter electrode 22, and vaporizes. Nano-sized micro-diameter droplets 3a are ejected to the outside, and the ionic liquid 3 is sprayed.

In the embodiment, the nozzle 21 is formed from a capillary having an inner diameter of about 0.1 mm at least near the tip, and ejects the ionic liquid 3 . Further, the nozzle 21 of the embodiment is made of a metal material such as stainless steel, which is a conductor, and has electrical conductivity. By using a very fine capillary as the nozzle 21, a strong electric field is easily induced at the sharp tip of the nozzle 21, the surface charge density is rapidly increased to exceed a critical value, and the ionic liquid 3 is electrosprayed to a nano size. droplets 3a are more reliably generated.

The counter electrode 22 is arranged to face the nozzle 21 . In the embodiment, the counter electrode 22 is ring-shaped, and the nozzle 21 is arranged so as to coincide with the central axis of the counter electrode 22 so that an electric field without distortion is concentrated at the tip of the nozzle 21, which is a capillary. be done. The material of the counter electrode 22 is not particularly limited. However, the ionic liquid 3 ejected from the nozzle 21 may adhere to the counter electrode 22, and metal materials having excellent corrosion resistance to the ionic liquid 3, such as tungsten, molybdenum, aluminum, stainless steel, and nickel, are used. Preferably, the counter electrode 22 is formed from an alloy.

The liquid sending means 30 can open and close the opening 10 a of the liquid collecting part 10 and sends the ionic liquid 3 from the liquid collecting part 10 to the discharging part 20 . In the embodiment, the liquid delivery means 30 includes a piston 31 , an infusion tube 33 and a moving means 32 .

The piston 31 is slidably inserted into the fitted portion 10 b through the opening 10 a and fitted with the liquid collecting portion 10 to push out the ionic liquid 3 from the liquid collecting portion 10 . The piston 31 of the embodiment is made of metal and has an elongated columnar shape, is electrically conductive, and has a liquid introduction hole 31a extending through it in the longitudinal direction along the central axis. One end of the liquid introducing hole 31 a opens toward the inside of the fitted portion 10 b in a state where the piston 31 and the liquid collecting portion 10 are fitted, and the other end opens so as to be connectable with the infusion tube 33 . are doing.

The infusion tube 33 sends the ionic liquid 3 extruded from the liquid collection section 10 by the piston 31 to the discharge section 20 . In the embodiment, the infusion tube 33 is made of stainless steel, which is a conductor, has electrical conductivity, and is electrically connected to the piston 31 by being connected to the liquid introduction hole 31a of the piston 31, The nozzle 21, which is a conductive capillary, and the piston 31 are electrically connected.

The moving means 32 moves at least one of the liquid collection part 10 and the piston 31 between the open state and the closed state. In the embodiment, the piston 31 is fixed to the vacuum vessel 50 by fixing means 34 including a support and a pedestal, and the liquid collection part 10 is moved between the open state and the closed state by the moving means 32. . The moving means 32 also has a function of moving the liquid collecting section 10 at a constant speed so as to push the ionic liquid 3 out of the liquid collecting section 10 in the closed state.

The open state is, as shown in FIG. 2, a state in which the liquid collection part 10 and the piston 31 are not fitted and the opening 10a is open. The closed state is, as shown in FIG. 1, a state in which the liquid collecting portion 10 and the piston 31 are fitted to close the opening 10a. As described above, in the embodiment, the piston 31 is an opening/closing member that opens and closes the opening 10a of the liquid collecting portion 10, and is accommodated in the vacuum vessel 50.

The moving means 32 includes an electric motor 32a, a linear introduction machine 32b, and a controller 32c. The electric motor 32a, the linear feeder 32b, and the controller 32c are supported by the vacuum vessel 50 outside the vacuum vessel 50 via the support portion 32d. Note that the controller 32c may be placed separately and connected to the electric motor 32a by a signal line or the like.

The electric motor 32a is a position-controllable stepping motor in the embodiment, and generates rotational driving force. The linear introduction device 32b converts the rotational driving force of the electric motor 32a into a linear driving force, and linearly moves the liquid collection part 10 forward and backward. The controller 32c controls the electric motor 32a. The liquid collection part 10 is moved between an open state and a closed state under the control of the controller 32c. In addition, the controller 32c controls the electric motor 32a so that a constant amount of the ionic liquid 3 per unit time is sent from the liquid collecting section 10 to the discharging section 20 in the closed state.

The power supply section 40 applies a voltage between the nozzle 21 and the counter electrode 22 of the discharge section 20 . In embodiments, the power supply section 40 is formed from a first power supply 41 . The first power supply 41 is a high-voltage power supply device with a maximum voltage of several kV, is connected to the piston 31 , and is connected to the nozzle 21 via the infusion tube 33 .

On the other hand, the counter electrode 22 is grounded, a potential difference of several kV at maximum is generated between the nozzle 21 and the counter electrode 22, an electric field is generated between the nozzle 21 and the counter electrode 22, and electrospray Droplets 3a of the ionic liquid 3 can be ejected from the ejection part 20 and the droplets 3a of the ionic liquid 3 can be sprayed.

The vacuum container 50 accommodates the liquid collecting part 10 . In the embodiment, the vacuum container 50 also houses a piston 31 that is part of the liquid transfer means 30 . The vacuum container 50 also has a cylindrical container body 51 and a pair of end plates 52 .

The container body 51 is arranged in the vertical direction, and the pair of end plates 52 hermetically closes the upper and lower openings of the container body 51 . Of the pair of end plates 52, the upper end plate 52A is provided with a hole (not shown) through which an electric wire connecting the first power source 41 and the piston 31 is airtightly inserted. An insertion hole (not shown) is formed in the lower end plate 52B, and a rod-like connecting member 32e is inserted therethrough so as to be airtight and movable back and forth. The connecting member 32e connects the linear introducer 32b and the liquid collector 10. As shown in FIG. Further, the piston 31 is fixed by the fixing means 34 to the lower end plate 52B.

Next, with reference to FIG. 3, the external device 1 according to the embodiment of the invention will be described. The external device 1 of the embodiment includes a synthesis chamber 61 to be evacuated, a connected portion 62, a resistance heating boat 63, a collection plate 64, a first external power source 65, and a second external power source 66. This apparatus uses droplets 3a of an ionic liquid 3 supplied from an ionic liquid spraying apparatus to purify an organic compound such as an organic EL chemical material.

A synthesis chamber 61 is formed from an airtight container and accommodates a resistance heating boat 63 and a collection plate 64 . The connected part 62 is connected to the connection part 2 of the ionic liquid spraying device, and connects the external device 1 to the ionic liquid spraying device of the embodiment.

The resistance heating boat 63 accommodates the purification target 4 which is an organic compound such as an organic EL chemical material, heats the purification target 4 with power supplied from the first external power supply 65, and heats the purification target 4 with the vapor of the purification target 4. A certain object vapor 4a is generated. The target vapor 4a generated by the resistance heating boat 63 and the droplets 3a of the ionic liquid 3 supplied from the ionic liquid spraying device are brought into contact inside the synthesis chamber 61, and the target vapor 4a is converted into the droplets 3a. is sprayed onto the collecting plate 64 by the movement of .

The collection plate 64 is arranged in the vertical direction, and cools the liquid droplets 3a and the object vapor 4a by electric power supplied from the second external power supply 66. As shown in FIG. By cooling the object vapor 4a, the object to be purified 4 precipitates on the surface of the collection plate 64, aggregates, and slides down together with the ionic liquid 3 to the collection dish 64a arranged below the collection plate 64. , is collected.

The ionic liquid spraying method according to the embodiment is a method of spraying the ionic liquid 3 using the ionic liquid spraying device according to the embodiment, comprising a degassing step, a liquid feeding step, a voltage applying step, and a releasing step. As described above, the droplets 3a of the ionic liquid 3 obtained by the ionic liquid spraying method of the embodiment can be used for purposes other than the purification of the organic EL chemical material.

The degassing step is a step of degassing the ionic liquid 3 by depressurizing the vacuum vessel 50 in an open state in which the opening 10a of the liquid collecting portion 10 is open. Gases such as oxygen and nitrogen in the air are dissolved in the ionic liquid 3 under atmospheric pressure, and the gases dissolved in the ionic liquid 3 appear as bubbles under reduced pressure. Therefore, in the open state in which the ionic liquid 3 is stored in the liquid collecting part 10 and the opening 10a is open, the pressure in the vacuum vessel 50 is reduced to the same high vacuum state as when the ionic liquid 3 is sprayed, The ionic liquid 3 is placed under reduced pressure for a certain period of time. By placing the ionic liquid 3 under reduced pressure for a certain period of time, the gas dissolved in the ionic liquid 3 can be separated from the ionic liquid 3 and the ionic liquid 3 can be degassed.

In the liquid transfer step, after the degassing step, the liquid transfer means 30 closes the opening 10a of the liquid collection section 10, and in the closed state where the opening 10a is blocked, the ionic liquid is transferred from the liquid collection section 10 to the discharge section 20. 3 is sent.

The voltage application step is a step in which the first power source 41 as the power source section 40 applies voltage between the nozzle 21 and the counter electrode 22 of the discharge section 20 .

The ejection step is a step in which the ejection section 20 ejects droplets 3 a of the ionic liquid 3 by the potential difference between the nozzle 21 and the counter electrode 22 .

As described above with reference to FIGS. 1 to 3, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the liquid collecting part 10 has the opening 10a, and the liquid sending means 30 has the opening 10a. , the opening 10 a can be opened and closed, and the vacuum vessel 50 accommodates the liquid collecting part 10 . Therefore, as in the ionic liquid spraying method according to the embodiment described above, the dissolved gas can be removed from the ionic liquid 3 sent to the discharge unit 20 by performing the liquid transfer step after performing the degassing step. can.

When the ionic liquid is placed under vacuum without being degassed, bubbles of dissolved gas are violently generated. Therefore, when spraying the ionic liquid under vacuum, it is necessary to deaerate the ionic liquid in advance. However, the work of injecting the ionic liquid into the liquid collecting part such as a syringe needs to be performed under atmospheric pressure, which halves the effect of degassing. As a result, for example, air bubbles may enter the infusion tube, causing problems such as the inability to transfer the liquid smoothly, or damage to the liquid collecting section if the liquid collecting section is thin.

According to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the dissolved gas can be removed in advance from the ionic liquid 3 sent to the discharge section 20, thereby preventing the above-described problems from occurring. Further, in an embodiment in which the liquid sending means 30 includes a piston 31 and the vacuum container 50 also accommodates the piston 31, which is an opening/closing member for the opening 10a, ions can be sent to the emitting portion 20 more easily and reliably. Dissolved gases can be removed from the liquid 3 .

Furthermore, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, by spraying the ionic liquid 3 using electrospray, there is no need to heat the ionic liquid 3, and deterioration of the ionic liquid 3 is suppressed. In addition, the ionic liquid 3 can be sprayed as minute droplets 3a that are not easily visible to the naked eye and are similar to vaporization. As a result, the surface area per unit volume of the ionic liquid 3 can be greatly increased. High efficiency can be achieved.

Then, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the ionic liquid 3 is sprayed by electrostatic spraying in the form of droplets with a small diameter that cannot be easily seen with the naked eye, so the ionic liquid 3 is heated. Since the ionic liquid does not need to be vaporized, discoloration or decomposition due to heating does not occur, so that even an ionic liquid that has been used once can be easily reused. As a result, when the ionic liquid spraying device is operated for a long period of time, it is possible to suppress an increase in operating costs.

Further, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the ionic liquid 3 can be sprayed as micro-diameter droplets 3a that are not heated to a high temperature, not limited to purification of various chemical substances. Therefore, it is possible to supply droplets 3a of the ionic liquid 3 with a small diameter, which is equivalent to vaporization, even in processes such as processes in which temperature rise is undesirable and processes in which it is difficult to use the ionic liquid that has been vaporized by heating. The ionic liquid spraying device and the ionic liquid spraying method of the present invention can also be applied to such processes.

Further, as described with reference to FIGS. 1 to 3, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the nozzle 21 has electrical conductivity, for example, the metal piston 31 and the stainless steel It is connected to a first power source 41 via a steel infusion tube 33 and a high voltage is applied. Therefore, even when a fine tube such as a capillary is used as the nozzle 21 in order to obtain nano-sized droplets 3a, the nozzle 21 is prevented from being charged and the nozzle 21 is prevented from being damaged by discharge. can be prevented.

As described above, under high vacuum of the order of 1×10 ⁻² Pa or less, discharge is less likely to occur than under atmospheric pressure. However, discharge is more likely to occur under a vacuum in a region of higher pressure. According to the ionic liquid spraying device of the embodiment, it is possible to prevent discharge even under vacuum in a pressure range in which discharge is likely to occur, and it is possible to more reliably prevent damage to the nozzle 21 . Further, if the nozzle 21 is formed of, for example, a resin capillary, the discharge may melt the resin and block the nozzle 21 . If the nozzle 21 is made of metal, even if discharge occurs, at least damage due to melting can be suppressed. For this reason, in the present embodiment, the inside of the vacuum vessel 50 is preferably adjusted to 1×10 ⁻³ to 1×10 ⁻⁵ Pa, and the vacuum vessel 50 has durability in this pressure range. preferably.

In the above-described embodiment, the nozzle 21 is provided with electrical conductivity and is electrically connected to the piston 31 or the like to prevent the nozzle 21 from being charged and to prevent the nozzle 21 from being damaged by discharge. ing. The present invention is not limited to this, but a bipolar power supply is used for the first power supply 41, and the polarity of the voltage applied to the nozzles 21 is constantly switched to prevent the nozzles 21 from being charged, and the discharge causes the nozzles 21 to It may be prevented from being damaged.

The bipolar power supply used for the first power supply 41 is preferably a high-voltage, high-frequency bipolar power supply with a maximum voltage of plus or minus several kV and a maximum frequency characteristic of several tens of kHz. When using a bipolar power source for the first power source 41, the first power source 41 can be connected to the piston 31 as shown in FIG. 1, or the first power source 41 can be directly connected to the nozzle 21. is also possible. Further, when the first power supply 41, which is a high-voltage, high-frequency bipolar power supply, is directly connected to the nozzle 21, the nozzle 21 is formed of a non-conductive resin capillary such as fused silica or polymer resin. You can also

Further, as described with reference to FIGS. 1 to 3, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the tapered portion 10c is formed between the opening 10a and the upper end of the liquid collecting portion 10. This prevents the piston 31 from coming into contact with the upper end of the liquid collecting part 10 when the piston 31 is fitted into the fitted part 10b, preventing the piston 31 from being fitted to the liquid collecting part 10. 31 and the liquid collection part 10 can be fitted more reliably.

Furthermore, as described with reference to FIGS. 1 to 3, according to the ionic liquid spraying device and the ionic liquid spraying method of the embodiment, the piston 31 is fixed with respect to the vacuum vessel 50, and the liquid collection part 10 moves. The ionic liquid 3 is moved by the means 32 , pushed out from the liquid collector 10 through the liquid introduction hole 31 a formed in the piston 31 , and sent to the discharge section 20 through the infusion tube 33 . Therefore, when the nozzle 21 is arranged above the liquid surface of the ionic liquid 3 to prevent dripping, the length of the infusion tube 33 can be shortened, and the ionic liquid 3 can be more stably supplied to the discharge section 20 .

In addition, since the piston 31 is fixed, when the piston 31 is made of a metal material, the infusion tube 33 can be connected to the fixed piston 31, and the infusion tube 33 can be made of an inflexible metal material. .

Another embodiment of the invention will now be described with reference to FIG. FIG. 4 is a partially enlarged view showing an ionic liquid spraying device according to another embodiment of the present invention. Hereinafter, the ionic liquid spraying device of FIG. 4 will be mainly described with respect to different parts from the ionic liquid spraying devices of FIGS. 1 and 2 .

As shown in FIG. 4, in this embodiment, the liquid collecting portion 10A has a plurality of fitted portions 10b. The liquid delivery means 30 has a plurality of pistons 31 fitted with the plurality of fitted portions 10 b and a plurality of infusion tubes 33 . The discharge section 20 has a plurality of nozzles 21 and a plurality of counter electrodes 22 (not shown).

A plurality of pistons 31 are fixed to the vacuum vessel 50 by fixing means 34 . Each of the plurality of pistons 31 has a liquid introduction hole 31a and is connected to a first power supply 41 (not shown). A stainless steel infusion tube 33 is connected to each of the liquid introduction holes 31a and formed of a conductor. It is electrically connected to the nozzle 21 to be connected. A plurality of counter electrodes 22 are arranged to face each of the plurality of nozzles 21 .

As described above with reference to FIG. 4, according to the present embodiment, the liquid collection part 10A has a plurality of fitted parts 10b, the liquid transfer means 30 has a plurality of pistons 31, and the discharge A portion 20 has a plurality of nozzles 21 and a plurality of counter electrodes 22 . Therefore, the amount of the droplets 3a of the ionic liquid 3 that can be sprayed per unit time can be increased, for example, the purification of organic EL chemical materials can be performed more efficiently, and mass production can be further facilitated. can.

Next, still another embodiment of the present invention will be described with reference to FIG. FIG. 5 is a front view showing an ionic liquid spraying device according to still another embodiment. Hereinafter, the ionic liquid spraying device of FIG. 5 will be mainly described with respect to the different parts from the ionic liquid spraying devices of FIGS. 1 and 2 .

In the ionic liquid spraying apparatus of this embodiment, the power supply unit 40 has a first power supply 41 that is a high voltage power supply similar to that in FIG. 1 and a second power supply 42 that is a low voltage bipolar power supply. A high voltage first power supply 41 is connected to the counter electrode 22, and a low voltage second power supply 42 is directly connected to the nozzle 21A. The voltage that the first power supply 41 applies to the counter electrode 22 is preferably several kV, and the voltage that the second power supply 42 applies to the nozzle 21 is preferably plus or minus several volts. Further, the nozzle 21A is formed from a metal or resin capillary. The material of the infusion tube 33A is not particularly limited and may be made of resin, and the material of the piston 31 is also not particularly limited, and may be made of metal or resin.

As described above with reference to FIG. 5, according to the present embodiment, the counter electrode 22 is connected to the high voltage first power supply 41 for electrospray, and the nozzle 21 is connected to the low voltage for antistatic. A second power supply 42, which is a voltage bipolar power supply, is connected. Therefore, discharge from the nozzle 21 can be prevented, and damage to the nozzle 21 can be prevented.

The embodiments of the present invention have been described above with reference to the drawings (FIGS. 1 to 5). However, the present invention is not limited to the above embodiments, and can be implemented in various aspects without departing from the scope of the invention (eg, (1) to (4) below).

(1) In each of the above embodiments, the piston 31 is fixed with respect to the vacuum vessel 50 and the liquid collecting portions 10 and 10A are moved by the moving means 32 . The present invention is not limited to this, and the liquid collecting parts 10, 10A may be fixed to the vacuum vessel 50, the piston 31 may be moved by the moving means 32, and both the liquid collecting parts 10, 10A and the piston 31 may be moved. may be

(2) In each of the above-described embodiments, the liquid introduction hole 31 a is formed so as to penetrate the piston 31 in the longitudinal direction, and the ionic liquid 3 is sent to the discharge section 20 through the inside of the piston 31 . The present invention is not limited to this. For example, an outlet for the ionic liquid 3 is provided at the bottom of the liquid collecting sections 10 and 10A, and the ionic liquid 3 is sent to the discharging section 20 through the outlets of the liquid collecting sections 10 and 10A. good too. At this time, the liquid collecting parts 10 and 10A are made of a metal material, are made conductive, are connected to the first power supply 41, and are fixed to the vacuum vessel 50. FIG. Moving the piston 31 by the moving means 32 is particularly preferable when connecting the infusion tube 33 made of metal to the outlets of the liquid collecting parts 10 and 10A.

(3) In the above embodiment, the nozzle 21 is made of a metal capillary so as to impart electrical conductivity. may be given.

(4) In the embodiment of FIG. 4, a plurality of fitted portions 10b, a plurality of pistons 31, and a plurality of nozzles 21 are provided. The infusion tube 33 may be branched so as to send the ionic liquid 3 from and to a plurality of nozzles 21 .

3... Ionic liquid 3a... Droplet 10, 10A... Liquid collection part 10a... Opening 10b... Fitted part 20... Ejection part 21, 21A... Nozzle 22... Counter electrode 30... Liquid sending means 31... Piston 32... Moving means 33 , 33A... Infusion tube 40... Power supply unit 41... First power supply 42... Second power supply 50... Vacuum vessel

Claims (6)

a liquid collection part having an opening and containing an ionic liquid;
an ejection unit that is formed of a conductor and includes a nozzle that ejects the ionic liquid, and a counter electrode arranged opposite to the nozzle, and that ejects droplets of the ionic liquid;
A liquid sending means capable of opening and closing the opening of the liquid collecting part and sending the ionic liquid from the liquid collecting part to the discharging part , the liquid sending means being formed of a conductor and electrically connected to the nozzle. a liquid delivery means including an infusion tube ;
a power supply unit that applies a voltage between the nozzle of the discharge unit and the counter electrode;
An ionic liquid spraying device comprising: a vacuum vessel that houses the liquid collecting part. The liquid sending means is made of a conductor, is housed in the vacuum container, is fitted with the liquid collecting portion through the opening, and is a piston for pushing out the ionic liquid from the liquid collecting portion; Moving means for moving the liquid portion , wherein the liquid collecting portion is moved between an open state in which the opening of the liquid collecting portion is opened and a closed state in which the opening of the liquid collecting portion is closed. and a moving means having a function of moving the liquid collecting part at a constant speed so as to push the ionic liquid out of the liquid collecting part in the closed state,
The liquid collecting portion is a fitted portion that is fitted with the piston, and includes a fitted portion into which the ionic liquid is injected, and the piston is formed to penetrate itself in the longitudinal direction. 2. The ionic liquid spraying device according to claim 1, further comprising a liquid introduction hole that communicates the inside of said fitting portion with said infusion tube, and is electrically connected to said infusion tube. The liquid collecting part has a plurality of the fitted parts,
3. The ionic liquid spraying device according to claim 2, wherein said liquid sending means includes a plurality of said pistons that are fitted with said plurality of fitted portions. The ionic liquid spraying device according to claim 2 or 3 , wherein the power supply unit is electrically connected to the nozzle through the piston and the infusion tube . a liquid collection part having an opening and containing an ionic liquid;
an ejection unit including a nozzle for ejecting the ionic liquid and a counter electrode arranged opposite to the nozzle, for ejecting droplets of the ionic liquid;
a liquid sending means capable of opening and closing the opening of the liquid collecting section and sending the ionic liquid from the liquid collecting section to the discharging section;
a power supply unit that applies a voltage between the nozzle of the discharge unit and the counter electrode;
A vacuum vessel that houses the liquid collecting part
and
The power supply unit includes a first power supply that applies a constant voltage between the nozzle and the counter electrode, and a bipolar power supply, and applies a voltage in a voltage range whose absolute value is smaller than that of the first power supply to the nozzle and the counter electrode. An ionic liquid spray device including a second power supply applied between the counter electrodes . An ionic liquid spraying method for spraying an ionic liquid using the ionic liquid spraying device according to any one of claims 1 to 5,
a degassing step of degassing the ionic liquid by depressurizing the vacuum vessel in an open state in which the opening of the liquid collecting portion is open;
After the degassing step, the liquid sending means closes the opening of the liquid collecting section, and in a closed state where the opening is closed, sends the ionic liquid from the liquid collecting section to the discharging section. a liquid process;
a voltage applying step in which the power supply unit applies a voltage between the nozzle of the discharge unit and the counter electrode;
and an ionic liquid spraying method, wherein the ejection section ejects droplets of the ionic liquid by a potential difference between the nozzle and the counter electrode.

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