JP6381363B2 - Bubble removing device and bubble removing method - Google Patents

Description

  The present invention relates to a bubble removing device and a bubble removing method.

  Gas-liquid mixing by stirring is known as a typical method for dissolving gas in a liquid (solvent). In performing this gas-liquid mixing, it is also known that gas can be efficiently dissolved in a liquid by stirring under a pressurized condition. For example, taking a carbonated beverage as an example, a large amount of carbon dioxide can be dissolved in water by applying pressure to carbon dioxide and stirring.

  By the way, bubbles are mixed in the solution obtained by a general stirring operation. These bubbles are known to have various effects. For example, the measurement accuracy of a flow meter is deteriorated, and the accuracy of finishing a painted surface or a printed surface by painting or ink printing is caused. Further, for example, when measuring the gas solubility (concentration) in a solution, it causes variation in measurement results, resulting in deterioration of measurement accuracy. Therefore, generally, after performing gas-liquid mixing by stirring, a defoaming operation for removing bubbles from the solution is performed.

Define defoaming and degassing.
Defoaming is removing bubbles of various sizes mixed in a solution. The bubbles are surrounded by liquid and the inside is gas.
In contrast, degassing changes the temperature environment or pressure environment of a solution in which the gas is dissolved in a saturated state, returns the gas component dissolved in the solution to bubbles by this change, and degass the bubbles. It is to reduce the gas concentration in the solution by bubbling. Therefore, by performing deaeration, the gas component dissolved in the solution is changed to bubbles and removed, so that the gas solubility of the solution decreases. In addition, the gas solubility of the solution in which the gas is dissolved in a saturated state follows Henry's law.

  As a method for performing the above-mentioned defoaming, for example, a method using heating boiling, a method using ultrasonic waves, a method using vacuum decompression, a method using centrifugal force, a gas permeable membrane (gas-liquid separation membrane) is used. Such a method and a stationary method are known.

  The method using heating boiling is a method of removing bubbles from the solution by heating the solution to increase the rising speed of the bubbles by lowering the viscosity of the solution and expanding the bubbles. However, since the solution is heated and boiled, the temperature environment changes greatly and the deaeration action works. For this reason, even gas components dissolved in the solution are vaporized to be changed into bubbles and easily removed from the solution. Therefore, there is a possibility that the gas solubility is lowered.

As a method using ultrasonic waves, for example, a method is known in which the volume is changed by applying ultrasonic vibration to a container containing a solution, and pressure reduction and pressurization in the container are alternately performed (Patent Document). 1). As a result, the volume of bubbles contained in the solution can be expanded and contracted to increase the rising speed of the bubbles, and the bubbles can be removed from the solution. However, ultrasonic vibration is applied to the solution. And a high-pressure part and a low-pressure part will exist alternately in the solution. Therefore, the deaeration action works in the low-pressure portion, and the gas component dissolved in the solution changes into bubbles, and expands to form large bubbles and floats on the solution surface and is easily removed from the solution. Therefore, there is a possibility that the gas solubility is lowered.

  The method using vacuum depressurization is a method of removing bubbles from the solution by increasing the bubble rising speed by expanding the volume of bubbles contained in the solution by depressurization. However, by reducing the pressure, even gas components dissolved in the solution are vaporized to be changed into bubbles and easily removed from the solution. Therefore, there is a possibility that the gas solubility is lowered. Thus, the method using vacuum depressurization is a method of simultaneously performing defoaming and degassing.

  As a method using a centrifugal force, for example, a method of removing bubbles contained in a solution by colliding the solution with an inner wall of a vacuum container using a centrifugal force of a rotating body is known (see Patent Document 2). In this method, the density difference between the solution and the bubbles is utilized, and the bubbles are easily removed from the solution by centrifugal force. However, when a centrifugal force is applied, a depressurized portion is generated in the solution. Therefore, a deaeration action works, and the gas component dissolved in the solution is easily changed to bubbles and easily removed from the solution. Therefore, there is a possibility that the gas solubility is lowered.

  The gas permeable membrane (gas-liquid separation membrane) is formed, for example, in the shape of an elongated pipe, and is usually used by bundling a plurality. Since this gas permeable membrane can remove bubbles without changing the composition of the solution, it is used in a wide range of fields. As a method using such a gas-liquid separation membrane, for example, a gas having the same component as the bubbles in the solution is present inside the gas-liquid separation membrane through which the solution (treatment liquid) passes, and the gas dissolved in the solution A method of moving a solution at a pressure equal to or lower than the saturated vapor pressure is known (see Patent Document 3). According to this method, it is possible to remove bubbles without changing the composition of the solution.

  However, in this method, since the pressure inside the gas-liquid separation membrane needs to be a pressure equal to or lower than the saturated vapor pressure of the solution, deaeration is performed in addition to the defoaming action, and the gas solubility may be reduced. was there. Furthermore, it is necessary to use a special membrane called a gas permeable membrane, which tends to be expensive. In addition, it is necessary to control a plurality of pressures, which is troublesome and difficult to handle.

  As mentioned above, heating boiling, ultrasonic waves, vacuum decompression, centrifugal force, and gas permeable membranes all involve not only defoaming but also degassing, so gas dissolved in the solution. The components are removed as bubbles, and the gas solubility tends to decrease.

  On the other hand, the stationary method is a method used in, for example, a solubility measurement experiment, and is known as a method capable of performing only defoaming without causing a deaeration action. Specifically, in the stationary method, a liquid and a gas are stirred for a predetermined time at a predetermined temperature and pressure to prepare a mixed solution, and then the temperature and pressure conditions during stirring are maintained. In this method, air bubbles are removed from the solution by standing for a certain time. As described above, in the standing method, the temperature condition and the pressure condition at the time of stirring are maintained, so that the deaeration action does not occur. Therefore, it is possible to perform only defoaming without reducing the gas solubility of the solution.

  Note that the standing time for allowing the solution to stand after stirring varies depending on, for example, the shape of the stirring container, the stirring method, and the like. For example, a method of spending 18 hours each for stirring and standing (see Non-patent Document 1), a method of spending 2 hours for stirring, and day and night standing (see Non-Patent Document 2), and spending 3 hours each for stirring and standing A method (see Non-Patent Document 3) is known.

Japanese Patent Laid-Open No. 2007-054680 JP 2011-206673 A JP-A-10-144604

S. Someya, two others, “Influence of pressure on the solubility of CO2 in water”, Transactions of the Japan Society of Mechanical Engineers (B), Vol. 71, No. 704 (2005-4), paper no. 04-1000, P1155-1160 Wei Yan and two others, “Measurement and modeling of CO2 solubility in NaCl brine and CO2-saturated NaCl brine density”, International Journal of Greenhouse Gas Control (2011), IJGGC-486, No. of Pages 18 Yoshihisa HAYASHI, “Direct Measurement of Solubility of Methane and Carbon Dioxide in High Pressure Water Using Gas Chromatography”, Journal of the Japan Petroleum Institute, Vol.57 No.3, May, 2014, P125-132

  The standing method is a method capable of performing only defoaming without lowering the gas solubility of the solution. However, the stirring method and the method of standing the solution mixed by stirring alternately (so-called so-called method) (Batch method). For this reason, labor and time are required, and it has been difficult to efficiently perform the work of removing bubbles (defoaming work) from the solution.

  The present invention has been made in view of such circumstances, and the object thereof is to make only bubbles from the solution while maintaining the gas solubility without affecting the gas components dissolved in the solution. It is providing the bubble removal apparatus and bubble removal method which can remove efficiently.

(1) The bubble removing apparatus according to the present invention is formed with an inflow port through which a solution in which a gas is dissolved in a solvent flows, and is disposed above the inflow port, a first storage unit that stores the solution therein. , A discharge path for discharging the solution flowing upward from the inflow port from the first storage section, the solution discharged through the discharge path being stored therein, and the stored solution flowing out A second accommodating portion in which an outlet is formed, a pressure adjusting portion that adjusts the internal pressure of the first accommodating portion and the second accommodating portion that communicate with each other through the discharge passage to the same pressure, and an arbitrary pressure; The first storage unit causes the solution to perform first gas-liquid separation before the solution is raised from the inflow port to the discharge path, and the discharge path includes the first storage The solution discharged from the inside of the second container While Tsutawa the placed guide member is supplied to the second housing portion, characterized in that to perform the second gas-liquid separation in the solution therebetween.

According to this bubble removing device, the solution can be raised from the inlet to the discharge path in the first container by allowing the solution to flow into the first container through the inlet. Then, in the process in which the solution rises, the bubbles contained in the solution rise faster than the solution due to the buoyancy due to the density difference from the solution, so that the bubbles can be separated from the solution.
In particular, since the liquid column pressure of the solution gradually decreases from the inlet side toward the discharge path side, as the bubbles rise, the pressure difference between the inside and outside of the bubbles gradually increases, and the volume of the bubbles gradually increases. Inflate (increase). Therefore, since the velocity further increases as the bubbles rise, it becomes easier to separate from the solution quickly.
As described above, by raising the solution in the first housing portion, the solution can be subjected to the first gas-liquid separation, and the bubbles contained in the solution can be removed.

  And the solution which rose in the 1st accommodating part is discharged | emitted from a 1st accommodating part through a discharge channel, and is supplied in a 2nd accommodating part. At this time, the discharge path gently supplies the solution into the second accommodating portion while the guide member is transmitted without dropping the solution, for example. In this process, even if bubbles remain in the solution without being removed by the first gas-liquid separation, the bubbles can be separated from the solution and escaped. In this way, by supplying the solution into the second storage portion while being transmitted along the guide member, the solution can be subjected to the second gas-liquid separation, and for example, fine bubbles can be finally removed. it can. And the solution from which the bubble was removed can be accommodated in a 2nd accommodating part.

In particular, since the pressure adjusting unit adjusts the internal pressures of the first storage unit and the second storage unit communicating with each other through the discharge path to the same pressure, and adjusts them to an arbitrary pressure, the first storage unit, the discharge path, and the The internal pressure of the second container can be maintained at the pressure when the solution is produced. Therefore, since the pressure environment does not change, only the bubbles can be removed from the solution without causing a deaeration action that changes the gas component dissolved in the solution into bubbles. Therefore, the solution from which only the bubbles are removed can be stored in the second storage portion while maintaining the gas solubility.
Also, unlike the conventional standing method in which the solution is simply left for a long time, the first gas-liquid separation by raising the solution in the first housing portion and the solution while guiding the guide member in the second housing portion By actively performing the second gas-liquid separation by supplying the gas, it is possible to efficiently remove the bubbles from the solution. Therefore, the solution in which bubbles are removed and the gas solubility is maintained can be efficiently stored in the second storage portion, and the solution can be easily extracted and used through the outflow port.

(2) The guide member may be an inner wall surface of the second storage portion, and the discharge path may be configured such that the solution discharged from the first storage portion is transmitted along the inner wall surface of the second storage portion. You may supply in an accommodating part.

  In this case, since the inner wall surface of the second housing portion can be used as a guide member, it is not necessary to prepare a guide member separately from the second housing portion, and the configuration can be simplified.

(3) A space portion may be secured in a portion located above the discharge path in the first housing portion.

  In this case, the bubbles separated from the solution by the first gas-liquid separation in the first accommodating portion can be released to the space portion by being bounced on the liquid surface and removed. Therefore, it can suppress that the bubble isolate | separated from the solution will be supplied in a 2nd accommodating part through a discharge channel. Therefore, the bubbles can be removed more efficiently.

(4) You may provide the supply part which supplies the said solution continuously in the said 1st accommodating part through the said inflow port.

  In this case, since the supply unit continuously supplies the solution into the first storage unit, the work of removing bubbles from the solution can be performed more efficiently.

(5) A stirrer having a stirrer container connected to the first container through the inflow port and a stirrer that stirs the solvent and the gas in the stirrer container to produce the solution. The pressure adjusting unit may adjust the internal pressure of the first storage unit and the second storage unit so as to be the same pressure as the internal pressure of the stirring container.

  In this case, a stirrer can stir the solvent and gas in the stirring vessel to prepare a solution, and after the preparation of the solution, the solution can be supplied into the first storage portion through the inlet. As described above, since the stirrer for preparing a solution by stirring is provided, a solution in which bubbles are removed and gas solubility is maintained can be obtained more efficiently and continuously.

(6) The second container is provided with a stirring unit having a stirrer that stirs the solvent and the gas in the second container to produce the solution, and the first container and the second container Between the storage part, a liquid feeding part for supplying the stirred solution flowing out from the second storage part through the outlet to the first storage part through the inlet is provided, and the stirrer After the preparation of the solution, stirring may be stopped.

In this case, the stirrer can stir the solvent and gas in the second container, and the solution can be prepared. After the preparation of the solution, the solution feeding part transfers the stirred solution from the second container to the first container. Supply. As described above, since the stirrer for preparing a solution by stirring is provided, a solution in which bubbles are removed and gas solubility is maintained can be obtained more efficiently and continuously.
In particular, the second container can be used first as a stirring container, and then can also be used as a container for storing a solution from which bubbles are removed. Therefore, it is not necessary to prepare a separate stirring container, and the configuration is simplified. In addition, it is not necessary to secure an extra installation space for installing the stirring container. In addition, since stirring is stopped after preparation of a solution, there is no possibility that air bubbles may be mixed after preparation of the solution.

(7) The liquid feeding unit may supply the solution after the second gas-liquid separation into the first storage unit through the inlet.

  In this case, since the first gas-liquid separation in the first housing portion and the second gas-liquid separation in the second housing portion can be repeatedly performed, bubbles can be removed more efficiently. In addition, a solution with further stable quality can be obtained.

(8) You may provide the measurement part which measures the gas solubility of the gas component contained in the said solution after said 2nd gas-liquid separation.

  In this case, since the gas solubility of the solution contained in the solution after the second gas-liquid separation can be measured, the gas solubility can be appropriately confirmed as necessary to obtain a more stable quality solution. Can do.

(9) The bubble removing method according to the present invention includes a step of supplying the solution into the first housing part so that a solution in which a gas is dissolved in the solvent rises in the first housing part; and A step of causing the solution to perform a first gas-liquid separation while ascending in the container, and discharging the solution rising in the first container from the first container through a discharge path, A step of supplying into the two storage portions, and a step of adjusting the internal pressures of the first storage portion and the second storage portion communicating with each other through the discharge path to the same pressure and an arbitrary pressure . After performing the step of adjusting the internal pressure of the first storage unit and the second storage unit, the step of supplying the solution into the first storage unit, the step of performing the first gas-liquid separation, and the solution of the first performed supplying the second housing portion, said solution said second yield When supplying into the section, the solution is supplied into the second storage section while being guided by the guide member disposed in the second storage section, and the second gas-liquid separation is performed on the solution in the meantime. Features.

  According to this bubble removal method, the same effect as the above-described bubble removal device can be achieved.

  According to the present invention, it is possible to efficiently remove only the bubbles from the solution while maintaining the gas solubility without affecting the gas component dissolved in the solution.

It is a block diagram which shows 1st Embodiment of the bubble removal apparatus which concerns on this invention. It is a block diagram of the solubility measuring apparatus shown in FIG. It is a figure which shows the state which is removing the bubble by the bubble removal apparatus shown in FIG. It is a block diagram which shows 2nd Embodiment of the bubble removal apparatus which concerns on this invention. It is a block diagram which shows 3rd Embodiment of the bubble removal apparatus which concerns on this invention. It is a figure which shows the state which rotates the stirring element from the state shown in FIG. 5, and is stirring water and methane. It is a figure which shows the state which has removed the bubble from the solution produced by stirring after stopping a stirring element from the state shown in FIG. It is a figure which shows the state which drives the liquid feeding pump in the reverse direction from the state shown in FIG. 7, and is analyzing the composition of the methane in a 2nd storage tank with a solubility measuring apparatus. It is a figure which shows the numerical value of the methane solubility at the time of actually removing a bubble with the apparatus corresponded to the bubble removal apparatus shown in FIG. 1, and measuring methane solubility in multiple times.

(First embodiment)
Hereinafter, a first embodiment according to the present invention will be described with reference to the drawings.
(Configuration of bubble removal device)
As shown in FIG. 1, the bubble removing device 1 of the present embodiment stirs degassed water (solvent) W such as pure water and methane (gas) M, and provides a solution S in which methane M is dissolved in water W. A stirrer (stirring unit) 2 to be produced, a first storage tank (first storage unit) 3 that stores the solution S stirred by the stirrer 2, and a discharge that discharges the solution S from the first storage tank 3 A line (discharge path) 4, a second storage tank (second storage section) 5 for storing the solution S discharged in the discharge line 4, a stirrer 2, a first storage tank 3, a discharge line 4 and a second 2 and a pressure adjusting unit 6 for adjusting the internal pressure of the storage tank 5.

  In the present embodiment, water W and methane M will be described as examples, but the types of the solvent and gas are not limited to this case, and various types can be adopted. These solvents and gases may be freely selected according to the way.

  The stirrer 2 is, for example, a magnetic mixer type stirrer, in which water W and methane M are supplied, and a stirring tank (stirring container) 10 that stores the solution S prepared by stirring, and a stirring tank 10 includes a stirrer 11 that stirs the water W and methane M, and a drive unit 12 that rotates the stirrer 11 using magnetic force.

The agitation tank 10 is arranged in a standing state with respect to the ground or floor surface (not shown), and is stably supported via a gantry (not shown). A first supply line 20 to which water W is supplied and a second supply line 21 to which methane M is supplied are connected to the upper part of the stirring tank 10. The first supply line 20 and the second supply line 21 are composed of, for example, pressure-resistant hoses or pipes, and can supply water W and methane M to the agitation tank 10 with a certain pressure applied, respectively. It is said that.
In the stirring tank 10, a space (gas phase space) R1 is formed in the upper part.

  The first supply line 20 is also connected to a raw material tank 22 in which water W is accommodated. Thereby, the 1st supply line 20 has connected the raw material tank 22 and the stirring tank 10 mutually. In the middle of the first supply line 20, a liquid feed pump 23 is provided for supplying water W in the raw material tank 22 while pressurizing the water W toward the stirring tank 10. Thereby, by operating the liquid feed pump 23, the water W can be supplied into the stirring tank 10 in a pressurized state.

The operation of the liquid feed pump 23 is controlled by the control unit 7 that comprehensively controls the bubble removing device 1 and the supply amount of the water W is also controlled.
The first supply line 20 is provided with a pressure gauge 24 that measures the internal pressure of the first supply line 20 between the liquid feed pump 23 and the stirring tank 10.

The second supply line 21 is also connected to a gas supply unit 30 in which methane M is accommodated. Thereby, the 2nd supply line 21 has connected the gas supply part 30 and the stirring tank 10 mutually.
The gas supply unit 30 includes a cylinder unit 31 accommodated in a state in which methane M is pressurized therein, a piston unit 32 that introduces the methane M in the cylinder unit 31 from the cylinder unit 31 to the second supply line 21, and It has. Thus, by operating the piston portion 32, the pressurized methane M can be supplied to the space portion R1 in the stirring tank 10.

  The operation of the piston part 32 is controlled by the control part 7. The second supply line 21 is provided with a pressure gauge 33 that measures the internal pressure of the second supply line 21 between the gas supply unit 30 and the stirring tank 10. The control unit 7 monitors the measurement value of the pressure gauge 33.

As described above, the water W is supplied in a pressurized state through the first supply line 20 to the stirring tank 10, and the methane M is supplied in a pressurized state through the second supply line 21. A storage chamber 15 in which the drive unit 12 described above is stored is provided at the lower part of the bottom wall 10 a of the stirring tank 10.
The drive unit 12 includes a motor 12a and a magnetic body 12b such as a magnet connected to a rotation shaft portion of the motor 12a. The motor 12a is, for example, a motor with a variable rotational speed, and the operation is controlled by the control unit 7 and the rotational speed is also controlled. The magnetic body 12b rotates in a plane parallel to the bottom wall 10a of the stirring tank 10 with the operation of the motor 12a.

The stirrer 11 is disposed on the bottom wall 10a side in the stirring tank 10, and rotates in a plane parallel to the bottom wall 10a while following the rotation of the magnetic body 12b by the magnetic force from the magnetic body 12b. Thereby, it is possible to stir the water W and methane M supplied into the stirring tank 10.
The stirrer 11 may be made of, for example, a metal having magnetism, or may be a metal having magnetism sealed with a resin material. In addition, the shape of the stirring bar 11 may be, for example, an elongated rod shape or a blade shape such as a windmill. The material, shape, and the like of the stirrer 11 may be freely selected according to the stirring efficiency, load, and the like. In the illustrated example, the case where the stirrer 11 is formed in a blade shape is taken as an example.

  Since the stirrer 2 is configured as described above, the water W and the methane M supplied into the stirring tank 10 can be stirred and gas-liquid mixed by rotating the stirrer 11 in a pressurized state. A high-pressure solution S in which methane M is dissolved in water W can be produced.

  The 1st storage tank 3 is arrange | positioned in the state standing up with respect to the ground or floor surface which is not shown in figure, and is stably supported via the mount frame which is not shown in figure. The first storage tank 3 is arranged side by side with the stirring tank 10, for example.

An inlet 40 through which the solution S flows is formed in the bottom wall 3 a of the first storage tank 3, and a connection line 41 is connected through the inlet 40. The connection line 41 is constituted by, for example, a pressure-resistant hose or pipe, and is also connected to the stirring tank 10. Thereby, the solution S in the stirring tank 10 receives the liquid column pressure of the solution S in the stirring tank 10 and flows into the first storage tank 3 through the connection line 41 and the inflow port 40.
At this time, since the inlet 40 is formed in the bottom wall 3 a of the first storage tank 3, the solution S that has flowed into the first storage tank 3 flows upward in the first storage tank 3. In this process, the solution S can be subjected to the first gas-liquid separation (first gas-liquid separation), and the bubbles contained in the solution S can be removed. This will be described in detail later.

The liquid feed pump 23 not only simply supplies the water W into the stirring tank 10 as described above, but also supplies the solution S in the stirring tank 10 through the connection line 41 and the inlet 40 into the first storage tank 3. It also functions as a supply unit for continuously supplying to the printer.
The solution S that has flowed into the first storage tank 3 is stored (stored) in the first storage tank 3. At this time, the liquid level of the solution S stored in the first storage tank 3 is set to a height equivalent to the liquid level of the solution S in the stirring tank 10 (the liquid level of the solution S in a state where stirring is not performed). Yes.

The discharge line 4 is composed of, for example, a pressure-resistant hose or pipe, and is connected to the first storage tank 3 above the inflow port 40. In the illustrated example, the discharge line 4 is connected to the first storage tank 3 at a position equivalent to the liquid level of the solution S. The discharge line 4 is also connected to the second storage tank 5. As a result, the discharge line 4 discharges the solution S (solution S after the first gas-liquid separation) flowing upward from the inlet 40 from the first storage tank 3, and enters the second storage tank 5. Supply.
In the first storage tank 3, a space (gas phase space) R <b> 2 is formed in a portion located above the discharge line 4.

  The second storage tank 5 is arranged in a standing state with respect to the ground or floor surface not shown, and is stably supported via a gantry not shown. For example, the second storage tank 5 is arranged side by side with the agitation tank 10 and the first storage tank 3.

  An outlet 42 through which the solution S flows out is formed on the bottom wall 5 a of the second storage tank 5, and an outlet line 43 is connected via the outlet 42. The outflow line 43 functions as a main outflow route, and is configured by, for example, a pressure-resistant hose or pipe. A first outflow valve 44 is provided in the middle of the outflow line 43. The first outflow valve 44 is a valve that opens and closes the outflow line 43, and its operation is controlled by the control unit 7. Accordingly, by opening the first outflow valve 44, the solution S stored in the second storage tank 5 can be discharged from the second storage tank 5 through the outflow port 42 and the outflow line 43 and extracted. ing.

The second storage tank 5 is provided with a liquid level gauge 50 for measuring the liquid level of the solution S stored therein.
The liquid level gauge 50 is, for example, a capacitance type liquid level gauge, and has an internal electrode 51 disposed in the second storage tank 5 and an external provided along the inner wall surface 5b of the second storage tank 5. The electrode 52 and the calculation part 53 which calculates a liquid level height based on the electrostatic capacitance between the internal electrode 51 and the external electrode 52 are provided.

The internal electrode 51 is a rod-like electrode that extends over almost the entire length of the second storage tank 5, and is disposed in the second storage tank 5 in a non-contact state with respect to the second storage tank 5 and the external electrode 52. Yes. The external electrode 52 is an electrode formed along the inner wall surface 5 b over almost the entire length of the second storage tank 5. However, when the second storage tank 5 is made of metal, the second storage tank 5 itself may be used as the external electrode 52.
Since the internal electrode 51 and the external electrode 52 are arranged in this way, the solution S in the second storage tank 5 accumulates between the internal electrode 51 and the external electrode 52. Thereby, the electrostatic capacitance between the internal electrode 51 and the external electrode 52 changes according to the amount of the solution S stored in the second storage tank 5.

The calculation unit 53 includes the internal electrode 51 and the external electrode 52 in an empty state where the solution S is not stored in the second storage tank 5 (the state where the solution S does not exist between the internal electrode 51 and the external electrode 52). Between the internal electrode 51 and the external electrode 52 in a state where the solution S is fully stored in the second storage tank 5. We grasp as electric capacity.
Thereby, the calculation part 53 calculates the accommodation rate of the solution S based on the measured electrostatic capacitance between the internal electrode 51 and the external electrode 52 and the reference electrostatic capacitance previously grasped. Can do. For example, it can be calculated that the solution S is stored up to 50% of the total capacity of the second storage tank 5. Thereby, the calculation unit 53 can calculate the liquid level of the solution S from the relationship between the capacity of the second storage tank 5 and the storage rate of the solution S.

  The control unit 7 always maintains a position where the liquid level of the solution S in the second storage tank 5 calculated by the calculation unit 53 is lower than the liquid level of the solution S in the first storage tank 3. Thus, the outflow amount of the solution S by the first outflow valve 44 and the supply amount of water W by the liquid feed pump 23 are comprehensively controlled. As a result, a space (gas phase space) R <b> 3 is formed in the second storage tank 5 in a portion located above the discharge line 4.

  By the way, the discharge line 4 described above uses the inner wall surface 5b of the second storage tank 5 as a guide member, and supplies the solution S into the second storage tank 5 while being transmitted along the inner wall surface 5b (see FIG. 3). ). Thereby, the solution S flows along the inner wall surface 5b and is stored in the second storage tank 5 without foaming, for example. In this process, the solution S can be subjected to the second gas-liquid separation (second gas-liquid separation), and bubbles remaining in the solution S can be removed. This will be described in detail later.

An adjustment line 35 for pressure adjustment is further connected to the second supply line 21 that connects the gas supply unit 30 and the stirring tank 10. Similar to the second supply line 21, the adjustment line 35 is configured by a pressure-resistant hose or pipe, for example, and is connected to the first storage tank 3 and the second storage tank 5, respectively.
Thereby, the space R1 located in the upper part in the stirring tank 10, the space R2 located in the upper part in the first storage tank 3, the space R3 located in the upper part in the second storage tank 5, and the first The discharge line 4 that connects the space R2 in the first storage tank 3 and the space R3 in the second storage tank 5 communicates with each other through the second supply line 21 and the adjustment line 35. Therefore, the internal pressures of the stirring tank 10, the first storage tank 3, the second storage tank 5 and the discharge line 4 are the same.

A relief valve 36 for releasing the pressure in the first storage tank 3 is provided at the top of the first storage tank 3. Further, the second supply line 21 is provided with a relief valve 37 for releasing the pressure in the second supply line 21. The operation of these relief valves 36 and 37 is controlled by the control unit 7.
Then, the control unit 7 comprehensively controls the piston unit 32 of the gas supply unit 30 and the two escape valves 36 and 37, so that the agitation tank 10, the first storage tank 3, the second storage tank 5, and the discharge are discharged. In addition to adjusting the internal pressure of the line 4 to the same pressure, it is possible to adjust to an arbitrary pressure.

  Accordingly, the second supply line 21, the adjustment line 35, the gas supply unit 30, the two relief valves 36 and 37, and the control unit 7 function as the pressure adjustment unit 6 described above. In particular, the pressure adjusting unit 6 only adjusts the internal pressure of the stirring tank 10 to an optimum pressure for stirring, and the internal pressures of the first storage tank 3 and the second storage tank 5 that communicate with each other through the discharge line 4 are also adjusted. It can be adjusted to the same pressure as the internal pressure.

  The adjustment line 35 is provided with a pressure gauge 38 for measuring the pressure in the adjustment line 35. The control unit 7 monitors the measurement value of the pressure gauge 38 and the measurement value of the pressure gauge 33 provided in the second supply line 21, and based on these measurement values, the stirring tank 10 and the first storage tank. 3. The internal pressure of the entire second storage tank 5 and the discharge line 4 is accurately adjusted.

  A branch line 45 made of, for example, a pressure resistant hose or pipe is connected to the outflow line 43 for extracting the solution S from the second storage tank 5 upstream of the first outflow valve 44. This branch line 45 functions as a sub (auxiliary) outflow route. Therefore, for example, the branch line 45 may have a smaller diameter than the outflow line 43 that is the main outflow route, and the outflow amount may be suppressed. The branch line 45 is provided with a solubility measuring device (measuring unit) 60 for measuring the solubility of the methane component (gas component) dissolved in the solution S flowing out from the outlet 42.

  Examples of the solubility measuring apparatus 60 include an apparatus described in Japanese Patent No. 5004112, and can be incorporated in the present specification. Specifically, the solubility measuring device 60 includes a gas chromatograph 61 and a data processing unit 62.

  As shown in FIG. 1 and FIG. 2, the gas chromatograph 61 includes a sampling valve 65 into which the solution S is introduced, a heating vaporizer 66 that heats and vaporizes the solution S, and a methane component and water W A pre-column 67 and a main column 68, a detector 69 for detecting the separated methane component and water W, a first supply unit 70 for supplying a carrier gas to the gas chromatograph 61, and a carrier for the heating vaporizer 66. And a second supply unit 71 for supplying gas.

The sampling valve 65 includes a valve body 65a having a ring shape in plan view, and a valve rotor 65b having a circular shape in plan view that is disposed inside the valve body 65a and is rotatable around the rotation axis O. .
Two slots 72 and 73 are formed in the inner wall of the valve rotor 65b. In the illustrated example, the two slots 72 and 73 are arranged so as to face each other with the rotation axis O therebetween. However, the number of slots 72 and 73 is not limited to two, and may be one or three or more.

The valve body 65 a is formed with two connection ports 75 and 76 connected to the slot 72 and two connection ports 77 and 78 connected to the slot 73.
Since the positions of the slots 72 and 73 are switched by rotating the valve rotor 65b halfway, the slot 72 and the two connection ports 77 and 78 are connected, and the slot 73 and the two connection ports 75 and 76 are connected. Connected.

  The branch line 45 described above is connected to connection ports 75 and 76. Thereby, the solution S flowing through the branch line 45 can be introduced into the slot 72. In the branch line 45, a second outflow valve 46 is provided in a portion located upstream from the connection port 75, and a third outflow valve 47 is provided in a portion located downstream from the connection port 76. The second outflow valve 46 and the third outflow valve 47 are valves that open and close the branch line 45, and their operations are controlled by the control unit 7.

The heating vaporizer 66 is connected to the connection port 78, and the first supply unit 70 is connected to the connection port 77. Thereby, the slot 72 into which the solution S is introduced is positioned on the two connection ports 77 and 78 side by the rotation of the valve rotor 65b, so that the solution S is transferred from the slot 72 to the heating vaporizer 66 using the carrier gas. It is possible to introduce.
Note that a valve member such as a check valve (not shown) is provided between the first supply unit 70 and the connection port 77, and the carrier gas supplied from the first supply unit 70 toward the connection port 77 is provided. The backflow is prevented.

The heating vaporizer 66 has a heater (not shown) that rapidly heats the solution S. The pre-column 67 and the main column 68 are connected to the heating vaporizer 66. The second supply unit 71 is also connected to the heating vaporizer 66. Thereby, the solution S heated and vaporized using the carrier gas is introduced into the pre-column 67 and the main column 68 from the heat vaporizer 66 and reliably separated into water W and methane M by the pre-column 67 and the main column 68. Is possible.
Note that a valve member such as a check valve (not shown) is provided between the heating vaporizer 66 and the second supply unit 71, and is supplied from the second supply unit 71 toward the heating vaporizer 66. Backflow of carrier gas is prevented.

  The pre-column 67 and the main column 68 can be appropriately selected from known ones according to the component to be detected dissolved in the solution S. The detector 69 is connected to the main column 68. Similarly, this detector 69 can employ a known detector as appropriate according to the component to be detected.

  The data processing unit 62 processes the data output from the gas chromatograph 61 configured as described above, and calculates the solubility of the methane component dissolved in the solution S. Thus, the solubility measuring device 60 can measure the methane solubility (gas solubility) in the solution S. The control unit 7 monitors the measured methane solubility.

(Operation of the bubble removal device)
Next, by using the bubble removing device 1 configured as described above, only bubbles from the solution S are removed while maintaining the methane solubility without affecting the methane component dissolved in the solution S. An efficient removal method (bubble removal method) will be described.

  In addition, all the component parts which comprise the bubble removal apparatus 1 are temperature-controlled, and are controlled so that it may become the same or comparable temperature. Further, at the initial stage of the bubble removing device 1, the stirring tank 10, the first storage tank 3, and the second storage tank 5 are all empty. However, in order to make the following description easy to understand, the stirring tank 10 is in a state where water W and methane M are supplied as shown in FIG. 1, and in the first storage tank 3 and the second storage tank 5 It demonstrates as the state in which the solution S is accommodated.

  First, the stirrer 2 is operated and the stirring operation of the water W and the methane M in the stirring tank 10 is started. Specifically, as shown in FIG. 3, the motor 12a is driven in response to an instruction from the control unit 7 to rotate the magnetic body 12b. Thereby, the stirring bar 11 arrange | positioned in the stirring tank 10 can be rotated so that the magnetic body 12b may be followed using the magnetic force of the magnetic body 12b. By rotating the stirrer 11, the water W and methane M in the stirring tank 10 can be stirred and gas-liquid mixed, and a high-pressure solution S in which the methane M is dissolved in the water W can be produced. It should be noted that bubbles are contained in the solution S by stirring.

When the solution S is prepared by stirring, the liquid feed pump 23 operates in response to an instruction from the control unit 7 and supplies new water W into the stirring tank 10. The produced solution S receives the liquid column pressure of the solution S in the stirring tank 10 and flows toward the connection line 41, and flows into the first storage tank 3 through the inlet 40.
Thereafter, the liquid feed pump 23 continuously supplies the water W into the stirring tank 10. Thereby, while being able to continue producing the solution S continuously in the stirring tank 10, the produced solution S can be continuously flowed into the first storage tank 3 through the connection line 41 and the inlet 40. it can.

  The solution S that has flowed into the first storage tank 3 rises upward from the inlet 40. Then, in the process in which the solution S rises, the bubbles contained in the solution S rise faster than the solution S due to the buoyancy due to the density difference from the solution S, so that the bubbles can be separated from the solution S.

In particular, the liquid column pressure of the solution S gradually decreases from the inlet 40 side (the bottom wall 3a side of the first storage tank 3) toward the discharge line 4 side (the liquid surface side). The pressure difference between the inside and outside of the bubble gradually increases, and the volume of the bubble gradually expands (increases). Therefore, since the velocity further increases as the bubbles rise, it becomes easy to separate from the solution S quickly.
Thus, by raising the solution S in the first storage tank 3, the solution S can be subjected to the first gas-liquid separation (first gas-liquid separation).

  The solution S that has risen in the first storage tank 3 is discharged from the first storage tank 3 through the discharge line 4 and then supplied into the second storage tank 5. At this time, the discharge line 4 gently supplies the solution S into the second storage tank 5 while being transmitted along the inner wall surface 5b of the second storage tank 5 without dripping the solution S, for example. In this process, even if the solution S cannot be completely removed by the first gas-liquid separation and bubbles remain in the solution S, the bubbles are further separated from the solution S to form a space portion. Can be released to R3.

In this way, the second gas-liquid separation (second gas-liquid separation) is performed on the solution S by supplying the solution S into the second storage tank 5 while being transmitted along the inner wall surface 5 b of the second storage tank 5. For example, even fine bubbles can be finally removed. Then, the solution S from which bubbles are removed can be stored in the second storage tank 5.
In particular, in the first storage tank 3, the bubbles separated from the solution S can be released to the space portion R <b> 2 by being bounced at the liquid level and removed, so that the bubbles separated from the solution S are secondly discharged through the discharge line 4. Supplying into the storage tank 5 can be suppressed. Therefore, it is possible to efficiently remove bubbles.

In addition, since the pressure adjusting unit 6 adjusts the internal pressures of the stirring tank 10, the discharge line 4, the first storage tank 3, and the second storage tank 5 to the same pressure, the solution S is prepared in the stirring tank 10. The pressure can be maintained. Therefore, since the pressure environment does not change, only the bubbles can be removed from the solution S without causing a deaeration action that changes the methane component dissolved in the solution S into bubbles. Therefore, only bubbles can be removed from the solution S while maintaining methane solubility.
In addition, since all the components constituting the bubble removing device 1 are temperature-controlled, it is possible to suppress changes in the temperature environment and to degas the methane component dissolved in the solution S into bubbles. The action is less likely to occur.

Further, unlike the conventional standing method in which the solution S is simply left standing for a long time, the first gas-liquid separation by raising the solution S in the first storage tank 3 and the inside of the second storage tank 5 are performed. By actively performing the second gas-liquid separation by supplying the solution S while being transmitted along the wall surface 5b, the work of removing bubbles from the solution S can be performed efficiently. Therefore, the solution S in which bubbles are removed and the methane solubility is maintained can be efficiently stored in the second storage tank 5.
In particular, the liquid feed pump 23 continuously supplies the water W into the stirring tank 10 and continuously causes the solution S prepared in the stirring tank 10 to flow into the first storage tank 3. Compared to the stationary method in which the stationary operation is performed alternately, the operation of removing bubbles from the solution S can be performed much more efficiently.

As described above, according to the bubble removal device 1 and the bubble removal method of the present embodiment, the methane solubility is maintained without affecting the methane component dissolved in the solution S, and the methane solubility is maintained from the solution S. Only bubbles can be removed efficiently.
Further, by opening the first outflow valve 44, the solution S in the second storage tank 5 can be withdrawn continuously or periodically through the outflow port 42 and the outflow line 43. Therefore, the solution S from which bubbles are removed and the methane solubility is stably maintained can be taken out while maintaining the quality, and can be used for various purposes thereafter.

By the way, since the solubility measuring device 60 is provided, the solubility of the methane component contained in the solution S extracted from the second storage tank 5 can be appropriately confirmed as necessary, and the solution S having a more stable quality. Can be obtained.
The case where methane solubility is measured will be briefly described below.

In this case, for example, the first outflow valve 44 is closed, the second outflow valve 46 is opened, and the third outflow valve 47 is closed, so that the second outflow line 43 is extracted from the second storage tank 5 through the outflow port 42. Solution S can flow through branch line 45 and can be introduced into slot 72 of gas chromatograph 61.
When the solution S is introduced into the slot 72, as shown in FIG. 2, the valve rotor 65b is rotated halfway to position the slot 72 on the connection ports 77 and 78 side. Further, the first supply unit 70 supplies the carrier gas and sends the solution S in the slot 72 to the heating vaporizer 66. Thereby, the solution S is heated and vaporized by the heating vaporizer 66.

  The heated and vaporized solution S is sent to the pre-column 67 and the main column 68 by the supply of the carrier gas by the second supply unit 71, and is separated into water W (water vapor) and a methane component. The separated water W and methane components are detected for each component by the detector 69. This detection value is expressed, for example, by the relationship between the retention time and the voltage value (or current value, etc.) of the component concentration or mass change. This relationship is called a gas chromatogram.

The data processing unit 62 calculates the solubility of the methane component in the water W based on the gas chromatogram (detection value). For example, it can be calculated by preparing a standard gas and water W having the same components as the methane component and high purity, and preparing these calibration curves in advance.
In this way, methane solubility can be measured easily and simply. Therefore, the methane solubility of the solution S can be quickly confirmed as necessary.

(Second Embodiment)
Next, a second embodiment according to the present invention will be described.
The difference from the first embodiment is that, in the first embodiment, the stirring tank 10, the first storage tank 3, and the second storage tank 5 are separate tanks, but in the second embodiment, the stirring tank 10, The first storage tank 3 and the second storage tank 5 are integrated.
In the second embodiment, the same components as those in the first embodiment are denoted by the same reference numerals, and the description thereof is omitted.

As shown in FIG. 4, the bubble removing device 70 of the present embodiment includes a unit tank 71 in which the stirring tank 10, the first storage tank 3, and the second storage tank 5 are integrally connected. In the present embodiment, the liquid level gauge 50 is not shown.
The space R1 of the stirring tank 10 and the space R2 of the first storage tank 3 are connected via a first connection pipe 72. Further, the space portion R <b> 2 of the first storage tank 3 and the space portion R <b> 3 of the second storage tank 5 are connected via a second connection pipe 73. Thereby, the inside of the stirring tank 10, the 1st storage tank 3, and the 2nd storage tank 5 is mutually connected.

The first connection pipe 72 and the second connection pipe 73 are configured to restrict the solution S that has risen in the first storage tank 3 from flowing toward the stirring tank 10 and allow the solution S to flow into the second tank. Has been placed.
The second connection pipe 73 functions as a discharge path for discharging the solution S that has risen in the first storage tank 3 into the second storage tank 5 while being transmitted along the inner wall surface 5 b of the second storage tank 5.

Even if it is the bubble removal apparatus 70 comprised in this way, the effect similar to the bubble removal apparatus 1 of 1st Embodiment can be achieved.
In particular, in the case of the present embodiment, the agitation tank 10, the first storage tank 3, and the second storage tank 5 are unit tanks 71 that are integrally connected. Therefore, the adjustment line 35 in the first embodiment is unnecessary. It becomes. Therefore, the number of parts can be reduced and the configuration can be simplified.

(Third embodiment)
Next, a third embodiment according to the present invention will be described.
The difference from the first embodiment is that the stirring tank 10 is provided in the first embodiment, but the second storage tank also serves as the stirring tank in the third embodiment.
In the third embodiment, the same components as those in the first embodiment are denoted by the same reference numerals, and the description thereof is omitted.

  As shown in FIG. 5, the bubble removing device 80 of the present embodiment includes a first storage tank 3, a discharge line 4 that discharges the solution S from the first storage tank 3, and a solution S that has been discharged from the discharge line 4. A second storage tank (second storage section) 81 stored in the interior and a pressure adjustment section 6 are provided.

As described above, the second storage tank 81 also serves as the stirring tank 10 in the first embodiment. Accordingly, a first supply line 20 to which water W is supplied and a second supply line 21 to which methane M is supplied are connected to the upper portion of the second storage tank 81. In the present embodiment, illustration of the raw material tank 22, the liquid feed pump 23, and the pressure gauge 24 is omitted.
Accordingly, water W and methane M are supplied into the second storage tank 81 through the first supply line 20 and the second supply line 21.

The second storage tank 81 is provided with a stirring unit 82 having a stirrer 11 that stirs the water W and methane M in the second storage tank 81 to produce the solution S. Under the bottom wall 81 a of the second storage tank 81, a storage chamber 83 that stores the drive unit 12 that rotates the stirrer 11 is provided.
Therefore, by rotating the stirrer 11, the water W and the methane M supplied into the stirring tank 10 can be stirred and gas-liquid mixed in a pressurized state, and the high pressure at which the methane M is dissolved in the water W. It is possible to prepare the solution S. The stirrer 11 stops stirring as the motor 12a of the driving unit 12 stops after the solution S is produced.

  An outlet 84 through which the solution S flows out is formed in a portion of the peripheral wall of the second storage tank 81 located on the bottom wall 81a side. A connection line 41 connected to the inlet 40 of the first storage tank 3 is connected to the outlet 84. The connection line 41 is provided with a liquid feed pump (liquid feed unit) 85 that supplies the solution S that has flowed out of the second storage tank 81 through the outlet 84 into the first storage tank 3 through the inlet 40. .

  The liquid feed pump 85 is a pump whose operation is controlled by the control unit 7 and whose internal motor (not shown) rotates forward and backward. Therefore, the liquid feed pump 85 can supply the solution S in the second storage tank 81 to the first storage tank 3 as described above by the forward rotation of the internal motor, and on the contrary, the internal motor is reversed. By rotating, the solution S in the first storage tank 3 can be supplied to the second storage tank 81.

  In addition, an outflow line 43 provided with a first outflow valve 44 is connected to the connection line 41 at a portion located between the second storage tank 81 and the liquid feed pump 85. Thereby, for example, after the removal of the bubbles from the solution S is completed, the solution S stored in the second storage tank 81 is extracted to the outside through the outlet 84 and the outlet line 43 by opening the first outlet valve 44. It is possible.

The discharge line 4 is connected to the top wall 3 b of the first storage tank 3 and to the peripheral wall on the upper side of the second storage tank 81. As a result, the discharge line 4 discharges the solution S flowing upward from the inlet 40 from the first storage tank 3 and supplies the solution S into the second storage tank 81. At this time, the discharge line 4 supplies the solution S into the second storage tank 81 while being transmitted along the inner wall surface 81b of the second storage tank 81 (see FIGS. 6 and 7).
In the present embodiment, since the discharge line 4 is connected to the top wall 3b of the first storage tank 3, after the solution S fills the inside of the first storage tank 3, the solution S is removed through the discharge line 4. 1 Discharge from the storage tank 3.

  A branch line 90 and a return line 91 are connected to the discharge line 4. The branch line 90 is connected between the discharge line 4 and the connection port 76 of the solubility measuring device 60. The return line 91 is connected to a portion of the discharge line 4 that is located closer to the second storage tank 81 than the connection portion of the branch line 90, and is connected to the connection port 75 of the solubility measuring device 60.

Further, the discharge line 4 is provided with a switching valve 92 between the connection part of the branch line 90 and the connection part of the return line 91. The switching valve 92 is a valve that opens and closes the discharge line 4, and its operation is controlled by the control unit 7. By opening the switching valve 92, the solution S can be discharged preferentially toward the second storage tank 81, and by closing the switching valve 92, the solution S can be discharged to the branch line 90 side. By discharging the solution S to the branch line 90 side, the solubility of the solution S can be measured using the solubility measuring device 60, and the measured solution S is directed toward the second storage tank 81 through the return line 91. It is possible to flow.
Thus, the solubility of the solution S can be measured by operating the switching valve 92 as necessary.

By the way, the space part R3 located in the upper part in the second storage tank 81 and the space part R2 of the first storage tank 3 communicate with each other through the discharge line 4. Therefore, the internal pressures of the first storage tank 3 and the second storage tank 81 are the same. Note that when the liquid feed pump 85 is driven, the interior of the first storage tank 3 is filled with the solution S, so that the space R2 of the first storage tank 3 is filled with the solution S (see FIGS. 6 and 7). ).
The second supply line 21 is provided with a relief valve 36 for releasing the pressure in the second storage tank 81 and a relief valve 37 for releasing the pressure in the second supply line 21. The control unit 7 comprehensively controls the piston unit 32 of the gas supply unit 30 and the two relief valves 36 and 37, so that the entire internal pressure of the first storage tank 3 and the second storage tank 81 can be set to an arbitrary pressure. It is possible to adjust to.

(Operation of the bubble removal device)
Next, a method for removing only bubbles from the solution S using the bubble removing device 80 configured as described above will be described.
In the initial stage of the bubble removing device 80, the first storage tank 3 and the second storage tank 81 are all empty. However, in order to make the following description easy to understand, the second storage tank 81 is supplied with water W and methane M as shown in FIG. 5, and the first storage tank 3 contains the solution S. It will be described as being in a state.

First, the process of preparing the solution S by stirring the water W and the methane M will be described.
In this case, as shown in FIG. 6, the motor 12 a of the drive unit 12 is driven to rotate the stirrer 11. Thereby, the water W and methane M in the 2nd storage tank 81 can be stirred and gas-liquid mixed, and the high voltage | pressure solution S which the methane M melt | dissolved in the water W can be produced. It should be noted that bubbles are contained in the solution S by stirring.

Further, the liquid feed pump 85 is driven by rotating the internal motor of the liquid feed pump 85 in the forward direction simultaneously with the stirring. Thereby, the liquid feed pump 85 discharges the solution S from the second storage tank 81 through the outlet 84 and the connection line 41 and supplies the solution S into the first storage tank 3 through the inlet 40. As a result, the inside of the first storage tank 3 is filled with the solution S, and then the solution S is discharged from the first storage tank 3 through the discharge line 4. Then, the solution S discharged from the first storage tank 3 is returned to the second storage tank 81 while being transmitted through the inner wall surface 81 b of the second storage tank 81, and is stirred again by the stirrer 11.
Thus, since the stirring operation can be performed while circulating the solution S, gas-liquid mixing can be performed more appropriately, and the solution S in which the methane M is sufficiently dissolved in the water W can be produced.

  During the agitation, the solution S rises in the first storage tank 3 and circulates along the inner wall surface 81 b of the second storage tank 81, so that the first gas is generated in the first storage tank 3. Liquid separation is performed, and second gas-liquid separation is performed in the second storage tank 81. However, since stirring with the stirrer 11 is performed, bubbles are included in the solution S, and bubbles are not substantially removed from the solution S at this stage.

Next, a step of removing bubbles from the solution S is performed.
As shown in FIG. 7, after the above-described stirring is sufficiently performed to prepare the solution S, the motor 12a of the drive unit 12 is stopped. Thereby, rotation of the stirring bar 11 can be stopped and stirring can be stopped. The liquid feed pump 85 is continuously driven.

  Thereby, the liquid feed pump 85 discharges the solution S from the second storage tank 81 through the outlet 84 and the connection line 41 and continuously supplies the solution S into the first storage tank 3 through the inlet 40. be able to. Then, the solution S that has flowed into the first storage tank 3 rises upward from the inflow port 40, so that bubbles contained in the solution S are lifted by buoyancy due to a density difference from the solution S in the rising process. Rise faster than S. Thereby, bubbles can be separated from the solution S (first gas-liquid separation).

  In the present embodiment, since the inside of the first storage tank 3 is filled with the solution S, the air bubbles separated from the solution S in the first storage tank 3 pass through the discharge line 4 in the space portion of the second storage tank 81. R3 is quickly reached and released into the space R3. Thereby, the air bubbles separated by the first gas-liquid separation can be discharged and removed into the space R3 of the second storage tank 81.

  Then, the solution S that has risen in the first storage tank 3 is discharged from the first storage tank 3 through the discharge line 4, and then quietly enters the second storage tank 81 while being transmitted along the inner wall surface 81 b of the second storage tank 81. To be supplied. Thus, in this process, even if bubbles remain in the solution S without being removed by the first gas-liquid separation, the bubbles are further separated from the solution S and released into the space R3. can do. Fine bubbles can be finally removed by the second gas-liquid separation (second gas-liquid separation). Then, the solution S from which bubbles are removed can be stored in the second storage tank 81.

Therefore, even in the bubble removing device 80 of the present embodiment, without affecting the methane M component dissolved in the solution S, only bubbles are efficiently removed from the solution S while maintaining the methane solubility. can do.
In particular, in the present embodiment, the second storage tank 81 can be used as a stirring tank first, and can also be used as a tank for storing the solution S from which bubbles have been removed, so there is no need to prepare a separate stirring tank. Therefore, the configuration can be simplified. Further, it is not necessary to secure an extra space for installing the stirring tank.

Furthermore, in the case of this embodiment, since the solution S can be circulated by the liquid feed pump 85, the first gas-liquid separation and the second gas-liquid separation described above can be repeatedly performed. Therefore, it is possible to sufficiently remove bubbles from the solution S.
At this time, as shown in FIG. 7, the switching valve 92 is closed as necessary, and the solution S discharged from the first storage tank 3 can be flowed to the solubility measuring device 60, so that the methane solubility can be measured quickly. For example, the first gas-liquid separation and the second gas-liquid separation can be repeatedly performed while appropriately confirming the measurement result. Therefore, the operation of removing bubbles from the solution S can be performed more reliably.

  In addition, after removing bubbles from the solution S, the solution S in the second storage tank 81 can be extracted through the outlet 84, the connection line 41, and the outlet line 43 by opening the first outlet valve 44. Therefore, as in the first embodiment, the solution S from which bubbles are removed and the methane solubility is stably maintained can be taken out while maintaining the quality, and can be used for various applications.

  By the way, in the case of this embodiment, it is possible to perform a vapor phase composition analysis. Specifically, the composition of methane M remaining in the space R3 of the second storage tank 81 can be analyzed after the bubble removal operation. This makes it possible to compare the composition of the initial stage methane M supplied to the space R3 of the second storage tank 81 when performing the stirring operation, and to accurately grasp the state of composition change from the comparison result.

  In this case, as shown in FIG. 8, after the removal of bubbles from the solution S is completed, the internal motor of the liquid feeding pump 85 is rotated in the reverse direction so that the solution S in the first storage tank 3 flows into the inlet 40. The second storage tank 81 is supplied through the connection line 41 and the outlet 84. As a result, the liquid level of the solution S in the first storage tank 3 can be lowered and the liquid level of the solution S in the second storage tank 81 can be raised, so that the inside of the space R3 of the second storage tank 81 The methane M remaining in the gas can be pushed out from the second storage tank 81 and can flow to the solubility measuring device 60 side through the discharge line 4 and the return line 91. As a result, composition analysis of methane M can be performed using the solubility measuring device 60 on the same principle as that of the solution S.

  The technical scope of the present invention is not limited to the above embodiment, and various modifications can be made without departing from the spirit of the present invention.

For example, in the first and second embodiments, the stirrer 2 and the solubility measuring device 60 are provided. However, these are not essential and may not be provided.
For example, a solution in which a gas is dissolved in a solvent may be collected from the formation or the seabed, and the collected solution may be flowed into the first storage tank 3 through the inflow port 40. In this case, the internal pressures of the first storage tank 3, the second storage tank 5, and the discharge line 4 may be adjusted by the pressure adjustment unit 6 so as to match the pressure environment from which the solution is collected.

  In the case where the stirrer 2 is provided, the magnetic mixer type stirrer has been described as an example in each of the above embodiments, but the present invention is not limited to this method. In any case, it is sufficient if the solvent and the gas can be gas-liquid mixed by stirring.

Further, in each of the above embodiments, the solution S is supplied to the second storage tank 5 while being transmitted along the inner wall surface 5b of the second storage tank 5, but instead of using the inner wall surface 5b of the second storage tank 5, A dedicated guide member may be arranged in the second storage tank 5, and the solution S may be supplied into the second storage tank 5 along the guide member.
For example, you may arrange | position in the 2nd storage tank 5 by using a rod-shaped member and a plate-shaped member as a guide member. Even in this case, the same effect can be achieved.

However, by using the inner wall surface 5b of the second storage tank 5 as a guide member, it is not necessary to prepare a separate guide member, so that the number of parts can be reduced and the configuration can be simplified. . The internal electrode 51 disposed in the second storage tank 5 may be used as a guide member, and the solution S may be supplied into the second storage tank 5 while being transmitted through the internal electrode 51.
When the inner wall surface 5b of the second storage tank 5 is used as a guide member, the second storage tank 5 is installed in an inclined state so that the inner wall surface 5b is not a vertical wall surface but an inclined wall surface. May be. In this case, when the solution S is supplied into the second storage tank 5, the inner wall surface 5 b can be more reliably transmitted, so that dripping of the solution S can be effectively prevented.

  In the first and second embodiments, a pump is further provided in the connection line 41 that connects the stirring tank 10 and the first storage tank 3, and the solution S in the stirring tank 10 is first stored through the inlet 40. It may be supplied into the tank 3. In this case, since the inflow of the solution S into the first storage tank 3 can be assisted, the solution S can be supplied into the first storage tank 3 more stably.

Furthermore, in the said 1st Embodiment, although the discharge line 4 was arrange | positioned in the height equivalent to the liquid level of the solution S, it is not limited to this case, The 1st storage tank 3 is below the liquid level. It may be connected.
In this case, the volume of the solution S stored in the first storage tank 3 and the distance between the inlet 40 and the liquid surface are taken into consideration, and bubbles are generated in the process of the solution S rising from the inlet 40. The position of the discharge line 4 may be determined in consideration of not inhibiting the action of separating from S.

Next, the high-pressure solution S stored in the second storage tank 5 is removed using an experimental apparatus configured in the same manner as the bubble removal apparatus 1 of the first embodiment and configured in a small scale. An embodiment in which the solubility of methane was actually measured by the solubility measuring device 60 will be described.
In the present embodiment, the solution S that has passed through the solubility measuring device 60 is caused to flow again into the stirring tank 10 via the third outflow valve 47 and the liquid feed pump 23. The measurement was performed under the following conditions.

The flow rate of the liquid feed pump 23 was set to 1 cc / min, and water W was continuously supplied to the stirring tank 10. 1 μL of the solution S was introduced into the slot 72 of the solubility measuring device 60, and methane solubility was measured.
The temperature condition was maintained at 45 ° C. On the other hand, as pressure conditions, the internal pressures of the stirring container, the first storage tank 3, the second storage tank 5 and the discharge line 4 are set to 23.0 (atm), 89.0 (atm) and 136.9 (atm). Measurements were made with three different patterns. The result obtained under the pressure condition of 23.0 (atm) is referred to as Example A, and the result obtained under the pressure condition of 89.0 (atm) as Example B. The measurement was performed under the pressure condition of 136.9 (atm). The result is referred to as Example C.
In the three patterns described above, methane solubility was measured multiple times with a 60 minute time interval. The results are shown in Table 1 and FIG.

Further, in order to compare the measurement results, the bubbles of the solution S are removed using a conventional standing method, and the methane solubility of the solution S after standing after the bubbles are removed is measured. A comparison was made. In the standing method, 2 hours were spent for stirring, and 2 hours to overnight were spent standing.
Moreover, the temperature conditions in the case of performing the stationary method were the same, and the measurement was performed under pressure conditions of 23.0 (atm), 89.0 (atm), and 136.9 (atm), respectively. The comparison results are shown in Table 1.

As a result of the measurement, as is clear from FIG. 9, in any case of Examples A to C, a stable methane solubility value could be obtained in a plurality of measurements. When bubbles were mixed in the solution S, the measured value of the methane solubility rapidly increased and a characteristic showing an abnormal peak appeared, but such a phenomenon did not appear. In addition, as shown in Table 1, the variation coefficient of the measurement result over a plurality of times in Example A is 0.8%, and the variation coefficient of the measurement result over a plurality of times in Example B is 3.0%. In Example C, the coefficient of variation of the measurement results over a plurality of times was 3.4%, all of which were low and good.
From these results, it was actually confirmed that the solution S from which bubbles were reliably removed could be stably stored in the second storage tank 5.

  In addition, the average value of the methane solubility in Example A is 0.52 (cc / g), the average value of the methane solubility in Example B is 1.61 (cc / g), and the methane solubility in Example C The average value of was 2.20 (cc / g).

Furthermore, as a result of comparing the average value of the methane solubility in Examples A to C with the methane solubility measured by the conventional stationary method, the error from the methane solubility measured by the stationary method is (−) 8. It was 5% to (+) 0.9%, and good results were obtained.
That is, according to the present invention, it was actually confirmed that methane solubility comparable to that of the conventional stationary method can be maintained.

From the above, according to the present invention, bubbles are generated from the solution S without affecting the methane component dissolved in the solution S, while maintaining the methane solubility at the same level as the conventional stationary method. We were able to confirm that it was possible to remove only with certainty.
In addition, according to the present invention, it is possible to perform the work of removing bubbles more efficiently than the conventional stationary method, and to achieve an excellent effect of being able to continuously obtain a solution S having a stable methane solubility. it can.

  According to the present invention, it is possible to efficiently remove only the bubbles from the solution while maintaining the gas solubility without affecting the gas component dissolved in the solution. Therefore, it has industrial applicability.

For example, the present invention can be used for the following applications, and therefore, industrial applicability is great.
(1) As a countermeasure for optimizing manufacturing conditions in the manufacturing process, removal of unnecessary volatile substance bubbles in the raw material or intermediate product liquid containing volatile substances supplied to a reaction tank or the like.
(2) Removal of bubbles in the paint containing volatile substances in the coating process using a coating apparatus such as a flow coater.
(3) Carbon dioxide capture & storage (CCS) in the aquifer and recovery of dissolved methane gas by injecting carbon dioxide into water-soluble natural gas fields where methane gas is dissolved in water Removal of bubbles mixed by gas-liquid agitation in a solubility measurement device that acquires basic data on the solubility of methane gas in high pressure carbon dioxide and water under high pressure, such as research.

M ... Methane (gas)
W ... Water (solvent)
S ... Solution R2 ... Spaces 1, 70, 80 in the first housing part ... Bubble removing device 2 ... Stirrer (stirring part)
3 ... 1st accommodation tank (1st accommodation part)
4 ... Discharge line (discharge path)
5, 81 ... 2nd accommodation tank (2nd accommodation part)
5b ... Inner wall surface of the second storage tank (inner wall surface of the second storage part)
6 ... Pressure adjusting part 10 ... Stirring tank (stirring container)
11 ... Stirrer 23 ... Liquid feed pump (supply unit)
40 ... Inlet 42, 84 ... Outlet 60 ... Solubility measuring device (measurement unit)
73 ... Second connection pipe (discharge path)
82 ... Stirrer 85 ... Liquid feed pump (liquid feed part)

Claims (9)

An inflow port through which a solution in which a gas is dissolved in a solvent flows is formed, and a first storage unit that stores the solution therein;
A discharge path that is disposed above the inlet and discharges the solution that has flowed upward from the inlet from the first container;
A second storage part in which the solution discharged through the discharge path is stored inside, and an outflow port for discharging the stored solution is formed;
A pressure adjustment unit that adjusts the internal pressure of the first storage unit and the second storage unit that communicate with each other through the discharge path to the same pressure, and a pressure adjustment unit;
The first container causes the solution to perform first gas-liquid separation until the solution is raised from the inlet to the discharge path,
The discharge path supplies the solution discharged from the first storage portion into the second storage portion while being guided through a guide member disposed in the second storage portion, and the second gas-liquid is supplied to the solution during that time. A bubble removing apparatus characterized by causing separation. The bubble removing apparatus according to claim 1,
The guide member is an inner wall surface of the second housing portion,
The bubble removing device, wherein the discharge path supplies the solution discharged from the first container into the second container while being transmitted along an inner wall surface of the second container. In the bubble removal apparatus according to claim 1 or 2,
A bubble removing device characterized in that a space is secured in a portion located above the discharge path in the first accommodating portion. In the bubble removal apparatus of any one of Claim 1 to 3,
A bubble removing device comprising a supply unit that continuously supplies the solution into the first storage unit through the inlet. In the bubble removal apparatus according to any one of claims 1 to 4,
A stirrer having a stirrer connected to the first container through the inlet and a stirrer for stirring the solvent and the gas in the stirrer to produce the solution;
The bubble removing apparatus, wherein the pressure adjusting unit adjusts internal pressures of the first storage unit and the second storage unit so as to be equal to an internal pressure of the stirring container. In the bubble removal apparatus according to claim 1 or 2,
The second container is provided with a stirrer having a stirrer that stirs the solvent and the gas in the second container to produce the solution,
Between the first storage part and the second storage part, a solution that supplies the stirred solution that has flowed out of the second storage part through the outlet and into the first storage part through the inlet. Part is provided,
The bubble removing device, wherein the stirring bar stops stirring after the solution is produced. The bubble removing apparatus according to claim 6, wherein
The liquid supply unit supplies the solution after the second gas-liquid separation into the first storage unit through the inflow port. The bubble removing apparatus according to any one of claims 1 to 7,
A bubble removing apparatus comprising a measuring unit that measures gas solubility of a gas component contained in the solution after the second gas-liquid separation. Supplying the solution into the first container so that a solution in which a gas is dissolved in the solvent rises in the first container;
Allowing the solution to undergo a first gas-liquid separation while the solution rises in the first container;
Discharging the solution that has risen in the first container from the first container through a discharge path and supplying the solution into the second container;
Adjusting the internal pressure of the first storage portion and the second storage portion communicating with each other through the discharge path to the same pressure, and adjusting to an arbitrary pressure,
After performing the step of adjusting the internal pressure of the first storage unit and the second storage unit, the step of supplying the solution into the first storage unit, the step of performing the first gas-liquid separation, and the solution Performing a process of supplying the second container;
When the solution is supplied into the second storage portion, the solution is supplied into the second storage portion while being guided by a guide member disposed in the second storage portion, and the second gas is supplied to the solution during that time. A method for removing bubbles, wherein liquid separation is performed.

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