Method for distilling or extracting liquid mixture or mixture containing the same, and microwave extraction device using the same

Abstract

To provide a method for distilling or extracting a liquid mixture or a mixture containing the same (hereinafter referred to as raw material), of recovering a to -be-recovered component (hereinafter referred to as target component) that is contained in the raw material and to be recovered as a distillate by distillation or extraction by an operator, in which the target component is recovered by distilling or extracting under reduced pressure at a preset distillation temperature, regardless of whether or not the concentration of the target component is known, and regardless of the concentration of the target component in the raw material which constantly changes over time during the distillation (extraction) process.SOLUTION: A method for distilling or extracting a raw material comprises: detecting boiling of the raw material while reducing pressure, and calculating a concentration of a target component in the raw material from the detected pressure and temperature at a time of boiling using a vapor-liquid equilibrium curve for the target component; and newly detecting the boiling while reducing the pressure to continue to newly calculate the concentration of the target component in the raw material, so as to cope with a concentration of a target component changing constantly over time in the raw material during the distillation (extraction) process.SELECTED DRAWING: Figure 2-1

Description

[Technical Field]

[0001] The present invention relates to a method for distilling or extracting a liquid mixture or a mixture containing the same (hereinafter referred to as "raw material"), and more particularly to a method for distilling or extracting a raw material in which a target component (hereinafter referred to as "target component") contained in the raw material and recovered as a distillate by distillation or extraction by an operator is recovered by distillation or extraction under reduced pressure at a target distillation temperature, regardless of whether the concentration of the target component is known or not, and regardless of the concentration of the target component in the raw material, which constantly changes over time during the distillation (extraction) process. [Background technology]

[0002] Conventionally, a vacuum distillation method or a vacuum extraction method has been known. For example, Patent Document 1 proposes a vacuum distillation apparatus that makes it possible to efficiently regenerate a liquid to be treated, such as a non-aqueous solvent containing various contaminants. Patent Document 2 proposes an extraction device and extraction method that involves a decompression step in order to efficiently extract a target component. Patent Document 3 proposes an extraction device that uses microwaves to extract and recover useful components such as essential oils contained in a processing object such as biomass by irradiating the processing object with microwaves and heating it. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] JP-A-7-136402 (Patent No. 3394815) [Patent Document 2] Japanese Patent Application Laid-Open No. 2011-016061 [Patent Document 3] JP 2012-030167 A (Patent No. 4849578) Summary of the Invention [Problem to be solved by the invention]

[0004] However, during the distillation (extraction) process, the concentration of the target component in the raw material constantly changes over time, and the boiling point of the target component also constantly changes in conjunction with this concentration change, presenting a technical challenge in that it is difficult to control the distillation (extraction) at a constant temperature. Furthermore, when distilling or extracting target components under reduced pressure, the state of the raw material may not be clearly understood by the operator prior to distillation or extraction. As a result, operators cannot easily predict the conditions under which distillation or extraction will begin (the raw material's reduced pressure, determined from the concentration of the target component in the raw material and the operator's desired distillation temperature), and it takes time to understand these conditions. For example, when distilling a raw material containing alcohol (ethanol) at the desired distillation temperature and recovering alcohol (ethanol) as the distillate, the reduced pressure value can be determined by measuring the alcohol (ethanol) concentration in the raw material. This requires a process of measuring the concentration using a spirit hydrometer or other device, and then determining the reduced pressure value based on the measured concentration and the desired distillation temperature. Determining the reduced pressure value without measuring the alcohol (ethanol) concentration in the raw material requires a process of determining the boiling point of the raw material by reducing the pressure until the raw material boils. Furthermore, this reduced pressure must be applied gradually to prevent the raw material from bumping. If bumping occurs, an excessive amount of the target component will be distilled, exceeding the capacity of the cooling trap (cold trap), and the distilled target component will disperse directly into the atmosphere, making it impossible to properly recover the target component as a distillate, or the excess target component may flow back into the vacuum pump, causing the vacuum pump to break down, so it must be prevented.Since these steps must be performed to understand the above conditions, it takes time for the raw material in the distillation process to first boil, which creates the problem of longer total operating time required for the distillation (extraction) process. Furthermore, in the distillation (extraction) process, which is carried out at a constant temperature, the concentration of the target component in the raw material constantly changes over time, and the boiling point of the target component constantly changes along with this concentration change. Therefore, it is desirable to change the pressure (reduce the pressure) whenever the concentration in the raw material changes, but it is not easy for the operator to predict the concentration changes that occur from moment to moment, and therefore it is difficult for the operator to determine how much pressure should be reduced. Excessive pressure reduction causes the above-mentioned bumping of the raw material, and conversely, insufficient pressure reduction prevents distillation (extraction) from occurring.

[0005] In view of the above circumstances, the present invention aims to provide a method for distilling or extracting a raw material, which recovers a target component contained in the raw material by distilling or extracting under reduced pressure at a set distillation temperature, regardless of whether the concentration of the target component is known or not, and regardless of the concentration of the target component in the raw material, which constantly changes over time during the distillation (extraction) process. [Means for solving the problem]

[0006] The invention of claim 1 relates to a vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component, wherein the raw material has a lower saturated vapor pressure (i.e., a higher boiling point) as the concentration (or content) of the target component decreases, and the concentration (or content) of the target component in the raw material decreases as the target component is separated from the raw material by distillation. The vacuum distillation method includes, in an airtight tank that can be depressurized, (A) a step of heating the raw material to and maintaining the target distillation temperature, (B) a step of gradually reducing the pressure in the tank if the raw material is not boiling, and (C) a step of maintaining the pressure in the tank if the raw material is boiling, and relates to a vacuum distillation method for boiling the raw material at the target distillation temperature and distilling at a constant temperature while capturing the saturated vapor pressure of the raw material, which changes over time due to distillation.

[0007] The invention according to claim 2 relates to the reduced pressure distillation method according to claim 1, which utilizes the phenomenon that, in the steps (B) and (C), the steam temperature is compared with the raw material temperature in an environment where the ambient temperature is lower than the target distillation temperature, and when boiling occurs, the steam temperature and the raw material temperature become equal, and when boiling ceases, the steam temperature becomes lower than the raw material temperature.

[0008] The invention of claim 3 relates to the reduced-pressure distillation method of claim 1, wherein, for the decompression in step (B), first, a vapor-liquid equilibrium surface, which is determined by temperature, concentration, and pressure, is utilized and which represents a mixture of a target component and a solvent component mixed with the target component, is rapidly reduced in pressure while heating to and maintaining the target distillation temperature in accordance with the conditions of (a) or (b), (a) when the concentration (or content) of the target component in the raw material is unknown, the target distillation temperature and the saturated vapor pressure are increased to the saturated vapor pressure determined on the vapor-liquid equilibrium surface from the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximized, or (b) when the concentration (or content) of the target component in the raw material is known, the target distillation temperature and the saturated vapor pressure are increased to the saturated vapor pressure determined on the vapor-liquid equilibrium surface from the target distillation temperature and the concentration of the target component.

[0009] The invention according to claim 4 is characterized in that the pressure reduction in the step (B) is performed at a rate utilizing the value of the gradient of the saturated vapor pressure versus the concentration of the target component on a vapor-liquid equilibrium curved surface representing a mixed system of the target component and a solvent component mixed with the target component, which is determined by the raw material temperature and the pressure inside the tank, and the value of the gradient of the saturated vapor pressure versus the concentration of the target component is

[0010]

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[0011] The invention according to claim 5 relates to the method for reducing the pressure in the step (B), which first utilizes a vapor-liquid equilibrium surface that represents a mixture of a target component and a solvent component that is mixed with the target component, and is determined by temperature, concentration, and pressure; (a) if the concentration (or content) of the target component in the raw material is unknown, the pressure is reduced to the saturated vapor pressure determined on the vapor-liquid equilibrium surface from the target distillation temperature and the concentration of the target component that maximizes the saturated vapor pressure; (b) if the concentration (or content) of the target component in the raw material is known, the pressure is reduced quickly while heating to the target distillation temperature and maintaining the temperature in accordance with the conditions of (a) or (b); and then, for the second and subsequent pressure reductions, the pressure is reduced at a rate that utilizes the value of the slope of the saturated vapor pressure versus the concentration of the target component on the vapor-liquid equilibrium surface that is determined by the raw material temperature and the pressure inside the tank; and the value of the slope of the saturated vapor pressure versus the concentration of the target component is

[0012]

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[0013] The invention according to claim 6 is a reduced-pressure distillation method in which the pressure is reduced in the step (B) in an environment where the ambient temperature is lower than the target distillation temperature, in order to perform distillation at a more stable temperature, when all of the following conditions (1) to (3) described in Condition 1 are met, wherein: (1) the distillation is not boiling, or

[0014]

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[0015]

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[0016]

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[0017] The invention of claim 7 relates to the reduced pressure distillation method of claim 1, which includes a step of determining the liquid phase molar fraction and the vapor phase molar fraction of the target component in the tank from the raw material temperature and the pressure inside the tank during boiling in the distillation, using a vapor-liquid equilibrium surface represented by a mixed system of the target component and a solvent component mixed with the target component.

[0018] The invention of claim 8 relates to the reduced pressure distillation method of claim 7, which further comprises a step of estimating the mass concentration of the target component in the raw material and / or distillate from the liquid phase molar fraction and / or gas phase molar fraction of the target component and the mass of the raw material and / or distillate, when the mass of the raw material and / or distillate can be measured.

[0019] The invention of claim 9 relates to the reduced pressure distillation method of claim 1, further comprising a step of, when the target distillation temperature is changed during the distillation, quickly changing the pressure in the tank to the saturated vapor pressure calculated from the gas-liquid equilibrium surface represented by a mixture system of the target component and the solvent component mixed with the target component, based on the concentration of the target component calculated before the change and the target distillation temperature after the change, and continuing the distillation.

[0020] The invention of claim 10 relates to the reduced pressure distillation method of claim 1, further comprising a step of detecting, in the case of a raw material containing a target component and a solvent component to be mixed with the target component, a state in which the concentration of the target component calculated by a gas-liquid equilibrium surface representing a mixed system of the target component and the solvent component to be mixed with the target component becomes 0, or a state in which the target internal tank pressure calculated by the gas-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone, during the distillation, and stopping the distillation when the concentration of the target component becomes 0 or when the target internal tank pressure becomes equal to the saturated vapor pressure of the solvent component alone.

[0021] The invention of claim 11 relates to the reduced pressure distillation method of claim 1, wherein the heating is performed by microwave irradiation, and microwave irradiation is stopped, microwave oscillation is started, switching to pulse irradiation, switching to continuous irradiation, microwave output is decreased, or microwave output is increased depending on the difference between the raw material temperature and the target distillation temperature.

[0022] The invention according to claim 12 relates to the reduced pressure distillation method according to claim 1, wherein the raw material contains alcohol and the target component is alcohol.

[0023] The invention according to claim 13 relates to the vacuum distillation method according to claim 1, wherein the raw material contains ethanol and the target component is ethanol.

[0024] The invention of claim 14 relates to a microwave extraction apparatus used in the reduced pressure distillation method of claim 1, the extraction apparatus comprising: a tank for accommodating raw materials; a microwave generator for generating microwaves; a wave-guiding means and a microwave transmission means for guiding the microwaves to the tank; a stirring device for stirring the raw materials accommodated in the tank; a vacuum pump for adjusting the pressure in the tank; an atmospheric release valve for adjusting the pressure in the tank; a cooling condenser or cooling device for cooling and condensing the vapor of the raw materials evaporated from the tank by heating; a recovery device for recovering the components condensed by the cooling condenser; a control device for controlling the operations of pressure, cooling, and microwave irradiation; and sensors for measuring the pressure, raw material temperature, and vapor temperature in the tank.

[0025] The invention of claim 15 relates to the microwave extraction device of claim 14, which has the function of calculating the liquid phase molar fraction and gas phase molar fraction of the target component in the tank from the raw material temperature and the pressure inside the tank during boiling in the distillation, using a gas-liquid equilibrium curved surface representing a mixed system of the target component and a solvent component mixed with the target component, and if a scale capable of measuring the mass of the raw material and / or distillate is available, has the function of estimating the mass concentration of the target component in the raw material and / or distillate from the liquid phase molar fraction and / or gas phase molar fraction of the target component and the mass of the raw material and / or distillate.

[0026] The invention of claim 16 relates to the microwave extraction apparatus of claim 14, which has a function of quickly changing the pressure in the tank to the saturated vapor pressure calculated from the gas-liquid equilibrium surface represented by a mixture of the target component and the solvent component mixed with the target component, based on the concentration of the target component calculated before the change and the target distillation temperature after the change, when the target distillation temperature is changed during the distillation, and continuing the distillation.

[0027] The invention of claim 17 relates to the microwave extraction device of claim 14, which, in the case of a raw material containing a target component and a solvent component to be mixed with the target component, is capable of detecting, during the distillation, a state in which the concentration of the target component calculated by a gas-liquid equilibrium surface representing a mixed system of the target component and the solvent component to be mixed with the target component becomes zero, or a state in which the target internal tank pressure calculated by the gas-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone, and has a function of stopping the distillation when the concentration of the target component becomes zero or when the target internal tank pressure becomes equal to the saturated vapor pressure of the solvent component alone.

[0028] The invention of claim 18 relates to the microwave extraction device of claim 14, wherein the heating is performed by microwave irradiation, and microwave irradiation is stopped, microwave oscillation is started, switching to pulse irradiation, switching to continuous irradiation, microwave output is decreased, or microwave output is increased depending on the difference between the raw material temperature and the target distillation temperature.

[0029] The invention according to claim 19 relates to the microwave extraction device according to claim 14, wherein the raw material contains alcohol and the target component is alcohol.

[0030] The invention according to claim 20 relates to the microwave extraction device according to claim 14, wherein the raw material contains ethanol and the target component is ethanol. [Effects of the Invention]

[0031] According to the invention of claim 1, there is provided a vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component, in which the raw material has a lower saturated vapor pressure (higher boiling point) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, thereby decreasing the concentration (or content) of the target component in the raw material, and the vacuum distillation method includes the steps of: (A) heating the raw material to a target distillation temperature and maintaining the temperature; (B) gradually reducing the pressure in the tank if the raw material has not boiled; and (C) gradually reducing the pressure in the tank if the raw material has boiled. The method is characterized by being a reduced-pressure distillation method in which the raw material is boiled at a target distillation temperature while capturing the saturated vapor pressure of the raw material, which changes over time due to distillation, and the pressure in the tank is maintained, and distillation is performed at a constant temperature.Therefore, it is possible to provide a method for distilling or extracting a raw material containing a desired target component concentration or content at a desired temperature (desired distillation temperature), in which the target component contained in the raw material is recovered by distillation or extraction under reduced pressure at a set distillation temperature, regardless of the target component concentration (or content) in the raw material, which constantly changes over time during the distillation (extraction) process.

[0032] According to the invention of claim 2, the vacuum distillation method of claim 1 utilizes the phenomenon that, in the steps (B) and (C), the steam temperature and the raw material temperature are compared in an environment where the ambient temperature is lower than the target distillation temperature, and if boiling occurs, the steam temperature and the raw material temperature become equal, and if boiling ceases, the steam temperature becomes lower than the raw material temperature. Therefore, it is possible to provide a method for distilling or extracting a raw material containing a desired concentration or content of a target component at a desired temperature (desired distillation temperature) by automatically detecting boiling of the raw material by comparing the steam temperature and the raw material temperature in an environment where the ambient temperature is lower than the target distillation temperature, and automatically controlling the pressure applied to the raw material depending on whether boiling occurs.

[0033] According to the invention of claim 3, the pressure reduction in step (B) is first achieved by utilizing a vapor-liquid equilibrium surface, which represents a mixture of the target component and the solvent component mixed with the target component, and which is determined by temperature, concentration, and pressure. (a) If the concentration (or content) of the target component in the raw material is unknown, the pressure is reduced to the saturated vapor pressure determined by the vapor-liquid equilibrium surface from the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximized, or (b) If the concentration (or content) of the target component in the raw material is known, the pressure is reduced to the saturated vapor pressure determined by the vapor-liquid equilibrium surface from the target distillation temperature and the concentration of the target component, according to the conditions of (a) or (b). Therefore, regardless of whether the concentration (or content) of the target component is known or unknown, by first reducing the pressure in one go to the saturated vapor pressure that can be read from the vapor-liquid equilibrium surface for the target component, the time required to detect the first boiling of the raw material can be shortened, and the total operating time required for the method of distilling or extracting a raw material of the present invention can be shortened.

[0034] According to the invention of claim 4, the pressure reduction in the step (B) is performed at a rate utilizing the value of the gradient of the saturated vapor pressure versus the concentration of the target component on a vapor-liquid equilibrium curved surface representing a mixed system of the target component and a solvent component mixed with the target component, which is determined by the raw material temperature and the pressure inside the tank, and the value of the gradient of the saturated vapor pressure versus the concentration of the target component is

[0035]

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[0036] According to the invention of claim 5, in the depressurization in the step (B), first, a vapor-liquid equilibrium surface representing a mixture of a target component and a solvent component mixed with the target component, which is determined by temperature, concentration, and pressure, is utilized, and (a) when the concentration (or content) of the target component in the raw material is unknown, the pressure is reduced to the saturated vapor pressure determined on the vapor-liquid equilibrium surface from the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximized, or (b) when the concentration (or content) of the target component in the raw material is known, the pressure is reduced quickly while heating to the target distillation temperature and maintaining the temperature in accordance with the conditions of (a) or (b), and then, for the second and subsequent depressurizations, the pressure is reduced at a rate utilizing the value of the slope of the saturated vapor pressure versus the concentration of the target component on the vapor-liquid equilibrium surface, which is determined by the raw material temperature and the pressure inside the tank, and the value of the slope of the saturated vapor pressure versus the concentration of the target component is

[0037]

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[0038] According to the invention of claim 6, in order to perform the distillation at a more stable temperature, the pressure reduction in the step (B) is performed in an environment where the ambient temperature is lower than the target distillation temperature, when all of the following conditions (1) to (3) described in Condition 1 are met, and the pressure reduction is performed in the step (B) at a more stable temperature, and the following conditions (1) to (3) are met:

[0039]

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[0040]

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[0041]

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[0042] According to the invention of claim 7, the reduced pressure distillation method of claim 1 includes a step of determining the liquid phase molar fraction and the gas phase molar fraction of the target component in the tank from the raw material temperature and the pressure inside the tank during boiling in the distillation, using a gas-liquid equilibrium surface represented by a mixed system of the target component and the solvent component mixed with the target component. Therefore, the constantly changing liquid phase molar fraction and the gas phase molar fraction of the target component in the raw material after the raw material boils can be calculated and the user can grasp them in real time.

[0043] According to the invention of claim 8, the reduced pressure distillation method of claim 7 further includes a step of estimating the mass concentration of the target component in the raw material and / or distillate from the liquid phase molar fraction and / or gas phase molar fraction of the target component and the mass of the raw material and / or distillate when the mass of the raw material and / or distillate can be measured.Therefore, in the process of producing a distillate, the user can grasp in real time whether the obtained distillate and the raw material (remaining material) after the distillate has been removed have the desired quality (for example, whether they have the desired mass concentration), and it becomes easier to predict the end time of the distillation and the remaining amount of distillate to be recovered from the estimated calculation of the target component remaining in the raw material.

[0044] According to claim 9, when the target distillation temperature is changed during the distillation, the vacuum distillation method of claim 1 further includes a step of rapidly changing the pressure in the tank to the saturated vapor pressure calculated from the vapor-liquid equilibrium surface, which represents the mixture of the target component and the solvent component mixed with the target component, based on the target distillation temperature and the concentration of the target component calculated before the change, and continuing the distillation.This allows users of the present invention to further distill or extract the raw material at any temperature (target distillation temperature).For example, for the purpose of sterilization, the raw material can be heated at the start of operation (e.g., to 80°C), and then the distillation set temperature can be changed to perform distillation or extraction.For similar sterilization purposes, heating can be performed as the final step in the distillation or extraction process (e.g., heating the raw material to 80°C).

[0045] According to the invention of claim 10, in the case of a raw material containing a target component and a solvent component that is mixed with the target component, a state in which the concentration of the target component calculated by the gas-liquid equilibrium surface representing the mixed system of the target component and the solvent component that is mixed with the target component becomes zero during the distillation, or a state in which the target internal tank pressure calculated by the gas-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone, can be detected, and the reduced pressure distillation method of claim 1 further includes a step of stopping the distillation when the concentration of the target component becomes zero or when the target internal tank pressure becomes equal to the saturated vapor pressure of the solvent component alone.This prevents the process from being continued when the target component is not contained in the raw material, and prevents the concentration of the target component in the distillate from being diluted (for example, due to an increase in the amount of components other than the solvent component or the target component), so the quality of the distillate (the concentration of the target component contained in the distillate) can be maintained at the desired quality (concentration).

[0046] According to the invention of claim 11, the heating is performed by microwave irradiation, and microwave irradiation is stopped, microwave oscillation is started, switching to pulsed irradiation, switching to continuous irradiation, microwave output is reduced, or microwave output is increased depending on the difference between the raw material temperature and the target distillation temperature.This is characterized by being a reduced-pressure distillation method as described in claim 1, and therefore it is possible to provide a method for distilling or extracting raw materials that can maintain the quality (concentration) of the distillate (concentration of the target component contained in the distillate) at a target quality (concentration) by controlling the raw material temperature during reduced pressure by microwave irradiation.

[0047] According to the invention of claim 12, the reduced pressure distillation method of claim 1 is characterized in that the raw material contains alcohol and the target component is alcohol. Therefore, by specifying the target component as alcohol, it is possible to provide a method for removing organic solvents contained in raw materials, or for distilling or extracting raw materials containing alcohol of any concentration at any temperature when producing distilled spirits.

[0048] According to the invention of claim 13, the reduced pressure distillation method of claim 1 is characterized in that the raw material contains ethanol and the target component is ethanol. Therefore, by specifying the target component as ethanol, it is possible to provide a method for distilling or extracting a raw material containing ethanol of any concentration at any temperature when producing distilled spirits.

[0049] According to the invention of claim 14, there is provided a microwave extraction apparatus for use in the reduced pressure distillation method of claim 1, the extraction apparatus comprising: a tank for accommodating raw materials; a microwave generator for generating microwaves; a wave-guiding means and a microwave transmission means for guiding the microwaves to the tank; a stirring device for stirring the raw materials accommodated in the tank; a vacuum pump for adjusting the pressure in the tank; an atmospheric release valve for adjusting the pressure in the tank; a cooling condenser or cooling device for cooling and condensing the vapor of the raw materials evaporated from the tank by heating; a recovery device for recovering the components condensed by the cooling condenser; a control device for controlling the pressure, cooling, and microwave irradiation operations; and sensors for measuring the pressure in the tank, the raw material temperature, and the vapor temperature. Thus, a microwave extraction apparatus for distilling or extracting raw materials containing any target component concentration at any temperature can be provided.

[0050] According to the invention of claim 15, the microwave extraction device of claim 14 has the function of calculating the liquid phase molar fraction and gas phase molar fraction of the target component in the tank from the raw material temperature and the pressure inside the tank during boiling in the distillation using a gas-liquid equilibrium curve representing a mixed system of the target component and the solvent component mixed with the target component, and if a scale capable of measuring the mass of the raw material and / or distillate is available, the microwave extraction device has the function of estimating the mass concentration of the target component in the raw material and / or distillate from the liquid phase molar fraction and / or gas phase molar fraction of the target component and the mass of the raw material and / or distillate.Therefore, the user of the present invention can grasp in real time the liquid phase molar fraction and gas phase molar fraction of the target component in the raw material, which are constantly changing after the raw material boils, whether the resulting distillate and the raw material (residue) after the distillate has been removed have the desired quality (for example, whether they have the desired mass concentration), and the expected end time of the distillation and the expected recovery amount of the remaining distillate based on the estimated content of the target component remaining in the raw material.

[0051] According to claim 16, if the target distillation temperature is changed during the distillation, the microwave extraction apparatus of claim 14 has the function of quickly changing the internal tank pressure to the saturated vapor pressure calculated from the vapor-liquid equilibrium surface, which represents the mixture of the target component and the solvent component mixed with the target component, based on the target distillation temperature and the concentration of the target component calculated before the change, and continuing the distillation.This allows users of the present invention to further distill or extract the raw material at any temperature (target distillation temperature).For example, for the purpose of sterilization, the raw material can be heated at the start of operation (e.g., to 80°C), and then the distillation temperature can be changed to perform distillation or extraction.For similar sterilization purposes, heating can be performed as the final step in the distillation or extraction process (e.g., heating the raw material to 80°C).

[0052] According to the invention of claim 17, in the case of a raw material containing a target component and a solvent component that is mixed with the target component, the microwave extraction apparatus of claim 14 has the function of detecting, during the distillation, a state in which the concentration of the target component calculated by the gas-liquid equilibrium surface representing the mixed system of the target component and the solvent component that is mixed with the target component becomes zero, or a state in which the target internal tank pressure calculated by the gas-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone, and has the function of stopping the distillation when the concentration of the target component becomes zero or when the target internal tank pressure becomes equal to the saturated vapor pressure of the solvent component alone.This means that the microwave extraction apparatus of claim 14 is characterized in that it does not continue the present invention when the target component is not contained in the raw material, and it is possible to prevent the concentration of the target component in the distillate from becoming diluted (for example, due to an increase in the amount of components other than the solvent component or the target component).Therefore, the quality of the distillate (the concentration of the target component contained in the distillate) can be maintained at the desired quality (concentration), and costs can be reduced by not operating the apparatus more than necessary.

[0053] According to the invention of claim 18, the heating is performed by microwave irradiation, and the microwave irradiation is stopped, microwave oscillation is started, switching to pulsed irradiation, switching to continuous irradiation, microwave output is reduced, or microwave output is increased depending on the difference between the raw material temperature and the target distillation temperature. Therefore, it is possible to provide a microwave extraction device that can maintain the quality of the distillate (the concentration of the target component contained in the distillate) at a target quality (concentration) by controlling the raw material temperature during decompression by microwave irradiation.

[0054] According to the invention of claim 19, the raw material contains alcohol, and the microwave extraction device is characterized in that the target component is alcohol, and is the microwave extraction device of claim 14. Therefore, by specifying the target component as alcohol, it is possible to provide a microwave extraction device that can remove organic solvents contained in raw materials or distill or extract raw materials containing alcohol of any concentration at any temperature when producing distilled spirits.

[0055] According to the invention of claim 20, the microwave extraction device of claim 14 is characterized in that the raw material contains ethanol and the target component is ethanol. Therefore, by specifying the target component as ethanol, it is possible to provide a microwave extraction device that can distill or extract raw materials containing ethanol of any concentration at any temperature when producing distilled spirits. [Brief explanation of the drawings]

[0056] [Figure 1] The present invention relates to a vacuum distillation apparatus used in a method for distilling or extracting a raw material. [Figure 2-1] 1 is a control flow chart of a method for distilling or extracting a raw material according to the present invention (1). [Figure 2-2] 2 is a control flow chart of a method for distilling or extracting a raw material according to the present invention (2). [Figure 3] 1 is a graph showing the pressure-temperature-concentration vapor-liquid equilibrium curves for a binary system of ethanol and water according to the present invention. [Figure 4] 1 is a chart showing the results of vacuum distillation of a raw material having an unknown concentration of a target component (ethanol) according to the present invention. [Figure 5] 1 is a chart showing the results of vacuum distillation of a raw material having a known concentration of a target component (ethanol) according to the present invention. [Figure 6] 1 shows the xy curve and vapor-liquid equilibrium curve, as well as the xy surface, at 50°C for the conventional ethanol-water binary system. DETAILED DESCRIPTION OF THE INVENTION

[0057] Hereinafter, embodiments of the method for distilling or extracting a raw material according to the present invention will be described in detail, but the technical scope of the present invention should not be limited by these descriptions.

[0058] As described above, conventional distillation or extraction methods have technical challenges, such as the difficulty of controlling distillation (extraction) at a constant temperature, the potentially lengthy operating time required for the distillation or extraction process, the possibility of bumping of the raw material due to excessive pressure reduction, and the possibility that distillation or extraction of the raw material will not occur due to insufficient pressure reduction.

[0059] Conventional microwave extraction equipment can only produce distilled spirits using raw materials with an alcohol (ethanol) concentration of 35%, and can only perform distillation (extraction) at two distillation temperatures of 40°C and 60°C, which are set based on pre-measured distillation test data (a microwave extraction equipment that can handle 25 kg of raw material and has a total microwave output of 6 kW). This means that if there is variation in the concentration of the target component (in this case, alcohol (ethanol)) contained in the raw material, the change in concentration from the start to the end of the distillation will differ from the test data, and distillation or extraction may not occur because the pressure cannot be reduced sufficiently to boil the raw material. In addition, there is a need for a versatile distillation (extraction) method that can distill or extract any target component targeted by the user of the present invention at any temperature while maintaining the quality of the recovered material or the raw material (residue) after the target component has been removed.

[0060] In order to solve the technical problems, the present invention provides a method for distilling or extracting a raw material, in which a target component contained in the raw material is recovered by distilling or extracting under reduced pressure at a set distillation temperature, regardless of whether the concentration of the target component is known or not, and regardless of the concentration of the target component in the raw material, which constantly changes over time during the distillation (extraction) process. Specifically, the present invention compares the vapor temperature and raw material temperature during distillation in real time, and utilizes the physical phenomenon that if boiling occurs, the vapor temperature is equal to the raw material temperature, and if not boiling, the vapor temperature is lower than the raw material temperature to detect whether or not boiling occurs, and by gradually lowering the pressure when not boiling, it controls the pressure by searching for the boiling point (concentration). In addition, the temperature is controlled by adjusting the heating mechanism so that the raw material temperature is equal to the desired distillation temperature (set distillation temperature). These techniques provide control over alcohol distillation at any concentration and temperature.

[0061] Here, when the raw material is not boiling, the vapor temperature is easily affected by the ambient temperature of the distillation or extraction apparatus of the present invention, and the vapor temperature will be lower than the raw material temperature. Therefore, it should be noted that the present invention cannot be applied when the distillation setting temperature is lower than the ambient temperature (e.g., distillation setting temperature 35°C, ambient temperature 40°C). This is because, in the distillation (extraction) apparatus of the present invention, the vapor temperature sensor is farther from the heat source than the raw material (i.e., the raw material temperature sensor that measures the raw material temperature). The term "ambient temperature" here refers to the ambient temperature when using the distillation or extraction method of the present invention, or the temperature around the apparatus for using such a method. It is sometimes referred to as the room temperature if indoors or the outdoor temperature if outdoors. For example, if the apparatus of the present invention is located indoors, the user can control the temperature (ambient temperature) using air conditioning equipment. Also, when "gradually reducing the pressure" (decompressing gradually), it is important to note that the degree of decompression is not clear and is therefore left to the discretion of the operator. For example, if the decompression process is carried out at a very slow speed, it will be possible to accurately determine the saturated vapor pressure, but it will take time. Conversely, if the pressure is reduced at a fast speed, the pressure may fall below the saturated vapor pressure, which could cause bumping of the raw material. To provide an overview of the xy curve and vapor-liquid equilibrium curve represented by the target component and solvent component, the xy curve and vapor-liquid equilibrium curve for ethanol as the target component and water as the solvent component are shown in Figure 6. The boiling point of an ethanol solution (see Figure 6) decreases as the ethanol concentration increases (however, there is a region where this is reversed at high concentrations of approximately 0.9 mole fraction or higher (approximately 97% or higher in alcohol (ethanol) content)). Furthermore, the boiling point of an ethanol solution is lower than that of water, and its saturated vapor pressure is high.

[0062] The vapor-liquid equilibrium surface is a surface determined by three variables: temperature, pressure, and concentration of the target component (for example, liquid phase molar fraction or mol%, for example, and other embodiments (e.g., embodiments expressing the content of the target component in the raw material) are not particularly limited as long as they can be converted into these embodiments), which can be obtained by arranging the vapor-liquid equilibrium curves (see FIG. 6) of pressure and concentration at a certain temperature for a mixture of a target component (e.g., ethanol) and a solvent component (e.g., water) mixed with the target component, for each temperature. When the concentration is expressed as a liquid phase molar fraction, it can be expressed using the amount of substance (mol) of the first component as the target component and the amount of substance (mol) of the second component as the solvent component. For example, when distilling a raw material whose ethanol concentration (or ethanol content) is unknown, the saturated vapor pressure is highest when the concentration is highest (here, the concentration of the ethanol solution is 90 mol%) under the condition that the boiling point of ethanol is low. Therefore, by determining the distillation setting temperature, it is possible to quickly reduce the pressure to the saturated vapor pressure (the pressure at which boiling never occurs) determined by the vapor-liquid equilibrium curve, and by starting pressure control to search for the boiling point from there, it is possible to shorten the operating time. If the ethanol concentration (or ethanol content) of the raw material is known, the saturated vapor pressure can be determined from the vapor-liquid equilibrium curve once the distillation temperature setting is determined, and the pressure can be reduced to that pressure in one go. Furthermore, after reducing the pressure all at once, the pressure is gradually reduced while searching for the boiling point (concentration). The amount of this reduction can be determined by using the value of the slope of the vapor-liquid equilibrium curve (the differential value of the pressure curve with respect to concentration [ΔkPa / Δconcentration of the target component (expressed, for example, as liquid phase mole fraction, or mol%))]) determined from the current pressure and feed temperature, allowing the pressure to be gradually reduced at an appropriate amount corresponding to the concentration. Here, "Δ" represents the amount of change in physical quantities such as "pressure" and "concentration" of the target component according to the present invention. In the present invention, when using this slope value, it is preferable to use the following formula (rate):

[0063]

number

[0064] Furthermore, while conventional technology has made it difficult to grasp the concentration of a target component contained in the distillate (extract) after vacuum distillation in real time during the distillation (extraction) process, this technology provides a function that calculates the weight deviation [g / sec] of the distillate (extract) from the liquid-vapor phase curve (xy curve) of the target component (see Figure 6), which is determined from the vapor-liquid equilibrium curve by constantly measuring the weight of the distillate (extract) and detecting the boiling of the raw material, and calculates the weight deviation [g / sec] of the target component from the vapor phase molar fraction of the target component, and integrates this over time to calculate the estimated concentration of the distillate (extract) during distillation (for example, the mass concentration of the target component in the distillate (wt% = kg of target component / kg of distillate × 100)). If the target component is ethanol when calculating this mass concentration, the alcohol (ethanol) content of the distillate can also be calculated simultaneously from the calculated mass concentration in wt%. Here, the gas-liquid equilibrium surface used in the present invention is expressed using the gas-liquid equilibrium curve of the raw material at each temperature. Therefore, by using the liquid-gas curve (xy curve) at each temperature obtained from the gas-liquid equilibrium curve at each temperature, a three-dimensional liquid-gas surface (xy curve) (see FIG. 6) can be expressed. Furthermore, if the weight of the liquid mixture (total weight of the target component and solvent component) of the input raw material is known, the weight of the liquid mixture contained in the raw material during distillation (extraction) can be determined by subtracting the weight of the recovered distillate (extract), so a function is provided to calculate the target component concentration of the raw material during distillation (extraction) (for example, the mass concentration of the target component relative to the target component and solvent component in the raw material (wt% = target component kg / target component + solvent component kg × 100)) from the liquid phase molar fraction (or mol%) at the time of boiling detection. When calculating this mass concentration, if the target component is ethanol, the alcohol (ethanol) content of the raw material is also calculated at the same time from the calculated mass concentration in wt%. For example, to monitor the alcohol (ethanol) concentration (concentration of the target component) of a distilled spirit (distillate) being distilled under reduced pressure in real time during the distillation (extraction) process, the weight of the spirit (distillate) is constantly measured, and the boiling of the raw material is detected to obtain a liquid-vapor phase curve (xy curve) (see Figure 6) from the vapor-liquid equilibrium curve. From this, the ethanol weight deviation (g / sec) is calculated from the weight deviation (g / sec) of the spirit and the vapor phase mole fraction. By integrating this over time, the estimated concentration and alcohol (ethanol) content of the spirit during distillation can be calculated. Here, since the ethanol-water vapor-liquid equilibrium surface used in this example is expressed using the ethanol-water vapor-liquid equilibrium curves of the raw material at each temperature, the ethanol-water liquid-vapor phase curves (xy curves) at each temperature obtained from the ethanol-water vapor-liquid equilibrium curves at each temperature can be used to represent the three-dimensional ethanol-water liquid-vapor phase curve (xy curve) (see Figure 6). Furthermore, if the weight of the ethanol solution of the raw material added (the weight of ethanol and water added together) is known, the weight of the ethanol solution of the raw material during distillation can be estimated by subtracting the weight of the recovered distilled spirits (distillate), and from this and the liquid phase molar fraction, the alcohol (ethanol) concentration of the raw material during distillation (the concentration of the target component and the alcohol (ethanol) content) can also be calculated. Here, the weight deviation [g / sec] is calculated by dividing g by sec (seconds), but g and sec can be set arbitrarily by the user as long as they are units that represent weight and time, respectively.

[0065] In addition, the system provides the following functions: (1) the function of providing distillation control of a target component (e.g., alcohol (ethanol)) at any concentration and temperature by controlling the pressure by gradually lowering the pressure when not boiling by comparing the steam temperature with the raw material temperature in real time, thereby searching for the boiling point (concentration), and by controlling the temperature by controlling the heating mechanism so that the raw material temperature is equal to the distillation setting temperature; (2) the function of providing stable distillation control that shortens operation time and prevents bumping by utilizing the vapor-liquid equilibrium curve of the target component-solvent component and performing efficient and appropriate pressure control; and (3) the function of calculating the estimated concentration of the target component contained in the distillate (extract) and raw material by utilizing the xy curve of the target component and constantly measuring the weight of the distillate (extract), thereby enabling automatic shutdown of an operating distillation (extraction) device depending on the concentration of the target component contained in the distillate (extract) being distilled under reduced pressure and the concentration of the target component contained in the raw material (e.g., liquid phase molar fraction). For example, in conventional technology, it was not possible to know the concentration of the distilled spirits or the concentration of ethanol contained in the raw material during vacuum distillation (e.g., liquid phase molar fraction), so it was not possible to automatically shut down the equipment depending on the concentration of the distilled spirits or the concentration of ethanol contained in the raw material, but this invention makes this possible.

[0066] Finally, in conventional technology, operators could not easily decide to change the distillation set temperature during reduced pressure distillation in order to maintain the quality of the distillate and residue, but by utilizing the vapor-liquid equilibrium surface, we provide a function that makes this possible. For example, when reducing the pressure of a raw material whose concentration of a target component is unknown for boiling detection, the concentration at that time can be determined from the vapor-liquid equilibrium surface based on the pressure at the time the distillation set temperature is changed and the distillation set temperature before the change. Therefore, the concentration at the time the distillation set temperature is changed is temporarily stored, and the pressure is controlled by changing the pressure to the saturated vapor pressure determined from that concentration and the changed distillation set temperature. This makes it possible to change the distillation set temperature during distillation when searching for boiling conditions for a raw material whose concentration of a target component is unknown, because the process used to search for the boiling conditions up to that point is stored even if the distillation set temperature is changed during distillation. If the concentration of the target component in the raw material is known, the set pressure is changed to the saturated vapor pressure determined from the changed distillation set temperature and the concentration of the target component via the vapor-liquid equilibrium surface, and the pressure is controlled. If boiling has already been detected and the concentration of the raw material (e.g., liquid phase mole fraction) is known, when the distillation set temperature is changed, the set pressure is changed to the saturated vapor pressure calculated via the vapor-liquid equilibrium surface from the changed distillation set temperature and the concentration of the target component (e.g., liquid phase mole fraction), and the pressure is controlled. However, when changing from a high distillation temperature setting to a low one, bumping may occur, so it is important to remember that the setting must be lowered gradually. A suitable example of changing the distillation set temperature during distillation (extraction) is when the purpose is sterilization. The distillation set temperature can be set to a high temperature (e.g., 80°C) to raise the temperature of the raw material (target component) and sterilize the raw material, and then the distillation set temperature can be reset to a lower temperature to start distillation or extraction.

[0067] The functions provided by the present invention can be summarized as follows: (1) By comparing the steam temperature and the raw material temperature in real time, the pressure is gradually reduced when the material is not boiling, thereby controlling the pressure to find the boiling point (concentration), and by controlling the heating mechanism so that the raw material temperature is equal to the distillation setting temperature, the function provides distillation control of the target component (e.g., alcohol (ethanol)) at any concentration and temperature. (2) The function of utilizing the vapor-liquid equilibrium curve of the target component and solvent component to perform efficient and appropriate pressure control, thereby shortening operation time and providing stable distillation control without bumping. (3) A function to calculate the estimated concentration of the target component contained in the distillate (extract) and raw material by utilizing the xy curve of the target component and constantly measuring the weight of the distillate (extract). (4) A function that automatically shuts down the device depending on the concentration of the target component by utilizing the technologies in (1) to (3). (5) A function that utilizes the vapor-liquid equilibrium curve of the target component (e.g., ethanol) to change the distillation temperature setting even while the distillation (extraction) equipment is in operation.

[0068] The vapor-liquid equilibrium surface may be a surface created by approximating and calculating a non-existent data range using multiple existing vapor-liquid equilibrium curves. For example, if data on the vapor-liquid equilibrium curves of ethanol-water at 30°C, 40°C, and 50°C are available, data on the vapor-liquid equilibrium curves from 31°C to 39°C and from 41°C to 49°C can be estimated by connecting the saturated vapor pressure values ​​at each concentration present in the vapor-liquid equilibrium curves at 30°C and 40°C, and at 40°C and 50°C, with approximation curves. A vapor-liquid equilibrium surface can be created using this estimated data. The calculations for this estimation may be performed using publicly known software. Furthermore, although the present invention assumes the use of a vapor-liquid equilibrium curve for a two-component system consisting of a target component and a solvent component (e.g., ethanol and water), it is also possible to distill (extract) the raw material by using the vapor-liquid equilibrium curve for a one-component system (e.g., water alone) (for example, in the case of water alone, this is equivalent to drying the raw material).

[0069] In the present invention, the user can freely change the settings of the operation time and the distillation volume recovered during vacuum distillation. Therefore, the present invention can provide a method for distilling or extracting raw materials with greater flexibility. For example, the user can change the operation time or distillation volume at any time from the start to the end of the method, improving the operability of the present invention. Since the operation time setting or the distillation volume recovered can be changed at any time from the start to the end of the method, multiple settings can be changed simultaneously or at different times as needed.

[0070] Hereinafter, embodiments of the method for distilling or extracting a raw material according to the present invention will be described in detail with reference to the drawings, but the technical scope of the present invention should not be limited by these descriptions.

[0071] FIG. 1 shows a vacuum distillation apparatus (1) used in the method for distilling or extracting raw materials according to the present invention. The reduced pressure distillation apparatus (1) requires a heating mechanism, a reducing pressure mechanism, a cooling mechanism, and sensors and control devices for controlling these mechanisms in order to distill or extract the raw material (M). For example, in the case of a microwave extraction device, the heating mechanism is a microwave generator (2) and microwave-transparent material (3), the pressure reduction mechanism is a tank (T), a vacuum pump (4) and an atmospheric release valve (5), the cooling mechanism is a cooling condenser (6) and a cooling device such as a chiller (7), the sensors are a pressure sensor inside the tank (8), a steam temperature sensor (9) and a raw material temperature sensor (12) (or a temperature sensor on the side of the tank), and the control device is a control panel (10) equipped with a PLC or touch panel.

[0072] The tank (T) is a container for storing the raw material (M) and is equipped with an agitator for agitating the raw material (M). The agitator in the present invention is composed of an agitator blade (11) disposed at the center of the inner bottom of the tank and a motor (15) disposed at the outer bottom of the tank, and the agitator blade (11) rotates around a vertical axis when driven by the motor (15). The tank (T) is used to process the raw material (M) therein, and its shape may be a rectangular parallelepiped, a cylindrical shape, or the like, but is not particularly limited. The motor (15) is controlled by the control panel (10) so that its rotating shaft can rotate in the forward or reverse direction, or in both the forward and reverse directions regularly or irregularly, thereby enabling the agitating blades (11) to rotate in the forward and reverse directions inside the tank.

[0073] A waveguide (13) is connected to the bottom of the tank (T) as a wave-guiding means for guiding microwaves generated by the microwave generator (2) into the tank (T). Although the number of waveguides (13) may be one, it is preferable to connect multiple waveguides (13) at multiple locations around the center of the bottom of the tank, as this allows the raw material (M) inside the tank (T) to be uniformly irradiated with microwaves. When multiple waveguides (13) are used, a microwave generator (2) may be connected to each waveguide (13), or a waveguide (13) from one microwave generator (2) may be branched into multiple waveguides (13).

[0074] The material of the tank (T) is not limited to a particular one, but for example, stainless steel is preferably used from the viewpoint of corrosion resistance. The capacity of the tank (T) is also not limited, but for example, 15 L, 100 L, 150 L, or 400 L can be used. The tank (T) may be equipped with a scale (or weighing scale) for measuring the mass of the raw material (M), and the user of the present invention may measure the weight of the raw material (M) in real time and understand the status. Note that the mass of the raw material (M) may be a value obtained by measuring it in advance before it is poured into the tank (T).

[0075] A microwave irradiation unit that irradiates microwaves into the tank (T) is provided at the bottom of the tank (T). The configuration of the microwave irradiating section is not particularly limited, and any configuration can be used as long as it can irradiate microwaves into the tank (T). As described above, the configuration of the microwave irradiation unit is not limited, but for example, the microwave irradiation unit includes a microwave generator (2) that generates microwaves, and a waveguide (13) that guides the microwaves generated by the microwave generator (2) into the tank (T).

[0076] It is preferable to install a plurality of microwave generators (2) so that the raw material (M) in the tank (T) can be uniformly irradiated with microwaves.

[0077] A magnetron is preferably used as the microwave generator (2), but other known microwave generators may also be used depending on the raw material (M), such as oscillators using electron tubes such as gyrotrons, klystrons, and traveling wave tubes, and solid-state oscillators that amplify the natural vibrations of crystal oscillators.

[0078] The tank (T) is provided with a microwave transmitting material (3) as a microwave transmitting means that transmits microwaves to the connection portion of the waveguide (13). The microwave-transmitting material (3) is formed from a dielectric material that allows microwaves to pass through (for example, resins such as PTFE, ceramics such as quartz and alumina, glasses, etc.), and the microwaves introduced into the waveguide (13) pass through the microwave-transmitting material (3) and are guided into the tank (T), where they heat the raw material (M) in the tank (T). The microwave-transmitting material (3) has a truncated cone shape whose diameter increases from the inner surface to the outer surface of the tank (T). A mounting hole having a truncated cone shape whose diameter increases from the inner surface to the outer surface of the tank (T) is formed in the bottom of the tank (T), and the microwave-transmitting material (3) is fitted into this mounting hole.

[0079] The top and / or side of the tank (T) is connected to a passage for extracting vapor containing the components (target components) in the raw material (M) that have been heated and evaporated in the tank (T) by microwave irradiation from the tank (T) and directing the vapor to the cooling condenser (6).

[0080] The refrigerant flowing through the cooling condenser (6) is once taken out to the outside, cooled by a cooling device (7), stored in a refrigerant tank, and then returned to the cooling condenser (6). The steam supplied into the cooling condenser (6) from the upper part or side part of the tank (T) through the passage is cooled and liquefied by the refrigerant supplied from the cooling device (7) and is collected in the container (14) connected to the bottom of the cooling condenser (6).

[0081] The cooling condenser (6) is not limited to either an air-cooled type or a water-cooled type, but a water-cooled type is preferable from the viewpoint of efficiency. The refrigerant for the cooling condenser (6) can be water or antifreeze. The antifreeze can be one whose main component is alcohol or one whose main component is ethylene glycol or the like. Although not particularly limited, water is preferably used as the refrigerant because it is inexpensive. The cooling device (7) is not particularly limited in type, but a chiller or the like is preferably used.

[0082] The container (14) contains a liquid (for example, water) containing the target component, which has been vaporized by heating and liquefied by passing through the cooling condenser (6). The upper part of the container (14) is connected via piping to a vacuum pump (4) which is a pressure reducing means. When the vacuum pump (4) is driven, the pressure inside the tank (T) is reduced through the piping, the cooling condenser (6) and the passage. By reducing the pressure inside the tank (T), the boiling point is lowered, allowing the raw material (M) to be distilled (extracted) at a low temperature.

[0083] The control device (control panel (10)) is equipped with a storage medium having written therein a program for controlling an atmospheric release valve (5) for allowing or blocking the inflow of outside air into the tank (T) and for adjusting the pressure inside the tank (T), a vacuum pump (4) configured to adjust (mainly reduce pressure) the pressure inside the tank (T), the microwave generator (2), and a stirring device for stirring the raw material (M) contained in the tank (T). The atmospheric release valve (5) is not limited to a specific valve, but in this embodiment, if the open / closed state is known, a program is provided to correct the deviation by applying correction in that state and convert and control the opening degree based on the cumulative time of the command. This control device (control panel (10)) can arbitrarily change the rotation speed and direction of the stirring blades (11), the output of the vacuum pump (4), the output, oscillation / stop, pulse irradiation and its oscillation time / stop time of the atmosphere release valve (5) and microwave generator (2) according to the raw material temperature of the raw material (M) and / or the vapor temperature of the raw material (M) during operation of the extraction device (1).

[0084] The control device (control panel (10)) has a non-volatile memory (e.g., ROM) and a volatile memory (e.g., RAM) as the storage medium, and the user can freely set target values ​​in advance and register or re-register them as recipes. This allows the user to devise and improve recipes and develop products independently. The items that the user can register in the program as a recipe include microwave output, oscillation / stop, pulse irradiation and its oscillation time / stop time, stirring speed, direction of rotation and its normal rotation time / reverse rotation time, distillation set temperature, etc., according to the elapsed operation time or recovery amount (distillation amount). Not only step control but also ramp control settings can be registered for the rotation speed and direction of rotation (normal rotation / reverse rotation) of the stirring blade (11), microwave output, pulse irradiation oscillation time / stop time, and distillation set temperature. Furthermore, regarding microwave pulse irradiation, if there are multiple microwave irradiators, for example, four (No. 1 to No. 4), the start timing of each pulse irradiation can be shifted (by setting an offset value for each). For example, No. 1 and No. 3 can be oscillated, No. 2 and No. 4 can be stopped, then No. 1 and No. 3 can be stopped, No. 2 and No. 4 can be oscillated, and the cycle can be repeated alternately. Alternatively, No. 1 can be oscillated, No. 2 to No. 4 can be stopped, No. 2 can be oscillated, No. 1, No. 3, and No. 4 can be stopped, then No. 3 can be oscillated, No. 1, No. 2, and No. 4 can be stopped, No. 4 can be oscillated, No. 1 to No. 3 can be stopped, and the cycle can be repeated in order. If the start timing of pulse irradiation is the same, No. 1 to No. 4 can be oscillated and stopped simultaneously, resulting in pulse irradiation.

[0085] The control device (control panel (10)) has the function of controlling the rotation speed of the vacuum pump (4) by PID (proportional, integral, derivative) control and opening / closing the air release valve (5) by PD (proportional, differential) control in order to control the pressure in the tank (T) to a target value. In this embodiment, the rotation speed of the vacuum pump (4) is PID controlled and the opening of the air release valve (5) is PD controlled based on the pressure deviation. A PLC, for example, is preferably used as the control device, and this PLC is equipped with a program that enables pressure control and temperature control. For example, in the case of a microwave extraction device (1), pressure control is PID control of the rotation speed of the vacuum pump (4) and / or PD control of the opening of the atmospheric release valve (5), and temperature control is control of the microwave generator (2) by oscillating / stopping, pulse irradiation, and output. Parameters corresponding to a gas-liquid equilibrium surface and an xy curve (a curve in the program) are also equipped. These parameters may be values ​​determined from experimental values, values ​​determined from theoretical values ​​such as Wilson's constant and Atwan's constant, or the theoretical formula itself. In the case of a gas-liquid equilibrium surface, they may be created by using multiple existing gas-liquid equilibrium curves to interpolate and estimate a range of data that does not already exist.

[0086] The length of each blade of the stirring blade (11) in the longitudinal direction is not limited, but may be, for example, 32 cm to 120 cm, and the pitch angle is not limited, but may be, for example, 30 degrees to 35 degrees.

[0087] The control device (control panel (10)) has a step control function and a ramp control function. The step control controls the rotation speed and direction (forward / reverse) of the stirring blade (11) and its time, the microwave output for heating the raw material (M), the microwave oscillation / stop, pulse irradiation and its oscillation / stop by ON / OFF operation. Ramp control controls the rotation speed and direction (forward / reverse) of the stirring blade (11), the microwave output for heating the raw material (M) in the tank (T), the pulse irradiation oscillation time / stop time, and the change in the distillation set temperature. By controlling the ramp, it is possible to gradually change the rotation speed of the stirring blade (11), the rotation direction (forward / reverse) time, microwave output, and pulse irradiation oscillation / stop time, for example, in accordance with the state of distillation (extraction) of the target component from the raw material (M) and / or the temperature rise. In other words, compared to when gradual changes are not possible, more precise stirring is possible, and microwave irradiation can be performed efficiently, thereby shortening the distillation (extraction) time.

[0088] The tank pressure sensor (8) is a pressure sensor installed in the tank (T) to detect the pressure. The pressure sensor is not particularly limited, and for example, a diaphragm type pressure sensor can be used. The present invention also has a control means for automatically controlling the pressure in the tank (T) by controlling the rotation speed of the vacuum pump (4) and opening and closing the atmospheric release valve (5), which is an electrically operated valve, based on the detection result of the tank pressure sensor (8).

[0089] The steam temperature sensor (9) is a sensor that detects and measures the temperature of steam generated from the raw material (M). The raw material temperature sensor (12) is a sensor that detects the raw material temperature or a temperature equivalent thereto. For example, in the case of the microwave extraction device (1), since the temperature at the bottom of the side of the tank is approximately equivalent to the raw material temperature, it may be installed at the bottom of the side of the tank (in this case, the raw material temperature sensor (12) may also be referred to as a tank side temperature sensor). The steam temperature sensor (9) and the raw material temperature sensor (12) for measuring the temperature of the raw material (M) may be configured in any manner, but it is preferable to use a thermocouple or an infrared radiation thermometer because they are inexpensive and easy to install. Other examples include a resistance temperature detector, an optical fiber thermometer, etc.

[0090] The raw material (M) is the source of the distillation and extraction according to the present invention, and may be a mixture of liquids, solids, or a mixture of both liquids and solids. There are no particular limitations on the form of the raw material, as long as it contains a solvent component (e.g., water) and a target component. When the raw material is a solid mixture and the target component adhering to the raw material is to be distilled (extracted), the raw material can be dispersed in a solvent (e.g., water) in which the target component dissolves, thereby utilizing the vapor-liquid equilibrium curve of the target component-solvent component (water), thereby enabling the present invention to be implemented.

[0091] The liquid mixture refers to the liquid components contained in the raw material (M). The liquid components contained in the raw material (M) may take into account the water content (or oil content) of each component constituting the raw material (M), but since the target component and the solvent component are often predominantly present in the raw material (M), the liquid mixture is often expressed as the sum of the target component and the solvent component. When using the vapor-liquid equilibrium surface according to the present invention, attention is focused on the state change of this liquid mixture.

[0092] The target component is the component recovered as a distillate (extract or recovered product) after the distillation and extraction according to the present invention. In the present invention, the target component is preferably used as the first component on the vapor-liquid equilibrium curve. The target component is determined arbitrarily by the user of the distillation or extraction method according to the present invention, depending on the user's purpose. For example, the user may need a distillate containing the target component after the distillation or extraction according to the present invention, or may need the residue of the raw material from which the target component has been removed. The user will determine the target component arbitrarily depending on the purpose. The target component is preferably a liquid, in view of the fact that the present invention involves distillation and extraction. Possible target components include alcohols such as methanol, ethanol, 1-propanol, 2-propanol, t-butyl alcohol, 1-butanol, and 2-butanol, organic solvents such as acetone, 3-butene, and acetonitrile, and odor components (e.g., volatile organic compounds with a molecular weight of 350 or less that contain at least one of the following elements: hydrogen, carbon, nitrogen, oxygen, and sulfur). As the target component, methanol or ethanol is particularly suitable.

[0093] The solvent component is a component that is uniformly mixed with the target component and is intended to function as a solvent for the target component in the present invention. In the present invention, the solvent component is preferably used as the second component on the vapor-liquid equilibrium surface. Examples of the solvent component include water, toluene, hexane, heptane, cyclohexane, dioxane, tetrachloromethane, p-xylene, m-xylene, o-xylene, benzene, toluene, triethylamine, diethyl ether, cyclopentyl methyl ether (CPME), chloroform, chlorobenzene, ethyl acetate, acetic acid, dimethyl ether, Me-THF, 1,2-dimethoxyethane, diethylene glycol, diethylene glycol diethyl ether, THF, dichloromethane, ethylene glycol, 1,2-dichloroethane, N-methyl-2-pyrrolidone (NMP), hexamethylphosphoric triamide (HMPA), N,N-dimethylformamide (DMF), pyridine, nitromethane, glycerin, dimethyl sulfoxide (DMSO), methyl tert-butyl ether (MTBE), octane, and mixed solvents thereof. However, there is no particular limitation as long as it is uniformly mixed with the target component and functions as a solvent for the target component in the present invention.

[0094] The distillation set temperature (also referred to as the distillation temperature or target distillation temperature) is the set temperature for distillation and extraction according to the present invention. Since the present invention involves a decompression process, reducing the pressure can lower the boiling point of the target component, allowing distillation and extraction to be performed at low temperatures. For example, the distillation set temperature can be set between 10°C and 100°C. When microwave heating is performed, a setting between 30°C and 100°C is preferable. This is because performing distillation or extraction under low-temperature, low-pressure conditions increases the probability of microwave-induced plasma generation, which may significantly damage the equipment. For example, the distillation or extraction method according to the present invention can be safely performed by defining the saturated vapor pressure of 6.67 kPa when the boiling point of water is 38°C as the limit value under low-temperature, low-pressure conditions. Here, the saturated vapor pressure of ethanol, one of the target components, when its boiling point is 30°C (i.e., the lowest temperature suitable for microwave heating) is approximately 10.44 kPa at a molar fraction of 0.9, allowing users to safely perform the distillation or extraction method according to the present invention. Furthermore, when producing distilled spirits containing components that are susceptible to thermal degradation, such as citrus essential oil components, it is preferable to set the distillation temperature between 30°C and 70°C.

[0095] The distillation volume (recovery volume or extraction volume) is the weight of the distillate (extract or recovered product). In the apparatus used for the distillation or extraction method of the present invention, the vessel (14) for recovering the distillate (e.g., a distillate recovery tank or recovery vessel) can be equipped with a scale (or weighing scale) to measure the mass of the distillate.

[0096] The operating time is the operating time of the distillation and extraction according to the present invention, and there is no particular limitation on the range thereof.

[0097] The raw material temperature refers to the temperature of the raw material (M) present in the tank (T). In addition to measuring the temperature of the raw material (M) by directly contacting the raw material (M) with the raw material temperature sensor (12), it is also possible to measure the temperature of the raw material (M) indirectly via the tank (T) using a raw material temperature sensor (12) attached to the side of the tank. In this case, the raw material temperature measured by the raw material temperature sensor (12) attached to the side of the tank is also referred to as the tank side temperature. In addition, in the practice of the present invention, it is preferable to measure the temperature of the raw material (M) by attaching the raw material temperature sensor (12) to the side of the tank, in consideration of preventing damage to the raw material temperature sensor (12) and making it easier to handle.

[0098] The vapor temperature refers to the temperature of the vapor generated by the distillation and extraction according to the present invention, and is measured using a vapor temperature sensor (9).

[0099] The distillate (extract, or recovered product) is the product recovered from the distillation and extraction procedures of the present invention and contains the target component.

[0100] FIG. 2 is a control flow chart for the method of distilling or extracting raw materials of the present invention. The present invention is achieved by the following steps starting from (1). It should be noted that in order to practice the present invention, a vapor-liquid equilibrium surface represented by a mixture of the target component and the solvent component must be prepared in advance and used as a parameter in the present invention. (1) Set the operating time or distillation volume (recovery volume). (2) Set the distillation temperature. (3) The distillation set temperature is different from the ambient temperature by ΔT. A Determine whether the set temperature difference ΔT is higher than the set temperature difference ΔT. A If it is higher than this, proceed to (4). A If it is less than this, return to (2). This judgment is made because boiling is detected based on the deviation between the raw material temperature (temperature on the side of the tank) and the steam temperature, so if the indoor temperature is higher than the distillation set temperature, boiling cannot be detected. For example, the set temperature difference ΔT A A temperature of 3°C or higher is preferable. (4) Is the concentration of the target component contained in the raw material (liquid phase mole fraction or mol%) known? If known, proceed to (5). If unknown, start operation and proceed to (7). (5) The concentration (liquid phase mole fraction or mol%) of the target component contained in the raw material is set, and operation is started. (6) The saturated vapor pressure at the set concentration (liquid phase mole fraction or mol%) of the target component is derived from the vapor-liquid equilibrium surface, and the pressure in the tank is reduced to the derived saturated vapor pressure. When the pressure in the tank reaches the set pressure difference ΔP A for a certain time t A The pressure is stabilized until it is reached. After the pressure is stabilized, proceed to (8). For example, the pressure at this time (set pressure difference ΔP A ) for 4 seconds (a certain time t A ) It is preferable that the pressure inside the tank is maintained within ±0.4 kPa. (7) The pressure in the tank is reduced to the saturated vapor pressure value obtained (determined) when the concentration (liquid phase mole fraction or mol%) of the target component at the maximum saturated vapor pressure at which the raw material does not boil, obtained from the vapor-liquid equilibrium surface of the target component (for example, if ethanol is the target component, a value of 90 mol% is used) and the distillation set temperature are applied to the vapor-liquid equilibrium surface, and the pressure in the tank is reduced to the saturated vapor pressure value obtained (determined) when the pressure in the tank is equal to the set pressure difference ΔP B for a certain time tB The pressure is stabilized until it is reached. After the pressure is stabilized, proceed to (8). For example, the pressure at this time (set pressure difference ΔP B ) for 4 seconds (a certain time t B ) It is preferable that the pressure inside the tank is maintained within ±0.4 kPa. (8) Start stirring the ingredients. (9) After (8), the pressure in the tank becomes equal to the set pressure difference ΔP C for a certain time t C The pressure is adjusted until the pressure is reached. For example, the pressure adjustment at this time (set pressure difference ΔP C ) for 5 seconds (a certain time t C ) is preferably within ±0.3 kPa. (10) After (9), heating is started, for example, by oscillating microwaves (continuous irradiation). In the operations after (10), The difference between the raw material temperature (temperature on the side of the tank) and the distillation temperature is ΔT. B If it is above this level, stop heating by, for example, stopping microwave generation, and wait until the raw material temperature (temperature on the side of the tank) minus the distillation set temperature is equal to the set temperature difference ΔT C If the temperature is less than 1.5℃, the temperature is (re)heated. For example, if the raw material temperature (temperature on the side of the tank) - the distillation set temperature is ≥ 1.5℃ (set temperature difference ΔT B ), it is preferable to stop heating (stop microwave generation). Also, if the raw material temperature (temperature on the side of the tank) - distillation set temperature < 1.0°C (set temperature difference ΔT C ), it is preferable to (re)heat ((re)oscillate microwaves). In addition, for temperature control, the set temperature difference ΔT B and / or set temperature difference ΔT C In the case of microwave heating, the set temperature difference ΔT can be used to stop microwave irradiation, oscillate microwaves, switch to pulse irradiation, switch to continuous irradiation, reduce microwave output, or increase microwave output, depending on the temperature difference between the raw material temperature and the distillation set temperature. B and / or set temperature difference ΔT C You can set the following. (11) After (10), the pressure in the tank becomes equal to the set pressure difference ΔP D Within a certain time t D The pressure in the tank is stabilized until it is reached, and it is determined whether the raw material temperature (temperature on the side of the tank) is equal to or higher than the set distillation temperature. D Within a certain time t D The temperature is stabilized until the temperature is reached, and if the raw material temperature (temperature on the side of the tank) is equal to or higher than the distillation set temperature, proceed to (12). ΔP D The value range of t is within ±0.01~0.2. D The value of ΔP can be in the range of 0.5 to 5, and can be set arbitrarily by the operator depending on the distillation temperature setting. D and t D The setting of the value of can be programmed by the operator so that it can be changed to any value under any condition from the start to the end of the present invention. For example, the pressure stabilization at this time (set pressure difference ΔP D ) for 1 second (a fixed time t D ) is preferably within ±0.1 kPa. (12) When all of the following conditions are met, the pressure in the tank is further reduced at a rate according to the slope ΔkPa / Δconcentration of the vapor-liquid equilibrium curve between the target component and the solvent component. conditions (I) It is not boiling, or

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[0105] The step (10) of starting heating does not have to be after (9), but may be after (4) or (5), for example. In the present invention, each step can be stopped automatically at any time. When the step is stopped automatically, the decision is made based on the concentration of the target component contained in the distillate (extract) being distilled under reduced pressure and the concentration of the target component contained in the raw material (e.g., liquid phase molar fraction) using a function for calculating the estimated concentration of the target component contained in the distillate (extract) and raw material. Other cases where the system will automatically stop include when the operating time set in (1) has elapsed or when the distillation volume (recovery volume) has been reached. The present invention utilizes the vapor-liquid equilibrium curve of the target component (for example, ethanol) and can change the distillation set temperature even during operation of the distillation (extraction) apparatus. The present invention calculates the estimated concentration of the distillate (extract) during distillation from the liquid-gas phase surface (xy surface) of the target component, which is determined from the gas-liquid equilibrium surface by constantly measuring the weight of the distillate (extract) and detecting the boiling of the raw material (see Figure 6).In addition, if the weight of the liquid mixture in the raw material (the sum of the weight of the target component and the solvent component) is known, the concentration of the target component in the raw material during distillation (extraction) can be calculated. [Example]

[0106] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to these examples.

[0107] Example 1 As shown in Figure 3, the pressure-temperature-concentration vapor-liquid equilibrium surface for the binary ethanol-water system was created by using multiple existing vapor-liquid equilibrium curves.

[0108] Example 2 As shown in Figure 4, 50 kg of raw material with an unknown concentration of the target component (ethanol) was subjected to reduced pressure distillation according to the present invention. The distillation temperature was set to 40°C, and the distillation amount (recovery amount) was set to 16 kg. First, the operation time according to the present invention was shortened by reducing the pressure to a saturated vapor pressure of 90 mol%, which is calculated from the vapor-liquid equilibrium surface of ethanol-water and does not cause boiling of the raw material. Next, the raw materials were stirred, and the microwave generator was started. The microwave generator was set to stop when the raw material temperature minus the distillation set temperature was ≥ 1.5°C, and to (re)oscillate when the raw material temperature minus the distillation set temperature was < 1.0°C. Then, in order to find the concentration of the target component (ethanol) contained in the raw material, the pressure was further reduced at a rate corresponding to the slope of the vapor-liquid equilibrium curve ΔkPa / Δmol% until all of the following conditions were not met:

[0109] conditions (1) The system is not boiling, or the difference between the steam temperature and the distillation set temperature is 0.8°C or more. Here, boiling is determined to occur when the difference between the raw material temperature and the steam temperature when the first boiling is detected is 1.0°C or less, and when the difference between the raw material temperature and the steam temperature when the second or subsequent boiling is detected is 0.5°C or less. (2) Depending on the concentration of the target component, the difference between the saturated vapor pressure calculated from the vapor-liquid equilibrium surface and the actual measured pressure is within ±0.1 kPa per second. (3) The difference between the raw material temperature and the distillation set temperature must be 0.3°C or more. Rate = [ΔkPa / Δmol%] / sec × a (In this case, a=1.)

[0110] Under these conditions, the first boiling was detected approximately 21 minutes and 30 seconds after the start of decompression, and the raw material was calculated to have an alcohol (ethanol) content of 8.68 mol%, an alcohol (ethanol) content of 23.9%, and a mass concentration of 19.5 wt%. The second boiling was confirmed approximately 24 minutes and 30 seconds after the start of decompression.

[0111] Assuming that the concentration of the target component (ethanol) contained in the raw material would decrease over time, the vacuum distillation process was carried out while maintaining the above conditions and rate, and while monitoring the concentrations of the raw material and distillate in real time, the vacuum distillation was stopped when the recovered amount (distilled amount) reached 16 kg. The concentration of the distillate was 23.2 mol%, alcohol (ethanol) content 51.1%, and mass concentration 43.5 wt%.

[0112] From the start to the end of the vacuum distillation in Example 2, the raw material temperature and vapor temperature could be maintained at around 40° C. The room temperature was about 32° C. to about 34° C. from the start to the end of the vacuum distillation.

[0113] Example 3 As shown in Figure 5, 50 kg of raw material with a target component (ethanol) concentration of 18.7°C (6.55 mol%, mass concentration 15.19 wt%) measured by an alcohol meter was subjected to vacuum distillation according to the present invention. The distillation temperature was set to 40°C, and the distillation volume (recovery volume) was set to 16 kg. First, the pressure was reduced to the saturated vapor pressure value when the concentration of the target component (ethanol) was 6.55 mol% from the vapor-liquid equilibrium curve of ethanol-water. Next, the raw materials were stirred, and the microwave generator was started. The microwave generator was set to stop when the raw material temperature minus the distillation set temperature was ≥ 1.5°C, and to (re)oscillate when the raw material temperature minus the distillation set temperature was < 1.0°C. Thereafter, the pressure was further reduced at a rate according to the slope of the vapor-liquid equilibrium surface ΔkPa / Δmol% until all of the following conditions were no longer met:

[0114] conditions (1) The system is not boiling, or the difference between the steam temperature and the distillation set temperature is 0.8°C or more. Here, boiling is determined to occur when the difference between the raw material temperature and the steam temperature when the first boiling is detected is 1.0°C or less, and when the difference between the raw material temperature and the steam temperature when the second or subsequent boiling is detected is 0.5°C or less. (2) Depending on the concentration of the target component, the difference between the saturated vapor pressure calculated from the vapor-liquid equilibrium surface and the actual measured pressure is within ±0.1 kPa per second. (3) The difference between the raw material temperature and the distillation set temperature must be 0.3°C or more. Rate = [ΔkPa / Δmol%] / sec × a (In this case, a=1.)

[0115] Under these conditions, the first boiling was detected approximately 17 minutes after depressurization began.

[0116] Assuming that the concentration of the target component (ethanol) contained in the raw material would decrease over time, the vacuum distillation process was carried out while maintaining the above conditions and rate, and while monitoring the concentrations of the raw material and distillate in real time, the vacuum distillation was stopped when the recovered amount (distilled amount) reached 16 kg. The concentration of the distillate was 23.3 mol%, alcohol (ethanol) content 51.3%, and mass concentration 43.7 wt%.

[0117] From the start to the end of the vacuum distillation in Example 3, the raw material temperature and vapor temperature could be maintained at around 40° C. The room temperature was about 32° C. to about 34° C. from the start to the end of the vacuum distillation. Compared to Example 2, the time from the start to the end of vacuum distillation was shortened by about 5 minutes. [Industrial Applicability]

[0118] The method of distilling or extracting raw materials according to the present invention can recover target components from various types of raw materials by distillation or extraction, and can be widely used, for example, in the production of distilled spirits, the removal of organic solvents contained in raw materials, and recycling for the purpose of removing odorous components adhering to resin containers (where the raw material is a solid (container), the target component is an odorous component, and the solvent component is water). Furthermore, in the production of distilled spirits, even when producing distilled spirits containing components that are susceptible to thermal degradation, such as essential oil components contained in citrus fruits such as yuzu, the present invention allows distillation (extraction) to be performed at low temperatures (e.g., 35°C), making it possible to produce distilled spirits that do not impair the citrus aroma. [Explanation of symbols]

[0119] 1. Vacuum distillation (extraction) apparatus 2. Microwave generator 3. Microwave-transmitting materials 4. Vacuum pump 5. Atmospheric release valve 6 Cooling condenser 7 Cooling device 8. Tank pressure sensor 9 Steam temperature sensor 10 Control Panel 11 Stirring blade 12 Raw material temperature sensor 13 Waveguide 14 Container 15 motor M Raw material T Tank

Claims

1. A vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component, The saturated vapor pressure of the raw material decreases (the boiling point of the raw material increases) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, thereby decreasing the concentration (or content) of the target component in the raw material. In an airtight tank that can be decompressed, (A) heating the feedstock to and maintaining a desired distillation temperature; (B) gradually reducing the pressure in the tank if the material is not boiling; and (C) maintaining pressure in the tank if the material is boiling; This involves boiling the raw material at the target distillation temperature while capturing the saturated vapor pressure of the raw material, which changes over time due to distillation, and distilling at a constant temperature.

2. Regarding the steps (B) and (C), In an environment where the ambient temperature is lower than the target distillation temperature, the steam temperature and raw material temperature are compared.

2. The vacuum distillation method according to claim 1, wherein the phenomenon that the vapor temperature becomes equal to the raw material temperature when boiling occurs and the vapor temperature becomes lower than the raw material temperature when boiling ceases is utilized.

3. Regarding the pressure reduction in the step (B), First, a vapor-liquid equilibrium surface is used, which represents a mixture of a target component and a solvent component that is mixed with the target component, and is determined by temperature, concentration, and pressure. (a) When the concentration (or content) of the target component in the raw material is unknown, the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximized are measured to the saturated vapor pressure determined by the vapor-liquid equilibrium curve. (b) When the concentration (or content) of the target component in the raw material is known, the target distillation temperature and the target component concentration are determined from the saturated vapor pressure determined by the vapor-liquid equilibrium curve.

2. The vacuum distillation method according to claim 1, wherein the pressure is rapidly reduced while heating is performed up to and maintaining the target distillation temperature under the conditions (a) or (b).

4. Regarding the pressure reduction in the step (B), The pressure is reduced at a rate that utilizes the value of the gradient of saturated vapor pressure versus concentration of the target component on a vapor-liquid equilibrium curved surface that represents a mixed system of the target component and the solvent component that is mixed with the target component, which is determined by the raw material temperature and the pressure inside the tank, and the value of the gradient of saturated vapor pressure versus concentration of the target component is [Equation 1] That is, The vacuum distillation method according to claim 1.

5. Regarding the pressure reduction in the step (B), First, a vapor-liquid equilibrium surface is used, which represents a mixture of a target component and a solvent component that is mixed with the target component, and is determined by temperature, concentration, and pressure. (a) When the concentration (or content) of the target component in the raw material is unknown, the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximized are measured to the saturated vapor pressure determined by the vapor-liquid equilibrium curve. (b) When the concentration (or content) of the target component in the raw material is known, the target distillation temperature and the target component concentration are determined from the saturated vapor pressure determined by the vapor-liquid equilibrium curve. heating to and maintaining the desired distillation temperature according to the conditions of (a) or (b), while rapidly reducing the pressure; Next, regarding the second and subsequent decompressions, The pressure is reduced at a rate utilizing the value of the gradient of the saturated vapor pressure with respect to the concentration of the target component on the vapor-liquid equilibrium curve determined by the raw material temperature and the pressure inside the tank, and the value of the gradient of the saturated vapor pressure with respect to the concentration of the target component is [Equation 2] That is, The vacuum distillation method according to claim 1.

6. Regarding the pressure reduction in the step (B), in order to perform the distillation at a more stable temperature, In an environment where the ambient temperature is lower than the target distillation temperature, A vacuum distillation method in which the pressure is reduced when all of the following conditions (1) to (3) described in Condition 1 are met: (1) It is not boiling, or [Equation 3] and (2) The absolute value of the difference between the target and actual tank pressure remains constant for a certain period of time t Ｅ At this point, the set pressure difference ΔP Ｅ and （３） [Equation 4] That is, Here, the condition for detecting boiling in (1) is (4) described in condition 2 below, (4) Boiling detection: [Equation 5] That is, The vacuum distillation method according to any one of claims 1 to 5, wherein

7. 2. The reduced pressure distillation method according to claim 1, further comprising a step of determining the liquid phase molar fraction and the vapor phase molar fraction of the target component in the tank from the raw material temperature and the pressure in the tank during boiling in the distillation, using a vapor-liquid equilibrium surface represented by a mixed system of the target component and a solvent component miscible with the target component.

8. 8. The vacuum distillation method according to claim 7, further comprising a step of estimating the mass concentration of the target component in the raw material and / or distillate from the liquid phase molar fraction and / or gas phase molar fraction of the target component and the mass of the raw material and / or distillate, when the mass of the raw material and / or distillate can be measured.

9. 2. The reduced pressure distillation method according to claim 1, further comprising the step of: when the target distillation temperature is changed during the distillation, quickly changing the pressure in the tank to the saturated vapor pressure calculated from the gas-liquid equilibrium surface represented by a mixture system of the target component and the solvent component mixed with the target component, based on the concentration of the target component calculated before the change and the target distillation temperature after the change, and continuing the distillation.

10. 2. The reduced pressure distillation method according to claim 1, further comprising the step of detecting, during the distillation, a state in which the concentration of the target component calculated by a gas-liquid equilibrium surface representing a mixed system of the target component and the solvent component mixed with the target component becomes zero, or a state in which the target internal tank pressure calculated by the gas-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone, in the case of a raw material containing a target component and a solvent component mixed with the target component, and stopping the distillation when the concentration of the target component becomes zero or when the target internal tank pressure becomes equal to the saturated vapor pressure of the solvent component alone.

11. The reduced pressure distillation method according to claim 1, wherein the heating is performed by microwave irradiation, and microwave irradiation is stopped, microwave oscillation is started, switching to pulse irradiation, switching to continuous irradiation, microwave output is decreased, or microwave output is increased depending on the difference between the raw material temperature and the target distillation temperature.

12. The vacuum distillation method according to claim 1 , wherein the raw material contains alcohol and the target component is alcohol.

13. The vacuum distillation method according to claim 1 , wherein the raw material contains ethanol and the target component is ethanol.

14. A microwave extraction apparatus used in the reduced pressure distillation method according to claim 1, the extraction apparatus comprising: a tank containing raw materials; a microwave generator that generates microwaves; a wave-guiding means and a microwave-transmitting means for guiding the microwaves to the tank; an agitator that agitates the raw material contained in the tank; a vacuum pump for adjusting the pressure in the tank; an atmospheric release valve for adjusting the pressure inside the tank; a cooling condenser or cooling device for cooling and condensing the vapor of the raw material evaporated from the tank by heating; a recovery unit that recovers the components condensed by the cooling condenser; a control device for controlling the operation of pressure, cooling, and microwave irradiation; sensors for measuring the pressure, raw material temperature, and steam temperature in the tank; A microwave extraction device comprising:

15. a function of calculating the liquid phase molar fraction and the vapor phase molar fraction of the target component in the tank from the raw material temperature and the pressure in the tank during boiling in the distillation, using a vapor-liquid equilibrium curved surface represented by a mixture system of the target component and a solvent component mixed with the target component; When a scale capable of measuring the mass of the raw material and / or distillate is available, the mass concentration of the raw material and / or distillate of the target component can be estimated from the liquid phase molar fraction and / or gas phase molar fraction of the target component and the mass of the raw material and / or distillate. The microwave extraction apparatus according to claim 14, having a function of estimating the mass concentration of the raw material and / or distillate.

16. 15. The microwave extraction apparatus according to claim 14, wherein when the target distillation temperature is changed during the distillation, the pressure in the tank is quickly changed to the saturated vapor pressure calculated from the gas-liquid equilibrium surface represented by a mixed system of the target component and the solvent component mixed with the target component, based on the concentration of the target component calculated before the change and the target distillation temperature after the change.

17. In the case of a raw material containing a target component and a solvent component that is mixed with the target component, the microwave extraction apparatus according to claim 14, which has the function of detecting, during the distillation, a state in which the concentration of the target component calculated by a gas-liquid equilibrium surface representing a mixed system of the target component and the solvent component that is mixed with the target component becomes 0, or a state in which the target internal tank pressure calculated by the gas-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone, and stopping the distillation when the concentration of the target component becomes 0 or the target internal tank pressure becomes equal to the saturated vapor pressure of the solvent component alone.

18. The heating is performed by microwave irradiation, and microwave irradiation is stopped, microwave oscillation is started, switching to pulsed irradiation, switching to continuous irradiation, microwave output is reduced, or microwave output is increased depending on the difference between the raw material temperature and the target distillation temperature. The microwave extraction apparatus according to claim 14.

19. 15. The microwave extraction apparatus of claim 14, wherein the raw material contains alcohol and the target component is alcohol.

20. 15. The microwave extraction apparatus of claim 14, wherein the raw material comprises ethanol and the target component is ethanol.

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