Method for distilling or extracting a liquid mixture or a mixture containing the same, and microwave extraction apparatus using the method

Abstract

A method for distilling or extracting a raw material is provided, which involves a component (hereinafter referred to as the target component) contained in a liquid mixture or a mixture containing the same (hereinafter referred to as the raw material), and which the operator aims to recover as a distillate by distillation or extraction. Regardless of whether the concentration of the target component is known, and regardless of the concentration of the target component in the raw material that continuously changes over time during the distillation (extraction) process, the raw material is recovered by distilling or extracting under reduced pressure at a set distillation temperature. 【Solution means】Detecting the boiling of the raw material while reducing the pressure, and calculating the concentration of the target component in the raw material by using the vapor-liquid equilibrium surface for the target component from the detected pressure and temperature at the time of boiling. Also, in the distillation (extraction) process, continuously calculating the new concentration of the target component in the raw material by newly detecting the boiling while reducing the pressure, even for the concentration of the target component in the raw material that continuously changes over time, thereby providing a method for distilling or extracting.

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 specifically, to a component (hereinafter referred to as the target component) contained in the raw material and intended to be recovered as a distillate by the operator through distillation or extraction. Regardless of whether the concentration of the target component is known, and regardless of the concentration of the target component in the raw material that continuously changes over time during the distillation (extraction) process, the present invention relates to a method for distilling or extracting the raw material, which is recovered by distilling or extracting under reduced pressure at the target distillation temperature.

Background Art

[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 enables efficient regeneration of a liquid to be treated, such as a non-aqueous solvent containing various dirt components. Patent Document 2 proposes an extraction apparatus and an extraction method involving a vacuum step for efficiently extracting a target component. Patent Document 3 proposes an extraction apparatus using microwaves that extracts and recovers useful components, such as essential oils, contained in an object to be treated, such as biomass, by irradiating the object to be treated with microwaves for heating.

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Patent Document 2

Patent Document 3

Summary of the Invention

Problems to be Solved by the Invention

[0004] However, in the distillation (extraction) process, the concentration of the target component in the raw material continuously changes over time, and the boiling point of the target component also continuously changes along with the concentration change. Therefore, there is a technical problem that it is difficult to control the distillation (extraction) at a constant temperature. In addition, when distilling or extracting the target component under reduced pressure, the state of the raw material may not be clearly grasped by the operator before distillation or extraction. Therefore, it is difficult for the operator to predict under what conditions (the concentration of the target component contained in the raw material and the reduced pressure value of the raw material determined from the target distillation temperature of the operator) the distillation or extraction will start, and it takes time to grasp these conditions. For example, when distilling a raw material containing alcohol (ethanol) at the target distillation temperature and recovering the alcohol (ethanol) as a distillate, when measuring the alcohol (ethanol) concentration contained in the raw material to obtain the reduced pressure value, it is necessary to measure the concentration using an alcohol hydrometer or the like, and then perform a step of determining the reduced pressure value from the measured concentration and the target distillation temperature. When obtaining the reduced pressure value without measuring the alcohol (ethanol) concentration contained in the raw material, it is necessary to perform a step of searching for the boiling point of the raw material by reducing the pressure until the raw material boils. Furthermore, this pressure reduction must be carried out gradually to prevent bumping of the raw material. If bumping occurs, an excessive amount of the target component will be distilled beyond the capacity of the cold trap, and the distilled target component will atomize into the atmosphere as it is, making it impossible to successfully recover the target component as a distillate. Or, an excessive amount of the target component may flow back into the vacuum pump, causing the vacuum pump to malfunction. Therefore, it is necessary to prevent this. Since it is necessary to perform these steps to grasp the above conditions, there is a problem that it takes time until the raw material in the distillation process first boils, and the total operation time required for the distillation (extraction) process becomes redundant. Furthermore, in the distillation (extraction) process carried out at a constant temperature, as time passes, the concentration of the target component in the raw material constantly changes, and accompanying this concentration change, the boiling point of the target component also constantly changes. Against this background, every time a concentration change occurs in the raw material, it is desirable to change (reduce) the pressure, but it is not easy for an operator to predict the constantly occurring concentration changes, and therefore it is difficult for the operator to determine how much the pressure should be reduced. Excessive pressure reduction causes bumping in the raw material as described above, and conversely, if the pressure reduction operation is insufficient, distillation (extraction) will not occur.

[0005] In view of the above circumstances, the present invention aims to provide a method for distilling or extracting a raw material, which recovers the target component contained in the raw material by distilling or extracting it under reduced pressure at a set distillation set 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 that constantly changes over time during the distillation (extraction) process.

Means for Solving the Problems

[0006] The invention according to claim 1 is a vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component. The raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and as the target component is separated from the raw material by distillation, the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes performing, in an airtight depressurizable tank, (A) a step of heating and maintaining the raw material to 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 while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling it at the target distillation temperature and distilling at a constant temperature For the steps (B) and (C), in an environment where the ambient temperature is lower than the target distillation temperature, compare the vapor temperature with the raw material temperature. Utilize the phenomenon that if it boils, the vapor temperature and the raw material temperature become equal, and if boiling stops, the vapor temperature becomes lower than the raw material temperature. relates to a vacuum distillation method.

[0008] Claim 2The invention according to uses, with regard to the reduced pressure in the step (B), first, the gas-liquid equilibrium surface represented by a mixing system of a target component and a solvent component that mixes with the target component, which is determined by temperature, concentration, and pressure. When (a) the concentration (or content) of the target component in the raw material is unknown, the target distillation temperature 、 and At the target distillation temperature reduce the pressure rapidly while heating and maintaining up to the target distillation temperature according to the conditions of (a) or (b) from the concentration of the target component in the raw material to the saturation vapor pressure determined by the gas-liquid equilibrium surface, where the saturation vapor pressure is up to the maximum saturation vapor pressure of the target component. This relates to the reduced-pressure distillation method according to claim 1.

[0009] Claim 3 The invention according to A vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component. The raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases. As the target component is separated from the raw material by distillation, the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes, in an airtight depressurizable tank, (A) a step of heating and maintaining the raw material to 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. While capturing the saturated vapor pressure of the raw material that changes with time by distillation, it is boiled at the target distillation temperature and distilled at a constant temperature. with regard to the reduced pressure in the step (B), uses the value of the slope of the saturation vapor pressure with respect to the concentration of the target component on the gas-liquid equilibrium surface represented by a mixing system of a target component and a solvent component that mixes with the target component, which is determined by the raw material temperature and the tank internal pressure, to reduce the pressure at a rate. The value of the slope of the saturation vapor pressure with respect to the concentration of the target component is

[0010]

Number

[0011] Claim 4 The invention according to uses, with regard to the reduced pressure in the step (B), first, the gas-liquid equilibrium surface represented by a mixing system of a target component and a solvent component that mixes with the target component, which is determined by temperature, concentration, and pressure. When (a) the concentration (or content) of the target component in the raw material is unknown, the target distillation temperature 、 and At the target distillation temperature From the concentration of the target component at which the saturated vapor pressure is maximum to the saturated vapor pressure determined on the vapor-liquid equilibrium surface, (b) when the concentration (or content) of the target component in the raw material is known, from the target distillation temperature and the concentration of the target component to the saturated vapor pressure determined on the vapor-liquid equilibrium surface, in accordance with the conditions of (a) or (b), while heating and maintaining to the target distillation temperature, rapidly reduce the pressure. Next, for the subsequent pressure reductions, reduce the pressure at a rate using the value of the slope of the saturated vapor pressure with respect to the concentration of the target component on the vapor-liquid equilibrium surface determined by the raw material temperature and the tank internal pressure. The value of the slope of the saturated vapor pressure with respect to the concentration of the target component is

[0012] [Number] It relates to the vacuum distillation method according to claim 1.

[0013] Claim 5 The invention according to relates to a vacuum distillation method in which, for the pressure reduction in the step (B), in order to perform distillation at a more stable temperature, in an environment where the ambient temperature is lower than the target distillation temperature, when all of (1) to (3) described in the following condition 1 are satisfied, the pressure is reduced. (1) Not in boiling, or

[0014] [Number] being that, and (2) the absolute value of the difference between the target and actual tank internal pressures is within the range of the set pressure difference ΔP E in a certain time t E and (3)

[0015] [Number] being that. Here, the condition for detecting boiling in (1) is (4) described in the following condition 2, and (4) the boiling detection is

[0016] [Number] being, is, according to any one of claims 1 to 4 relates to the vacuum distillation method described in any one of them.

[0017] Claim 6 The invention according to relates to A vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component. The raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases. As the target component is separated from the raw material by distillation, the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes, in an airtight depressurizable tank, (A) a step of heating and maintaining the raw material to 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. While capturing the saturated vapor pressure of the raw material that changes with time by distillation, it is boiled at the target distillation temperature and distilled at a constant temperature. a step of obtaining the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the tank by means of the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component from the raw material temperature and the tank internal pressure during boiling in the distillation. , reduction relates to a pressure distillation method.

[0018] Claim 7 The invention according to further includes a step of estimating the mass concentration of the target component in the raw material and / or distillate from the liquid-phase mole fraction and / or gas-phase mole 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. 6 relates to the vacuum distillation method described in.

[0019] Claim 8 The invention according to relates to A vacuum distillation method for recovering a target component by distilling or extracting a raw material containing the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes, in an airtight depressurizable tank: (A) a step of heating and maintaining the raw material to a 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. This includes performing the steps while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature. During the distillation, when changing the target distillation temperature, from the concentration of the target component determined before the change by means of the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component and the target distillation temperature after the change, the tank internal pressure is quickly changed to the saturated vapor pressure obtained from the vapor-liquid equilibrium surface, and the distillation is further continued. , de relates to a pressure distillation method.

[0020] Claim 9The invention according to claim 1 further includes a step of stopping the distillation when, in the case of a raw material containing a target component and a solvent component that mixes with the target component, during the distillation, the concentration of the target component obtained from the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component that mixes with the target component becomes 0, or the target tank internal pressure obtained from the vapor-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone.

[0021] Claim 10 The invention according to claim 1 is related to the vacuum distillation method according to claim 1, wherein the heating is performed by microwave irradiation, and depending on the difference between the raw material temperature and the target distillation temperature, the microwave irradiation is stopped, the microwave oscillation is started, the switching to pulse irradiation is performed, the switching to continuous irradiation is performed, the output of the microwave is decreased, or the output of the microwave is increased.

[0022] Claim 11 The invention according to claim 1 is related to the vacuum distillation method according to claim 1, wherein the raw material contains alcohol and the target component is alcohol.

[0023] Claim 12 The invention according to claim 1 is related to the vacuum distillation method according to claim 1, wherein the raw material contains ethanol and the target component is ethanol.

[0024] Claim 13The invention according to claim 1 is a microwave extraction device used in the vacuum distillation method described in claim 1. The extraction device includes a tank for accommodating raw materials, a microwave generator for generating microwaves, waveguide means and 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 air release valve for adjusting the pressure in the tank, a cooling condenser or a 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. It relates to a microwave extraction device.

[0025] Claim 14 The invention according to claim has a function of obtaining the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the tank from the raw material temperature and the pressure in the tank by the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component during boiling in the distillation. When there is a scale capable of measuring the mass of the raw materials and / or the distillate, it has a function of estimating the mass concentration of the target component in the raw materials and / or the distillate from the liquid-phase mole fraction and / or the gas-phase mole fraction of the target component and the mass of the raw materials and / or the distillate. 13 It relates to the microwave extraction device described in claim

[0026] Claim 15 The invention according to claim has a function that when changing the target distillation temperature during the distillation, the pressure in the tank is quickly changed from the concentration of the target component obtained before the change by the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component to the saturated vapor pressure obtained from the vapor-liquid equilibrium surface based on the target distillation temperature after the change, so that the distillation can be continued. 13 It relates to the microwave extraction device described in claim

[0027] Claim 16The invention according to claim 13 relates to a microwave extraction device as described in claim

[0028] Claim 17 The invention according to claim 13 relates to a microwave extraction device as described in claim

[0029] Claim 18 The invention according to claim 13 relates to a microwave extraction device as described in claim

[0030] Claim 19 The invention according to claim 13 relates to a microwave extraction device as described in claim

Advantages of the Invention

[0031] According to the invention of claim 1, a vacuum distillation method for recovering a target component by distilling or extracting a raw material containing the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes, in an airtight depressurizable tank, (A) a step of heating and maintaining the raw material to a 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. While capturing the saturated vapor pressure of the raw material that changes with time by distillation, it boils at the target distillation temperature and distills at a constant temperature. It is characterized in that it is a vacuum distillation method. Therefore, in the distillation (extraction) process, the target component contained in the raw material can be recovered by depressurizing and distilling or extracting at the set distillation set temperature regardless of the concentration (or content) of the target component in the raw material that continuously changes with the passage of time. A method for distilling or extracting a raw material containing an arbitrary target component concentration or content at an arbitrary temperature (target distillation temperature) can be provided. Also, Regarding the above steps (B) and (C), in an environment where the ambient temperature is lower than the target distillation temperature, the vapor temperature and the raw material temperature are compared. When boiling occurs, the vapor temperature and the raw material temperature become equal, and when boiling stops, the vapor temperature becomes lower than the raw material temperature. Utilizing this phenomenon, the vacuum distillation method according to claim 1 is characterized in that by comparing the vapor temperature and the raw material temperature in an environment where the ambient temperature is lower than the target distillation temperature, the boiling of the raw material is automatically detected, and by automatically controlling the pressure applied to the raw material according to the presence or absence of boiling, a method for distilling or extracting a raw material containing an arbitrary target component concentration or content at an arbitrary temperature (target distillation temperature) can be provided.

[0033] Claim 2 According to the invention related thereto, regarding the pressure reduction in the step (B), first, using the gas-liquid equilibrium surface represented by a mixing system of the target component and a solvent component that mixes with the target component, which 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 At the target distillation temperature From the concentration of the target component at which the saturated vapor pressure is maximum to the saturated vapor pressure determined on the vapor-liquid equilibrium surface, (b) when the concentration (or content) of the target component in the raw material is known, from the target distillation temperature and the concentration of the target component to the saturated vapor pressure determined on the vapor-liquid equilibrium surface, heating and maintaining to the target distillation temperature in accordance with the condition of (a) or (b) and then rapidly reducing the pressure. According to the vacuum distillation method described in claim 1, regardless of whether the concentration (or content) of the target component is unknown or known, by rapidly reducing the pressure all at once to the saturated vapor pressure that can be read from the vapor-liquid equilibrium surface for the target component first, the time required to detect the initial boiling of the raw material can be shortened, so the total operation time in the method for distilling or extracting the raw material of the present invention can be shortened.

[0034] Claim 3 According to the invention according to A vacuum distillation method for recovering a target component by distilling or extracting a raw material containing the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes, in an airtight depressurizable tank: (A) a step of heating and maintaining the raw material to a 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. This includes performing the steps while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature. Regarding the pressure reduction in the step (B), at a rate using the value of the slope of the saturated vapor pressure with respect to the concentration of the target component on the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component, which is determined by the raw material temperature and the tank internal pressure. The value of the slope of the saturated vapor pressure with respect to the concentration of the target component is

[0035]

Number

[0036] Claim 4According to the invention according to claim 0, regarding the decompression in the step (B), first, using the vapor-liquid equilibrium surface represented by a mixing system of a target component and a solvent component to be mixed with the target component, which 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 At the target distillation temperature from the concentration of the target component at which the saturated vapor pressure is maximized to the saturated vapor pressure determined by the vapor-liquid equilibrium surface, (b) when the concentration (or content) of the target component in the raw material is known, from the target distillation temperature and the concentration of the target component to the saturated vapor pressure determined by the vapor-liquid equilibrium surface, in accordance with the conditions of (a) or (b), while heating and maintaining to the target distillation temperature, rapidly decompress, and then, regarding the decompression after the second time, decompress at a rate using the value of the slope of the saturated vapor pressure with respect to the concentration of the target component on the vapor-liquid equilibrium surface determined by the raw material temperature and the tank internal pressure. The value of the slope of the saturated vapor pressure with respect to the concentration of the target component is

[0037]

Number

[0038] Claim 5 According to the invention according to claim 19, regarding the decompression in the step (B), in order to perform distillation at a more stable temperature, in an environment where the ambient temperature is lower than the target distillation temperature, it is a vacuum distillation method in which decompression is performed when all of (1) to (3) described in condition 1 below are satisfied. (1) Not boiling, or

[0039]

Number

[0040]

Number

[0041]

Number

[0042] Claim 6 According to the invention according to A vacuum distillation method for distilling or extracting a raw material containing a target component to recover the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes performing, in an airtight and depressurizable tank, (A) a step of heating and maintaining the raw material to a 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, while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature. at the time of boiling in the distillation, from the raw material temperature and the tank internal pressure, a step of obtaining the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the tank by means of the vapor-liquid equilibrium surface represented in the mixing system of the target component and the solvent component mixed with the target component is included , reduction a pressure distillation method, characterized in that the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the constantly changing raw material after the raw material has boiled are calculated and can be grasped by the user in real time.

[0043] Claim 7 According to the invention according to, when the mass of the raw material and / or the distillate can be measured, a step of further estimating the mass concentration of the target component in the raw material and / or the distillate from the liquid-phase mole fraction and / or the gas-phase mole fraction of the target component and the mass of the raw material and / or the distillate is further included, claim 6Since it is a vacuum distillation method described in [reference], in the process of producing a distillate, the user can grasp in real time whether the obtained distillate or the raw material (residue) after the distillate is removed has the target quality (for example, whether it has the target mass concentration). From the estimated calculation of the target component remaining in the raw material, it becomes easier to predict the end time of distillation and the remaining recovery amount of the distillate.

[0044] Claim 8 According to the invention according to [reference], A vacuum distillation method for distilling or extracting a raw material containing a target component to recover the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes performing, in an airtight and depressurizable tank, (A) a step of heating and maintaining the raw material to a 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, while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature. During the distillation, when changing the target distillation temperature, the tank internal pressure is quickly changed from the concentration of the target component determined before the change by the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component to the saturation vapor pressure obtained from the vapor-liquid equilibrium surface at the target distillation temperature after the change, and the process further includes continuing the distillation. , reduction Since it is a pressure distillation method, the user of the present invention can further distill or extract the raw material at an arbitrary temperature (target distillation temperature). For example, for the purpose of sterilization, the raw material is heated at the start of operation (for example, at 80°C), and then the distillation set temperature is changed to perform distillation or extraction, or for the same purpose of sterilization, heating is performed as the last step in the distillation or extraction process (for example, heating the raw material at 80°C). Such modes are possible.

[0045] Claim 9According to the invention according to claim 1, in the case of a raw material containing a target component and a solvent component that mixes with the target component, during the distillation, the concentration of the target component obtained from the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component that mixes with the target component becomes 0, or the state where the target tank internal pressure obtained from the vapor-liquid equilibrium surface becomes equal to the saturated vapor pressure of the solvent component alone can be detected. When the concentration of the target component becomes 0, or when the target tank internal pressure becomes equal to the saturated vapor pressure of the solvent component alone, a step of stopping the distillation is further included. Since the present invention is not continued in a state where 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 being diluted (for example, by an increase in the amount of components other than the solvent component and the target component), the quality of the distillate (the concentration of the target component contained in the distillate) can be maintained at the target quality (concentration).

[0046] Claim 10 According to the invention according to claim 1, the heating is performed by microwave irradiation, and depending on the difference between the raw material temperature and the target distillation temperature, the microwave irradiation is stopped, the microwave oscillation is started, the switching to pulsed irradiation, the switching to continuous irradiation, the reduction of the microwave output, or the increase of the microwave output is performed. Since it is a vacuum distillation method according to claim 1, by controlling the raw material temperature during vacuum by microwave irradiation, it is possible to maintain the quality of the distillate (the concentration of the target component contained in the distillate) at the target quality (concentration), and it is possible to provide a method for distilling or extracting the raw material.

[0047] Claim 11 According to the invention according to claim 1, the raw material contains alcohol and the target component is alcohol. Since it is a vacuum distillation method according to claim 1, by specifying the target component as alcohol, it is possible to provide a method for removing the organic solvent contained in the raw material and for distilling or extracting a raw material containing alcohol at an arbitrary concentration at an arbitrary temperature when manufacturing distilled liquor.

[0048] Claim 12According to the invention according to claim 1, the raw material contains ethanol and the target component is ethanol. By specifying the target component as ethanol, it is possible to provide a method for distilling or extracting a raw material containing ethanol at an arbitrary concentration at an arbitrary temperature in the production of distilled spirits.

[0049] Claim 13 According to the invention according to claim 1, a microwave extraction device used in the vacuum distillation method according to claim 1, the extraction device comprising: a tank for accommodating the raw material; a microwave generator for generating microwaves; waveguide means and microwave transmission means for guiding the microwaves to the tank; a stirring device for stirring the raw material accommodated in the tank; a vacuum pump for adjusting the pressure in the tank; an air release valve for adjusting the pressure in the tank; a cooling condenser or a cooling device for cooling and condensing the vapor of the raw material 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 a sensor for measuring the pressure in the tank, the raw material temperature, and the vapor temperature. Therefore, it is possible to provide a microwave extraction device for performing a method of distilling or extracting a raw material containing an arbitrary target component concentration at an arbitrary temperature.

[0050] Claim 14 According to the invention according to claim 1, at the time of boiling in the distillation, from the raw material temperature and the pressure in the tank, a function of obtaining the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the tank by means of the vapor-liquid equilibrium surface represented in the mixing system of the target component and the solvent component mixed with the target component. If there is a scale capable of measuring the mass of the raw material and / or the distillate, it has a function of estimating the mass concentration of the target component in the raw material and / or the distillate from the liquid-phase mole fraction and / or the gas-phase mole fraction of the target component and the mass of the raw material and / or the distillate. Claim 13Since it is characterized by being the microwave extraction device described in [reference], 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 that is constantly changing after the raw material boils, the distillate obtained, whether the raw material (residue) after the distillate is removed has the target quality (for example, whether it has the target mass concentration), and the estimated end time of distillation and the remaining estimated recovery amount of the distillate by estimating the content of the target component remaining in the raw material.

[0051] Claim 15 According to the invention according to [claim], when changing the target distillation temperature during the distillation, the concentration of the target component previously determined before the change and the target distillation temperature after the change are used based on the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component. The pressure inside the tank is quickly changed to the saturated vapor pressure obtained from the vapor-liquid equilibrium surface, and it has the function of being able to continue the distillation. Claim 13 Since it is characterized by being the microwave extraction device described in [reference], the user of the present invention can further distill or extract the raw material at an arbitrary temperature (target distillation temperature). For example, for the purpose of sterilization, the raw material is heated at the start of operation (for example, at 80°C), and then the distillation set temperature is changed to perform distillation or extraction. Or for the same purpose of sterilization, it is possible to heat as the last step in the distillation or extraction process (for example, heat the raw material at 80°C).

[0052] Claim 16 According to the invention according to [claim], in the case of a raw material containing a target component and a solvent component mixed with the target component, during the distillation, the state where the concentration of the target component obtained from the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component becomes 0, or the state where the target pressure inside the tank obtained from the vapor-liquid equilibrium surface is equal to the saturated vapor pressure of the solvent component alone can be detected. When the concentration of the target component becomes 0, or when the target pressure inside the tank is equal to the saturated vapor pressure of the solvent component alone, it has the function of stopping the distillation. Claim 13Since it is characterized by being the microwave extraction device described in [reference], the present invention will not continue in a state where 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 decreasing (for example, due to an increase in the amount of components other than the solvent component and the target component). Therefore, the quality of the distillate (the concentration of the target component contained in the distillate) can be maintained at the target quality (concentration), and cost reduction can be achieved by not operating the device more than necessary.

[0053] Claim 17 According to the invention according to [claim], the heating is performed by microwave irradiation, and depending on the difference between the raw material temperature and the target distillation temperature, stopping of microwave irradiation, oscillation of microwaves, switching to pulse irradiation, switching to continuous irradiation, decreasing the output of microwaves, or increasing the output of microwaves is performed. Claim 13 Since it is characterized by being the microwave extraction device described in [claim], 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 the target quality (concentration) by controlling the temperature of the raw material under reduced pressure by microwave irradiation.

[0054] Claim 18 According to the invention according to [claim], the raw material contains alcohol and the target component is alcohol. Claim 13 Since it is characterized by being the microwave extraction device described in [claim], by specifying the target component as alcohol, it is possible to provide a microwave extraction device that removes the organic solvent contained in the raw material and distills or extracts a raw material containing alcohol at an arbitrary concentration at an arbitrary temperature in the production of distilled liquor.

[0055] Claim 19 According to the invention according to [claim], the raw material contains ethanol and the target component is ethanol. Claim 13 Since it is characterized by being the microwave extraction device described in [claim], by specifying the target component as ethanol, it is possible to provide a microwave extraction device that distills or extracts a raw material containing ethanol at an arbitrary concentration at an arbitrary temperature in the production of distilled liquor.

Brief Description of the Drawings

[0056]

Figure 1

Figure 2-1

Figure 2-2

Figure 3

Figure 4

Figure 5

Figure 6

Modes for Carrying Out the Invention

[0057] Hereinafter, embodiments of the method for distilling or extracting raw materials 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, in the conventional distillation or extraction method, there are problems such as difficulty in controlling distillation (extraction) at a constant temperature, the operating time required for the distillation or extraction process can be long, bumping may occur in the raw material due to excessive vacuum, and distillation or extraction of the raw material may not occur due to insufficient vacuum. These are cited as technical problems.

[0059] Conventional microwave extraction devices can only distill (extract) in two cases where the distillation temperature is 40°C and 60°C, which are set based on pre-measured distillation test data (a microwave extraction device with a raw material input of 25 kg and a total microwave output of 6 kW) when producing distilled spirits from a raw material with an alcohol (ethanol) concentration of 35 degrees. That is, it can only distill at fixed temperatures and concentrations. Therefore, when there are variations in the concentration of the target component (here, alcohol (ethanol)) contained in the raw material, the concentration change from the start to the end of distillation may differ from the test data, resulting in insufficient vacuum reduction to cause the raw material to boil, and thus distillation or extraction may not occur. In addition, there is a need for a highly versatile distillation (extraction) method that can distill or extract any target component aimed at by the user of the present invention at an arbitrary temperature while maintaining the quality of the recovered product or the raw material (residue) after the target component has been removed.

[0060] To solve the technical problem, the present invention provides a method for distilling or extracting a raw material, which recovers the target component contained in the raw material by performing distillation or extraction under reduced pressure at a set distillation set temperature, regardless of whether the concentration of the target component is known and regardless of the concentration of the target component in the raw material that continuously changes over time during the distillation (extraction) process. Specifically, the present invention utilizes the physical phenomenon that during distillation, the vapor temperature and the raw material temperature are compared in real time. If it is boiling, the vapor temperature is equal to the raw material temperature; if it is not boiling, the vapor temperature is lower than the raw material temperature. By detecting the presence or absence of boiling and gradually reducing the pressure when it is not boiling, the pressure is controlled to find the boiling point (concentration). Also, the heating mechanism is adjusted to control the temperature so that the raw material temperature becomes equal to the temperature to be distilled (distillation set temperature). By these methods, alcohol distillation control at arbitrary concentrations and temperatures is provided.

[0061] Here, when the raw material is not boiling, the steam temperature is likely to affect the ambient temperature of the distillation or extraction device according to the present invention. Since the steam temperature is lower than the raw material temperature, if the distillation set temperature is lower than the ambient temperature, it should be noted that the present invention cannot be applied (for example, distillation set temperature 35°C, ambient temperature 40°C). This is due to the fact that, regarding the distillation (extraction) device according to the present invention, the steam 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 "ambient temperature" mentioned here refers to the ambient temperature when using the distillation or extraction method according to the present invention, or the ambient temperature of the device for using those methods. If it is indoors, it may also be referred to as the indoor temperature, and if it is outdoors, it may be referred to as the outdoor temperature. For example, if the device according to the present invention exists indoors, the user can control that temperature (ambient temperature) using air conditioning equipment. Also here, when "gradually reducing the pressure" (gradually depressurizing), since the degree is not clear, it should be noted that it depends on the operator's decision. For example, if the depressurization process is carried out at a very slow speed, the accurate saturated vapor pressure can be captured, but it takes time. Conversely, if the pressure is reduced at a fast speed, it will be below the saturated vapor pressure, and there is a possibility of bumping in the raw material. Also here, in order to explain the outline of the x - y curve and the vapor - liquid equilibrium curve represented by the target component and the solvent component, the x - y curve and the vapor - liquid equilibrium curve with ethanol as the target component and water as the solvent component are shown in FIG. 6. The boiling point of the ethanol solution (see FIG. 6) is lower the higher the concentration of ethanol (however, there is a region where it reverses at high concentrations of about 0.9 mole fraction or more (about 97 degrees or more in alcohol (ethanol) proof)). Also, the boiling point of the ethanol solution is lower than that of water, and the saturated vapor pressure is higher.

[0062] The vapor-liquid equilibrium surface is a surface determined by three variables: temperature, pressure, and the concentration of the target component (e.g., ethanol concentration, which can be represented in terms of liquid-phase mole fraction or mol%, etc., and other modes that can be converted to these modes, such as the content of the target component contained in the raw material, are not particularly limited). It is formed by arranging the vapor-liquid equilibrium curves (see Figure 6) of pressure and concentration at a certain temperature for a mixing system of the target component (e.g., ethanol) and the solvent component (e.g., water) that mixes with the target component for each temperature. When expressing the concentration in terms of liquid-phase mole fraction, there is a mode of expressing it using the amount of substance (mol) with the first component as the target component and the amount of substance (mol) with the second component as the solvent component. For example, when distilling a raw material with an unknown ethanol concentration (or ethanol content), under the condition that the boiling point of ethanol is low, since the saturated vapor pressure is the highest when the concentration is the highest (here, the concentration of the ethanol solution is 90 mol%), if the distillation set temperature is determined, the pressure can be rapidly reduced to the saturated vapor pressure determined by the vapor-liquid equilibrium surface (the pressure at which boiling will definitely not occur), and by starting the pressure control to find the boiling point from there, the operation time can be shortened. If the ethanol concentration (or ethanol content) of the raw material is known, when the distillation set temperature is determined, the saturated vapor pressure is determined from the vapor-liquid equilibrium surface, so the pressure can also be rapidly reduced to that pressure. Also, after rapidly reducing the pressure, while searching for the boiling point (concentration), the pressure is gradually reduced. By using the value of the slope of the vapor-liquid equilibrium surface determined from the current pressure and raw material temperature (the differential value of the pressure curve with respect to the concentration [ΔkPa / Δ concentration of the target component (e.g., represented by liquid-phase mole fraction or mol%)]), the pressure can be gradually reduced with an appropriate reduction width corresponding to the concentration. Here, "Δ" represents the change amount of physical quantities such as "pressure" and "concentration" of the target component according to the present invention. In the present invention, when using the value of this slope, it is preferable to use the following formula (rate).

[0063]

Equation

[0064] Furthermore, in the conventional technology, it was difficult to grasp in real time the concentration of the target component contained in the distillate (extract) after vacuum distillation during the distillation (extraction) process. However, by constantly measuring the weight of the distillate (extract) and detecting the boiling of the raw material, the weight deviation [g / sec] of the distillate (extract) and the weight deviation [g / sec] of the target component are calculated from the liquid-vapor curve (x-y curve) (see Figure 6) of the target component obtained from the vapor-liquid equilibrium curve. By integrating this over time, a function is provided 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)). When calculating this mass concentration, if the target component is ethanol, the alcohol (ethanol) content of the distillate is also calculated simultaneously from the calculated mass concentration in wt% units. Here, since the vapor-liquid equilibrium surface used in the present invention is represented by using the vapor-liquid equilibrium curves at each temperature of the raw material, by using the liquid-vapor curves (x-y curves) at each temperature obtained from the vapor-liquid equilibrium curves at each temperature, a three-dimensional liquid-vapor surface (x-y surface) (see Figure 6) can be represented. Furthermore, if the weight of the input raw material, i.e., the weight of the liquid mixture (the sum of the target component and the solvent component), is known, subtracting the weight of the recovered distillate (extract) allows us to determine the weight of the liquid mixture contained in the raw material during distillation (extraction). Thus, a function is provided to calculate the concentration of the target component in the raw material during distillation (extraction) (e.g., the mass concentration of the target component with respect to the target component and the solvent component in the raw material (wt% = kg of target component / (kg of target component + kg of solvent component) × 100)) from the liquid-phase mole 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 simultaneously calculated from the calculated mass concentration in wt% units. For example, in order to grasp the alcohol (ethanol) concentration (concentration of the target component) of the distilled liquor (distillate) being vacuum-distilled in real time during the distillation (extraction) process, the weight of the distilled liquor (distillate) is constantly measured, and by detecting the boiling of the raw material, the ethanol weight deviation [g / sec] is calculated from the weight deviation [g / sec] of the distilled liquor and the gas-phase mole fraction from the liquid-phase - gas-phase curve (x - y curve) (see Figure 6) obtained from the vapor-liquid equilibrium curve. By integrating this over time, the estimated concentration of the distilled liquor and the alcohol (ethanol) content during distillation can be calculated. Here, since the ethanol - water vapor-liquid equilibrium surface used in this example is represented by the ethanol - water vapor-liquid equilibrium curves at each temperature of the raw material, by using the ethanol - water liquid-phase - gas-phase curves (x - y curves) at each temperature obtained from the ethanol - water vapor-liquid equilibrium curves at each temperature, the three-dimensional ethanol - water liquid-phase - gas-phase surface (x - y surface) (see Figure 6) can be represented. Also, if the weight of the ethanol solution of the input raw material (the sum of ethanol and water) is known, subtracting the weight of the recovered distilled liquor (distillate) allows us to estimate the weight of the ethanol solution of the raw material during distillation, and from this and the liquid-phase mole fraction, the alcohol (ethanol) concentration (concentration of the target component or alcohol (ethanol) content) of the raw material during distillation can also be calculated. Here, the weight deviation [g / sec] divides g by sec (seconds), but g and sec can be arbitrarily set by the user as long as they represent weight and time units respectively.

[0065] In addition, by comparing the steam temperature and the raw material temperature in real time as described above, and gradually reducing the pressure when not boiling to search for the boiling point (concentration) and performing pressure control, and performing temperature control by controlling the heating mechanism so that the raw material temperature becomes equal to the distillation set temperature, a function of providing distillation control of a target component (e.g., alcohol (ethanol)) at any concentration and temperature is provided. (2) By utilizing the vapor-liquid equilibrium surface of the target component-solvent component and performing efficient and appropriate pressure control, a function of shortening the operation time and providing stable distillation control without bumping is provided. And (3) by utilizing the x-y curve of the target component and constantly measuring the weight of the distillate (extract), a function of calculating the estimated concentration of the target component contained in the distillate (extract) and the raw material is provided, so that according to the concentration of the target component contained in the distillate (extract) being vacuum-distilled and the concentration of the target component contained in the raw material (e.g., liquid-phase mole fraction), a function of enabling automatic stop of the operating distillation (extraction) apparatus is provided. For example, in the prior art, since the concentration of the distilled liquor during vacuum distillation and the concentration of ethanol contained in the raw material (e.g., liquid-phase mole fraction) were unknown, the apparatus could not be automatically stopped according to the concentration of the distilled liquor and the concentration of ethanol contained in the raw material, but the present invention enables this.

[0066] Finally, in the prior art, in order to maintain the quality of the distillate and the residue, the operator could not make a judgment to easily change the distillation set temperature during vacuum distillation, but by utilizing the vapor-liquid equilibrium surface, a function of enabling this is provided. For example, when reducing the pressure of a raw material with an unknown concentration of the target component for boiling detection, the concentration at that time can be obtained from the vapor-liquid equilibrium surface based on the pressure at the time of changing the distillation set temperature and the distillation set temperature before the change. Therefore, once the concentration at the time of changing the distillation set temperature is memorized, the pressure is controlled by changing the pressure from that concentration to the saturated vapor pressure obtained from the distillation set temperature after the change. As a result, when searching for the boiling conditions of a raw material with an unknown concentration of the target component, even if the distillation set temperature is changed during distillation, the process of searching for the boiling conditions up to that point is memorized, so it becomes possible to change the distillation set temperature during distillation. When the concentration of the target component in the raw material is known, the set pressure is changed from the changed distillation set temperature to the saturated vapor pressure obtained through the vapor-liquid equilibrium surface based on the concentration of the target component, and the pressure is controlled. When boiling has already been detected and the concentration of the raw material (for example, liquid-phase mole fraction) is known, when the distillation set temperature is changed, the set pressure is changed from the distillation set temperature after the change and the concentration of the target component (for example, liquid-phase mole fraction) to the saturated vapor pressure obtained through the vapor-liquid equilibrium surface, and the pressure is controlled. However, when changing from a high distillation set temperature to a low distillation set temperature, there is a possibility of bumping, so it should be noted that the set value needs to be gradually decreased. A suitable example of changing the distillation set temperature during distillation (extraction) is, for example, when the purpose is sterilization. The distillation set temperature can be set to a high temperature (for example, 80 °C) once to raise the temperature of the raw material (target component) to sterilize the raw material, and then the distillation set temperature can be reset to a low temperature to start distillation or extraction.

[0067] Summarizing the functions provided by the present invention, it is as follows. (1) By comparing the vapor temperature and the raw material temperature in real time, when not boiling, gradually reducing the pressure to search for the boiling point (concentration) and controlling the pressure, and controlling the heating mechanism so that the raw material temperature becomes equal to the distillation set temperature to perform temperature control, a function of providing distillation control of the target component (for example, alcohol (ethanol)) at an arbitrary concentration and temperature (2) By utilizing the vapor-liquid equilibrium surface of the target component - solvent component and performing efficient and appropriate pressure control, it provides a function to shorten the operation time and offer stable distillation control without bumping. (3) By utilizing the x-y curve of the target component and constantly measuring the weight of the distillate (extract), it calculates the estimated concentrations of the target component contained in the distillate (extract) and the raw material. (4) By utilizing the technologies of (1) to (3), it provides a function to automatically stop the device according to the concentration of the target component. (5) By utilizing the vapor-liquid equilibrium surface of the target component (for example, ethanol), it provides a function to change the distillation set temperature even during the operation of the distillation (extraction) device.

[0068] The vapor-liquid equilibrium surface may be created by approximating and calculating a data range that does not exist by using a plurality of existing vapor-liquid equilibrium curves and then estimating. For example, when there are data of the vapor-liquid equilibrium curves of ethanol-water at 30 °C, 40 °C, and 50 °C, the data of the vapor-liquid equilibrium curves from 31 °C to 39 °C and from 41 °C to 49 °C can use the data estimated by connecting the saturated vapor pressure values at each concentration existing within the vapor-liquid equilibrium curves of 30 °C and 40 °C, and 40 °C and 50 °C with an approximate curve. By using this estimated data, the vapor-liquid equilibrium surface can be created. The calculation for this estimation may be performed using software that is already known. Furthermore, although the present invention assumes using the vapor-liquid equilibrium surface of a two-component system of the target component and the solvent component (for example, ethanol and water), it is possible to perform distillation (extraction) of the raw material by using the vapor-liquid equilibrium curve of a one-component system (for example, water alone) (for example, in the case of water alone, it is synonymous with drying the raw material).

[0069] In the present invention, the user can arbitrarily change the setting of the operation time and the amount of distillate to be recovered during vacuum distillation. Therefore, the present invention can provide a method for distilling or extracting raw materials with a higher degree of freedom. For example, since the user can change the operation time or the distillation amount at any timing from the start to the end of the present invention, the operability of the present invention is improved. Since the setting of the operation time or the setting of the distillation amount to be recovered can be changed at any timing from the start to the end of the present invention, a plurality of setting changes can be made simultaneously or at different times as necessary.

[0070] Hereinafter, embodiments of the method for distilling or extracting raw materials 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 vacuum distillation apparatus (1) requires a heating mechanism, a decompression mechanism, a cooling mechanism, and sensors and a control device for controlling these mechanisms in order to distill or extract the raw material (M). For example, in the case of a microwave extraction apparatus, the heating mechanism includes a microwave generator (2) and a microwave transmission material (3), the decompression mechanism includes a tank (T), a vacuum pump (4), and an air release valve (5), the cooling mechanism includes a cooling condenser (6) and a cooling device (7) such as a chiller, the sensors include a tank internal pressure sensor (8), a vapor temperature sensor (9), and a raw material temperature sensor (12) (or a tank side surface temperature sensor), and the control device is a control panel (10) equipped with a PLC and a touch panel.

[0072] The tank (T) is a container for storing the raw material (M), and is provided with a stirring device for stirring the raw material (M). The stirring device in the present invention is composed of a stirring 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. The stirring blade (11) rotates around a vertical axis by driving the motor (15). The tank (T) is for processing the raw material (M) inside it, and examples of its shape include a rectangular parallelepiped and a cylindrical shape, but it is not particularly limited. The motor (15) is controlled by the control panel (10) such that its rotating shaft can be rotated in the forward direction, reverse direction, or both the forward and reverse directions regularly or irregularly. As a result, the stirring blade (11) can rotate forward and reverse inside the tank.

[0073] At the bottom of the tank (T), a waveguide tube (13) for waveguide means for guiding the microwave generated by the microwave generator (2) into the tank (T) is connected. The number of waveguide tubes (13) may be one, but it is preferable to connect a plurality of them at a plurality of locations sandwiching the center of the bottom of the tank, because it becomes possible to irradiate the raw material (M) inside the tank (T) with microwaves evenly. When a plurality of waveguide tubes (13) are provided, the microwave generator (2) may be connected to each waveguide tube (13), or a plurality of waveguide tubes (13) may be branched from one microwave generator (2).

[0074] The material of the tank (T) is not limited to a specific one, but for example, stainless steel or the like is preferably adopted from the viewpoint of corrosion resistance. Also, the capacity of the tank (T) is not limited, but for example, 15L, 100L, 150L, 400L can be adopted. The tank (T) can be provided with a scale (or weighing meter) for measuring the mass of the raw material (M), and the user of the present invention can measure the weight of the raw material (M) in real time and grasp the situation. Note that the mass of the raw material (M) may be a value obtained by measuring in advance before being charged into the tank (T).

[0075] At the bottom of the tank (T), a microwave irradiation unit for irradiating the inside of the tank (T) with microwaves is provided. The configuration of the microwave irradiation unit 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. For example, the microwave irradiation unit includes a microwave generator (2) that generates microwaves and a waveguide tube (13) that guides the microwaves generated by the microwave generator (2) into the tank (T).

[0076] The number of microwave generators (2) is preferably a plurality, respectively, so as to be able to irradiate the raw material (M) in the tank (T) with microwaves evenly.

[0077] As the microwave generator (2), a magnetron is preferably used. However, depending on the raw material (M) and the like, other known microwave generators such as an oscillator using an electron tube such as a gyrotron, a klystron, or a traveling wave tube, or a solid-state oscillator that amplifies the natural vibration such as a crystal oscillator can also be used.

[0078] The tank (T) is provided with a microwave transmission material (3) for a microwave transmission means that transmits microwaves at the connection portion of the waveguide (13). The microwave transmission material (3) is formed of a dielectric through which microwaves can pass (for example, resins such as PTFE, ceramics such as quartz and alumina, glasses, etc.). The microwaves introduced into the waveguide (13) pass through the microwave transmission material (3) and are guided into the tank (T), heating the raw material (M) in the tank (T). The microwave transmission material (3) has a frustoconical shape that becomes larger in diameter from the inner surface to the outer surface of the tank (T). At the bottom of the tank (T), a mounting hole having a frustoconical shape that becomes larger in diameter from the inner surface to the outer surface of the tank (T) is formed, and the microwave transmission material (3) is fitted into this mounting hole.

[0079] At the upper part and / or side surface part of the tank (T), a passage for taking out the vapor containing the component (target component) in the raw material (M) heated and evaporated in the tank (T) by microwave irradiation to the outside of the tank (T) and guiding it to the cooling condenser (6) is connected.

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

[0081] The cooling condenser (6) is not limited to either an air-cooling method or a water-cooling method, but the water-cooling method is preferable from the viewpoint of efficiency. As the refrigerant of the cooling condenser (6), water or an antifreeze can be used, and as the antifreeze, those mainly composed of alcohol or those mainly composed of ethylene glycol or the like can be used. Although not particularly limited, water is preferably used as the refrigerant because it is inexpensive. The cooling device (7) is not particularly limited in its aspect, but a chiller or the like is preferably used.

[0082] In the container (14), a liquid (for example, water) containing the target component, which becomes vapor by heating and liquefies by passing through the cooling condenser (6), accumulates. The upper part of the container (14) is connected to a vacuum pump (4) which is a decompression means via a pipe. When the vacuum pump (4) is driven, the inside of the tank (T) is decompressed through the pipe, the cooling condenser (6) and the passage. By taking advantage of the fact that the boiling point decreases by decompressing the inside of the tank (T), the raw material (M) can be distilled (extracted) at a low temperature.

[0083] The control device (control panel (10)) includes a storage medium in which a program for controlling an atmosphere release valve (5) for allowing or blocking the inflow of outside air into the tank (T) and adjusting the pressure inside the tank (T), a vacuum pump (4) configured to adjust the pressure inside the tank (T) (mainly for decompression), a microwave generator (2), and a stirring device for stirring the raw material (M) accommodated in the tank (T) is written. The atmosphere release valve (5) is not limited to a specific valve. However, in this embodiment, if the open state / closed state is distinguishable, correction is applied in that state to correct the deviation, and a program is provided to convert and control the opening degree based on the integrated time of the command. During the operation of the extraction device (1), this control device (control panel (10)) can arbitrarily change the rotation speed and direction of rotation of the stirring blade (11), the output of the vacuum pump (4), the outputs of the atmosphere release valve (5) and the microwave generator (2), oscillation / stop, pulse irradiation, and its oscillation time / stop time, according to the raw material temperature of the raw material (M) and / or the vapor temperature of the raw material (M).

[0084] The control device (control panel (10)) has a non-volatile memory (e.g., ROM) and a volatile memory (e.g., RAM) as the aforementioned storage medium, and the user can arbitrarily set a target value in advance and register or re-register it as a recipe. As a result, the user can devise or improve a recipe and independently develop a product on their own. What the user can register as a program in the recipe includes microwave output, oscillation / stop, pulse irradiation and its oscillation time / stop time, rotation speed of stirring, direction of rotation and its forward rotation time / reverse rotation time, distillation set temperature, etc., according to the operation elapsed time or the recovery amount (distillation amount). For the rotation speed and direction of rotation (forward rotation / reverse rotation) time of the stirring blade (11), the output of the microwave, the oscillation time / stop time of the pulse irradiation, and the distillation set temperature, not only Step control but also Ramp control settings can be registered. Also, regarding the pulsed irradiation of microwaves, when there are multiple microwave irradiation units, for example, four units numbered No.1 to No.4, it can be irradiated by shifting the pulse irradiation start timing for each (by setting offset values for each). For example, after oscillating No.1 and No.3 and stopping No.2 and No.4, it is also possible to stop No.1 and No.3, oscillate No.2 and No.4, and repeat alternately as follows. Or, after oscillating No.1 and stopping No.2 to No.4, then oscillate No.2 and stop No.1, No.3, and No.4, then oscillate No.3 and stop No.1, No.2, and No.4, and then oscillate No.4 and stop No.1 to No.3, and repeat in order as follows. If the start timing of the pulse irradiation is the same, it will be a pulse irradiation where No.1 to No.4 oscillate and stop simultaneously.

[0085] The control device (control panel (10)) has a function of controlling the rotation speed of the vacuum pump (4) by PID (proportional, integral, differential) control and controlling the opening and closing of the atmosphere release valve (5) by PD (proportional, differential) control in order to control the pressure in the tank (T) to the target value. In this embodiment, the rotation speed of the vacuum pump (4) is PID-controlled and the opening degree of the atmosphere release valve (5) is PD-controlled according to the pressure deviation. As the control device, for example, a PLC is preferably used, and a program that enables pressure control and temperature control is incorporated into this PLC. For example, in the case of the microwave extraction device (1), the pressure control is the PID control of the rotation speed of the vacuum pump (4) and / or the PD control of the opening degree of the atmosphere release valve (5), and the temperature control is the oscillation / stop, pulse irradiation, and output control of the microwave generator (2). Also, parameters corresponding to the gas-liquid equilibrium surface and the x-y curve (a surface on the program) are incorporated. This parameter may be a value obtained from experimental values, or a value obtained from theoretical values such as Wilson constants or Atwone constants, or the theoretical formula itself. In the case of the gas-liquid equilibrium surface, it may also be created by using a plurality of existing gas-liquid equilibrium curves to complement and estimate a data range that does not exist.

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

[0087] The control device (control panel (10)) has a function of Step control and a function of Ramp control. Step control controls the rotation speed and rotation direction (forward / backward rotation) of the stirring blade (11) and its time, the output of the microwave for heating the raw material (M), the oscillation / stop of the microwave, pulse irradiation, and its oscillation / stop by ON / OFF operation. Ramp control controls the rotation speed and rotation direction (forward / backward rotation) time of the stirring blade (11), the output of the microwave for heating the raw material (M) in the tank (T), the oscillation time / stop time of pulse irradiation, and the change of the distillation set temperature. By performing Ramp control, for example, while the target component is being distilled (extracted) from the raw material (M) and / or while the temperature is rising, the rotation speed of the stirring blade (11), the rotation direction (forward / backward rotation) time, the output of the microwave, and the oscillation time / stop time of pulse irradiation can be gradually changed. That is, compared with the case where it cannot be gradually changed, finer stirring is possible, and since the microwave can be efficiently irradiated, the distillation (extraction) time can be shortened.

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

[0089] The vapor temperature sensor (9) is a sensor that detects the temperature of the vapor generated from the raw material (M) and measures that temperature. The raw material temperature sensor (12) is a sensor that detects the raw material temperature or a temperature corresponding thereto. For example, in the case of the microwave extraction device (1), since the temperature at the lower part of the tank side surface is approximately equivalent to the raw material temperature, an embodiment of installing it at the lower part of the tank side surface (the raw material temperature sensor (12) at this time is also referred to as the tank side surface temperature sensor) can be considered. The embodiments of the steam temperature sensor (9) and the raw material temperature sensor (12) for measuring the temperature of the raw material (M) are not particularly limited, but it is preferable to use a thermocouple or an infrared radiation thermometer for reasons of low cost and easy installation. Others include resistance temperature detectors, optical fiber thermometers, etc.

[0090] The raw material (M) is the basis for performing the distillation and extraction according to the present invention, and is a liquid mixture, a solid mixture, or a mixture in which a liquid and a solid coexist. If it contains a solvent component (e.g., water) and a target component, its embodiment is not particularly limited. When the raw material is a solid mixture and the target component attached to the raw material is distilled (extracted), by dispersing the raw material in a solvent (e.g., water) in which the target component dissolves, the gas-liquid equilibrium surface of the target component - solvent component (water) can be used, and the present invention can be implemented.

[0091] The liquid mixture refers to the liquid components contained in the raw material (M). When considering the water content (or oil content) of each component constituting the raw material (M) for the liquid components contained in the raw material (M), since in the raw material (M), the target component and the solvent component often dominantly exist, it is often expressed as the sum of the target component and the solvent component. When using the gas-liquid equilibrium surface according to the present invention, attention will be paid to the state change of this liquid mixture.

[0092] The target component is what is recovered as a distillate (extract, or recovered product) after performing the distillation and extraction according to the present invention. In the present invention, it is preferable that the target component is used as the first component on the gas-liquid equilibrium surface. The target component is arbitrarily determined by the user of the distillation or extraction method according to the present invention according to the user's purpose. For example, it is conceivable that the user needs a distillate containing the target component or a residue of the raw material from which the target component has been removed after performing the distillation or extraction according to the present invention. Depending on this difference in purpose, the user arbitrarily determines the target component. In view of the fact that the present invention performs distillation and extraction, it is desirable that the target component is a liquid. Examples of the target component 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 (for example, volatile organic compounds having a molecular weight of 350 or less and having at least one of hydrogen, carbon, nitrogen, oxygen, and sulfur as a constituent element). Methanol or ethanol is particularly suitable as the target component.

[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, it is preferable that the solvent component is used as the second component on the gas-liquid equilibrium surface. Examples of the solvent component include water, toluene, hexane, heptane, cyclohexane, dioxane, carbon tetrachloride, 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, or a mixed solvent thereof. However, it is not particularly limited 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 the target distillation temperature) is the set temperature for distillation and extraction according to the present invention. Since the present invention performs a vacuum step and can lower the boiling point of the target component by reducing the pressure, distillation and extraction at a low temperature can be performed. For example, the distillation set temperature can be set between 10°C and 100°C. When heating is performed by microwave, it is preferably set between 30°C and 100°C. This is because when distillation or extraction is performed under low temperature and low pressure conditions, the probability of generating plasma derived from microwave increases, which may significantly damage the apparatus. For example, by setting the saturated vapor pressure of 6.67 kPa when the boiling point of water is 38°C as the limit value under low temperature and low pressure conditions, the distillation or extraction method according to the present invention can be safely performed. Here, since the saturated vapor pressure when the boiling point of ethanol, which is one of the target components, is 30°C (i.e., the lowest temperature that can be preferably used in microwave heating) is about 10.44 kPa at a molar fraction of 0.9, the user can safely perform the distillation or extraction method according to the present invention. In addition, when producing distilled spirits containing components prone to thermal degradation, such as the essential oil components of citrus fruits, it is preferable to set the distillation set temperature between 30°C and 70°C.

[0095] The distillation amount (recovery amount, or extraction amount) is the weight of the distillate (extract, or recovered product). In the apparatus used for the distillation or extraction method according to the present invention, it can be measured by providing a scale (or weighing scale) for measuring the mass of the distillate in a container (14) for recovering the distillate (for example, a distillate recovery tank or a recoverer).

[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 its range.

[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), a mode of indirectly measuring through the tank (T) by the raw material temperature sensor (12) attached to the side of the tank is conceivable. The raw material temperature measured by the raw material temperature sensor (12) attached to the side of the tank at this time is also referred to as the side surface temperature of the tank. Further, in the implementation of the present invention, considering the prevention of damage to the raw material temperature sensor (12) and the ease of handling of the raw material temperature sensor (12), 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.

[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 what is recovered by the distillation and extraction operations according to the present invention and contains the target component.

[0100] Figure 2 is a control flowchart relating to the method for distilling or extracting the raw material of the present invention. The present invention is achieved by the following steps starting from (1). It should be noted that in the implementation of the present invention, it is necessary to prepare in advance the gas-liquid equilibrium surface represented by the mixed system of the target component and the solvent component, and it should be noted that this is required to be adopted as a parameter in the present invention. (1) Set the operation time or the distillation amount (recovery amount). (2) Set the distillation set temperature. (3) Determine whether the distillation set temperature is higher than the ambient temperature by the set temperature difference ΔT A or more. If the set temperature difference ΔT A is higher or more, proceed to (4). If the set temperature difference ΔT A is less than that, return to (2). This determination is because in order to detect boiling by the deviation amount between the raw material temperature (tank side surface temperature) and the vapor temperature, boiling detection cannot be performed when the indoor temperature is higher than the distillation set temperature. For example, the set temperature difference ΔT A at this time is preferably 3°C or more. (4) Do you know the concentration (liquid-phase mole fraction or mol%) of the target component contained in the raw material? If you know, proceed to (5). If you don't know, start the operation and proceed to (7). (5) Set the value of the concentration (liquid-phase mole fraction or mol%) of the target component contained in the raw material and start the operation. (6) Derive the saturated vapor pressure at the set concentration (liquid-phase mole fraction or mol%) of the target component from the gas-liquid equilibrium surface, lower the pressure in the tank to the derived saturated vapor pressure, and keep the pressure in the tank at the set pressure difference ΔP A for a certain time t A until it is achieved. After the pressure is adjusted, proceed to (8). For example, the pressure adjustment at this time (set pressure difference ΔP A ) is preferably such that the pressure in the tank reaches within ±0.4 kPa in 4 seconds (certain time t A ). (7) Lower the pressure in the tank to the value of the saturated vapor pressure obtained (determined) when the gas-liquid equilibrium surface of the target component is adopted, 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 (for example, when ethanol is the target component, adopt the value of 90 mol%), and the distillation set temperature are adopted on the gas-liquid equilibrium surface, and keep the pressure in the tank at the set pressure difference ΔP B for a certain time tB Adjust the pressure until it is achieved. After adjusting the pressure, proceed to (8). For example, the pressure adjustment at this time (set pressure difference ΔP B ) is preferably such that the pressure inside the tank reaches within ±0.4 kPa within 4 seconds (constant time t B ). (8) Start stirring the raw materials. (9) After (8), adjust the pressure until the pressure inside the tank reaches the set pressure difference ΔP C for a constant time t C . For example, the pressure adjustment at this time (set pressure difference ΔP C ) is preferably such that it reaches within ±0.3 kPa within 5 seconds (constant time t C ). (10) After (9), start heating, for example, by oscillating microwaves (continuous irradiation). In the operations after (10), if the raw material temperature (tank side surface temperature) - distillation set temperature is equal to or greater than the set temperature difference ΔT B , stop heating, for example, by stopping the oscillation of microwaves. If the raw material temperature (tank side surface temperature) - distillation set temperature is less than the set temperature difference ΔT C , (re)heat. For example, it is preferably to stop heating (stop the oscillation of microwaves) if the raw material temperature (tank side surface temperature) - distillation set temperature ≥ 1.5 °C (set temperature difference ΔT B ). Also, it is preferably to (re)heat (re-oscillate the microwaves) if the raw material temperature (tank side surface temperature) - distillation set temperature < 1.0 °C (set temperature difference ΔT C ). In addition, for temperature control, depending on the temperature difference between the raw material temperature and the distillation set temperature, the set temperature difference ΔT B and / or the set temperature difference ΔT C can be set so that the output of the heating (heat source) can be appropriately decreased or increased. In the case of heating by microwaves, depending on the temperature difference between the raw material temperature and the distillation set temperature, the stop of microwave irradiation, the oscillation of microwaves, the switching to pulse irradiation, the switching to continuous irradiation, the decrease in the output of microwaves, or the increase in the output of microwaves can be appropriately performed by setting the set temperature difference ΔT B and / or the set temperature difference ΔT C . (11)(10) Subsequently, the pressure in the tank is leveled until it reaches within the set pressure difference ΔP D within a certain time t D is achieved, and it is determined whether the raw material temperature (tank side surface temperature) is a value equal to or higher than the distillation set temperature. The pressure in the tank is leveled until it reaches within the set pressure difference ΔP D within a certain time t D is achieved. If the raw material temperature (tank side surface temperature) is equal to or higher than the distillation set temperature, proceed to (12). ΔP D The value range of is within ±0.01 to 0.2, and t D The value range of is considered to be in the range of 0.5 to 5 and can be arbitrarily set by the operator according to the distillation set temperature. Also, ΔP D and t D The values can also be programmed by the operator so that they can be changed to arbitrary values under arbitrary conditions from the start to the end of the present invention. For example, the pressure leveling at this time (set pressure difference ΔP D ) preferably achieves within ±0.1 kPa in 1 second (certain time t D ). (12) When all of the following conditions are satisfied, the pressure in the tank is further reduced at a rate corresponding to the slope ΔkPa / Δ concentration of the vapor-liquid equilibrium curve of the target component and the solvent component. Condition (I) Not boiling, or

[0101]

Number

[0102]

Number

[0103] [Number] When this is achieved, it is determined that boiling has been detected. ΔT F Values of can be set in plural, and the value of ΔT F when detecting the first boiling (the first time boiling occurs), and the value of ΔT F when detecting the second boiling, and the value of ΔT F when detecting the third boiling may be different, and the values of ΔT F after the fourth time can also be set similarly. Furthermore, ΔT F may adopt a value that is changed in real time according to the deviation between the distillation set temperature and the room temperature. For example, in (I), it is preferable that the set temperature difference ΔT D is 0.8 °C. For example, in (II), the difference between the value of the saturated vapor pressure calculated by the vapor-liquid equilibrium surface and the actually measured pressure value (set pressure difference ΔP E ) preferably achieves within ±0.1 kPa in 1 second (constant time t E ). For example, in (III), it is preferable that the set temperature difference ΔT E is 0.3 °C. The set temperature difference ΔT F is basically 0.5 °C, and the set temperature difference ΔT F may be different values for the first and second boiling detections. In that case, it is desirable that the first time is 1.0 °C and the second time is 0.5 °C. Also, it may be changed similarly for the third time and later. Furthermore, the set temperature difference ΔT F may be variable according to the deviation between the distillation set temperature and the room temperature. Here, the rate is represented by the following formula.

[0104] [Number] Here, a is an arbitrary constant. The range of the value of a is considered to be in the range of 0.5 to 1.5. For example, a = 1 is preferred, but it can be arbitrarily set according to the type of raw material, the type of target component, the operation time, the distillation amount, and the position on the vapor-liquid equilibrium curve. The setting of the value of a can also be programmed by the operator so that it can be changed to any value under any conditions from the start to the end of the present invention. Here, the rate is obtained by dividing [ΔkPa / Δ concentration] by sec (seconds) as described above, but the units of pressure and time such as kPa and sec can be arbitrarily set by the user. (13)(12) The target component is recovered (distilled) at any time, and the present invention ends when the operation time or the distillation amount (recovery amount) set in (1) is reached. (14)(13) When the concentration of the target component contained in the raw material becomes 0, or when the pressure in the tank reaches the saturated vapor pressure of the solvent component alone, it is determined that the target component cannot be recovered (distilled) even if the operation continues, and a message to that effect is displayed on the control panel.

[0105] The step of starting the heating in (10) does not have to be after (9), and can be, for example, after (4) or after (5). The present invention can be arbitrarily (automatically) stopped in each step. When automatically stopping, it is determined according to the concentration of the target component contained in the distillate (extract) being vacuum distilled and the concentration of the target component contained in the raw material (for example, the liquid-phase mole fraction) by a function that calculates the estimated concentration of the target component contained in the distillate (extract) and the raw material. In other cases where automatic stop occurs, it may be after the lapse of the operation time set in (1) or when the distillation amount (recovery amount) is achieved. 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 the operation of the distillation (extraction) apparatus. The present invention constantly measures the weight of the distillate (extract), detects the boiling of the raw material, and calculates the estimated concentration of the distillate (extract) during distillation from the liquid-vapor surface (x-y surface) of the target component (see Figure 6) obtained from the vapor-liquid equilibrium surface. When the weight of the liquid mixture in the raw material (the sum 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] Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited by such examples.

[0107] (Example 1) As shown in Figure 3, the vapor-liquid equilibrium surface of pressure-temperature-concentration for an ethanol-water binary system was created by using a plurality of 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 vacuum distillation according to the present invention. At this time, the distillation set temperature was set to 40 °C, and the distillation amount (recovery amount) was set to 16 kg. First, the operating time according to the present invention was shortened by reducing the pressure to the value of the saturated vapor pressure of 90 mol% at which boiling of the raw material does not occur, calculated from the vapor-liquid equilibrium surface of ethanol-water. Next, the raw material was stirred and the microwave generator was started. At this time, the microwave generator was set to stop when the raw material temperature - distillation set temperature ≥ 1.5 °C and (re)oscillate when the raw material temperature - distillation set temperature < 1.0 °C. After that, in order to find the concentration of the target component (ethanol) contained in the raw material, further pressure reduction was performed at a rate according to the slope ΔkPa / Δmol% of the vapor-liquid equilibrium surface until all of the following conditions were not met.

[0109] Condition (1) Not boiling, or the difference between the vapor temperature and the distillation set temperature is 0.8 °C or more, where the boiling is determined to be boiling when the difference between the raw material temperature and the vapor temperature at the time of detecting the first boiling is 1.0 °C or less, and the difference between the raw material temperature and the vapor temperature at the time of detecting the second and subsequent boilings is 0.5 °C or less. (2) Depending on the concentration of the target component, the difference between the value of the saturated vapor pressure calculated by the vapor-liquid equilibrium surface and the value of the actually measured pressure is within ±0.1 kPa per second. (3) The difference between the raw material temperature and the distillation set temperature is 0.3 °C or more. Rate = [ΔkPa / Δmol%] / sec × a (At this time, let a = 1.)

[0110] Under these conditions, the first boiling was detected about 21 minutes and 30 seconds after starting the vacuum reduction, and it was calculated that the raw material contained 8.68 mol%, the alcohol (ethanol) degree was 23.9 degrees, and the mass concentration was 19.5 wt%. The second boiling could be confirmed about 24 minutes and 30 seconds after starting the vacuum reduction.

[0111] Assuming that the concentration of the target component (ethanol) contained in the raw material decreases over time, the vacuum distillation process was carried out while maintaining the above conditions and rate, and the vacuum distillation was terminated when the recovery amount (distillation amount) reached 16 kg while grasping the concentrations of the raw material and the distillate in real time. The concentration of the distillate was 23.2 mol%, the alcohol (ethanol) degree was 51.1 degrees, and the mass concentration was 43.5 wt%.

[0112] From the start to the end of the vacuum distillation in Example 2, the raw material temperature and the vapor temperature could be maintained at around 40 °C. The indoor 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 Fig. 5, 50 kg of a raw material with a concentration of the target component (ethanol) measured by an alcohol meter of 18.7 degrees (6.55 mol%, mass concentration 15.19 wt%) was subjected to vacuum distillation according to the present invention. At this time, the distillation set temperature was set to 40°C and the distillation amount (recovery amount) was set to 16 kg. First, the pressure was reduced to the value of the saturated vapor pressure when the concentration of the target component (ethanol) was 6.55 mol% from the ethanol-water vapor-liquid equilibrium surface. Next, the raw material was stirred and the microwave generator was started. The microwave generator at this time was set to stop when the raw material temperature - distillation set temperature ≥ 1.5°C and (re)oscillate when the raw material temperature - distillation set temperature < 1.0°C. Thereafter, further pressure reduction was performed at a rate according to the slope ΔkPa / Δmol% of the vapor-liquid equilibrium surface until all of the following conditions were not met.

[0114] Condition (1) Not boiling or the difference between the vapor temperature and the distillation set temperature is 0.8°C or more. Here, the boiling is determined to be boiling when the difference between the raw material temperature and the vapor temperature at the time of detecting the first boiling is 1.0°C or less, and the difference between the raw material temperature and the vapor temperature at the time of detecting the second and subsequent boilings is 0.5°C or less. (2) The difference between the value of the saturated vapor pressure calculated by the vapor-liquid equilibrium surface and the value of the actually measured pressure is within ±0.1 kPa per second according to the concentration of the target component. (3) The difference between the raw material temperature and the distillation set temperature is 0.3°C or more. Rate = [ΔkPa / Δmol%] / sec × a (At this time, let a = 1.)

[0115] Under this condition, the first boiling was detected about 17 minutes after the start of pressure reduction.

[0116] Assuming that the concentration of the target component (ethanol) contained in the raw material decreases over time, the vacuum distillation process was carried out while maintaining the above-mentioned conditions and rates. While grasping the concentrations of the raw material and the distillate in real time, the vacuum distillation was terminated when the recovery amount (distillation amount) reached 16 kg. The concentration of the distillate was 23.3 mol%, the alcohol (ethanol) degree was 51.3 degrees, and the mass concentration was 43.7 wt%.

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

Industrial Applicability

[0118] The method for distilling or extracting the raw material according to the present invention can recover the target component from various types of raw materials by distillation or extraction. For example, in the production of distilled liquor, the removal of organic solvents contained in the raw material, and recycling for the purpose of removing odor components adhering to resin containers (the raw material is a solid (container), the target component is an odor component, and the solvent component is water), etc., can be widely used. In addition, in the production of distilled liquor, when producing a distilled liquor containing components that are prone to thermal degradation, such as essential oil components contained in citrus fruits such as yuzu, the present invention can perform distillation (extraction) at a low temperature (for example, 35°C), so that a distilled liquor that does not damage the aroma of citrus fruits can be produced.

Explanation of Symbols

[0119] 1 Vacuum distillation (extraction) device 2 Microwave generator 3 Microwave transmission material 4 Vacuum pump 5 Atmosphere release valve 6 Cooling condenser 7 Cooling device 8 Tank internal 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 recovering a target component by distilling or extracting a raw material containing the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes inside an airtight tank capable of being depressurized, (A) a step of heating and maintaining the raw material to 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, including performing the above steps, while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature, Regarding the above steps (B) and (C), in an environment where the ambient temperature is lower than the target distillation temperature, the vapor temperature and the raw material temperature are compared, A vacuum distillation method that utilizes the phenomenon that the vapor temperature and the raw material temperature become equal when boiling occurs, and the vapor temperature becomes lower than the raw material temperature when boiling stops.

2. Regarding the pressure reduction in the above step (B), first, using the vapor-liquid equilibrium surface represented by a mixing system of the target component and the solvent component mixed with the target component, which is determined by temperature, concentration, and pressure, (a) When the concentration (or content) of the target component in the raw material is unknown, from the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximum at the target distillation temperature, to the saturated vapor pressure determined by the vapor-liquid equilibrium surface, (b) When the concentration (or content) of the target component in the raw material is known, from the target distillation temperature and the concentration of the target component, to the saturated vapor pressure determined by the vapor-liquid equilibrium surface, According to the conditions of (a) or (b), while heating and maintaining to the target distillation temperature, rapidly reduce the pressure. The vacuum distillation method according to Claim 1.

3. A vacuum distillation method for recovering a target component by distilling or extracting a raw material containing the target component, wherein the raw material has a lower saturated vapor pressure (higher boiling point of the raw material) as the concentration (or content) of the target component decreases, and the target component is separated from the raw material by distillation, so that the concentration (or content) of the target component in the raw material decreases. The vacuum distillation method includes inside an airtight tank capable of being depressurized, (A) a step of heating and maintaining the raw material to the target distillation temperature, Step of gradually reducing the pressure in the tank if the raw material is not boiling, and Step of maintaining the pressure in the tank if the raw material is boiling, including performing the above steps, while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature, Regarding the pressure reduction in the step (B), reduce the pressure at a rate using the value of the slope of the saturated vapor pressure with respect to the concentration of the target component on the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component, which is determined by the raw material temperature and the pressure in the tank. The value of the slope of the saturated vapor pressure with respect to the concentration of the target component is 【Number 1】 a vacuum distillation method.

4. Regarding the pressure reduction in the step (B), first, utilize the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component, which is determined by temperature, concentration, and pressure. When the concentration (or content) of the target component in the raw material is unknown, from the target distillation temperature and the concentration of the target component at which the saturated vapor pressure is maximum at the target distillation temperature, to the saturated vapor pressure determined by the vapor-liquid equilibrium surface. When the concentration (or content) of the target component in the raw material is known, from the target distillation temperature and the concentration of the target component, to the saturated vapor pressure determined by the vapor-liquid equilibrium surface. According to the conditions of (a) or (b), while heating and maintaining to the target distillation temperature, rapidly reduce the pressure. Next, regarding the pressure reduction for the second and subsequent times, reduce the pressure at a rate using the value of the slope of the saturated vapor pressure with respect to the concentration of the target component on the vapor-liquid equilibrium surface determined by the raw material temperature and the pressure in the tank. The value of the slope of the saturated vapor pressure with respect to the concentration of the target component is 【Number 2】 as follows. The vacuum distillation method according to claim 1.

5. Regarding the pressure reduction in the step (B), in order to perform 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 pressure reduction is performed when all of (1) to (3) described in condition 1 below are satisfied. (1) Not boiling, or 【Number 3】 being in a certain state, and (2) The absolute value of the difference between the target and actual tank internal pressures is within the range of the set pressure difference ΔP Ｅ at a constant time t Ｅ and （３） [Number 4] being in a certain state. Here, the condition for detecting boiling in (1) is (4) described in condition 2 below. (4) Boiling detection is 【Number 5】 in a certain state. The vacuum distillation method according to any one of claims 1 to 4.

6. A vacuum distillation method for distilling or extracting a raw material containing a target component and recovering the target component. The raw material has a lower saturated vapor pressure (higher boiling point of the raw material) 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 is as follows: Inside an airtight tank capable of being depressurized, (A) A step of heating and maintaining the raw material to 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, including performing the above steps, while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature. A vacuum distillation method including a step of obtaining the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the tank by means of a vapor-liquid equilibrium surface represented by a mixing system of the target component and a solvent component that mixes with the target component, based on the raw material temperature and the pressure in the tank during boiling in the distillation.

7. When the mass of the raw material and / or the distillate can be measured, the method further includes a step of estimating the mass concentration of the target component in the raw material and / or the distillate from the liquid-phase mole fraction and / or the gas-phase mole fraction of the target component and the mass of the raw material and / or the distillate. The vacuum distillation method according to claim 6.

8. A vacuum distillation method for distilling or extracting a raw material containing a target component to recover the target component, The raw material has a lower saturated vapor pressure (higher boiling point of the raw material) 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 is as follows: Inside an airtight tank capable of being depressurized, (A) A step of heating and maintaining the raw material to 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, including performing the above steps, while capturing the saturated vapor pressure of the raw material that changes with time by distillation, boiling at the target distillation temperature, and distilling at a constant temperature. In the case of changing the target distillation temperature during the distillation, when changing the target distillation temperature, the pressure inside the tank is promptly changed from the concentration of the target component determined before the change according to the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component to the saturation vapor pressure obtained from the vapor-liquid equilibrium surface based on the target distillation temperature after the change, and the distillation is continued, further including a step of a vacuum distillation method.

9. In the case of a raw material containing a target component and a solvent component mixed with the target component, during the distillation, the state where the concentration of the target component obtained from the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component becomes 0, or the state where the target tank internal pressure obtained from the vapor-liquid equilibrium surface becomes equal to the saturation vapor pressure of the solvent component alone can be detected. When the concentration of the target component becomes 0, or when the target tank internal pressure becomes equal to the saturation vapor pressure of the solvent component alone, the vacuum distillation method according to claim 1, further including a step of stopping the distillation.

10. The heating is performed by microwave irradiation, and according to the difference between the raw material temperature and the target distillation temperature, the vacuum distillation method according to claim 1 is performed, including stopping microwave irradiation, oscillating microwaves, switching to pulse irradiation, switching to continuous irradiation, decreasing the output of microwaves, or increasing the output of microwaves.

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

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

13. A microwave extraction device used in the vacuum distillation method according to claim 1, wherein the extraction device includes a tank for accommodating the raw material, a microwave generator for generating microwaves, waveguide means and microwave transmission means for guiding the microwaves to the tank, a stirring device for stirring the raw material accommodated in the tank, a vacuum pump for adjusting the pressure inside the tank, an air release valve for adjusting the pressure inside the tank, a cooling condenser or a cooling device for cooling and condensing the vapor of the raw material evaporated from the tank by heating, a recovery device for recovering the components condensed by the cooling condenser, a control device for controlling operations of pressure, cooling, and microwave irradiation, a sensor for measuring the pressure inside the tank, the raw material temperature, and the vapor temperature, A microwave extraction device comprising.

14. During boiling in the distillation, based on the raw material temperature and the tank internal pressure, a function is provided to obtain the liquid-phase mole fraction and the gas-phase mole fraction of the target component in the tank according to the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component. When there is a scale capable of measuring the mass of the raw material and / or the distillate, the microwave extraction device according to claim 13 has a function of estimating the mass concentration of the target component in the raw material and / or the distillate from the liquid-phase mole fraction and / or the gas-phase mole fraction of the target component and the mass of the raw material and / or the distillate.

15. During the distillation, when changing the target distillation temperature, according to the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component, the internal pressure of the tank is quickly changed from the concentration of the target component obtained before the change to the saturation vapor pressure obtained from the vapor-liquid equilibrium surface based on the target distillation temperature after the change, and the distillation can be continued. The microwave extraction device according to claim 13 has this function.

16. In the case of a raw material containing a target component and a solvent component mixed with the target component, during the distillation, a state where the concentration of the target component obtained according to the vapor-liquid equilibrium surface represented by the mixing system of the target component and the solvent component mixed with the target component becomes 0, or a state where the target internal pressure of the tank obtained according to the vapor-liquid equilibrium surface is equal to the saturation vapor pressure of the solvent component alone can be detected. When the concentration of the target component becomes 0, or when the target internal pressure of the tank is equal to the saturation vapor pressure of the solvent component alone, the microwave extraction device according to claim 13 has a function of stopping the distillation.

17. The heating is performed by microwave irradiation. According to the difference between the raw material temperature and the target distillation temperature, the microwave extraction device according to claim 13 performs stopping of microwave irradiation, oscillation of microwaves, switching to pulse irradiation, switching to continuous irradiation, decreasing the output of microwaves, or increasing the output of microwaves.

18. The raw material contains alcohol, and the target component is alcohol. The microwave extraction device according to claim 13.

19. The raw material contains ethanol, and the target component is ethanol. The microwave extraction device according to claim 13.

Images