JP3087211B2 - Distillation separation method and distillation separation apparatus - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for distilling and separating a specific component from a material containing a plurality of chemical components. Particularly suitable for distillation separation from natural materials such as plants, and without the use of organic chemical reagents or reagents, the oiliness of natural materials composed of complex chemical components by the activation energy of photochemical reactions and thermal reactions The molecular characteristics of each of the components and the water-soluble components can be separated by distillation while maintaining the state of being contained in the natural material. For this reason, natural materials are contained, especially by creating an electron transfer state between hydrogen and hydrogen monoxide in water vapor and utilizing organic electronistic effects such as conjugate addition reactions of electrons and thermodynamic effects of water vapor. The present invention relates to a distillation separation method and apparatus capable of separating an oily component and a water-soluble component contained in a natural material by distillation while bringing the oily component and the water-soluble component closer to a natural state as much as possible.

[0002]

2. Description of the Related Art Preferred fragrance and flavor active ingredients of vegetable oil (perfume, cologne, cream, lotion, lotion, lipstick, white powder, foundation, pomade, tic, hair cream, and other cosmetics and fragrances of foods, etc.), pharmaceuticals Active ingredients (eg, cardiotonic, diuretic, hormonal, antiviral, anti-immune, metabolic improving, appetite-enhancing, intestinal, mental-stabilizing, antibacterial, antifungal, anti-mite insects) Action and anti-cancer action) and active ingredients as nutrients such as foods, as well as active ingredients necessary for daily living space such as rubber, dyes and fuels. Since ancient times, human beings have gathered and used wisdom. It is well known that Also, with the accumulation of knowledge on organic chemistry, useful primary compounds present in vegetable oils, even though those that are relatively easy to synthesize, are mostly artificially synthesized, have complex primary structural formulas and It may be technically and economically difficult to synthesize a compound with configuration and conformation. In addition, the synthesis of a compound or derivative having a structure similar to that of a known compound and the production of a useful new compound or a complex thereof in the form of a naturally occurring form thereof are extremely low in efficiency and naturally occur. In some cases, unnatural substance compositions and composition ratios as well as by-products harmful to the human body may be mixed.

Conventionally, oily components contained in natural materials and organic components contained therein have been obtained by a steam distillation method (Japanese Patent Laid-Open Nos. 64-38496, 61-279247, 62-143997, 62-143997, and 62-143997). 60-161929) and a solvent extraction method (JP-A-5-86396, JP-A-5-345).
899, JP-A-3-91456, JP-A-2-22839
6, JP-A-2-235996, JP-A-62-14399
7, JP-A-61-222299, JP-A-55-343
4, JP-A-59-24795, JP-A-58-9669
9, JP-A-58-187497, or a rhodium complex or a cobalt complex (JP-A-59-8139).
9, JP-A-63-68991) and composite iron salts (JP-A-2-
208398), and a gaseous phase fluid such as carbon dioxide (JP-A-4-246500, JP-A-2-18099).
7, JP-A-2-235996, JP-A-63-11029
1, JP-A-61-221299, JP-A-61-1290
03, distillation or separation using JP-A-60-99793).

[0004] However, in oily components separated by distillation or extraction by these methods and in essential oils subjected to washing and deodorizing treatments, aromatic organic components which are easily deteriorated by heat and are easily oxidized are present. In some cases, a method capable of extracting and separating the aromatic organic component qualitatively and quantitatively in a manner similar to a state in which it is contained in a natural state has not been exemplified at this stage. Although many methods and devices as described above have been published based on various organic chemical reaction theories, at present they are still qualitatively and quantitatively maximally approximating the state contained in the natural state. There is no method of distillation separation or extraction separation, and no method of distillation or extraction separation of a chemically stable complex product.

[0005] Particularly, vegetable oils and the like contain a large amount of terpenes and aliphatic hydrocarbon compounds. In the method and operation of distilling and separating vegetable oils, substances having electron orbits which are not originally present in vegetable oils. Transformation into a substance having a different configuration or conformation is a reason that can be reasonably considered from current knowledge of organic chemistry. Furthermore, in the conventional method of separating and distilling vegetable oil, oxygen radicals and hydrogen oxide radicals which can occur in the method and operation of distillation and separation of vegetable oil due to the activation energy of photochemical reaction and thermal reaction and organic chemical reaction theory. For the purpose of preventing the deterioration and deterioration of vegetable oil due to the generation of the above-mentioned substances, the main object was distillation separation of substances which can be crystallized and whose primary structure is considered to be stable.

In order to provide a method for modulating the odor of a compound having an unsaturated double bond and an essential oil contained as a component thereof, a method of treating the compound with hydrogen and carbon dioxide using a rhodium complex or a cobalt complex and a hydroformylation catalyst is also available. It has been proposed (JP-A-59-81399). But,
In this method, benzene, aromatic compounds such as toluene,
Hexane, heptane, solvents such as saturated hydrocarbons such as cyclohexane, tetrahydrofuran, chloroform, halogenated hydrocarbons such as methylene chloride are used,
In addition to solving the above-mentioned problems, while it is possible to extract and separate a specific aromatic organic component for a limited purpose in a state close to nature, the organic chemical reason is not described. However, no consideration is given to the effective use or deterioration of other composite components contained in natural materials other than the target substance.

[0007] A method of recovering a refined oil by hydrogenation using a nickel-containing catalyst is also disclosed (JP-A-63-68991). Further, a method in which an allylation reactant prepared by adding copper cyanide and lithium chloride utilizes a conjugate catalytic reaction of an allyl halide type compound (JP-A-3-27123)
6) is also shown, which was proposed based on the conjugate catalysis of an allyl halide type compound for hydrogenation. Methods using these conjugated catalytic reactions are:
In any case, the reaction must be carried out by mixing and heating with the resin or the essential oil itself, and the specified reaction product must be recovered by some method such as adsorption.

[0008] As described above, as a principle of distilling and separating natural materials composed of complex chemical substances of complex components, particularly, vegetable oils such as trees, there are organic electron theory, molecular orbital theory, quantum mechanics and thermodynamics. There is no method proposed with a simple logical configuration, and the conventionally proposed methods of distillation separation and solvent extraction separation using steam have the natural scientific significance of plants such as trees and the scientific history of their industrial use. There is a problem that the development of civilized history is restricted.

Here, a molecule generally has a configuration, a conformation, and a molecular orbital, has a spatial region corresponding to the electron distribution, and has an energy state based on the structure, physicochemical characteristics, and another molecule of the molecule itself. It is well-known that the interaction and reaction rate such as the bond with the carbon can be explained by the wave equation and the frontier orbital theory (Reference: Explanation of Organic Electronics, 4th edition, Minoru Imoto, Tokyo Doujin, 1990) Year: Introduction to Frontier Orbital Method, by Fleming, supervised by Kenichi Fukui, translated by Tomoda Takeuchi, Kodansha, 199
2nd year: How to understand molecular orbital method, 2nd edition, Masayuki Yoshida, Tokyo Kagaku Dojin, 1992). On the other hand, many theoretical explanations of chemical reactions have been made on the basis of organic electron theory, molecular orbital theory and quantum theory in organic chemistry of each molecule (for example, Woodward-Hoffman rule first law: Electrocyclic reaction HOMO for thermal reaction and LUMO for photoreaction
Determines the reaction mode. The second rule: The electron ring-opening reaction occurs so that the generated π-electron system takes the form of HOMO in a thermal reaction and LUMO in a photoreaction. The third rule: (1, j) HOMO for thermal reaction in the following sigmatropy, LUMO for photoreaction
Decides the reaction. Fourth rule: In the prototype, two π-electron systems are generated at the cut sigma-bonding points, and each of them becomes two planes to form a transition system that is vertically parallel. In the thermal reaction, both are HOMO, and in the photoreaction, one is HOMO and the other is LUM.
React with O. Fifth rule: In the cycloaddition of two molecules, the reaction is regulated by the HOMO of the diene and the LUMO of the parent diene in the thermal reaction, and the reaction is regulated by the LUMO in both of the photoreactions. Sixth rule: When the generated π-electron system is 4π-system or more, in the thermal reaction, when the number of electrons is an integer multiple of 4, it is a reverse rotation, and when it is an integer multiple of 4, plus 2, the reaction is a concentric reaction.
The opposite is true for photoreactions).

[0010] The intermolecular compound is composed of an electron donor (supplier) for giving an electron to a partner and an electron acceptor (acceptor) for receiving an electron from the partner. Examples of the former include an aromatic compound molecule that provides electrons in a π molecular orbital, a molecule of an unsaturated compound having a double bond, or a device that provides an electron of an unshared electron pair such as alcohols (a nitrogen atom is The same applies to molecules of organic bases included), and these are generally referred to as D. Receptors include, for example, chlorine, bromine,
There are halogen molecules of iodine, organic halogen compounds such as bromoform, iodoform, and chloroform, and nitro compounds such as nitrobenzene. Now, assuming that D and A are close to each other, van der Waals force (attraction between molecules)
Works to form a weak bond between D and A. This state is termed "non-bonded structure". . It is denoted by D. When the distance between A and D is further reduced, the electron clouds begin to overlap with each other, possibly causing the electrons to move.
If one electron moves from D to A, each is 1
In order to have a shape having a number of unpaired electrons, these electrons form a new electron pair, so that A-D bonding occurs. This state is referred to as A. . It can be represented as D-. This is a state called "charge transfer structure".
Therefore, the structure of such an intermolecular compound is represented by AD and A.D. . It is also well known that it must be expressed as a resonance structure with D +. Further, when titanium oxide, which is a transition metal, is irradiated with ultraviolet light, it is split into electrons (-) and protons (+), and the generated protons convert oxygen to active oxygen (OH radicals) in the air. In the case of a reaction in water, it is known that water is decomposed into oxygen and hydrogen, and at the same time, active oxygen is produced. Transition metals having such an effect on light energy are known as photocatalytic metals, and have contributed to the development of organic chemistry and synthetic chemistry in recent years. However, the conventional use of transition metals has been used for the synthesis, isolation, and improvement of concentration of specific molecules, and oily components and water-soluble components contained in plants such as trees, which are natural materials. Complex chemicals are qualitative and quantitative ratios, the conformation of each molecule,
No distillation separation method or specific apparatus has been proposed in consideration of keeping the configuration or electron density close to the natural state. Furthermore, a method and a distillation separation device that can separate and separate oily and water-soluble components of natural materials composed of multiple molecular compositions and molecular structures including unknown molecules by additionally controlling the electron transfer state of water vapor Is not mentioned.

[0011] Further, in the conventional steam distillation method, oil and
The distillate (distillate) contains a large number of organic chemical components having water-soluble phenolic hydroxyl groups and carboxyl groups. Such as aromatic hydrocarbons such as hexane, heptane, and cyclohexane, and extracted organic solvents such as halogenated hydrocarbons such as tetrahydrofuran, chloroform, and methylene chloride, and by-products thereof, and are hardly used. Has been discarded. In a large amount of distillate water and other aqueous solutions generated, even though useful components are dissolved, their recovery is complicated, so that they cannot be used as harmful substances and almost have to be discarded. In addition, waste contains the organic solvent used for extraction and its by-products, etc.To prevent environmental pollution, it is necessary to treat neutralized wastewater for waste. Have been forced.

Furthermore, a distillation separation and concentration method and apparatus for utilizing a useful component present in a distillate or other aqueous solution by a steam distillation method, and a structural form of a basic skeleton of a plant such as a tree which is a natural material. There has been no proposal for a method or apparatus capable of separating oily components and water-soluble organic chemical components by distillation without destroying the structural skeleton of the residual substrate material such as a fiber structure which maintains the above.

In view of the above, in order to promote future industrial development utilizing natural materials (particularly, trees and other plants) in the natural world, particularly preferred aromatic and flavor active ingredients such as vegetable oils, active ingredients as pharmaceuticals, Active ingredients as food, furthermore, active ingredients such as rubber, dyes and fuels, and useful ingredients in distillates and other aqueous solutions by the steam distillation method, as well as residual substrate materials such as natural materials such as plant fibers such as trees. There has been a long-awaited proposal of a series of processing methods and specific devices that can be effectively used without breaking the image. In addition, it does not cause steric hindrance of the complex components separated by distillation and changes in the molecular structure generated during the distillation separation process, and minimizes the alteration due to light, heat, etc., and is stable from plants such as trees, which are natural materials. There has been a long-awaited proposal of a method and an apparatus capable of distilling and separating the composite chemical component thus obtained.

[0014]

SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and its main purpose is to use a plurality of chemical components contained in a material by using an organic chemical reagent or a reactant. Instead of separating by distillation. In addition, for natural materials, while maintaining the molecular state of each oil-based component and water-soluble component composed of composite chemical components in the natural state as it is contained in natural materials to the maximum,
It is intended to separate by distillation. Furthermore, by separating useful components without waste, it is possible not only to improve the efficiency of the industry, but also to clarify and use unknown active components that are currently unknown, and to identify active components that are difficult to synthesize synthetically at present. It is intended to be useful for separation, prevention of environmental pollution and destruction of nature. Still another object of the present invention is to suppress the production of free radicals and the like, and to carry out distillation separation while making the chemical composition and molecular structure of oily components and water-soluble components such as vegetable oils and animal oils as close to the natural state as possible.

[0015]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies on the above problems, and as a result, have been able to activate a photochemical reaction or a thermal reaction without using an organic chemical reagent, a reactant or a solvent. In order to modulate or regulate the molecular characteristics of each of the composite chemical components by energy, etc., in addition to the molecular interaction of each of the chemical components composed of these multiple
It was decided to thermodynamically create an electron transfer state of hydrogen and hydrogen monoxide in water vapor in an addition reaction system between each molecule of the complex chemical substance. That is, in the present invention, the solvent vapor (particularly water vapor) supplied to the material in the process of distillation separation
An electron transfer state of water molecules is created by adding electrons to a mixed gas containing components discharged from materials and / or before condensation and separation.

The electron transfer state refers to a state in which an electron is transited to an antibonding molecular orbit through an appropriate resonance or resonance phenomenon by applying activation energy or the like to a molecule. Here, the energy of the difference between the quantum states is generated, and a suitable distillation separation can be realized by causing the instability of the high energy state in the excited state to return to a new ground state by vibrational cascade. Further, according to this configuration, in the extraction method using an organic solvent, the components to be extracted are different depending on the solvent to be selected, so that not only the entire low-boiling fraction cannot be efficiently extracted, but also some nonvolatile components can be simultaneously extracted. The inconvenience of extraction can be solved. There are various methods for adding electrons, for example, a method of contacting with a transition metal, a method of applying an electromagnetic wave such as discharge, microwave, ultraviolet light, and visible light, and the like.

Further, of the liquid separated into a low-boiling substance and a high-boiling substance, or a component soluble in a solvent (water-soluble component) and an insoluble component (oil-based component), the liquid containing the majority of the solvent By recycling the (distillate), the molecules contained in the distillate recreate the electron transfer state,
The excited state of the contained composite chemical component is induced, and each component containing the composite chemical component can be obtained in a state closer to that before the distillation separation.

In the process of separation by distillation of the present invention, the structure-maintaining substrate such as fibers other than the oily component and the water-soluble component possessed by the plant such as a tree, which is a natural material, does not undergo destructive alteration, and the structure-maintaining substrate Not only can it be returned to nature as compost and the like, but it can also increase the value of industrial use of household goods such as building materials, pulp, furniture, and nonwoven fabric.

The material which can be treated by the distillation separation method and the distillation separation apparatus according to the present invention is not limited to plants and animals such as trees, which are natural materials, but is involved in the separation and purification of crude oil for petroleum and coal liquefaction. It can be used for distillation operation, concentration and recovery of enzymes, hormones, vitamins, etc. in the field of food and medical products, purification of chemicals, distillation of spices and spices, and the like. Natural materials of plants such as trees, as well as fragrance oils such as citrus oil and laurel oil extracted and separated by another method, fruits and vegetables, seeds and general tree materials and leaves, and plant plants such as herbs Can be used for the distillation operation, but the present invention is not limited thereto.

When operation at a relatively low temperature is required, the apparatus can be filled with liquefied carbon dioxide gas or the like, and a supercritical fluid distillation separation can be added. Conventionally, various organic solvents (eg, acetone, hexane, benzene, formaldehyde, ether, acetonitrile, tetrahydrofuran, alcohol, etc.) are used as solvents to effectively separate and separate specific target chemical substances by distillation. It is needless to say that the present invention can be applied to a distillation method and a distillation apparatus.

[0021]

DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the method according to the present invention will be described with reference to FIG. The method of the present invention is roughly composed of a steam generating section A, an evaporating section B, a condensing section C, a separating section D, and an electron addition control section E, roughly classified from the mechanical point of view.
The electron transfer state of hydrogen and hydrogen monoxide is added and accelerated by the electron addition control unit E to the water vapor generated in the water vapor generation unit A. This water vapor is sprayed on the target material contained in the evaporating section B. The steam containing the distillate is cooled in the condensing section C, and separated in the separating section D into two layers of an oil component and a water soluble component. The water-soluble component is returned to the steam generating section A again, passes through the electron addition control section E, and is used in the above-mentioned distillation separation circuit. An electron addition control unit E may be interposed between the evaporation unit B and the condensation unit C.

FIG. 2 shows a specific example of an apparatus for an industrial production process according to this method. However, it goes without saying that the present example does not impose any restrictions on the method and apparatus described in the claims of the present invention.

According to the apparatus shown in FIG. 2, first, natural materials such as sawdust and chips such as trees are transferred by the conveyor 2,
It is charged into a material input device 3 which is a hopper. The natural material falls into the rotary evaporator 4 through the valve V3. When a predetermined amount of natural material is charged, the valve V3 is closed, the motor 8 is started, and the rotary evaporator 4 is rotated around the horizontal axis. By rotating the rotary evaporator 4, heat can be uniformly transmitted to materials such as natural materials.

Next, the valve V6 is opened, and the water treated with the ion exchange resin is
To supply. The water supplied to the steam generator 1 receives heat from the temperature-controllable boiler 19 via the valve V5, and turns into steam. When the valve V2 is opened, the steam supplied from the steam generator 1 flows into the jacket 5 of the rotary evaporator 4, and the rotary evaporator 4 is warmed. When the internal temperature of the rotary evaporator 4 reaches a predetermined temperature, the control valve V16
Adjust the amount of water vapor. In this example, the steam generator 1 supplies 200 kg / h of steam at a pressure of 1 kg / cm ² G.

Inside the rotary evaporator 4, a steam generator 1 is provided.
Is supplied through the electron addition device 9 and is evenly sprayed on the natural material by the blowing pipe 6. As shown in FIG. 3, the electron addition device 9 is a wire mesh 9a arranged in a water vapor passage. The wire mesh 9a is made of copper oxide, which is one of the transition metals, and has a cylindrical shape with a diameter of 5 cm filled with a mesh of 0.2 mm in diameter and 5 × 5 mm.

When water vapor passes through the wire mesh 9a, the wire mesh 9
When it comes into contact with a, the water molecules are brought into a state (transition state) having activation energy by the heat of the steam. That is, the metal mesh 9a made of copper oxide, which is a transition metal, acts as an electron complex. Examples of the transition metal complex that can be used in addition to copper oxide include Fe, Ni, Co, Cu, and Ti. However, the transition metal complex is not limited thereto. For example, it is not limited to a wire mesh.

The steam can be evenly sprayed on the natural material due to the rotation of the rotary evaporator 4, whereby the target composite chemical substance evaporates from the natural material and mixes with the steam to form a mixed gas. Become. The mixed gas passes through the exhaust port 7 and is led to the distillation condenser 10.

The pressure inside the rotary evaporator 4 is controlled by a valve V17.
And the inside of the rotary evaporator 4 is 1 kg
/ Cm ² G pressure is maintained by the steam amount and pressure of 200 kg / hour.

The pressure regulator 18, the valve V4 and the valve V
By controlling the opening and closing with 14, the pressure control from the outlet of the rotary evaporator 4 to the distillation condensing device 10, the separation device 11, and the low-boiling substance recovery device 22 can be performed. Normally, the outlet pressure is set to the atmospheric pressure by closing the valve V4 and opening the valve 14.

The mixed gas is led to the distillation condensing device 10, where it is condensed into a liquid mixture. Cooling water is circulated from the cooling device 14 to the distillation condensing device 10. Temperature is valve V1
1 is adjusted by opening and closing. The cooling device 14 is also used for cooling the low-boiling-point substance recovery device 22.

In order to homogenize the mixed gas in the distillation condenser 10, the distillation condenser is provided with an automatic stirring device 21. The automatic stirring device 21 is provided with a blade driven by a motor, and can stir the mixed gas in the distillation condensing device 10 by driving it appropriately.

The mixed liquid condensed in the distillation condensing device 10 flows into the separating device 11 and is separated into two phases. The upper portion is an oily component, which flows into the separated material collector 12 by opening the valve V12. The oil component can be appropriately collected by opening the valve V13.

The distillate containing the water-soluble components below the two phases can be recycled to the steam generator 1 and reused by opening the valve V8 as appropriate. At this time, an adsorption filter (synthetic adsorbent, ion-exchange resin, activated carbon, reverse-phase partition type adsorbent) may be provided on the recirculation circuit 13 for the purpose of removing acidic substances contained in the distillate. The substance attached to the adsorption filter can be desorbed and recovered by an appropriate secondary treatment.

The gas that is not condensed and liquefied in the distillation condensing device 10 is guided to the low-boiling substance recovery unit 22 and condensed and liquefied at a lower temperature. The low-boiling-point substance recovery device 22 is maintained at a low temperature by a cooling jacket 23 that receives a supply of cooling water from the cooling device 14. Low boiling substances are recovered by opening valve V15.

The natural material remaining in the rotary evaporator 4 is dried by opening the valve V17, introducing steam into the jacket 5 and heating while evacuating the rotary evaporator 4 with the vacuum pump 24. . The dried natural material passes through a residue recovery device 15 and is conveyed on a conveyor 16 to be reused or processed. In addition, the water-soluble component in the distillate remaining in the steam generator 1 is guided to the dissolved matter recovery device 17 via the valve V9, and the water-soluble component can be collected as needed by opening the valve V10.

In the apparatus shown in FIG. 2, steam distillation using water as a solvent has been exemplified. However, when a planned organic solvent is used, the processing temperature is 25 to 200 degrees Celsius, particularly 3 to 200 degrees Celsius.
0-120 ° C is preferred.

In the apparatus shown in FIG. 2, steam is distilled using steam. In this circuit, the wire mesh 9a shown in FIG. 3 is used to create an "electron transfer state" of steam. In order to bring about such an “electron transfer state”, an activation generator 20 as shown in FIG. 4 can be attached to the electron addition device 9 to supply activation energy to water vapor in the circuit.

The power generation device 20 applies a voltage to the positive and negative electrodes 201 which are alternately arranged at an appropriate distance (2 to 4 mm) between the upper and lower electrodes. The electrode is formed by forming a metal or a material such as silicon or carbon having heat resistance, chemical resistance, and conductivity in a net shape so that water vapor or the like can easily pass therethrough.

The energized pattern (strength, continuous energizing time, etc.) can be freely designed with reference to the display panel 203 by the charging on / off circuit 202, and furthermore, the pH electrode, the ammeter, etc. It is also possible to attach the detector 204 and automatically control the energization pattern while measuring the applied state by the applied control circuit 205. The applied voltage used in this case varies depending on the electric resistance of the electrode material and the like, but is preferably 10 to 1000 V, particularly 200 to 500 V from the viewpoint of voltage supply and safety management.

Further, by attaching an electromagnetic wave, a microwave or a magnetic field generator 30 to the electron adding device 9, an "electron transfer state" of a solvent gas molecule such as water vapor can be created (see FIG. 5). The electromagnetic wave, microwave, or magnetic field generator 30 generates an electromagnetic wave, microwave, or magnetic field from the electromagnetic wave, microwave, or magnetic field generating unit 301 to act on water vapor. The pattern of generation (intensity, duration of generation, etc.) can be freely designed by referring to the display panel 303 by the pulse power supply on / off control circuit 302. Further, the detector 304 is attached, and electromagnetic wave, microwave or The generated pattern can be automatically controlled while measuring the generated state by the magnetic field detecting device.

The microwave or electromagnetic wave in this case has a spectrum with a wavelength of 3 nanometers to 3 centimeters,
An activation energy of 250 to 500 kJ / mol is mentioned, but it goes without saying that the range of the spectrum is selected according to the purpose, and the temperature, pressure and the like in the apparatus can be automatically controlled. The magnetic field intensity used for the electron adding device 9 is preferably 500 to 30,000 Gauss, particularly preferably 100 to 5000 Gauss. For example, it is preferable to set the conditions such as 500-1000 Hertz for a duration of 0.1 millisecond.

Further, by attaching the solar beam converging device 40 and / or the ultraviolet light / visible light generating device 50 to the electron adding device 9, the “electron transfer state” of solvent gas molecules such as water vapor can also be obtained. (See FIG. 6). The solar ray convergence device 40 takes in the sunlight and converges it to act, and the ultraviolet light / visible light generating device 50 causes ultraviolet light or visible light to act. The amount of sunlight to be taken in is controlled by the sunlight convergence control circuit 401. The pattern of generation of ultraviolet light or visible light (intensity, duration of generation, etc.) can be freely designed while referring to the display panel 502 by the pulse power on / off control circuit 501, and the luminous intensity is detected by the luminous intensity detector 503. The detection pattern can be detected and the generated pattern can be automatically controlled. A reflection plate 504 is disposed on the inner surface of the steam flow path to reflect light so that the light sufficiently acts on the steam.

Each electron adding means may be used alone or in combination. The installation position is preferably between the steam generating section A and the evaporating section B, but since the apparatus is configured as a closed system, it may be between the evaporating section B and the condensing section C, or may be installed in both. Is also good. Furthermore, it is also possible to arrange inside the evaporation part B.

The substance separated by distillation collected from any one of the distillation separation circuits is analyzed by a molecular structure analyzer such as a mass spectrometer or a near-infrared spectroscopic spectrometer, and the results are used to determine conditions suitable for the target substance. (Heat amount, water vapor amount, water vapor pressure, applied voltage, electromagnetic wavelength, magnetic field intensity, etc.) can be set, and this setting can be set by installing an appropriate detector in the device,
It is also possible to automatically control by computer processing based on the output of the detector.

The apparatus and method of the present invention can be used not only for steam, but also for ether, acetonitrile, tetrahydrofuran,
It can be applied to distillation separation using an organic solvent such as alcohol, hexane, and benzene. In this case, the high and low boiling points of each organic solvent and the organic electronistic properties are used.

When applied to the apparatus shown in FIG.
Is an organic solvent supply device, and the steam generator 1 generates a solvent vapor. The saturated vapor of the organic solvent passes through the electron addition device 9 and is guided to the rotary evaporator 4. From the material input device 3, not only natural materials but also a solvent extract previously treated with an organic solvent such as ether, acetonitrile, tetrahydrofuran, alcohol, hexane, benzene, etc., can be input as materials.

The mixed gas is condensed in the distillation condensing device 10,
The target substance is obtained by separation by the separation device 11. Further, the separated substance containing a large amount of the organic solvent is recirculated to the steam generator 1, and the substances contained in the separated substance can be accelerated and reused together with the solvent in the electron transfer state by the electron adding device 9. By controlling the number of circulations, etc., a qualitative and quantitative difference in the components of the composition of the solution stored in the separation / recovery unit 12 or the dissolved product recovery unit 17 is created.
In addition, a chemically stable composition can be obtained.

The electronic adding device 9 in the device shown in FIG.
Is attached to a conventional distillation separation apparatus of the Aldershaw type, the filling type, the concentric type, and the rotating band type, which are already implemented, whereby the effect of the present invention can be obtained.
Furthermore, the electronic load device 9 can be applied to simple distillation. That is, the material is put into a solvent and heated, or the mixed liquid containing the solvent and the components extracted from the material is heated, and the electron load device 9 is actuated before the generated mixed gas is condensed, so that the electron transfer of the solvent molecules is performed. By creating a state, good distillation separation can be performed.

Although the control device of the distillation apparatus of the present invention is not shown, it performs pressure control, temperature control, liquid level control, weight control, sequence control and the like. For example, the liquid level control and the weight control are performed by detecting the liquid level of each device, the collecting device, and the like, and opening and closing a solenoid valve so as to have a predetermined level or a predetermined weight. The feed rate is controlled by a metering pump. In order to reduce heat loss in the distilled water tower or circuit, the steam temperature can be controlled by a compensating heater. The amount of vapor rise is measured by measuring the differential pressure of the distillation column during distillation, and is controlled so as to be constant. Steam generator 1,
The temperatures inside the electron addition device 9, the rotary evaporator 4 and the like are also measured and maintained at the set temperature.

[0050]

Next, the aromatic resin oil distilled off from the sawdust or chips of Kiso hinoki cypress, which is a typical Japanese cypress tree, using the above apparatus will be described. However, the method and apparatus of the present invention are not limited to those illustrated.

Using the above-mentioned industrial concrete apparatus, 100 kg of sawdust of dried cypress cypress genus Hinoki (produced by the Kisoyama system in Nagano Prefecture) (100 to 300 years old) was subjected to ion-exchanged water 100 for steam. The oil component and the water-soluble component were separated by distillation with a liter. At this time, the distillate was separated into an aqueous layer component and an oily layer component (average 3 liters). The oily component in the upper layer has an average pH of 7.1, and the fragrance is close to the fragrance produced by the raw materials.

The oily components obtained by distillation vapor from the cypress family Hinoki cypress were examined for their contents by gas chromatography. As a result of measurement with a gas chromatograph double focusing mass spectrometer (Hitachi M-2500), there were no C ₁₀ H ₁₂ O ₂ 7-membered hinokitiol or other 7-membered ring substances having a molecular weight of 164, and 76 kinds of substances were present. It was found to be present (FIG. 7). 6 of them
Three species were identified as having an approximate 82% probability of existing material. Its main components are endoborneol, 1-4
-Terpineol, α-terpineol, (+)-α-
Terpineol, epibicyclosesquiferrandrene,
β-selinen, α-amorphene, aromadendrene,
Monoterpenes such as kadinene, 1,2,3,4,4a, 7-hexahydro-1,6-dimethyl-4- (1-methylethyl) naphthalene and α-cadinol, diterpenes and sesquiterpenes are mainly used. There are also many linear aliphatic compounds and compounds of carboxylic acids.
According to the molecular weight distribution of each substance contained in this vegetable oil, 1
Three large peaks at 36, 154 and 204 were observed.

The sawdust after the distillation separation had the same appearance as that before the distillation separation without any carbonization (see FIG. 8). Further, no change in the morphology of the surface of the fiber structure before and after distillation was observed by observation with a scanning electron microscope. Also, by observation with a transmission electron microscope, no significant change is observed in the fiber structure before and after distillation, but high-density particles of about 2 to 30 nanometers are arranged in the conduit outside the fiber structure before distillation, and sometimes, A morphological image was seen that erupted into the conduit (see FIG. 9), but after distillation, their high-density fine particles were not observed (see FIG. 10). This indicates that the method of distillation separation according to the present invention does not destroy the basic skeleton of the structure forming body such as fiber.

<Basic Concept Related to the Present Invention and the Significance of the Present Invention> In general, the density of electrons changes as the distance from the nucleus increases, and the distance corresponding to the highest point of the mountain has the largest number of electrons. Is the place (equilibrium distance)
Furthermore, the existence probability of the electron cloud, that is, where the electrons can spread, is determined according to the energy. This is the logical construction that has been systematized as quantum theory. It is basically said that the equilibrium radius is proportional to the square of the principal quantum number. However, the second kind of orbit of principal quantum number 2 has changed, and it has a shape like two balls superimposed despite one orbit,
There is a nucleus between the superposition. That is, the p trajectory has directionality in the vertical direction, and the p trajectory has px, py, p
There will be three orbits of z. Also, it is a principle that orbits of the same energy level are always dispersed so as not to interfere with each other, and it is a hybrid that orbits of the same type can be created from different orbits of s orbital and p orbital, The new orbit is called a hybrid orbit. As an example for understanding such a molecular orbital theory, a bond (covalent bond) between C and H will be outlined. If C and H can overlap successfully, the two electrons belong to C and H at the same time, and are shared by C and H, so they are called shared electrons. It is important to note that when two electrons form one bond by reversing the spin, a large amount of energy such as overlapping energy (overlapping energy) is released. This is the generation of so-called binding energy, which is reduced and stabilized. Conversely, it is natural that this binding energy must be newly added in some way in order to split the C—H bond into the original atoms. In addition, molecules have orbits quantized from stable orbits to unstable orbits (which means that they are discontinuous and have a constant orbital energy). It is known that an electron goes into orbit with its spin reversed, and σ (sigma) of stable molecular orbital
The trajectory is one H. Has energy of only E2 as compared with C.I. The energy is further stabilized by the energy of E1, and the molecular orbital (electron pair) into which electrons for covalent bonding are inserted is obtained. Another new molecular orbital is E2 and E1
The trajectory is destabilized only and is expressed as σ *. Since the trajectories cannot overlap, the trajectory is destabilized. That is, regarding the overlap of the orbits, the phase (Ph) of (+) and (-)
), and only those having the same phase can overlap, that is, stabilize. Conversely, it is well known that if the phase is different between (+) and (-), they cannot overlap and repel each other and become unstable. Even from such a simple principle, the conventional steam distillation method itself supplies energy by heat and ionizes water (H ₂ O) by the energy. I.e. hydrogen ions is denoted as H ^+, H ⁺ is a proton i.e. proton itself is very unstable ones. Always where the presence of water, together with the H ₂ O has maintained a balanced relationship with the "H ₃ O" ⁺ of the state. But most H ⁺
Is released, the base that actually receives H ⁺ must always coexist, and H ₂ O, which is water, receives H ⁺ , and even in water vapor [H ₃ O
^+] Concentration and [OH - ^if] the product of the concentration is constant,
Due to the heat energy involved in the distillation and the protons, H ⁺ , the molecular orbitals of the target substance easily become thermally energetic in the direction of stabilization, ie, change in configuration, formation of stereoisomers, and localization of electrons. In addition, the molecular structure is stabilized by substitution (acidification) of a hydroxyl group. In other words, in the generation of the σ bond, the circular s orbitals overlap each other to become a σ bond and become stable, and the circular s orbit becomes sp
3, sp2, and sp trajectories overlap on the same axis and σ
The orbits of sp3, sp2, and sp also overlap on the same direction axis to form a σ coupling, and when the p orbitals also face each other in the same direction axis, they overlap and become σ coupling.
Furthermore, when the generated p orbitals of the π bond are arranged vertically in parallel, they overlap to form a π bond. If they cannot overlap, the circular s-orbit cannot be combined with the p-orbit with a different directional axis even if they overlap (that is, a phenomenon called orthogonal). Further, as a problem of the phase, when the p orbitals are on the same x-axis, they become σ-coupling, and when they are on the py orbital or px-orbital, they become parallel and become π-coupling.
The orbitals are perpendicular to each other and do not overlap because the directions are different, and if the phases are different, they become antibonding molecular orbitals and do not bind. Furthermore, the electron isomer effect (E effect) becomes a π bond of a double bond as compared to the case where the I effect is a σ bond,
It will be very different. From this point, adding an additional electron in steam distillation externally replenishes the delocalization energy, or resonance energy, to the molecule, and the π-electrons are dispersed together with the water vapor and its thermal energy, which is the purpose. A molecule becomes thermodynamically stable due to structural change, and the amount of energy equivalent to the stability becomes the delocalization energy of electrons, controlling, suppressing, or controlling the chain reaction system that promotes the stabilization of other molecular structures. Prevention is thought to be its role. In addition, complex compounds contained in oily components such as trees are mainly composed of carbon, hydrogen, oxygen and nitrogen atoms, but the growth of plants such as trees by chemically converting the light energy of sunlight with chlorophyll etc. In addition to synthesizing substances necessary for maintaining the life, the synthesized composite chemicals also serve as energy storage capacitors for maintaining the life of each. For example, as shown in the examples of the present invention, oily fine particles fixed to glutaraldehyde and stained with osnic acid at high density adhere to the surface in contact with the conduit around the fibrous structure, Some of these particles are scattered erupting or erupting into the conduit, and while these materials are chemically hydrophilic and hydrophobic in nature, they are thermodynamically energetic. By acting as a storage capacitor, in some cases it plays an important role as a pump driving source, as well as forming a pipeline for water movement in the tree from the root to the tip of the leaf spanning tens of meters it is conceivable that. The external enthalpy to the composite chemical is increased by the heat energy of water vapor and the binding energy of the organic solvent itself, and the vegetable oil composed of the composite chemical component as such an energy storage capacitor is increased in resin. It is fully conceivable that the properties of a substance as an energy storage capacitor will be converted to a substance separated from its natural state, and it will change the structure (including the three-dimensional structure) of the substance and the charge distribution (electron density) of molecular orbitals. This results in thermodynamic stabilization of the complex chemicals contained in the resin during the distillation separation operation. This is the point at which various distillation and extraction methods have been improved to date.These include thermodynamic considerations and molecular orbitals of complex chemicals necessary for life support contained in plants such as trees to be separated by distillation. The lack of theoretical considerations has been a scientific issue that has been left behind as a problem when dealing with natural materials. The present invention has been made in view of the above problems,
In addition, natural materials, especially complex chemical substances such as trees, are indispensable substances for the life support of trees and the like, and the substances involved in life support are each thermodynamically ordered in a "dynamic non-equilibrium open system". It is invented from the viewpoint of performing the above, and forms the basis of the present invention. More specifically, it is well known that vegetable oil contains many chemicals having side branches such as carboxyl group, carbonyl group, methyl group and hydroxyl group. = O) -OH is -C after which itself has a characteristic to structure donates H ⁺ to the other, it got out of H ⁺ as the second cause of easily emit H ⁺
Since electrons are dispersed in the anion which is O—O—, delocalization energy, that is, resonance energy is generated, and can be further stabilized by emitting H ⁺ , and this state is further increased by H 2. Make the first factor that releases ⁺ decisive again. Such a reaction system is easily generated by heat energy or light energy load, and is generally involved in a process of denaturing and altering a substance. It has been pointed out that similar changes occur in steam distillation to which heat energy is applied. TECHNICAL FIELD The present invention relates to a method and apparatus capable of controlling, suppressing, or preventing a thermodynamic molecular structure (including a three-dimensional structure) chain chemical reaction occurring in a distillation process by externally adding an electron. Not only can it logically explain that natural materials, especially plants such as trees, can distill the complex composition and complex molecular structure of natural substances in a state closer to nature, but also natural effects as well as industrial effects The significance of the present invention is considered to be great in further exploring the role of the effect on human beings from human beings and in exploring the involvement of humans in natural ecosystems.

[Brief description of the drawings]

FIG. 1 is a schematic view showing an embodiment of a method for distillation separation according to the present invention.

FIG. 2 is a diagram showing an example of a distillation separation device according to the present invention.

FIG. 3 is a diagram showing a wire mesh of an electronic addition control unit E of the apparatus shown in FIG. 2;

FIG. 4 is a diagram illustrating an example of a power generation device for electronic additional control.

FIG. 5 is a diagram illustrating an example of an electromagnetic wave, microwave, or magnetic field generation device for an electronic addition control unit.

FIG. 6 is a diagram illustrating an example of a solar beam converging device and an ultraviolet or visible light generating device for electronic additional control.

FIG. 7 is an analysis chart showing an example of gas chromatography analysis of a vegetable oil component distilled and separated from Kiso hinoki by the apparatus of FIG. 2;

FIG. 8 shows an appearance image of a material before and after an oil component and a water-soluble component are separated by distillation from Kiso hinoki by the apparatus of FIG.

FIG. 9 shows a state of high-density particles in a transmission electron microscope image of a material before an oily component and a water-soluble component are separated by distillation from Kiso Hinoki by the apparatus of FIG. 2;

FIG. 10 shows transmission electron microscope images of the material before and after the oily component and the water-soluble component were separated by distillation from Kiso Hinoki by the apparatus of FIG. 2;

Claims (15)

(57) [Claims] 1. A distillation separation method for condensing and separating a mixed gas containing components emitted from a material placed in a solvent vapor atmosphere, wherein the solvent vapor and the material before being supplied to the place where the material is placed are provided. And / or a mixed gas before condensation / separation of the mixed gas at the place where the liquid is placed, wherein an electron addition process is performed to create an electron transfer state of the solvent molecule. 2. The method according to claim 1, wherein the solvent is water. 3. A distillation separation method for condensing and separating a mixed gas containing a component derived from a material, the method including an electron adding step for forming an electron transfer state of a solvent molecule in the mixed gas before being condensed and separated. Distillation separation method. 4. A mixed gas generating means for generating a mixed gas containing a solvent and a solute, a condensing means for condensing the generated mixed gas, and a separation for separating the condensed mixed liquid into a high-boiling component and a low-boiling component. Means, wherein an electron adding means for generating an electron transfer state of the solvent molecule is arranged before the condensing means. 5. A solvent vapor generating means for supplying a solvent vapor, an evaporating means for supplying a solvent vapor and evaporating a component from a material to generate a mixed gas, and a condensing means for condensing the mixed gas sent from the evaporating means. Means, a distillation separation device including a separation means for separating the condensed mixed liquid into a high boiling component and a low boiling component, between the solvent vapor generating means and the evaporation means,
In the evaporating means and / or between the evaporating means and the condensing means,
A distillation separation device comprising an electron addition means for generating an electron transfer state of a solvent molecule. 6. The distillation separation device according to claim 5, wherein the solvent is water. 7. The distillation separation apparatus according to claim 5, wherein, of the liquid separated by the separation means, a liquid containing most of the solvent is recirculated to the solvent vapor generation means to form a vapor. 8. The distillation separation apparatus according to claim 5, wherein the electron adding means is a transition metal that comes into contact with water vapor and / or a mixed gas. 9. The distillation separation device according to claim 5, wherein the electron addition means is a discharge device that discharges into steam and / or a mixed gas. 10. The distillation separation device according to claim 5, wherein the electron addition means is a discharge device that discharges into steam and / or a mixed gas. 11. The distillation separation apparatus according to claim 5, wherein the electron addition means is an electromagnetic wave generator for applying an electromagnetic wave to water vapor and / or a mixed gas. 12. The distillation separator according to claim 11, wherein the electromagnetic wave generator is a microwave generator. 13. The distillation separation apparatus according to claim 11, wherein the electromagnetic wave generator is an ultraviolet ray generator. 14. The distillation separation device according to claim 11, wherein the electromagnetic wave generation device is a visible light generation device. 15. The distillation separation device according to claim 5, wherein the electron addition means is a solar beam converging device that applies sunlight converged to water vapor and / or a mixed gas.