Constant-temperature double-circulation substance separation method and application thereof

Abstract

The invention belongs to the technical field of substance separation, and particularly relates to a constant-temperature double-circulation substance separation method and application thereof. According to the invention, in a totally-enclosed treatment system, a high-temperature temperature control substance of which the phase change temperature is between the phase change temperature of a low-temperature treated substance and the phase change temperature of a high-phase change temperature component is in contact with the low-temperature treated substance for mass and heat transfer; according to the method, the low-phase-transition-temperature component and the high-phase-transition-temperature component of the low-temperature treated substance are separated, low-temperature dissipation of a treatment system is achieved through substance circulation of the high-temperature temperature control substance and substance circulation of the low-temperature treated substance, a totally-closed, continuous, stable and controllable microenvironment is formed, the low-temperature treated substance is heated uniformly, the component separation efficiency is high, and the treatment effect is good. The energy consumption is reduced, and zero emission of pollutants is realized.

Description

Technical Field

[0001] The present invention belongs to the technical field of material separation, and particularly relates to a constant-temperature double-cycle material separation method and its application. Background Art

[0002] When performing material separation and other treatments by utilizing different phase change temperatures, temperature control is crucial. The existing method is to directly or indirectly heat the material in advance (such as chemical rectification), and then perform subsequent treatments such as material separation. Usually, the low-temperature material to be treated needs to be heated to a certain temperature for all components before it can be used for subsequent treatments. In the actual treatment process, it is usually impossible to uniformly heat all components of the material to be treated within a limited time and space, resulting in problems such as too low or too high local temperatures. At the same time, the pretreatment process is time-consuming and energy-consuming, greatly increasing costs such as equipment, management, and labor. Therefore, the existing method has the disadvantages of low separation efficiency, high ineffective energy consumption, and uneven heating of the material to be treated during preheating. Summary of the Invention

[0003] In view of this, the present invention aims to provide a constant-temperature double-cycle material separation method and its application. This method can create a "fully enclosed, continuous, stable, and controllable" microenvironment for the treatment system, with the material to be treated being evenly heated, high component separation efficiency, and low energy consumption.

[0004] To achieve the above objectives, the present invention provides the following technical solutions:

[0005] The present invention provides a constant-temperature double-cycle material separation method, including:

[0006] Performing two cycles in a fully enclosed treatment system. The two cycles include the material cycle of the high-temperature temperature-controlled material and the material cycle of the low-temperature material to be treated. The low-temperature material to be treated includes a low-phase-change-temperature component and a high-phase-change-temperature component; the phase change temperature of the high-temperature temperature-controlled material is between the phase change temperature of the low-phase-change-temperature component and the phase change temperature of the high-phase-change-temperature component;

[0007] The material cycle of the low-temperature material to be treated is as follows: The high-temperature temperature-controlled material is heated and then contacts the low-temperature material to be treated for heat exchange. During the heat exchange process, the latent heat of phase change of the high-temperature temperature-controlled material causes the low-phase-change-temperature component in the low-temperature material to be treated to undergo a first-order phase change, and after being separated from the high-phase-change-temperature component, it is taken out. The high-phase-change-temperature component is separated and taken out or enters the next cycle process as the low-temperature material to be treated;

[0008] The material cycle of the high-temperature temperature-controlled material is as follows: The high-temperature temperature-controlled material after heat exchange with the low-temperature material to be treated is reheated through reflux and then enters the next cycle process.

[0009] Preferably, the high-temperature temperature control substance, the low-phase change temperature component, and the high-phase change temperature component are substances with first-order phase change properties.

[0010] Preferably, the feeding method of the low-temperature substance to be treated is batch feeding or unidirectional continuous cyclic feeding.

[0011] Preferably, the high-temperature temperature control substance is a gaseous substance or a liquid substance; the gaseous substance is a gaseous azeotrope or a gaseous non-azeotropic mixture.

[0012] Preferably, the low-temperature substance to be treated is a substance with fluidity;

[0013] When the low-temperature substance to be treated does not have fluidity, the low-temperature substance to be treated is made to have fluidity by pulverization.

[0014] Preferably, when the substance with first-order phase change properties in the treatment system is in a gaseous state, the phase change temperature of the substance with first-order phase change properties is changed by changing the pressure of the treatment system.

[0015] Preferably, when the pressure of the treatment system is a constant pressure, the temperature of the treatment system is controlled by controlling the phase change temperature properties and / or the reflux rate of the high-temperature temperature control substance.

[0016] Preferably, when the high-temperature temperature control substance is a gaseous non-azeotropic mixture, the temperature of the treatment system is controlled by controlling the proportion of each component in the high-temperature temperature control substance.

[0017] The present invention also provides an application of the constant-temperature double-cycle substance separation method described in the above technical solution in substance separation, concentration, and surface treatment.

[0018] Preferably, the substance separation includes preparing original brandy from Xanthoceras sorbifolium Bunge flowers; the surface treatment includes microbial inactivation; the microbial inactivation includes inactivating the surface microorganisms of freshly picked Datong yellow flowers in the wild;

[0019] In the process of preparing original brandy from Xanthoceras sorbifolium Bunge flowers, the high-temperature temperature control substance is a gaseous non-azeotropic mixture of ethanol and water, the low-temperature substance to be treated is Xanthoceras sorbifolium Bunge flowers dried at room temperature, and the temperature of the gaseous non-azeotropic mixture of ethanol and water is 80°C to 85°C;

[0020] In the process of inactivating the surface microorganisms of freshly picked Datong yellow flowers in the wild, the high-temperature temperature control substance is a gaseous non-azeotropic mixture of ethanol and water, the low-temperature substance to be treated is freshly picked Datong yellow flowers in the wild, and the temperature of the gaseous non-azeotropic mixture of ethanol and water is 80°C to 85°C.

[0021] The present invention provides a constant-temperature double-cycle material separation method, which includes the following steps: two cycles are carried out in a fully enclosed treatment system, and the two cycles include the material cycle of a high-temperature temperature-controlled substance and the material cycle of a low-temperature substance to be treated. The low-temperature substance to be treated includes a low-phase-transition-temperature component and a high-phase-transition-temperature component; the phase-transition temperature of the high-temperature temperature-controlled substance is between the phase-transition temperatures of the low-phase-transition-temperature component and the high-phase-transition-temperature component of the low-temperature substance to be treated; the material cycle of the low-temperature substance to be treated is as follows: the high-temperature temperature-controlled substance is heated and then contacts the low-temperature substance to be treated for heat exchange. During the heat exchange process, the latent heat of phase change of the high-temperature temperature-controlled substance causes the low-phase-transition-temperature component in the low-temperature substance to be treated to undergo a first-level phase change, and after being separated from the high-phase-transition-temperature component, it is taken out. The high-phase-transition-temperature component is separated and taken out or enters the next cycle process as the low-temperature substance to be treated; the material cycle of the high-temperature temperature-controlled substance is as follows: the high-temperature temperature-controlled substance after heat exchange with the low-temperature substance to be treated enters the next cycle process after being reheated by reflux.

[0022] The present invention uses a high-temperature temperature-controlled substance with a phase-transition temperature between the phase-transition temperatures of the low-phase-transition-temperature component and the high-phase-transition-temperature component of the low-temperature substance to be treated to contact the surface of the low-temperature substance to be treated for mass transfer and heat transfer. The heat transfer direction is from the high-temperature temperature-controlled substance with low density to the low-temperature substance to be treated with high density. The heat transfer method is non-penetrating surface homogeneous mass transfer and heat transfer. The direct contact surface between the high-temperature temperature-controlled substance and the low-temperature substance to be treated is static, and no phenomena such as bubbles and boiling occur, which is beneficial to improving the mass transfer and heat transfer efficiency, making the low-temperature substance to be treated heated evenly and having a high component separation efficiency. Moreover, only the surface of the low-temperature substance to be treated is heated, and the temperature rise is limited by the phase-transition temperature of the high-temperature temperature-controlled substance, having the advantages of high efficiency, low energy consumption, and precise temperature control. Moreover, through the double-cycle process, each component is separated more thoroughly and concentrated, improving the purity of the collected materials of each component. The material cycle of the high-temperature temperature-controlled substance takes away the low temperature while the high-temperature temperature-controlled substance exchanges heat with the low-temperature substance to be treated, realizing the low-temperature dissipation of the treatment system, thereby realizing a "fully enclosed, continuous, stable, and controllable" microenvironment for the treatment system, reducing the consumption of the high-temperature temperature-controlled substance, and also achieving zero pollutant emissions due to the use of a fully enclosed treatment. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of the working principle of the constant-temperature double-cycle material separation method provided by the present invention, wherein: 1-treatment system, 2-high-temperature temperature-controlled substance generating device, 3-high-temperature temperature-controlled substance, 4-low-temperature substance to be treated, 5-low-phase-transition-temperature component, 6-high-phase-transition-temperature component, 7-external pipeline 1, 8-unidirectional power device 1, 9-external pipeline 2, 10-unidirectional power device 2, 11-multi-layer horizontal tank;

[0024] Figure 2Schematic diagram of the method for preparing Xanthoceras sorbifolium flower crude brandy in the embodiment, where: 1 - distillation kettle, 2 - rectifying column, 3 - cooling tower, 4 - primary distillate, 5 - gaseous ethanol and water azeotrope mixture, 6 - tray, 7 - Xanthoceras sorbifolium flowers dried at normal temperature, 8 - low-boiling fraction collection device, 9 - high-boiling fraction collection device, 10 - liquor collection device, 11 - valve. Detailed implementation mode

[0025] The present invention provides a constant-temperature double-cycle material separation method, which includes the following steps:

[0026] Two cycles are carried out in a fully enclosed treatment system. The two cycles include the material cycle of the high-temperature temperature-controlled substance and the material cycle of the low-temperature substance to be treated. The low-temperature substance to be treated includes a low-phase-transition-temperature component and a high-phase-transition-temperature component; the phase-transition temperature of the high-temperature temperature-controlled substance is between the phase-transition temperature of the low-phase-transition-temperature component and the phase-transition temperature of the high-phase-transition-temperature component;

[0027] The material cycle of the low-temperature substance to be treated is as follows: the high-temperature temperature-controlled substance is heated and then contacts with the low-temperature substance to be treated for heat exchange. During the heat exchange process, the latent heat of phase change of the high-temperature temperature-controlled substance causes the low-phase-transition-temperature component in the low-temperature substance to be treated to undergo a first-order phase change, and is taken out after being separated from the high-phase-transition-temperature component. The high-phase-transition-temperature component is taken out separately or enters the next cycle process as the low-temperature substance to be treated;

[0028] The material cycle of the high-temperature temperature-controlled substance is as follows: the high-temperature temperature-controlled substance after heat exchange with the low-temperature substance to be treated is reheated by reflux and then enters the next cycle process.

[0029] Unless otherwise specified, the present invention has no special requirements for the sources of the raw materials used, and commercially available products well-known to those skilled in the art can be used.

[0030] As an implementation mode, the high-temperature temperature-controlled substance, the low-phase-transition-temperature component and the high-phase-transition-temperature component are substances with first-order phase change properties; the phase change of the substances with first-order phase change properties in the treatment system is temperature-constant and related to the internal environmental pressure of the treatment system. The present invention aims to control the upper temperature limit, that is, to control the temperature of the treatment system below the phase-transition temperature of the high-temperature temperature-controlled substance. For example, when the concentration of ethanol is 95.6% and the concentration of water is 4.4%, the azeotropic boiling point (i.e., the phase-transition temperature of the azeotrope) of the gaseous ethanol and water azeotrope is 78.13 °C. At this time, the temperature of the circulating treatment system is controlled below this temperature. Because the pressure remains unchanged, the proportion of the azeotrope components remains unchanged and the circulating treatment is adopted, although the temperature of the treatment system will change with the above influencing factors, the temperature of the treatment system cannot rise above the phase-transition temperature of the high-temperature temperature-controlled substance.

[0031] As an implementation manner, the high-temperature temperature control substance is a gaseous substance or a liquid substance; the gaseous substance or the liquid substance is a pure substance or a mixture; the gaseous substance is a gaseous azeotrope or a gaseous non-azeotropic mixture, and in a specific embodiment, it is a gaseous non-azeotropic mixture; for the gaseous non-azeotropic mixture, the boiling range of the mixture can be greatly changed by adjusting the components, so as to provide a simple and feasible temperature control method for a high-temperature temperature control substance.

[0032] As an implementation manner, when the high-temperature temperature control substance is a gaseous substance, it can be high-temperature steam; when the high-temperature temperature control substance is a liquid substance, it can be high-temperature liquid metal. During the circulation process, the high-temperature temperature control substance may instantaneously undergo a phase change locally, but due to the adoption of circulation treatment, only part of the latent heat of phase change is released by the high-temperature temperature control substance overall, and generally no phase change occurs. For example, when using high-temperature liquid copper as the high-temperature temperature control substance to separate a low-temperature substance containing aluminum and iron, aluminum melts first, mixes with copper and is separated from iron, and then cooling can cause the copper to undergo a phase change and solidify to be separated from aluminum, thereby removing aluminum, and the copper continues to be used as the high-temperature temperature control substance and added to the next circulation process.

[0033] As an implementation manner, the low-phase-change-temperature component in the low-temperature substance to be treated is gaseous, liquid or solid, and the high-phase-change-temperature component is liquid or solid. During the circulation separation process, the low-phase-change-temperature component may be separated through solid-liquid phase change or liquid-gas phase change, and the high-phase-change-temperature component may be separated through solid-liquid phase change.

[0034] The main difference between the first-order phase change and the second-order phase change lies in the continuity of the thermodynamic functions and their derivatives during the phase change process and whether latent heat and volume changes are accompanied. The present invention is only applicable to the first-order phase change substances accompanied by the release or absorption of latent heat of phase change. With partial release of the latent heat of phase change of the high-temperature temperature control substance, only the low-phase-change-temperature component in the low-temperature substance to be treated is released. Since the treatment process is cyclic, flowing, contacting, mass-transferring, and heat-transferring, the high-phase-change-temperature component in the low-temperature substance to be treated cannot undergo the same phase change as the low-phase-change-temperature component due to the existence of the latent heat of phase change, and thus is separated in a liquid or solid form.

[0035] In the material circulation process of the high-temperature temperature control substance in the present invention, the high-temperature temperature control substance exchanges heat with the low-temperature substance to be treated and simultaneously takes away the low temperature, realizing "low-temperature dissipation" of the treatment system, thereby realizing a "fully enclosed, continuous, stable, and controllable" microenvironment of the treatment system.

[0036] As an implementation method, the feeding method of the low-temperature substance to be treated is batch feeding or unidirectional continuous cyclic feeding, and in a specific embodiment, it is batch feeding; the above feeding method can increase the direct contact area between the high-temperature temperature-controlled substance and the low-temperature substance to be treated or improve the surface contact efficiency during the cyclic flow process. During the cyclic process of the low-temperature substance to be treated, it is equivalent to the high-temperature temperature-controlled substance contacting different surfaces of the low-temperature substance to be treated. For example, when the low-temperature substance to be treated is in a liquid state, during the flowing process, it is equivalent to continuously changing the interfacial molecules contacting the high-temperature temperature-controlled substance. Therefore, it is equivalent to increasing the liquid surface area, thereby greatly improving the heat exchange efficiency.

[0037] As an implementation method, when the low-temperature substance to be treated is added by the method of unidirectional continuous cyclic feeding, at the end of each cyclic process, the low-temperature substance to be treated that has not been completely treated is re-added to the treatment system as raw material along with the cycle and enters the next cyclic process; therefore, in the cyclic separation process of the present invention, it is not necessary to completely separate the substances of the low-temperature substance to be treated in each cyclic separation process.

[0038] As an implementation method, when the high-temperature temperature-controlled substance is a gaseous azeotrope, the azeotropic point of the gaseous azeotrope is between the phase change temperatures of the low-phase-change-temperature component and the high-phase-change-temperature component of the low-temperature substance to be treated. The gaseous azeotrope has the advantages of economy, easy availability, fast mass transfer and heat transfer speed, high efficiency, etc.; when the high-temperature temperature-controlled substance is a gaseous non-azeotropic mixture, the difference from the gaseous azeotrope is that it has a dynamic boiling range, and a wider temperature control range can be obtained by adjusting the proportion of each component of the gaseous non-azeotropic mixture under constant pressure. In the present invention, the composition of the gaseous azeotrope can be arbitrarily selected, and the selection principle is that it has the characteristics of a high-temperature temperature-controlled substance, that is, a first-order phase change property substance and the phase change temperature is between the phase change temperatures of the low-phase-change-temperature component and the high-phase-change-temperature component of the low-temperature substance to be treated, and it can be a multi-component mixture.

[0039] As an implementation method, the thermal conductivity of the high-temperature temperature-controlled substance is determined according to the selected high-temperature temperature-controlled substance, and in a specific embodiment, it is determined according to the proportion of ethanol and water in the selected gaseous ethanol-water azeotrope. The high thermal conductivity of the high-temperature temperature-controlled substance in the present invention is beneficial to improving the response speed, efficiency and long-term stability of the temperature control of the high-temperature temperature-controlled substance.

[0040] As an implementation manner, the high-temperature temperature control substance is monitored and replaced in a timely manner to prevent performance degradation of the high-temperature temperature control substance, such as a decrease in phase change enthalpy and a shift in phase change temperature, from affecting the temperature control effect. In the present invention, the thermal conductivity can be detected by sampling or in real time by a thermal conductivity measuring instrument. The principle generally uses the transient heat source method in the unsteady state method to measure. There are many factors affecting the thermal conductivity. For example, the factors causing the change in the thermal conductivity of water include temperature, pressure, purity and state of water, etc. Therefore, when the detection shows that it is inappropriate, the high-temperature temperature control substance can be directly replaced.

[0041] As an implementation manner, the low-temperature substance to be processed is a substance with fluidity; when the low-temperature substance to be processed does not have fluidity, the low-temperature substance to be processed is made to have fluidity by crushing; the non-fluid low-temperature substance to be processed is converted into a substance with fluidity through the pretreatment method of crushing to increase its surface area.

[0042] As an implementation manner, when the substance with first-order phase change properties in the treatment system is in a gaseous state, the phase change temperature of the substance with first-order phase change properties is changed by changing the pressure of the treatment system, thereby realizing the control of the temperature of the treatment system, which has the advantages of simplicity and rapidity.

[0043] As another implementation manner, the azeotropic point of the gaseous azeotrope as the high-temperature temperature control substance is changed by changing the pressure of the treatment system, thereby accurately controlling the upper temperature limit of the treatment system.

[0044] As an implementation manner, the phase change temperature of the high-temperature temperature control substance is adjusted by means of vacuum distillation or by pressurizing the treatment system. Vacuum distillation reduces the phase change temperature of the gaseous high-temperature temperature control substance, and the method of pressurizing the treatment system increases the phase change temperature of the high-temperature temperature control substance, thereby realizing temperature control by changing the pressure.

[0045] In the present invention, the quantitative relationship between pressure and temperature control changes with the selection of the high-temperature temperature control substance. For example, the temperature of the gaseous ethanol and water non-azeotropic mixture changes with the ratio of ethanol to water under normal pressure. The lower the proportion of ethanol component, the higher the temperature of the gaseous ethanol and water non-azeotropic mixture, which can vary between 78.13 °C and 100 °C. The boiling point of ethanol is 78.3 °C, and the boiling point of water is 100 °C. The azeotropic point of the ethanol and water azeotrope is 78.13 °C. At this time, the concentration of ethanol is 95.6%, and the concentration of water is 4.4%. Changing the component ratio will change the azeotropic point (boiling range) of the non-azeotropic mixture.

[0046] As an implementation manner, the heating of the high-temperature temperature control substance refers to the high-temperature temperature control substance generated by a high-temperature temperature control substance generating device; the high-temperature temperature control substance generating device is a distillation kettle or a furnace; the treatment system is a rectification tower or a furnace, specifically a rectification tower in a specific embodiment; the high-temperature temperature control substance generating device is communicated with the treatment system; the treatment system is provided with a collecting device for the low-phase-change-temperature component in the low-temperature substance to be treated; the treatment system is provided with a collecting device for the high-phase-change-temperature component in the low-temperature substance to be treated; the treatment system is provided with two sets of external pipelines and a unidirectional power device, one of which is used for the material circulation of the low-temperature substance to be treated, and the other is used for the circulation of the high-temperature temperature control substance; the unidirectional power device is an air pump or an exhaust fan, specifically an air pump in a specific embodiment. The present invention enables the high-temperature temperature control substance to form a unidirectional circulation power through the unidirectional power device. In the present invention, the internal and external pipelines of the treatment system form a circulation under the action of the unidirectional power to achieve temperature control of the treatment system. If only a circulation flow of the high-temperature temperature control substance is formed inside the treatment system, the properties of the high-temperature temperature control substance during the treatment process cannot be controlled, including the real-time consumption amount of the latent heat of phase change of the high-temperature temperature control substance. The main purpose of the external pipeline is to assist in control, construct a fully enclosed circulation, and achieve zero pollutant emissions.

[0047] As an implementation manner, when the high-temperature temperature control substance after heating the low-temperature substance to be treated is collected, a valve is provided between the external pipeline and the high-temperature temperature control substance generating device, and a cooling device and a collecting device are provided between the external pipelines; the cooling device is a cooling tower.

[0048] As an implementation manner, when the pressure of the treatment system is a constant pressure, the temperature of the treatment system is controlled by controlling the properties and / or the reflux speed of the high-temperature temperature control substance, which has the advantages of simplicity and rapidity. The high-temperature temperature control substance controls the upper temperature limit of all substances in the treatment system not to be higher than the phase change temperature of the high-temperature temperature control substance.

[0049] In the present invention, the constant pressure refers to the pressure selected by the treatment system. For example, the rectification tower selects atmospheric rectification, or vacuum rectification at different pressure levels can also be selected. The constant pressure of the treatment system can be effectively controlled by an external device, such as a vacuum distillation device.

[0050] In the present invention, when the selected constant pressure is different, the temperature of the gaseous high-temperature temperature control substance formed in the treatment system will change accordingly, which is directly related to the phase change temperatures of the high-temperature temperature control substance and the low-temperature substance to be treated in the treatment system. For example, if the high-temperature temperature control substance is water, when the pressure of the treatment system is 101.3 kPa, the boiling point of water is 100 °C; when the pressure drops to 12.34 kPa, the boiling point of water is 50 °C; when the pressure is 198.5 kPa, the boiling point temperature of water is 121.3 °C.

[0051] As an implementation manner, when the high-temperature temperature control substance is a gaseous azeotropic mixture, the temperature of the treatment system is controlled by controlling the proportion of each component in the high-temperature temperature control substance. The present invention changes the temperature of the treatment system by controlling the proportion of each component in the gaseous azeotropic mixture of the high-temperature temperature control substance.

[0052] In the present invention, the phase change temperature property of the high-temperature temperature control substance, for example, when the high-temperature temperature control substance is a gaseous mixture, the boiling range of the mixture can be changed by changing the proportion of each component of the mixture. Except for azeotropic mixtures, the mixture has no boiling point, so the boiling range is mentioned here.

[0053] In the present invention, the composition of the gaseous azeotropic mixture is related to the raw material selection in the gaseous azeotropic mixture generation device. The types and proportions of each component substance determine the boiling range of the gaseous azeotropic mixture. The raw material selection for generating the gaseous azeotropic mixture usually only needs to select a range value. For example, as long as the two components of ethanol and water exist, a gaseous ethanol-water azeotropic mixture can be formed. After formation, the boiling range of the gaseous ethanol-water azeotropic mixture is below 100 °C. In the embodiment of the present invention, the raw material for generating the gaseous ethanol-water azeotropic mixture is the primary distillate of fruit fermentation broth, which contains many impurities. However, when the volume ratio of ethanol is 26% - 29%, a gaseous ethanol-water azeotropic mixture can be effectively formed, and the cycle temperature can be stably controlled at about 80 °C. If the ethanol ratio is about 2%, the temperature of the formed gaseous azeotropic mixture will rise above 95 °C due to the too low ethanol proportion.

[0054] As an implementation manner, by controlling the proportion of each component of the gaseous azeotropic mixture in the cyclic separation process to be relatively constant, the temperature of the treatment system is controlled to be relatively constant.

[0055] The present invention controls the temperature change or constancy by changing the treatment system pressure and the properties of the high-temperature temperature control substance, and has the advantages of accuracy, simplicity, and rapidity. The treatment system pressure can be adjusted by external equipment devices of the treatment system. For example, vacuum distillation can be achieved by an air pump. The degree of pressure control needs to be determined according to the requirements of material separation and related treatments in the treatment system. For example, when treating Xanthoceras sorbifolium flowers, high pressure cannot be used, otherwise the food properties of Xanthoceras sorbifolium flowers will be changed (Xanthoceras sorbifolium flowers will become'mud' under high pressure). By changing the properties of the high-temperature temperature control substance, the temperature change or constancy is controlled. For example, in Example 1 of the present application, when the proportion of recycled ethanol decreases, the proportion of ethanol in the high-temperature temperature control substance generation device becomes smaller, so that the proportion of ethanol in the generated gaseous ethanol-water azeotropic mixture becomes smaller. At this time, the temperature of the treatment system will rise, and its upper limit is the boiling point temperature of water, that is, 100 °C. Correspondingly, by controlling the real-time reflux of ethanol to the high-temperature temperature control substance generation device and maintaining the ethanol within a certain concentration range in the high-temperature temperature control substance generation device, the temperature of the treatment system can be kept constant.

[0056] The present invention uses a gaseous azeotropic mixture as a high-temperature temperature control substance, which has the advantages of high penetrability while ensuring accurate temperature control. The penetrability of gaseous substances is higher than that of liquid substances. For example, when liquid water comes into surface contact with an object, it is often unable to effectively contact the object surface due to the formation of tiny bubbles on the object surface, which has a greater impact on killing microorganisms on the object surface. Microorganisms can survive due to the protection of tiny bubbles, but gaseous substances do not form a protective layer in the form of tiny bubbles and can effectively and thoroughly kill microorganisms. The gaseous azeotropic mixture as a high-temperature temperature control substance can simultaneously meet the requirements of high penetrability and accurate temperature control in the process of temperature control and microorganism inactivation during food processing, which is conducive to the surface contact, circulation, mass transfer, and heat transfer between the high-temperature temperature control substance and the low-temperature substance to be processed.

[0057] As an implementation manner, the low-temperature substance to be processed is placed in a multi-layer horizontal tank for circulating treatment. The multi-layer horizontal tank can increase the contact area between the low-temperature substance to be processed and the high-temperature temperature control substance, and can improve the mass transfer and heat transfer efficiency during the circulating flow. The heat exchange between the lower surface and the side surface of the multi-layer horizontal tank and the high-temperature temperature control substance plays a role in preheating the low-temperature substance to be processed flowing unidirectionally in the multi-layer horizontal tank. In the present invention, the multi-layer horizontal tank only provides a possibility for optimizing the effective treatment when the treatment amount of the low-temperature substance to be processed increases here. The qualitative and quantitative indicators such as the number of layers, size, and shape of the multi-layer horizontal tank need to be determined according to the properties, treatment amount, and design objectives of the treatment device of the low-temperature substance to be processed, and the present invention has no special restrictions on this.

[0058] As an implementation manner, after the low-phase-change-temperature component and the high-phase-change-temperature component of the low-temperature substance to be processed are separated, a small amount of known high-temperature temperature control substance impurities are removed by changing the pressure or temperature, which has the advantages of simplicity and convenience. Since the phase-change temperatures of the high-temperature temperature control substance and the low-phase-change-temperature component and the high-phase-change-temperature component of the low-temperature substance to be processed are different, when a small amount of known high-temperature temperature control substance is mixed with the low-phase-change-temperature component and the high-phase-change-temperature component of the low-temperature substance to be processed, only by effectively controlling the change of the pressure or temperature of the external circulation pipeline, the phase-change temperature or the temperature of the high-temperature temperature control substance can be changed to cause component separation. If a higher purity requirement is needed, existing purification technologies can be adopted in the design of the external circulation pipeline.

[0059] As an implementation manner, when the low-temperature substance to be treated is a multi-component separation, high-temperature temperature control substances with different phase change temperatures are used for stepwise separation. Only the high-temperature temperature control substance needs to be replaced, and there is no need to construct a multi-layer separation tower, thereby reducing production costs and improving production safety. The constant-temperature double-cycle substance separation method provided by the present invention has low requirements for equipment accuracy and can greatly reduce production costs. The replacement of the high-temperature temperature control substance needs to be determined according to the low-temperature substance to be treated. For example, when the temperature at which the component separation of two different low-phase change temperature components and high-phase change temperature components of the low-temperature substance to be treated needs to be controlled at 80 °C and 100 °C, it can be achieved by replacing the high-temperature temperature control substance with the corresponding phase change temperature. For example, changing from an ethanol-water azeotropic mixture to pure water.

[0060] As an implementation manner, the high-temperature temperature control substance, the low-temperature substance to be treated, and the separated low-phase change temperature component and high-phase change temperature component are all subjected to a fully enclosed circulation treatment, thereby achieving zero pollutant emissions.

[0061] As an implementation manner, the device used for the fully enclosed circulation treatment is the fully enclosed fluid pollutant purification device disclosed in CN115569474A.

[0062] In the present invention, while the high-temperature temperature control substance and the low-temperature substance to be treated perform surface contact mass transfer and heat transfer with each other during their respective unidirectional circulations, the heat transfer direction is from the high-temperature temperature control substance with low density to the low-temperature substance to be treated with high density, and the heat transfer method is non-penetrating surface homogeneous mass transfer and heat transfer. During the mass transfer and heat transfer process of the high-temperature temperature control substance and the low-temperature substance to be treated, the direct contact surface is static, and no phenomena such as bubbles and boiling occur, which is beneficial to improving the mass transfer and heat transfer efficiency.

[0063] Since the phase change temperature of the substance with first-order phase change properties in the treatment system is fixed, and under the same temperature and pressure, the heat absorbed or released when the substance changes from one phase to another, that is, the latent heat of phase change, is related to the type of substance, the type of phase change, and the energy conversion situation during the phase change process. During the treatment process, only the surface of the low-temperature substance to be treated is heated, and the temperature increase is limited by the phase change temperature of the high-temperature temperature control substance. Therefore, the constant-temperature double-cycle substance separation method provided by the present invention has the advantages of high efficiency, low energy consumption, precise temperature control, etc., thereby greatly reducing the energy consumption during the treatment process.

[0064] Figure 1 It is a schematic diagram of the working principle of the constant-temperature double-cycle substance separation method provided by the present invention. As Figure 1As shown, in the 1-treatment system, the phase change temperature of the 3-high-temperature temperature control substance generated by heating with the 2-high-temperature temperature control substance generating device is between the 5-low phase change temperature component and the 6-high phase change temperature component in the 4-low-temperature substance to be treated. During the treatment process, after the 3-high-temperature temperature control substance is generated, under the action of the 8-unidirectional power device 1 in the 7-external pipeline 1, a mass cycle of the 3-high-temperature temperature control substance between the 1-treatment system and the 7-external pipeline 1 is formed; after the 4-low-temperature substance to be treated is added, under the action of the 10-unidirectional power device 2 in the 9-external pipeline 2, a mass cycle of the 4-low-temperature substance to be treated between the 1-treatment system and the 9-external pipeline 2 is formed during the flow of the 4-low-temperature substance to be treated on the 11-multilayer horizontal tank; the mass cycle of the 3-high-temperature temperature control substance and the mass cycle of the 4-low-temperature substance to be treated are carried out in the 1-treatment system for surface contact, circulation, mass transfer, and heat transfer between the 3-high-temperature temperature control substance and the 4-low-temperature substance to be treated, so that the 5-low phase change temperature component and the 6-high phase change temperature component of the 4-low-temperature substance to be treated are separated due to the phase change temperature limit, and then a small amount of the known 3-high-temperature temperature control substance that may be mixed in the 5-low phase change temperature component and the 6-high phase change temperature component is removed, and finally the processes of component separation, enrichment, or food processing of the 4-low-temperature substance to be treated are completed. During this process, the temperature of the 1-treatment system can be controlled by changing the pressure of the 1-treatment system or changing the properties of the 3-high-temperature temperature control substance; the 5-low phase change temperature component is separated and collected first during the treatment process due to its lower phase change temperature; the 6-high phase change temperature component can be separated and taken out at any time in the 9-external pipeline 2 or enter the next mass cycle of the 4-low-temperature substance to be treated as the 4-low-temperature substance to be treated; during the treatment process, due to the phase change temperature limit, the highest temperature in the 1-treatment system is controlled below the phase change temperature of the 3-high-temperature temperature control substance. The method provided by the present invention has the advantages of high efficiency, low energy consumption, precise temperature control, etc., and at the same time realizes zero pollutant emission due to the use of a fully enclosed cycle.

[0065] The present invention separates substances through a constant-temperature double-cycle process. In a system with the same internal environmental pressure, the phase-transition temperature of substances with first-order phase-transition properties is constant and related to the internal environmental pressure. The constant-temperature double-cycle substance separation method provided by the present invention, under the condition of constant internal environmental pressure, uses a substance with a phase-transition temperature between the low-phase-transition-temperature component and the high-phase-transition-temperature component of the low-temperature substance to be treated as the high-temperature temperature-control substance. After heating, by controlling the double cycle in the same treatment system, that is, the substance cycle of the high-temperature temperature-control substance and the substance cycle of the low-temperature substance to be treated, surface contact, circulation, mass transfer, and heat transfer are carried out, so that the low-phase-transition-temperature component and the high-phase-transition-temperature component of the low-temperature substance to be treated are separated due to the phase-transition temperature limit. After separation, a small amount of the known high-temperature temperature-control substance can be removed to further purify the components. The substance cycle of the low-temperature substance to be treated is implemented by means of batch feeding or unidirectional continuous circulation feeding, etc., to increase the direct contact area between the high-temperature temperature-control substance and the low-temperature substance to be treated or improve the surface contact efficiency during the circulating flow process. When using unidirectional continuous circulation feeding, at the end of each cycle separation, the low-temperature substance to be treated that has not been completely treated can be used as raw material and re-added to the treatment system with the cycle separation process to enter the next cycle separation. Therefore, it is not necessary to completely separate the substances of the low-temperature substance to be treated in each cycle separation. Transient extraction with a non-azeotropic mixture of gaseous ethanol and water alone cannot concentrate aromatic substances, and at the same time, a large amount of the non-azeotropic mixture of gaseous ethanol and water is consumed, and a high-level reduction degree of the treated food cannot be achieved. When only using the non-azeotropic mixture of ethanol and water for extraction, there is a risk of incorporating allergic substances. The constant-temperature double-cycle substance separation method provided by the present invention makes the separation of each component more thorough through multiple cycle processes of the substance cycle of the high-temperature temperature-control substance and the substance cycle of the low-temperature substance to be treated, and enriches them, improves the purity of the collected substances of each component, and can realize a "fully enclosed, continuous, stable, and controllable" microenvironment in the treatment system, reducing the consumption of the high-temperature temperature-control substance.

[0066] The ethanol-water azeotrope-free mixture has a broad-spectrum effect of inactivating microorganisms, combining the penetrability of ethanol and high-temperature steam, the effect of denaturing microbial proteins, and the enhanced effect of inactivating microorganisms by releasing potential heat. Compared with using high-temperature steam alone to inactivate microorganisms, the temperature drops significantly. Compared with using ethanol solutions with different concentrations alone to inactivate microorganisms, the irreversible inactivation effect of releasing potential heat is added, overcoming the problem that microorganisms cannot be completely inactivated due to the reversibility of protein denaturation caused by ethanol. Moreover, the constant-temperature double-cycle material separation method can provide a "fully enclosed, continuous, stable, and controllable" microenvironment, which cannot be achieved simply with the ethanol-water azeotrope-free mixture. For example, when the gaseous ethanol-water azeotrope-free mixture contacts the low-temperature material to be treated, only "heat conduction from high temperature to low temperature" can be achieved, but low-temperature dissipation cannot be realized. If the low temperature of the microenvironment cannot dissipate or dissipates too slowly, as the low-temperature material to be treated is continuously added, the temperature of the microenvironment will gradually decrease, and the inactivation effect will gradually decrease, allowing some microorganisms to survive. At the same time, a large amount of the high-temperature temperature-control substance may also undergo a phase change, and a continuous and stable microenvironment cannot be obtained. The microenvironment loses balance, and complete inactivation of microorganisms cannot be achieved. The constant-temperature double-cycle material separation method provided by the present invention can realize the low-temperature dissipation of the treatment system through the material cycle of the high-temperature temperature-control substance, enabling heat exchange between the high-temperature temperature-control substance and the low-temperature material to be treated while taking away the low temperature, thereby realizing a "fully enclosed, continuous, stable, and controllable" microenvironment in the treatment system and completely inactivating microorganisms. Therefore, using the constant-temperature double-cycle material separation method based on the gaseous ethanol-water azeotrope-free mixture to inactivate microorganisms has obvious advantages.

[0067] The present invention also provides the application of the constant-temperature double-cycle material separation method described in the above technical solution in material separation, concentration, and surface treatment.

[0068] As an implementation manner, the material separation includes preparing original Xanthoceras sorbifolium Bunge flower brandy; the surface treatment includes microbial inactivation; the microbial inactivation includes inactivating the surface microorganisms of freshly picked Datong Flammulina velutipes in the wild.

[0069] As an implementation manner, during the process of preparing the original Xanthoceras sorbifolium Bunge flower brandy, the high-temperature temperature-control substance is a gaseous ethanol-water azeotrope-free mixture, and the low-temperature material to be treated is air-dried Xanthoceras sorbifolium Bunge flowers at room temperature. The temperature of the gaseous ethanol-water azeotrope-free mixture is 80°C to 85°C, and in a specific embodiment, it is 85°C.

[0070] As an implementation manner, during the process of inactivating the surface microorganisms of freshly picked Datong Flammulina velutipes in the wild, the high-temperature temperature-control substance is a gaseous ethanol-water azeotrope-free mixture, and the low-temperature material to be treated is freshly picked Datong Flammulina velutipes in the wild. The temperature of the gaseous ethanol-water azeotrope-free mixture is 80°C to 85°C, and in a specific embodiment, it is 85°C.

[0071] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, but they should not be construed as limiting the protection scope of the present invention.

[0072] Example 1 Preparation of Xanthoceras sorbifolium Bunge flower original brandy

[0073] Based on the constant-temperature double-cycle material separation method, this example uses the primary distillate obtained after distilling grape fermentation broth to treat air-dried Xanthoceras sorbifolium Bunge flowers at room temperature to obtain Xanthoceras sorbifolium Bunge flower original brandy with a unique flavor. During the treatment process, while removing harmful low-phase-transition-temperature components such as methanol and acetaldehyde and high-phase-transition-temperature components such as higher alcohols that cause sensory discomfort in the volatile components of the primary distillate and air-dried Xanthoceras sorbifolium Bunge flowers, the original aroma components such as alcohols, acids, and esters in the volatile components of the primary distillate and air-dried Xanthoceras sorbifolium Bunge flowers are incorporated into the gaseous ethanol-water azeotropic mixture. During the cyclic treatment process, since the main substance is the gaseous ethanol-water azeotropic mixture, the small amount of impurities incorporated has little effect on the boiling range of the gaseous ethanol-water azeotropic mixture. On the one hand, the gaseous ethanol-water azeotropic mixture acts as a high-temperature temperature-control substance to keep the temperature of the treatment system constant during the circulation process of the treatment system and the external pipeline, and does not exceed the boiling range of the gaseous ethanol-water azeotropic mixture. On the other hand, the original aroma components of air-dried Xanthoceras sorbifolium Bunge flowers are incorporated into the gaseous ethanol-water azeotropic mixture, and after cooling and collection, Xanthoceras sorbifolium Bunge flower original brandy with a unique flavor is formed. In addition, existing data shows that the boiling range of the gaseous ethanol-water azeotropic mixture is affected by the ethanol-water component ratio. When the mass percentage of ethanol in the gaseous ethanol-water azeotropic mixture is higher than 82.8%, the system temperature can be controlled below 80°C, which significantly reduces the treatment temperature compared with the treatment with 100°C steam under the same ambient pressure and enables precise temperature control.

[0074] The specific implementation process of this example is as Figure 2Perform with the shown wine still, where the 1 - distillation kettle (generation device of high - temperature controlled - temperature substance) is equipped with a 2 - rectifying column (treatment system) and a 3 - cooling tower (unidirectional power formed due to pressure change caused by volume change after the phase change of gaseous substances). Select organic Cabernet Sauvignon grapes, wash them after removing impurities, crush them, and ferment them. The filtered fermented liquid is distilled to obtain a 4 - primary distillate with an alcohol content of 26% - 29% (ABV) and add it to the 1 - distillation kettle. When the 1 - distillation kettle is heated under normal pressure (heated to the phase - change temperature of the gaseous high - temperature controlled - temperature substance, 80°C), the 4 - primary distillate is heated to form a 5 - gaseous ethanol - water azeotropic mixture (high - temperature controlled - temperature substance, containing a small amount of impurities), which comes into surface contact, circulation, mass transfer, and heat transfer with the 7 - air - dried Xanthoceras sorbifolium Bunge flowers (low - temperature substance to be treated, air - dried Xanthoceras sorbifolium Bunge flowers) added in batches on the 6 - tray in the 2 - rectifying column. During the unidirectional circulation treatment process, the gaseous ethanol - water azeotropic mixture is in direct surface contact with the air - dried Xanthoceras sorbifolium Bunge flowers and undergoes mass transfer and heat transfer. Part of the latent heat of phase change released by the gaseous ethanol - water azeotropic mixture causes the separation of the low - phase - change - temperature components and high - phase - change - temperature components of the volatile components in the air - dried Xanthoceras sorbifolium Bunge flowers, and they are respectively collected by the 8 - low - boiling - fraction collection device and the 9 - high - boiling - fraction collection device. At the same time, the surface microorganisms of the air - dried Xanthoceras sorbifolium Bunge flowers are inactivated by the gaseous ethanol - water azeotropic mixture; the harmful low - boiling - fraction components (low - phase - change - temperature components) such as methanol and acetaldehyde in the 4 - primary distillate and the volatile substances contained in the 7 - air - dried Xanthoceras sorbifolium Bunge flowers gather at the top of the 2 - rectifying column and are collected by the 8 - low - boiling - fraction collection device and removed; the high - boiling - fraction components (high - phase - change - temperature components) such as higher alcohols that cause sensory discomfort gather at the bottom of the 2 - rectifying column and are collected by the 9 - high - boiling - fraction collection device and removed; the original aroma components such as alcohols, acids, and esters in the air - dried Xanthoceras sorbifolium Bunge flowers are separated and collected by the 10 - wine - liquid collection device along with the 5 - gaseous ethanol - water azeotropic mixture and then circulated back to the 1 - distillation kettle and enter the next cycle of the high - temperature controlled - temperature substance. The 5 - gaseous ethanol - water azeotropic mixture forms a material cycle of the high - temperature controlled - temperature substance among the "2 - rectifying column, 3 - cooling tower, 10 - wine - liquid collection device, 11 - valve, 1 - distillation kettle" during the treatment process. After multiple cycles, the original aroma components of the air - dried Xanthoceras sorbifolium Bunge flowers are enriched in the 5 - gaseous ethanol - water azeotropic mixture. After cooling and collection, a Xanthoceras sorbifolium Bunge flower original brandy with a unique flavor is obtained in the 10 - wine - liquid collection device; during the implementation process, by controlling the reflux rate of the 4 - primary distillate with an alcohol content of 26% - 29% (ABV), the temperature of the 2 - rectifying column is kept constant below 85°C.

[0075] Example 2 Inactivate the surface microorganisms of wild freshly - picked Datong yellow flowers

[0076] This embodiment is based on the constant-temperature double-cycle material separation method and uses the device of Embodiment 1. Compared with Embodiment 1, the dried Xanthoceras sorbifolium Bunge flowers at room temperature are replaced with wild Datong yellow flowers picked immediately as the low-temperature material to be processed, for detecting the effect of the constant-temperature double-cycle material separation method on treating surface microorganisms of fresh food. During the implementation process, the wild Datong yellow flowers picked immediately are placed on the distillation column trays and processed by the constant-temperature double-cycle material separation method. The experiment shows that the surface microorganisms of the wild Datong yellow flowers picked immediately are inactivated and show regularity. In addition, similar to the treatment result of Embodiment 1, harmful low-boiling components such as methanol and acetaldehyde and high-boiling components such as higher alcohols that cause sensory discomfort in the primary distillate and the wild Datong yellow flowers picked immediately are separated and removed, and the original aroma components such as alcohols, acids, and esters in the wild Datong yellow flowers picked immediately are enriched, and Datong yellow flower original brandy with a unique flavor is obtained.

[0077] During the specific implementation process of this embodiment, the wild Datong yellow flowers picked immediately locally in Datong are placed on the distillation column trays and processed by the constant-temperature double-cycle material separation method. The experimental treatment time is counted as follows: When the non-azeotropic mixture of ethanol and water in the treatment device reaches a stable cycle, the power supply is suspended. After the sample is added to the treatment device, the power supply is turned on and the timing starts, until the treatment device suspends the power supply again. The treatment times are 3, 6, 9, and 12 min respectively.

[0078] Under normal pressure, the non-azeotropic mixture of gaseous ethanol and water contains 95.6% ethanol and 4.4% water. Generally, the azeotropic boiling point of the gaseous ethanol and water mixture is lower than the boiling points of the single components. The boiling point of ethanol is 78.3 °C, and the boiling point of water is 100 °C, while the gaseous ethanol and water mixture boils at 78.13 °C, which is lower than the boiling points of its components ethanol or water. This temperature is much lower than 100 °C. Compared with high-temperature steam for treating food, the loss of nutrients in food raw materials can be greatly reduced.

[0079] Comparative Example 1

[0080] The difference from Embodiment 1 is that the non-azeotropic mixture of gaseous ethanol and water formed by heating the primary distillate is directly brought into surface contact, circulation, mass transfer, and heat transfer with the dried Xanthoceras sorbifolium Bunge flowers at room temperature placed on the distillation column trays in the distillation column to obtain Xanthoceras sorbifolium Bunge flower original brandy, and the rest of the content is the same as that of Embodiment 1.

[0081] In Comparative Example 1, the transient simple extraction with the non-azeotropic mixture of gaseous ethanol and water cannot concentrate the aromatic substances, and at the same time, a large amount of the non-azeotropic mixture of gaseous ethanol and water needs to be consumed, and a high-level reduction degree of the treated food cannot be achieved. Moreover, if only the non-azeotropic mixture of ethanol and water is used for leaching, there is a risk of incorporating allergic substances.

[0082] The constant temperature double-circulation material separation method adopted in Example 1 enriches the original aroma components of the Xanthoceras sorbifolia flowers dried at room temperature in the non-azeotropic mixture of 5-gaseous ethanol and water through multiple cycles of material circulation of high-temperature temperature-controlled materials and material circulation of low-temperature treated materials, and is completely separated from other impurities. The flavor of the prepared Xanthoceras sorbifolia flower original brandy is richer than that in Comparative Example 1, and can achieve a "fully closed, continuous, stable, and controllable" microenvironment of the treatment system, reducing the consumption of the non-azeotropic mixture of gaseous ethanol and water.

[0083] Comparative Example 2

[0084] The difference from Example 1 is that the constant temperature double-circulation material separation method is not adopted, and the primary distillate is directly heated to form a non-azeotropic mixture of gaseous ethanol and water in a distillation tower to inactivate the surface microorganisms of wild Datong yellow flowers on the tower plate. The rest of the content is consistent with Example 1.

[0085] In Comparative Example 2, when the non-azeotropic mixture of gaseous ethanol and water comes into contact with the low-temperature treated substance, it can only "conduct from high temperature to low temperature", but cannot dissipate the low temperature. The low temperature of the microenvironment cannot dissipate or dissipates too slowly. Then, with the continuous addition of low-temperature treated substance, the temperature of the microenvironment will gradually decrease, and the inactivation effect will gradually decrease, allowing some microorganisms to survive. At the same time, the high-temperature temperature-controlling substance may also undergo a large number of phase changes, and a continuous and stable microenvironment cannot be obtained. The microenvironment loses balance and cannot completely inactivate the microorganisms.

[0086] The constant temperature double-circulation material separation method in Example 2 can realize the low temperature dissipation of the treatment system through the material circulation of the high-temperature temperature-controlling material, so that the high-temperature temperature-controlling material can exchange heat with the low-temperature treated material and take away the low temperature at the same time, thereby realizing a "fully closed, continuous, stable and controllable" microenvironment of the treatment system and completely inactivating the microorganisms.

[0087] Performance Testing

[0088] (1) The original brandy of Xanthoceras sorbifolia obtained by the preparation method of Example 1 was added with oak chips for aging as a sample group (JA), and a sample group of Xanthoceras sorbifolia flowers treated in parallel but without any room temperature drying was used as a blank control group (JH) for comparative experiments. The above two groups of samples were detected by gas chromatography-mass spectrometry and analyzed by metabolomics methods (commissioned by Shanghai Puling Biotechnology Co., Ltd.), and the VIP value of the first principal component of the OPLS-DA model (threshold>1) was combined with the p value of the unidimensional test (threshold<0.05) to find differentially expressed metabolites. The results are shown in Table 1. Among them, the qualitative method of differentially expressed metabolites uses a search of a self-built standard substance database.

[0089] Table 1 Differential metabolites between JA group and JH group

[0090]

[0091]

[0092] Note: VIP, i.e., variable projection importance, is obtained from the OPLS-DA model; P value is calculated from the Student's t-test; Log2FC, i.e., fold change value, is the logarithm (base 2) of the ratio of the mean normalized peak areas of the JA group and the JH group. A positive sign indicates that the average signal response value or concentration value of the substance in the JA group is greater than that in the JH group, while a negative sign indicates that the average signal response value or concentration value of the substance in the JA group is less than that in the JH group.

[0093] As can be seen from Table 1, a total of 31 differential metabolites were screened and identified in the JA group and the JH group, among which 15 substances decreased and 16 substances increased. It can be seen that the Xanthoceras sorbifolium Bunge flower raw brandy obtained by the constant temperature double-cycle substance separation method provided by the present invention does not detect harmful chemical components to the human body. At the same time, the original aroma components of the air-dried Xanthoceras sorbifolium Bunge flowers at room temperature are enriched, forming Xanthoceras sorbifolium Bunge flower raw brandy with a unique flavor.

[0094] (2) After the samples in Example 2 were processed and packaged for inspection, they were detected by Shandong Bayer Testing Co., Ltd. in accordance with GB4789.2-2022 (Food microbiological examination - Determination of total bacterial count) and GB4789.15-2016 (Food microbiological examination - Enumeration of molds and yeasts). The test results are shown in Table 2. The results show that when the treatment time is 6, 9, and 12 min, the total bacterial count, mold count, and yeast count are all < 10 CFU / g. According to the above national standard result judgment criteria, bacteria, molds, and yeasts are all "not detected"; when the treatment time is 3 min, the total bacterial count test result is 10 CFU / g, that is, the total bacterial colony detected is 1 CFU / g, and the mold count and yeast count test results are both < 10 CFU / g, that is, molds and yeasts are both "not detected". Compared with the blank control group samples without treatment by the constant temperature double-cycle substance separation method, the total bacterial count, mold count, and yeast count are 3.1×10 4 、1.2×10 2 、1.7×10 3 CFU / g respectively. The analysis shows that the inactivation of surface microorganisms on freshly picked wild Datong yellow flowers by the constant temperature double-cycle substance separation method provided by the present invention shows a regular change. The surface microorganisms on freshly picked wild Datong yellow flowers can be inactivated after 6 min of treatment. The surface microorganisms of types such as bacteria on freshly picked wild Datong yellow flowers cannot be completely inactivated after 3 min of treatment, but the microorganisms of types such as molds and yeasts can be completely inactivated.

[0095] Table 2 Detection results of the inactivation of surface microorganisms on freshly picked wild Datong yellow flowers by the constant temperature double-cycle substance separation method

[0096]

[0097] Note: When the detected colony counts (CFU / g) of the sample dilution ratios "1:10", "1:100", and "1:1000" are all "0, 0", the result is expressed as "<10".

[0098] Although the above embodiments have described the present invention in detail, they are only a part of the embodiments of the present invention rather than all of them. People can also obtain other embodiments based on these embodiments without creative efforts, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A constant temperature double circulation material separation method, characterized in that: include: Two cycles are carried out in a fully enclosed treatment system, the two cycles including a material cycle of a high-temperature temperature-controlling material and a material cycle of a low-temperature treated material, the low-temperature treated material including a low phase-change temperature component and a high phase-change temperature component; the phase-change temperature of the high-temperature temperature-controlling material is between the phase-change temperature of the low phase-change temperature component and the phase-change temperature of the high phase-change temperature component; The material cycle of the low-temperature processed material is as follows: the high-temperature temperature-controlling material is heated and then contacts the low-temperature processed material for heat exchange, during which the phase change latent heat of the high-temperature temperature-controlling material causes the low phase change temperature component in the low-temperature processed material to undergo a primary phase change, and is separated from the high phase change temperature component and then taken out, and the high phase change temperature component is separated and taken out or enters the next cycle as the low-temperature processed material; The material cycle of the high-temperature temperature-controlling material is as follows: the high-temperature temperature-controlling material after heat exchange with the low-temperature processed material is reheated by reflux and then enters the next cycle process.

2. The constant temperature double circulation material separation method according to claim 1, characterized in that: The high-temperature temperature-controlling substance, the low phase-change temperature component and the high phase-change temperature component are substances with primary phase-change properties.

3. The constant temperature double circulation material separation method according to claim 1, characterized in that: The low-temperature treated material is fed in batches or in a one-way continuous cycle.

4. The constant temperature double circulation material separation method according to claim 1 or 2, characterized in that: The high-temperature temperature-controlling substance is a gaseous substance or a liquid substance; the gaseous substance is a gaseous azeotrope or a gaseous non-azeotropic mixture.

5. The constant temperature double circulation material separation method according to claim 1 or 2, characterized in that: The low-temperature processed substance is a fluid substance; When the low-temperature processed material has no fluidity, the low-temperature processed material is made fluid by pulverizing.

6. The constant temperature double circulation material separation method according to claim 2, characterized in that: When the substance with the first-order phase change property in the processing system is in a gaseous state, the phase change temperature of the substance with the first-order phase change property is changed by changing the pressure of the processing system.

7. The constant temperature double circulation material separation method according to claim 1, characterized in that: When the pressure of the processing system is a constant pressure, the temperature of the processing system is controlled by controlling the phase change temperature property and / or the reflux rate of the high-temperature temperature-controlling material.

8. The constant temperature double circulation material separation method according to claim 4, characterized in that: When the high-temperature temperature-controlling substance is a gaseous non-azeotropic mixture, the temperature of the treatment system is controlled by controlling the ratio of each component in the high-temperature temperature-controlling substance.

9. Application of the constant temperature double circulation material separation method according to any one of claims 1 to 8 in material separation, concentration and surface treatment.

10. The use according to claim 9, characterized in that the substance separation includes preparing Xanthoceras sorbifolia flower original brandy; the surface treatment includes inactivating microorganisms; the inactivation of microorganisms includes inactivating the surface microorganisms of wild and collected Datong yellow flowers; In the process of preparing the Xanthoceras sorbifolia flower original brandy, the high-temperature temperature-controlling substance is a non-azeotropic mixture of gaseous ethanol and water, the low-temperature processed substance is Xanthoceras sorbifolia flower dried at room temperature, and the temperature of the non-azeotropic mixture of gaseous ethanol and water is 80° C. to 85° C.; In the process of inactivating microorganisms on the surface of wild freshly harvested Datong chrysanthemum, the high-temperature temperature-controlling material is a non-azeotropic mixture of gaseous ethanol and water, the low-temperature treated material is wild freshly harvested Datong chrysanthemum, and the temperature of the non-azeotropic mixture of gaseous ethanol and water is 80°C to 85°C.

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