阅读说明：本技术 一种用于分离酒类产品中乙醇的旋转带蒸馏装置及方法 (Rotary belt distillation device and method for separating ethanol in wine products ) 是由 刘卫 秦来来 韩兴博 马玉华 曾友石 于 2020-07-31 设计创作，主要内容包括：本发明公开一种用于分离酒类产品中乙醇的旋转带蒸馏装置及方法,装置由加热及控温系统、旋转搅拌系统、蒸馏柱组件、冷凝系统及回流比控制系统组成；加热及控温系统用于加热酒类产品,使可挥发组分以蒸汽形式进入蒸馏柱组件,并测量酒类混合液及蒸汽的温度；旋转搅拌系统驱动旋转带在蒸馏柱组件中高速旋转,迫使上升蒸汽和下降冷凝液进行气液交换,使乙醇在上升蒸汽不断富集；冷凝系统用于冷凝蒸馏柱组件顶部乙醇蒸汽,并将冷凝液导入回流比控制系统；回流比控制系统用于控制冷凝液馏出到收集瓶和回流至蒸馏柱组件的比例,以保证馏出液中乙醇的纯度。该装置具有残留量少,回收率高,馏出液中乙醇纯度高,安全性能好,易于实施的优点。(The invention discloses a rotary belt distillation device and a method for separating ethanol in wine products, wherein the device consists of a heating and temperature control system, a rotary stirring system, a distillation column component, a condensation system and a reflux ratio control system; the heating and temperature control system is used for heating the wine products, enabling the volatile components to enter the distillation column component in a steam form, and measuring the temperature of the wine mixed liquid and the steam; the rotary stirring system drives the rotary belt to rotate at a high speed in the distillation column component, so that ascending steam and descending condensate are forced to perform gas-liquid exchange, and ethanol is continuously enriched in the ascending steam; the condensing system is used for condensing ethanol steam at the top of the distillation column component and guiding the condensate into the reflux ratio control system; the reflux ratio control system is used for controlling the proportion of the condensed liquid distilled out to the collecting bottle and refluxed to the distillation column assembly so as to ensure the purity of the ethanol in the distillate. The device has the advantages of less residual quantity, high recovery rate, high purity of ethanol in distillate, good safety performance and easy implementation.)

1. A rotating belt distillation device for separating ethanol in wine products is characterized in that: comprises a heating temperature measuring system, a rotary stirring system, a distillation column component, a condensing system, a reflux ratio control system and a fraction collecting device;

the heating temperature control system is used for heating wine products, enabling volatile components to enter the distillation column assembly in a steam mode, and measuring the temperature of wine mixed liquid and the steam;

the distillation column assembly is inserted on the heating temperature control system, the top end of the distillation column assembly is communicated with the condensing system, the side surface of the distillation column assembly is communicated with the reflux ratio control system, and the distillation column assembly is used for guiding steam to rise into the condensing system;

the condensing system comprises a first condensing system and a second condensing system which are respectively arranged above and at one side of the distillation column component and communicated with the distillation column component;

the rotary stirring system penetrates through the inner cavities of the first condensation system and the distillation column assembly;

the reflux ratio control system comprises a flow guide swing part (11), an electromagnetic coil (12), a time relay (13), a liquid circulating pump (17) and a reflux chamber (26), the flow guide swing part (11) is arranged in the reflux chamber (26), the flow guide swing part (11) is hinged with the second condensation system, the electromagnetic coil (12) is arranged on one side of the flow guide swing part (11) and is positioned on the outer side of the reflux chamber (26), the time relay (13) is electrically connected with the electromagnetic coil (12), and the liquid circulating pump (17) is communicated with the reflux chamber (26) through a pipeline (27);

the fraction collecting device is arranged below one side of the diversion swing part (11) and communicated with the reflux chamber (26).

2. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 1, wherein: the distillation component comprises an outer sleeve (20) and a second inner sleeve (19) inserted in the outer sleeve (20), a condensate return opening (18) is formed in one side, close to the flow guide swing part (11), of the second inner sleeve (19), and the condensate return opening (18) is communicated with the liquid circulating pump (17) through a pipeline (27).

3. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 2, wherein: the first condensation system comprises a first-stage condensation sleeve (6), a first inner-layer sleeve (7) inserted in the first-stage condensation sleeve (6) and a drainage tip (24) fixedly connected to the bottom end of the first inner-layer sleeve (7), a transition cavity (25) is arranged between the first inner-layer sleeve (7) and the second inner-layer sleeve (19), the drainage tip (24) extends into the transition cavity (25), and the top end of the second inner-layer sleeve (19) is communicated with the transition cavity (25).

4. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 3, wherein: the second condensing system includes second grade condensation sleeve pipe (8), the inside vacuole formation (28) of second grade condensation sleeve pipe (8), cavity (28) slope sets up, cavity (28) top with transition chamber (25) communicate with each other, drainage tip (24) end stretches into cavity (28) top, cavity (28) bottom with water conservancy diversion goods of furniture for display rather than for use (11) are articulated.

5. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 1, wherein: the heating temperature measurement system comprises a tower kettle (23), an electric heating sleeve (22), a first temperature probe (9), a first temperature control instrument (10) and a second temperature probe (21), wherein the top end of the tower kettle (23) is connected with the bottom end of an outer sleeve (20) in an inserting mode, the tower kettle (23) is arranged above the electric heating sleeve (22), the first temperature probe (9) is connected to the side face of a transition cavity (25) in an inserting mode and stretches into the transition cavity (25), the second temperature probe (21) is connected to the side face of the tower kettle (23) in an inserting mode and stretches into the tower kettle (23), the first temperature probe (9) is electrically connected with the first temperature control instrument (10), and the second temperature probe (21) is electrically connected with the electric heating sleeve (22).

6. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 3, wherein: rotatory mixing system includes electric motor (1), speed controller (2), anchor clamps (3), sealing member (4) and rotatory area (5), electric motor (1) sets up one-level condensation sleeve pipe (6) top, electric motor (1) output with rotatory area (5) are passed through anchor clamps (3) fixed connection, anchor clamps (3) with cup joint between one-level condensation sleeve pipe (6) sealing member (4), electric motor (1) electric connection has speed controller (2).

7. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 6, wherein: the first inner layer sleeve (7) and the second inner layer sleeve (19) are coaxially arranged in the vertical direction, and the rotating belt (5) penetrates through the first inner layer sleeve (7) and the second inner layer sleeve (19) from top to bottom.

8. A rotary belt distillation apparatus for separating ethanol from an alcoholic product according to claim 4, wherein: the reflux chamber (26) is provided with a reflux side outlet (14) and a distillation side outlet (15), the reflux side outlet (14) is communicated with the liquid circulating pump (17) through a pipeline (27), the distillation side outlet (15) is communicated with the fraction collecting device, and the fraction collecting device is a collecting bottle (16).

9. A rotary belt distillation apparatus for separating ethanol from an alcoholic liquor product according to claim 8, wherein: first-order condenser tube (6) outside is provided with first water inlet (6A), first delivery port (6B), second grade condenser tube (8) outside is provided with second water inlet (8A), second delivery port (8B), second water inlet (8A) with return side export (14) are adjacent, first water inlet (6A), first delivery port (6B), second water inlet (8A), second delivery port (8B) are external to have the circulation cold water ware.

10. A method of using a rotary belt distillation apparatus for separating ethanol from alcoholic beverages according to any one of claims 1 to 9, the method comprising the steps of:

s1: putting the alcoholic liquor product to be separated into the tower kettle (23), starting the power supply of the electric heating sleeve (22), the time relay (13), the circulating water cooler and the liquid circulating pump (17), setting the electrifying time of the electromagnetic coil (12) to be 0, and starting to heat the alcoholic liquor product in the tower kettle (23);

s2: when the alcohol mixed liquid in the tower kettle (23) begins to boil, and the temperature measured by the first temperature probe (9) gradually rises to 78.0-78.5 ℃, the power supply of the electric motor (1) is started, the rotating speed is set to 1000-3000RPM, the heating power of the electric heating sleeve (22) is adjusted, so that the ethanol condensate in the reflux ratio control system is dripped along the flow guide swing part (11) gradually, slowly and uniformly, and the ethanol condensate is dripped for 5-30 minutes to reach an equilibrium state;

s3: after the balance state is reached, setting the ratio of the power-on time to the power-off time of the electromagnetic coil (12) to be 1:1-1:99, keeping the time ratio constant as a reflux ratio, and collecting distilled ethanol distillate when the temperature measured by the first temperature probe (9) is 78-78.5 ℃;

s4: when the temperature measured by the first temperature probe (9) exceeds 78.5 ℃, resetting the electrifying time of the electromagnetic coil (12) to be 0, and stopping collecting ethanol distillate for 5 minutes to avoid collecting water;

s5: when the temperature measured by the first temperature probe (9) falls back to 78.0 ℃, setting the reflux ratio according to the time proportion in the step S3, and collecting the ethanol distillate again until the temperature measured by the first temperature probe (9) exceeds 78.5 ℃;

s6: repeating the steps S4 and S5 until the temperature measured by the first temperature probe (9) is obviously higher than 78.5 ℃, and the ethanol does not fall back again, which indicates that the ethanol in the wine product is completely separated;

s7: closing the power supply of the electric heating sleeve (22) and the time relay (13), reducing the rotating speed of the electric motor (1) to 100-500RPM, closing the power supply of the electric motor (1) and the circulating water cooler after the temperature measured by the first temperature probe (9) falls back to the ambient temperature, and measuring the quality of the distillate and the purity of the ethanol in the collecting bottle (16);

s8: and (3) purging the rotary belt (5) distillation device for 10 minutes by using pure inert gas, pure nitrogen or dry air to remove residual water and ethanol in the device.

Technical Field

The invention relates to the field of liquid separation, in particular to a rotary belt distillation device and a rotary belt distillation method for separating ethanol in wine products.

Background

In recent years, with the continuous and high-speed development of the economy of China, the consumption of liquor products such as white spirit, wine and the like is rapidly increased. However, a few illegal vendors are driven by interests, and fraud behaviors such as adulteration, annual adulteration and the like occur in the production and sale processes of wine products. Currently, the counterfeiting behaviors existing in the wine product industry at home and abroad can be classified into the following categories: blending industrial alcohol; manufacturing a fake product in a production place, such as a domestic faking import or a domestic filling faking original bottle import; making fake by year, collecting original bottles aiming at the wine of famous brands, filling the wine of different years, or changing the years; water mixing, sugar mixing and counterfeiting, etc.

At present, methods commonly used in the field of food detection, such as an optical or electron microscope, a high performance liquid chromatography analysis method, a gas mass spectrometer method, a differential thermal scanner method, a near infrared spectroscopy method and the like, can only detect the composition and the content of the components of wine products, cannot determine whether the detected components are produced by wine brewing or are artificially added in the later period, cannot identify common production place faking, year faking and other faking modes of high-value wine products, and have technical defects.

The isotope ratio technology has unique advantages in the aspects of traceability of the production area of wine products, identification of water and sugar adulteration, year identification and the like. The stable isotope ratio of C, H, O elements in ethanol and water molecules in the wine has some 'fingerprint' characteristics of origin, and can reflect important information such as the type, the origin, whether adulteration is carried out or not of wine brewing raw materials. Wherein the D/H ratio at the methyl sites in the ethanol molecule depends on the geographical and biological origin of the fermentation sugars; the D/H ratio at the methylene sites is influenced by the climatic conditions of the grape production site (e.g., rainfall, light intensity, etc.). The method can be used for tracing the production place of wine products, identifying sugar doping before fermentation, identifying year information and the like by measuring the D/H ratio of methyl and methylene sites in the wine ethanol molecule by using a point-specific natural isotope fractionation nuclear magnetic resonance (SNIF-NMR) technology.

In order to avoid interference when performing isotope ratio measurements, the ethanol in the wine needs to be separated in advance. In order to ensure that the measured isotope ratio can truly reflect important information such as whether wine products are adulterated and how to make the wine products, the ethanol obtained by separation needs to meet the following requirements: the purity is more than or equal to 90 wt%, and the collection efficiency is more than or equal to 96% so as to reduce the isotope fractionation effect in the separation process as much as possible.

Although the liquor industry such as white spirit, wine and the like develops rapidly in China, the research on authenticity identification of liquor products based on an isotope ratio technology is still in the initial stage in China, no special equipment for separating ethanol in the liquor products with independent intellectual property rights exists in China, and the separation equipment required by the research is totally imported. When the ethanol in the wine products is separated by using conventional distillation equipment, the ethanol obtained by distillation has low purity and low recovery rate, so that the obvious isotope fractionation effect exists in the distillation process, and the requirement of isotope ratio determination on samples cannot be met.

Therefore, it is urgently needed to develop a separation device which can overcome the above-mentioned defects and has high ethanol separation purity and high collection efficiency, so as to separate ethanol from alcoholic products and can be used for measuring isotope ratio.

Disclosure of Invention

The invention aims to provide a rotary belt distillation device and a rotary belt distillation method for separating ethanol in wine products, which are used for solving the problems in the prior art and improving the purity and the collection efficiency of the ethanol so as to achieve the aim of reducing the isotope fractionation effect in the separation process.

In order to achieve the purpose, the invention provides the following scheme: the invention provides a rotary belt distillation device for separating ethanol in wine products, which comprises a heating and temperature measuring system, a rotary stirring system, a distillation column component, a condensing system, a reflux ratio control system and a fraction collecting device, wherein the heating and temperature measuring system is connected with the distillation column component;

the heating and temperature control system is used for heating wine products, enabling volatile components to enter the distillation column assembly in a steam mode, and measuring the temperature of wine mixed liquid and the steam;

the distillation column assembly is inserted on the heating and temperature control system, the top end of the distillation column assembly is communicated with the condensation system, the side surface of the distillation column assembly is communicated with the reflux ratio control system, and the distillation column assembly is used for guiding steam to rise into the condensation system;

the condensing system comprises a first condensing system and a second condensing system which are respectively arranged above and at one side of the distillation column component and communicated with the distillation column component;

the rotary stirring system extends into the first condensing system and the distillation assembly;

the reflux ratio control system comprises a flow guide swing part, an electromagnetic coil, a time relay, a liquid circulating pump and a reflux chamber, the flow guide swing part is arranged in the reflux chamber, the flow guide swing part is hinged with the second condensing system, the electromagnetic coil is arranged on one side of the flow guide swing part and is positioned outside the reflux chamber, the time relay is electrically connected with the electromagnetic coil, and the liquid circulating pump is communicated with the reflux chamber through a pipeline;

the fraction collecting device is arranged below one side of the diversion swing part and communicated with the reflux chamber.

Preferably, the distillation assembly comprises an outer sleeve and a second inner sleeve inserted into the outer sleeve, a condensate return port is formed in one side, close to the diversion swing part, of the second inner sleeve, and the condensate return port is communicated with the liquid circulating pump through a pipeline.

Preferably, the first condensation system comprises a first-stage condensation sleeve, a first inner-layer sleeve inserted into the first-stage condensation sleeve, and a drainage tip fixedly connected to the bottom end of the first inner-layer sleeve, a transition cavity is arranged between the first inner-layer sleeve and the second inner-layer sleeve, the drainage tip extends into the transition cavity, and the top end of the second inner-layer sleeve is communicated with the transition cavity.

Preferably, the second condensing system comprises a second-stage condensing sleeve, a cavity is formed inside the second-stage condensing sleeve, the cavity is obliquely arranged, the top end of the cavity is communicated with the transition cavity, the tail end of the drainage tip extends into the top end of the cavity, and the bottom end of the cavity is hinged to the flow guide swing part.

Preferably, the heating and temperature measuring system comprises a tower kettle, an electric heating sleeve, a first temperature probe, a first temperature control instrument and a second temperature probe, wherein the top end of the tower kettle is connected with the bottom end of the outer casing in an inserting mode, the tower kettle is arranged above the electric heating sleeve, the first temperature probe is connected with the side face of the transition cavity in an inserting mode and extends into the transition cavity, the second temperature probe is connected with the side face of the tower kettle in an inserting mode and extends into the tower kettle, the first temperature probe is electrically connected with the first temperature control instrument, and the second temperature probe is electrically connected with the electric heating sleeve.

Preferably, rotatory mixing system includes electric motor, speed controller, anchor clamps, sealing member and rotatory area, electric motor sets up one-level condensation sleeve pipe top, the electric motor output with rotatory area passes through anchor clamps fixed connection, anchor clamps with cup joint between the one-level condensation sleeve pipe the sealing member, electric motor electric connection has speed controller.

Preferably, the first inner layer sleeve and the second inner layer sleeve are coaxially arranged in the vertical direction, and the rotating belt penetrates through the first inner layer sleeve and the second inner layer sleeve from top to bottom.

Preferably, the reflux chamber is provided with a reflux side outlet and a distillation side outlet, the reflux side outlet is communicated with the liquid circulating pump through a pipeline, the distillation side outlet is communicated with the fraction collecting device, and the fraction collecting device is a collecting bottle.

Preferably, a first water inlet and a first water outlet are formed in the outer side of the first-stage condensation sleeve, a second water inlet and a second water outlet are formed in the outer side of the second-stage condensation sleeve, the second water inlet is adjacent to the outlet of the backflow side, and a circulating water cooler is externally connected to the first water inlet, the first water outlet, the second water inlet and the second water outlet.

A rotary belt distillation apparatus for separating ethanol from alcoholic products, the method of use comprising the steps of:

s1: putting the wine product to be separated into a tower kettle, starting an electric heating sleeve, a time relay, a circulating water cooler and a liquid circulating pump power supply, setting the power-on time of an electromagnetic coil to be 0, and starting to heat the wine product in the tower kettle;

s2: when the wine mixed liquid in the tower kettle begins to boil, and the temperature measured by the first temperature probe gradually rises to 78.0-78.5 ℃, starting the power supply of the electric motor, setting the rotating speed to 1000-3000RPM, and adjusting the heating power of the electric heating sleeve to enable the ethanol condensate in the reflux ratio control system to drip, slowly and uniformly along the flow guide swing part, and waiting for 5-30 minutes to reach a balanced state;

s3: after the balance state is reached, setting the ratio of the power-on time to the power-off time of the electromagnetic coil to be 1:1-1:99, keeping the time ratio constant as a reflux ratio, and collecting distilled ethanol distillate when the temperature measured by a first temperature probe is 78-78.5 ℃;

s4: when the temperature measured by the first temperature probe exceeds 78.5 ℃, resetting the electrifying time of the electromagnetic coil to be 0, and stopping collecting the ethanol distillate for 5 minutes to avoid collecting water;

s5: when the temperature measured by the first temperature probe falls back to 78.0 ℃, setting the reflux ratio according to the time proportion in the step S3, and collecting the ethanol distillate again until the temperature measured by the first temperature probe exceeds 78.5 ℃;

s6: repeating the steps S4 and S5 until the temperature measured by the first temperature probe is obviously higher than 78.5 ℃, and the alcohol does not fall back again, which indicates that the ethanol in the alcohol product is completely separated;

s7: closing the electric heating sleeve and the time relay power supply, reducing the rotating speed of the electric motor to 100-500RPM, closing the electric motor and the circulating water cooler power supply after the temperature measured by the first temperature probe falls back to the ambient temperature, and measuring the quality of the distillate and the purity of the ethanol in the collecting bottle;

s8: the rotary belt distillation apparatus was purged with pure inert gas, pure nitrogen or dry air for 10 minutes to remove residual water and ethanol from the apparatus.

The invention discloses the following technical effects:

the rotating belt is arranged to continuously act on ascending steam and descending liquid on the inner wall surface of the second inner-layer sleeve, so that gas and liquid phases are continuously and tightly contacted, and sufficient mass and energy transfer is carried out, so that a higher separation tower plate number is obtained, and the aim of continuously enriching ethanol in the ascending steam is fulfilled; the middle section of the rotating belt is positioned in the first inner-layer sleeve, and is used for driving the ethanol steam to be cooled into condensate on the inner wall surface of the first inner-layer sleeve with lower temperature during high-speed rotation and flow downwards along the inner wall surface so as to be beneficial to introducing the condensate into the secondary condensation sleeve;

the rotating direction of the rotating belt is driven by the electric motor, so that the rotating belt generates downward thrust on descending condensate when rotating, the condensate uniformly descends along the inner wall surface of the distillation column component, and the phenomenon of liquid flooding at the top of the distillation column component is prevented;

a second water inlet at the lower end of the second-stage condensation sleeve is positioned near the outlet of the reflux side of the reflux ratio control system and is used for forming a lower temperature area near the outlet of the reflux side, so that a small part of ethanol steam which is not condensed in the first-stage condensation sleeve and the second-stage condensation sleeve is condensed on the side wall surface of the reflux side and flows back to a distillation column assembly, and the phenomenon that the condensation on the side wall surface of the outlet of the distillation side influences the purity of ethanol in distillate is prevented;

the device has the advantages of small residual quantity, high recovery rate, high purity of ethanol in distillate, good safety performance and easiness in implementation;

the first temperature probe and the second temperature probe are matched for use, so that the purity and the collection efficiency of collected ethanol are ensured, and the 13C/12C non-isotope fractionation effect of ethanol before and after separation is finally realized, wherein the first temperature probe is used for measuring the temperature of steam reaching the top end of a distillation column component, the boiling point of the ethanol is 78.5 ℃, when the temperature of the steam is 78-78.5 ℃, the content of the ethanol in the steam is high, and the ethanol is collected at the moment, so that high-purity ethanol distillate can be obtained; if the steam temperature is below 78 ℃ or above 78.5 ℃, this indicates that the ethanol content in the steam is somewhat low, and it is not suitable to collect the distillate. The second temperature probe is used for measuring the boiling temperature of the alcohol mixed liquor in the tower kettle, the content of ethanol in the alcohol mixed liquor is positively correlated with the boiling point of the alcohol mixed liquor, and when the boiling point of the mixed liquor is lower than 100 ℃, the mixed liquor still contains ethanol and needs to be distilled continuously; when the boiling point of the mixed solution reaches 100 ℃, the mixed solution does not contain ethanol any more, and distillation can be stopped, so that the ethanol collection efficiency in the separation process is high.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.

FIG. 1 is a schematic view showing the structure of a rotary belt distillation apparatus for separating ethanol from alcoholic beverages according to the present invention;

fig. 2 is a partially enlarged view of a in fig. 1.

The system comprises an electric motor 1, a rotating speed controller 2, a clamp 3, a sealing element 4, a rotating belt 5, a primary condensing sleeve 6, a first inner layer sleeve 7, a secondary condensing sleeve 8, a first temperature probe 9, a first temperature control instrument 10, a diversion swing part 11, an electromagnetic coil 12, a time relay 13, a backflow side outlet 14, a distillation side outlet 15, a collecting bottle 16, a liquid circulating pump 17, a backflow port 18, a second inner layer sleeve 19, an outer layer sleeve 20, a second temperature probe 21, an electric heating sleeve 22, a tower kettle 23, a drainage pin 24, a transition cavity 25, a backflow chamber 26, a pipeline 27, a cavity 28, a first water inlet 6A, a first water outlet 6B, a second water inlet 8A and a second water outlet 8B.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.