CN113862106A - Electrochemical catalytic esterification method and device for improving total ester content of white spirit - Google Patents

Electrochemical catalytic esterification method and device for improving total ester content of white spirit Download PDF

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CN113862106A
CN113862106A CN202111127529.6A CN202111127529A CN113862106A CN 113862106 A CN113862106 A CN 113862106A CN 202111127529 A CN202111127529 A CN 202111127529A CN 113862106 A CN113862106 A CN 113862106A
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white spirit
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郑青
余有贵
熊阿媛
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Shaoyang University
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/12Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
    • C12H1/16Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation

Abstract

The invention provides an electrochemical catalytic esterification method for improving the total ester content of white spirit, which adopts a three-electrode system electrochemical catalytic esterification, wherein a working electrode is a gold electrode, a counter electrode is an inert electrode, a reference electrode is an electrode for a water phase, an electrolyte is a white spirit stock solution, and the surface area of the gold electrode is not less than 0.01 square centimeter; recording the acetic acid and total ester content in the white spirit stock solution before catalytic esterification, starting electrolysis when the acetic acid content is more than 0.6g/L, stopping electrolysis when the total ester content reaches a target value, and recording the acetic acid and total ester content after electrolysis. The method adopts an electrochemical catalysis method, and does not directly or indirectly add edible alcohol and color, aroma and flavor generation substances generated by non-self fermentation. On the premise of guaranteeing the safety of the white spirit, the content of total esters of the white spirit is increased, so that the effect of regulating and controlling the flavor of the white spirit is achieved, and the method has important significance for promoting the sustainable development of the white spirit industry.

Description

Electrochemical catalytic esterification method and device for improving total ester content of white spirit
Technical Field
The invention relates to the technical field of electrochemical wine brewing, in particular to an electrochemical catalytic esterification method for improving the content of total esters in white spirit.
Background
The white spirit is prepared with grains as main material and Daqu, Xiaoqu, bran koji, enzyme preparation, yeast, etc. as saccharifying ferment and through steaming, saccharifying, fermenting, distilling and ageing. Besides flavoring, the white spirit also has an important characteristic that edible alcohol and color, aroma and flavor developing substances generated by non-self fermentation are not directly or indirectly added. The esters contained in the white spirit are the key of the flavor source of the white spirit. Therefore, the method for improving the total ester content of the white spirit is a key technology for regulating and controlling the quality of the white spirit on the premise of not adding ester substances generated by non-self fermentation.
The thesis of the research on the optimization of the microbial action conditions and the improvement of the quality of the semi-solid multi-grain white spirit in the brewing process provides that the brewing process of the multi-grain white spirit is mainly optimized from the aspects of the spirit yield, the total acid content, the total ester content and the like. However, the biological activity of microorganisms is also significantly affected by the presence of numerous microorganisms and unclear modes of action among microorganisms during the brewing process of white spirit, and the environmental sensitivity of the microbial activity, such as the temperature difference of fermentation sites caused by weather reasons. Therefore, the method for improving the content of the total esters of the white spirit by optimizing the action conditions of the microorganisms has strict requirements on the environmental temperature. This is not favorable for the actual brewing and application of white spirit.
Chinese patent publication No. CN112029607A, electrochemical method for increasing total ester content in liquid fermentation base wine and liquid fermentation base wine, clearly indicates that the total ester content in liquid fermentation base wine can be increased by applying differential potential to different fermentation stages of fermentation microorganisms to optimize their physiological activities. However, this method uses a gold plate electrode as an alternative electron source to mediate the redox reaction of the fermenting microorganism, and it can be seen that the inclusion of the fermenting microorganism in the electrolytic system of this method requires that the entire electrolytic circuit be capable of conducting electricity. Therefore, the method can only be used for liquid fermentation of white spirit, but not for solid fermentation of white spirit: the water content of the environment where the microorganisms are located in the solid-state fermented white spirit is much lower than that of the environment where the microorganisms are located in the liquid-state fermented white spirit, and contained conductive ions cannot flow, so that the solid-state fermentation tank is almost non-conductive, and an effective electrolysis loop cannot be formed. The high-quality white spirit sold in the market at present is solid-state fermented white spirit without exception. For example, Luzhou-flavor liquor, Maotai-flavor liquor, fen-flavor liquor, etc. are all solid-state fermented liquor (see the national standard, the standard number: GB/T15109-.
Chinese patent publication No. CN111518664A, a method for electrochemical oxidation of aging spirit, specifically, an electrochemical method using a self-assembled film modified gold electrode as a working electrode to oxidize reducing substances in spirit. The characteristics of the patent include two aspects: firstly, modifying a gold electrode by using a self-assembly film as a working electrode, and covering the surface of the working electrode (the gold electrode) by using the self-assembly film so as to simulate the catalytic activity of the working electrode; secondly, the aim is to utilize the catalytic action of the working electrode to oxidize the reducing substances in the white spirit to generate acid substances, thereby indirectly improving the ester content and controlling the ester content in a controllable direction. According to the mechanism, the amount of the acid is increased, but not decreased. The mechanism is catalytic oxidation (i.e., catalytic oxidation of alcohols to acids). But the acid substances are also important related to the flavor of the white spirit, and the excessive acid substance content can obviously change the flavor of the white spirit, thereby reducing the quality of the white spirit. Therefore, the patent has the defects that the ester content can not be improved to a desired value, and only can be controlled within an effective range, so that the corresponding white spirit has single flavor and is not suitable for improving the flavor of all white spirits, in addition, the amount of acid substances is only increased and cannot be reduced, and the flavor of the white spirits is obviously changed by excessively high content of the acid substances, so that the quality of the white spirits is reduced.
Disclosure of Invention
The invention aims to solve the technical problem of providing an electrochemical catalytic esterification method for improving the total ester content of white spirit aiming at the defects of the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: an electrochemical catalytic esterification method for improving the content of total esters in white spirit is characterized by comprising the following steps:
preparing an electrochemical system: the working electrode is a gold electrode, the counter electrode is an inert electrode, the reference electrode is an electrode for a water phase, the electrolyte is a liquor stock solution, and the surface area of the gold electrode is not less than 0.01 square centimeter;
testing a white spirit stock solution: the acetic acid concentration was measured and recorded as A using a gas chromatograph prior to electrochemical treatment0(ii) a Measuring the content of total esters in the white spirit stock solution by an indicator method in the national standard (GB/T10345-2007)And is denoted by B0
Electrochemical catalytic esterification: placing the electrochemical system in a container containing liquor stock solution, connecting the components, and performing electrochemical reaction when A is0When the concentration is more than 0.6g/L, the electrolysis is started; the amount of the white spirit stock solution is not less than 0.05L, the electrolytic voltage of electrolysis is not less than 0.2V, and the electrolytic time is not less than 0.5 h;
stopping catalysis: stopping catalysis when the content of total esters in the stock solution of Chinese liquor reaches a target value, and recording the concentration of acetic acid in the stock solution of Chinese liquor as A1With a total ester content of B1
Further, the gold electrode is subjected to a pretreatment as follows: and polishing the gold electrode into a mirror surface by using alumina polishing powder with the particle sizes of 0.3 micron and 0.05 micron in sequence, and cleaning the surface of the gold electrode.
The inert electrode is any one of a platinum wire and a platinum net.
The electrode for the water phase is any one of a silver/silver chloride electrode and a calomel electrode.
Furthermore, in the electrochemical catalytic esterification in the step, the amount of the white spirit stock solution is further preferably 0.05L-5L.
Further, in the step of electrochemical catalytic esterification, the electrolytic voltage is further optimized to be 0.2V-1V.
Still further, in the step of electrochemically catalytic esterification, the electrolysis time is further optimized to be 0.5-24 h.
Based on the same invention concept, the invention also provides an electrochemical catalytic esterification device for improving the total ester content of the white spirit, which comprises a main box body, a working electrode, a reference electrode, a counter electrode and a potential controller, wherein the working electrode, the reference electrode and the counter electrode are arranged in the main box body, and the potential controller is positioned outside and electrically connected with the main box body, the working electrode, the reference electrode and the counter electrode.
Furthermore, the upper end of one side of the left side and the right side of the main box body is provided with a liquid injection port, and the lower end of the other side of the main box body is provided with a liquid outlet.
Further, the working electrode is a gold electrode, the counter electrode is an inert electrode, and the reference electrode is an electrode for aqueous phase.
Furthermore, the gold electrode is a gold electrode polished into a mirror surface by using 0.3 micron and 0.05 micron aluminum oxide polishing powder in sequence.
Further, the inert electrode is any one of a platinum wire and a platinum mesh.
Further, the electrode for aqueous phase is any one of a silver/silver chloride electrode and a calomel electrode.
The catalytic process of the esterification of alcohols with acids generally requires the addition of an additional catalyst. In order to ensure the safety of the white spirit, foreign substances cannot be added into the white spirit, so that the conventional esterification reaction is not suitable for the white spirit. The esterification reaction speed of alcohol and acid in the white spirit is very slow on the premise of not directly or indirectly adding edible alcohol and color, aroma and flavor substances generated by non-self fermentation. The invention adopts an electrochemical catalysis method to catalyze the esterification reaction of alcohol and acid on the surface of a working electrode (gold electrode), and no foreign substances enter the white spirit. By the electrochemical catalysis method, the esterification reaction speed of alcohol and acid in the white spirit is accelerated, and the total ester content of the white spirit is improved. The working principle is as follows: the gold electrode applied with voltage and acid substances generate electron exchange to form active carbon positive ions, and then alcohol reacts with the active carbon positive ions to remove water molecules to obtain ester; the counter electrode is only for forming a current loop and the reference electrode is only for indicating the operating voltage. In the whole process, no foreign substance enters the white spirit, and no gold ion is formed and enters the white spirit (the gold electrode only provides a catalytic action and cannot be dissolved).
Compared with the prior art, the invention has the beneficial effects that: firstly, the surface of the gold electrode is not covered with any substance, so that the simulation of surface covering on catalytic activity is avoided; secondly, a new mechanism is proposed, which utilizes the gold electrode to catalyze the esterification reaction of alcohol and acid (i.e. the reaction of alcohol and acid to generate ester), thereby increasing the content of ester substances. Thirdly, because the content requirements of esters of different varieties of white spirits are different, the method provides technical guidance for improving the content of required esters for different varieties of white spirits with different flavors, can improve the content of the esters to a desired value, can reduce the content of acids, and can effectively avoid the influence of overhigh content of the acids on the flavor of the white spirits. Fourthly, adopting an electrochemical catalysis method without directly or indirectly adding edible alcohol and coloring, fragrant and flavor-developing substances generated by non-self fermentation. On the premise of guaranteeing the safety of the white spirit, the content of total esters of the white spirit is increased, so that the effect of regulating and controlling the flavor of the white spirit is achieved, and the method has important significance for promoting the sustainable development of the white spirit industry.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment 6 of the present invention.
Wherein, 1 is a main box body, 2 is a working electrode, 3 is a reference electrode, 4 is a counter electrode, 5 is a potential controller, 6 is a liquid injection port, and 7 is a liquid outlet.
Detailed Description
Example 1
Preparing an electrochemical system: the working electrode is a gold electrode, the area of the gold electrode is 0.01 square centimeter, the gold electrode is polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micrometer and 0.05 micrometer in sequence, and the surface of the gold electrode is cleaned; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the liquor stock solution is 0.05L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage is 0.2V, the electrolysis time is 0.5 h, and the electrolysis temperature is room temperature (28 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.70g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.72 g/L.
Example 2
Preparing an electrochemical system: the working electrode is a gold electrode, the area of the gold electrode is 1 square centimeter, the gold electrode is polished into a mirror surface by using 0.3 micron and 0.05 micron aluminum oxide polishing powder in sequence, and the surface of the gold electrode is cleaned; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the quantity of the liquor stock solution is 5L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage is 0.2V, the electrolysis time is 0.5 h, and the electrolysis temperature is room temperature (28 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.73g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.73 g/L.
Example 3
Preparing an electrochemical system: the working electrode is a gold electrode, the area of the gold electrode is 0.01 square centimeter, the gold electrode is polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micrometer and 0.05 micrometer in sequence, and the surface of the gold electrode is cleaned; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the liquor stock solution is 0.05L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage was 0.2V, the electrolysis time was 0.5 hours, and the electrolysis temperature was room temperature (33 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.71g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.73 g/L.
Example 4
Preparing an electrochemical system: the working electrode is a gold electrode, the area of the gold electrode is 0.01 square centimeter, the gold electrode is polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micrometer and 0.05 micrometer in sequence, and the surface of the gold electrode is cleaned; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the liquor stock solution is 0.05L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage is 0.8V, the electrolysis time is 18 hours, and the electrolysis temperature is room temperature (28 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.66g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.83 g/L.
Example 5
Preparing an electrochemical system: the working electrode is a gold electrode, the area of the gold electrode is 0.01 square centimeter, the gold electrode is polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micrometer and 0.05 micrometer in sequence, and the surface of the gold electrode is cleaned; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the liquor stock solution is 0.05L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage is 1V, the electrolysis time is 24 hours, and the electrolysis temperature is room temperature (28 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.60g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.86 g/L.
Comparative example 1
Preparing an electrochemical system: the working electrode is a glassy carbon electrode, the area of the gold electrode is 0.01 square centimeter, and the gold electrode is polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micrometer and 0.05 micrometer in sequence to clean the surface of the gold electrode; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the liquor stock solution is 0.05L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage is 0.2V, the electrolysis time is 0.5 h, and the electrolysis temperature is room temperature (28 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.84g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Comparative example 2
Preparing an electrochemical system: the working electrode is a gold electrode, the area of the gold electrode is 0.01 square centimeter, the gold electrode is polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micrometer and 0.05 micrometer in sequence, and the surface of the gold electrode is cleaned; the counter electrode is a platinum wire electrode, and the reference electrode is a silver/silver chloride electrode; taking liquor stock solution without any substance as electrolyte, wherein the liquor stock solution is 0.05L; conventional glass containers are electrolytic cells.
Testing a white spirit stock solution: before electrochemical treatment, a gas chromatograph is used, and a standard substance is used for qualitative and quantitative determination to determine the acid content in the white spirit. The acetic acid concentration was measured to be 0.84g/L based on acetic acid. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.65 g/L.
Electrochemical catalytic esterification: and controlling the voltage of the electrochemical process by using an electrochemical workstation, connecting all the components, and electrolyzing the liquor stock solution in an electrochemical system. The electrolysis voltage was 0.2V, the electrolysis time was 10 minutes, and the electrolysis temperature was room temperature (28 ℃).
Stopping catalysis: after the electrolysis, the acid content in the white spirit is measured and is 0.81g/L by taking acetic acid as a standard. The content of total esters in the white spirit is measured by an indicator method in the national standard (GB/T10345-2007) and is 1.67 g/L.
TABLE 1 Effect of electrochemical catalytic esterification for white spirit in examples 1-5 and comparative examples 1-2
Figure BDA0003279366650000071
As can be seen from Table 1, the total ester content of examples 1 to 5 was higher than that of comparative examples 1 to 2, and the acetic acid content of examples 1 to 5 was lower than that of comparative examples 1 to 2. Comparative example 1 differs from example 1 in that a different working electrode is used, and comparative example 2 differs from example 1 in that a different electrochemically catalyzed esterification time is used. The results show that the working electrodes, the electrolytic voltage and the electrolytic time corresponding to the working electrodes, the electrolytic voltage and the electrolytic time in the preparation process can improve the total ester content of the white spirit and reduce the content of acid substances (acetic acid).
Example 6
As shown in fig. 1, the embodiment provides an electrochemical catalytic esterification apparatus for increasing the total ester content of white spirit, which includes a main tank 1, a working electrode 2, a reference electrode 3, a counter electrode 4 and a potential controller 5, wherein the working electrode 2, the reference electrode 3 and the counter electrode 4 are arranged inside the main tank 1, and the potential controller 5 is located outside the main tank 1 and electrically connected to the working electrode 2, the reference electrode 3 and the counter electrode 4.
In the left side and the right side of the main box body 1, the upper end of one side is provided with a liquid injection port 6, and the lower end of the other side is provided with a liquid outlet 7.
The working electrode 3 is a gold electrode polished into a mirror surface by using aluminum oxide polishing powder with the particle sizes of 0.3 micron and 0.05 micron in sequence; the counter electrode 4 is a platinum wire; the reference electrode 3 is a calomel electrode.
The use process of the device is as follows: firstly, white spirit is injected into the main box body 1 through the liquid injection port 6, then the three-electrode electrochemical catalysis system is connected according to the structure, so that the white spirit completely submerges the three electrode materials, finally, the electric controller 5 is adjusted, the catalysis time is set according to the total ester content required by different types of white spirit, and after the ester content reaches the standard, the qualified white spirit with unique flavor is obtained through the liquid outlet 7.

Claims (8)

1. An electrochemical catalytic esterification method for improving the content of total esters in white spirit is characterized by comprising the following steps:
preparing an electrochemical system: the working electrode is a gold electrode, the counter electrode is an inert electrode, the reference electrode is an electrode for a water phase, the electrolyte is a liquor stock solution, and the surface area of the gold electrode is not less than 0.01 square centimeter;
testing a white spirit stock solution: the acetic acid concentration was measured and recorded as A using a gas chromatograph prior to electrochemical treatment0(ii) a Measuring the content of total esters in the white spirit stock solution by using an indicator method in the national standard (GB/T10345-2007), and recording as B0
Electrochemical catalytic esterification: placing the electrochemical system in a container containing liquor stock solution, connecting the components, and performing electrochemical reaction when A is0When the concentration is more than 0.6g/L, the electrolysis is started; the amount of the white spirit stock solution is not less than 0.05L, the electrolytic voltage of electrolysis is not less than 0.2V, and the electrolytic time is not less than 0.5 h;
stopping catalysis: stopping catalysis when the content of total esters in the stock solution of Chinese liquor reaches a target value, and recording the concentration of acetic acid in the stock solution of Chinese liquor as A1With a total ester content of B1
2. The method of claim 1, wherein: the gold electrode needs to be pretreated, and the pretreatment is as follows: and polishing the gold electrode into a mirror surface by using alumina polishing powder with the particle sizes of 0.3 micron and 0.05 micron in sequence, and cleaning the surface of the gold electrode.
3. The method of claim 1, wherein: the inert electrode is any one of a platinum wire and a platinum net.
4. The method of claim 1, wherein: the electrode for the water phase is any one of a silver/silver chloride electrode and a calomel electrode.
5. The electrochemical catalytic esterification device for improving the total ester content of the white spirit is characterized by comprising a main box body (1), a working electrode (2), a reference electrode (3), a counter electrode (4) and a potential controller (5), wherein the working electrode (2), the reference electrode (3) and the counter electrode (4) are arranged in the main box body (1), the potential controller (5) is positioned outside the main box body (1) and is electrically connected with the working electrode (2), the reference electrode (3) and the counter electrode (4), a liquid injection port (6) is formed in the upper end of one side of the left side and the right side of the main box body (1), and a liquid outlet (7) is formed in the lower end of the other side of the main box body; the working electrode (3) is a gold electrode, the counter electrode (4) is an inert electrode, and the reference electrode (3) is an electrode for water phase.
6. The apparatus of claim 5, wherein the gold electrode is a mirror polished gold electrode with 0.3 micron and 0.05 micron particle size alumina polishing powders in sequence.
7. The apparatus of claim 5, wherein the inert electrode is any one of a platinum wire and a platinum mesh.
8. The device according to claim 5, wherein the electrode for aqueous phase is any one of a silver/silver chloride electrode and a calomel electrode.
CN202111127529.6A 2021-09-26 2021-09-26 Electrochemical catalytic esterification method and device for improving total ester content of white spirit Pending CN113862106A (en)

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