Disclosure of Invention
The technical problem to be solved by the invention is as follows: the prior method for separating alcohol ester by rectification has the problems of high energy consumption, high loss of alcohol substances and poor wine quality.
The technical scheme for solving the technical problems comprises the following steps: provides a method for reducing ethyl acetate in white spirit. The method comprises the following steps:
adding an alcohol ester water system into a closed sealed tank, wherein one end of the sealed tank is connected with an air inlet, the other end of the sealed tank is connected with an air outlet, and the air outlet is connected with a cooling tower; and (3) introducing gas from the gas inlet of the sealed tank at the temperature of 25-35 ℃, wherein the introducing time is 30-120min, and the residual liquid in the sealed tank is the white spirit with ethyl acetate reduced.
In the method for reducing ethyl acetate in the white spirit, the air inlet of the sealed tank is arranged at the bottom or below the sealed tank.
In the method for reducing ethyl acetate in the white spirit, the air inlet of the sealed tank is arranged at the top or above the sealed tank.
In the method for reducing ethyl acetate in the white spirit, the alcohol ester water system is the white spirit, wherein ethanol and water are more than or equal to 98%.
In the method for reducing ethyl acetate in white spirit, the volume ratio of the alcohol ester adding water system to the sealed tank is 1-2: 3.
In the method for reducing ethyl acetate in white spirit, the gas is nonpolar gas.
Further, in the method for reducing ethyl acetate in white spirit, the gas is at least one of nitrogen, helium or argon. Preferably nitrogen.
In the method for reducing ethyl acetate in white spirit, the gas can also be air.
In the method for reducing ethyl acetate in the white spirit, the gas is introduced at a flow rate of 0.3-1.5 times/min of the volume of the alcohol ester water system.
Preferably, in the method for reducing ethyl acetate in white spirit, the gas introduction flow rate is 0.5-1 time/min of the volume of the alcohol ester water system.
Preferably, in the method for reducing ethyl acetate in white spirit, the gas is introduced for 40-100 min.
The invention has the beneficial effects that:
the invention provides a method for reducing ethyl acetate in white spirit by introducing gas into the white spirit and bringing the ethyl acetate in the white spirit into the air by utilizing the adsorbability or entrainment effect of gas phase. The content of the ethyl acetate in the wine before the gas is introduced is 340mg/100ml, the content of the ethyl acetate in the wine after the reduction can be reduced to 100.69mg/100ml at least, the content of the ethyl acetate is obviously reduced, and simultaneously the content of other flavor substances is not influenced, so that the effect is better. Compared with the traditional rectification process, the treatment method has the advantages of simple process, low energy consumption and short production period, and can quickly improve the quality of the white spirit.
Detailed Description
The invention provides a method for reducing ethyl acetate in white spirit, which comprises the following steps:
adding an alcohol ester water system into a closed sealed tank, wherein one end of the sealed tank is connected with an air inlet, the other end of the sealed tank is connected with an air outlet, and the air outlet is connected with a cooling tower; and (3) introducing gas from the gas inlet of the sealed tank at the temperature of 25-35 ℃, wherein the introducing time is 30-120min, and the residual liquid in the sealed tank is the white spirit with ethyl acetate reduced.
In the method for reducing ethyl acetate in the white spirit, the air inlet of the sealed tank is arranged at the bottom or below the sealed tank.
In the method for reducing ethyl acetate in the white spirit, the air inlet of the sealed tank is arranged at the top or above the sealed tank.
In the method for reducing ethyl acetate in the white spirit, the alcohol ester water system is the white spirit, wherein ethanol and water are more than or equal to 98%.
In the method for reducing ethyl acetate in white spirit, the volume ratio of the alcohol ester adding water system to the sealed tank is 1-2: 3.
The invention obtains the adding amount of the alcohol ester water system in the sealed tank through a large number of experiments so as to ensure the aeration effect of the introduced gas; when the amount of the alcohol ester water system is small, the utilization rate of the gas phase is low, but when the amount of the alcohol ester water system is large, the aeration is easy to overflow the alcohol ester water system.
In the method for reducing ethyl acetate in white spirit, the gas is nonpolar gas.
Further, in the method for reducing ethyl acetate in white spirit, the gas is at least one of nitrogen, helium or argon. The nitrogen, the helium and the argon are inert gases, the chemical properties of the inert gases are stable, the inert gases are introduced into the white spirit, the formed micro bubbles absorb or carry the ethyl acetate, and the inert gases are not easy to react with alcohol compounds in the white spirit, so that the taste of the white spirit is not influenced, and the white spirit is safe, reliable and pollution-free.
The nitrogen is low in price and easy to obtain, and the nitrogen is the main component in the air, so that the used nitrogen can be directly discharged into the atmosphere, and the introduced gas is preferably the nitrogen.
In the method for reducing ethyl acetate in white spirit, the gas can also be air.
In the method for reducing ethyl acetate in the white spirit, the gas is introduced at a flow rate of 0.3-1.5 times/min of the volume of the alcohol ester water system.
The invention particularly designs that the gas introduction flow is 0.3-1.5 times/min, the introduction time is 30-120min, and the gas is introduced into an alcohol ester water system at a reasonable speed, so that the content of ethyl acetate is reduced, the content of alcohol compounds is ensured, and the white spirit keeps good taste and fragrance.
Preferably, in the method for reducing ethyl acetate in white spirit, the gas introduction flow rate is 0.5-1 time/min of the volume of the alcohol ester water system.
Preferably, in the method for reducing ethyl acetate in white spirit, the gas is introduced for 40-100 min.
The method comprises the steps of introducing gas into an alcohol ester water system at 25-35 ℃ to separate ethyl acetate from the alcohol ester water system, introducing gas into the alcohol ester water system, and taking away the ethyl acetate in the alcohol ester water system by the aid of micro bubbles formed by the flowing gas so as to reduce the content of the ethyl acetate in the alcohol ester water system.
The specific operation process is as follows: the gas enters the sealed tank from the gas inlet of the sealed tank, flows through the alcohol ester water system (namely white spirit) in the sealed tank, and is discharged from the gas outlet of the sealed tank. The gas inlet is arranged at the bottom or the lower part of the sealed tank, so that gas enters from the liquid level of the alcohol ester water system, the gas is fully mixed with the alcohol ester water system to adsorb ethyl acetate (forming gas-borne ester molecules, as shown in figure 2) in the alcohol ester water system, the gas-borne ester molecules are discharged from the gas outlet arranged at the top or the upper part of the sealed tank, and the discharged gas passes through the cooling tower to separate the gas from the ethyl acetate.
The following examples are intended to illustrate specific embodiments of the present invention without limiting the scope of the invention to the examples.
Example 1 reduction of Ethyl acetate in white spirit by the method of the invention
2.5L of brewed Chinese liquor is filled into a 5L sealed tank (shown in figure 1) at 26 deg.C, and nitrogen with purity of 99.9% is continuously introduced into the sealed tank through an air inlet of the sealed tank at a speed of 0.8 times liquid phase volume, i.e. 2L/min, for 40 min. And after the nitrogen flows through the white spirit, the nitrogen is discharged from the air outlet and then flows into a cooling tower, the nitrogen is separated from the ethyl acetate in the cooling tower, the separated nitrogen is directly discharged into the air, and the liquid ethyl acetate can be reused.
Example 2 reduction of Ethyl acetate in white spirit by the method of the invention
Filling 3L of brewed white spirit into a 5L sealed tank at 25 ℃, and arranging an aeration disc at the bottom of the sealed tank through an air inlet of the sealed tank; continuously introducing nitrogen into the sealed tank at a speed of 1.5L/min at a liquid phase volume of 0.5 times, wherein the nitrogen enters the white spirit through the aeration disc and is uniformly dispersed in the white spirit, the ethyl acetate in the white spirit is taken out by the nitrogen along with the continuous introduction of the nitrogen into the white spirit, and is discharged from the air outlet together with the nitrogen, and then the ethyl acetate and the nitrogen enter the cooling tower, and the nitrogen and the ethyl acetate are separated in the cooling tower. In this example, the nitrogen gas was introduced for 60 min.
Example 3 reduction of Ethyl acetate in white spirit by the method of the present invention
2.5L of brewed white spirit is filled into a 5L sealed tank at the temperature of 35 ℃, nitrogen is continuously introduced into the sealed tank through an air inlet of the sealed tank at the speed of 2L/min, wherein the liquid phase volume is 0.8 times of the liquid phase volume, and the introduction time is 40 min. After the air flows through the white spirit, the air is discharged from the air outlet and then flows into the cooling tower, nitrogen and ethyl acetate are separated in the cooling tower, the separated nitrogen is directly discharged into the air, and the liquid ethyl acetate can be reused.
Example 4 reduction of Ethyl acetate in white spirit by the method of the present invention
Filling 3L of brewed white spirit into a 5L sealed tank at 30 ℃, and continuously introducing nitrogen into the sealed tank at the speed of 3L/min by 1 time of liquid phase volume through an air inlet of the sealed tank, wherein the introducing time is 35 min. And after the nitrogen flows through the white spirit, the nitrogen is discharged from the air outlet and then flows into a cooling tower, the nitrogen is separated from the ethyl acetate in the cooling tower, the separated nitrogen is directly discharged into the air, and the liquid ethyl acetate can be reused.
Example 5 reduction of Ethyl acetate in white spirit by the method of the present invention
Filling 3L of brewed white spirit into a 5L sealed tank at 25 ℃, and arranging an aeration disc at the bottom of the sealed tank through an air inlet of the sealed tank; and continuously introducing argon into the sealed tank at a speed of 1.5L/min at a liquid phase volume of 0.5 times, wherein the argon enters the white spirit through an aeration disc and is uniformly dispersed in the white spirit, the ethyl acetate in the white spirit is taken out by the argon along with the continuous introduction of the argon into the white spirit, the ethyl acetate and the argon are discharged from an air outlet, and then the ethyl acetate and the argon enter a cooling tower, and the argon and the ethyl acetate are separated in the cooling tower. In this example, the argon gas was introduced for 60 min.
Example 6 reduction of Ethyl acetate in white spirit by the method of the present invention
Filling brewed 5L of white spirit into a 10L sealed tank at the temperature of 30 ℃, and arranging an aeration disc at the bottom of the sealed tank through an air inlet of the sealed tank; continuously introducing helium into the sealed tank at a speed of 5L/min, wherein the volume of the liquid phase is 1 time of that of the liquid phase, the helium enters the white spirit through the aeration disc, the helium is uniformly dispersed in the white spirit, the helium is continuously introduced into the white spirit, the ethyl acetate in the white spirit is taken out by the helium, the ethyl acetate and the helium are discharged from the gas outlet, and then the ethyl acetate and the helium enter the cooling tower, and the argon is separated from the ethyl acetate in the cooling tower. In this example, the helium gas was introduced for 90 min.
Example 7 reduction of Ethyl acetate in white spirit by the method of the present invention
Filling 25L of brewed white spirit into a 50L sealed tank at the temperature of 35 ℃, and arranging an aeration disc at the bottom of the sealed tank through an air inlet of the sealed tank; continuously introducing clean air into the sealed tank at a speed of 15L/min at a liquid phase volume of 0.6 times, wherein the air enters the white spirit through the aeration disc and is uniformly dispersed in the white spirit, the ethyl acetate in the white spirit is carried out by the air along with the continuous introduction of the air into the white spirit, the air and the ethyl acetate are discharged from the air outlet together, and then the air and the ethyl acetate are separated in the cooling tower. In this example, the air was introduced for 65 min.
Example 8 reduction of Ethyl acetate in Baijiu by the method of the present invention
Filling 30L of brewed white spirit into a 50L sealed tank at 25 ℃, and arranging an aeration disc at the bottom of the sealed tank through an air inlet of the sealed tank; continuously introducing clean air into the sealed tank at a speed of 24L/min at a liquid phase volume of 0.8 times, wherein the air enters the white spirit through an aeration disc and is uniformly dispersed in the white spirit, the ethyl acetate in the white spirit is carried out by helium along with the continuous introduction of the air into the white spirit, the air and the ethyl acetate are discharged from an air outlet together, and then the air and the ethyl acetate are introduced into a cooling tower, and the air and the ethyl acetate are separated in the cooling tower. In this example, the time for introducing air was 90 min.
Detecting the content of each component in the white spirit:
the content of ethyl hexanoate, ethyl lactate, ethyl butyrate, isoamyl alcohol, n-butanol, acetal, isobutanol, n-propanol, methanol and ethyl acetate in the original white spirit is measured by a gas chromatograph by adopting a detection method in the prior art. After the treatments of examples 1 to 4, the contents of the respective components in the treated white spirit were measured by the same method under the same conditions, and the results are shown in table 1 below.
TABLE 1 flavor substance content in Chinese liquor treated by different methods (mg/100ml)
From the detection results, the content of ethyl acetate in the white spirit is obviously reduced after the white spirit is treated by the treatment method, so that more ethyl acetate content in the white spirit is effectively removed, and the loss of alcohol compounds in the treated white spirit is less. The treatment method of the invention effectively removes the ethyl acetate in the white spirit, simultaneously ensures the alcohol compounds in the white spirit and reduces the loss of the alcohol compounds. It can also be obtained from the above table that the effect of removing ethyl acetate is good when nitrogen is used as the adsorption gas phase, and the effect is slightly poor when air is used as the adsorption gas phase, but compared with the rectification method in the prior art, the effect of removing ethyl acetate is superior to that of the rectification process in the prior art no matter nitrogen or air is used in the method, and the treatment method of the invention has the advantages of simple operation, low energy consumption, short treatment period and the like, and the white spirit treated by the method of the invention has good taste.