CN106834068B - Method for separating white spirit and harmful substances in white spirit - Google Patents

Method for separating white spirit and harmful substances in white spirit Download PDF

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Publication number
CN106834068B
CN106834068B CN201710250795.5A CN201710250795A CN106834068B CN 106834068 B CN106834068 B CN 106834068B CN 201710250795 A CN201710250795 A CN 201710250795A CN 106834068 B CN106834068 B CN 106834068B
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white spirit
harmful substances
control temperature
separation
temperature
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CN106834068A (en
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袁茂华
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Ecological Group Zhejiang Wine Co ltd
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Ecological Group Zhejiang Wine Co ltd
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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
    • C12H6/00Methods for increasing the alcohol content of fermented solutions or alcoholic beverages
    • C12H6/02Methods for increasing the alcohol content of fermented solutions or alcoholic beverages by distillation

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  • Food Science & Technology (AREA)
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  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)

Abstract

The invention provides a white spirit and a method for separating harmful substances of the white spirit, and relates to the technical field of food. According to the method for separating harmful substances in the white spirit, the contents of the harmful substances such as formaldehyde, methanol, lead, sulfur, plasticizer, free radicals and the like in the white spirit are effectively reduced through the steps of primary distillation separation, gas phase separation, liquid phase separation, secondary distillation separation and the like. The white spirit prepared by the separation method provided by the invention has extremely low content of harmful substances, wherein the content of lead ions and methanol is lower than 0.005mg/mL, which is greatly lower than the national standard, and the white spirit is ecological, safe and healthy.

Description

Method for separating white spirit and harmful substances in white spirit
Technical Field
The invention relates to the technical field of food, in particular to a method for separating white spirit and harmful substances of the white spirit.
Background
The white spirit is a special distilled spirit in China and is prepared by preparing fermented grains from starch or sugar raw materials or distilling after fermentation. As a special beverage, white spirit changes along with the continuous development of literature and art in the historical process of China, along with the joy, anger and sadness of the civilians and ink guests, and becomes a bright pearl of oriental culture. At present, liquor culture is still full of all aspects of life, and occasions such as gathering of friends, meeting of relatives, joint of people and the like are avoided to drink one or two cups of liquor to show celebration.
Wine is a mixture of many chemical components, water and ethanol being the most important components. In addition, however, some trace elements harmful to human bodies are generated in the process of preparing the white spirit, and although the content of the trace elements is low, if the white spirit is drunk too much, the trace elements can cause great harm to the health of human bodies. For example, formaldehyde, methanol, sulfur, plasticizer, lead, free radicals and the like are common harmful substances in the white spirit, and the control on the content of the harmful substances in the white spirit should be increased in the production process of the white spirit. At present, although some methods for removing harmful substances in white spirit exist, some problems still exist, such as poor removal effect, high cost and the like. Therefore, there is a need to provide a separation and purification method to effectively remove harmful substances in white spirit, improve the safety of white spirit, and enable people to enjoy the taste of white spirit without worrying about the harm caused by white spirit.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a method for separating harmful substances in white spirit, and the second purpose of the invention is to provide white spirit so as to relieve the problem of high content of harmful substances in white spirit in the prior art.
The invention provides a method for separating harmful substances in white spirit, which comprises the following steps:
first distillation separation: controlling the temperature in the distiller to be a first control temperature so as to separate harmful substances with boiling points lower than the first control temperature; then, controlling the temperature in the distiller to be a second control temperature to separate harmful substances with boiling points higher than the second control temperature, and enabling the white spirit to enter a gas separation process in the form of steam;
gas separation: removing harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like from the white spirit steam through a filter material, condensing the white spirit steam into a liquid state, and entering a liquid separation process;
liquid state separation: removing harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like from the liquor liquid through a filter material, and performing a second distillation separation process;
and (3) second distillation separation: controlling the temperature in the distiller to be a first control temperature so as to separate harmful substances with boiling points lower than the first control temperature; then, controlling the temperature in the distiller to be a second control temperature to separate harmful substances with boiling points higher than the second control temperature, and enabling the white spirit to enter a condensing device in the form of steam, and condensing the white spirit steam to obtain white spirit with separated harmful substances;
the first control temperature is below 75 ℃, and the second control temperature is above 80 ℃.
Further, the first control temperature is 70-75 ℃.
Further, the second control temperature is 80-95 ℃.
Further, the filter material includes minerals.
Further, the filter material comprises activated carbon.
Further, the filter material further comprises a quantum energy releasing substance capable of ionizing the inert substance.
Further, the filter material further comprises a quantum energy releasing substance capable of ionizing the inert substance.
In addition, the invention also provides the white spirit, and the separation method of the white spirit removes harmful substances.
Further, the content of lead ions in the white spirit is lower than 0.005 mg/mL.
Further, the content of methanol in the white spirit is lower than 0.005 mg/mL.
According to the method for separating harmful substances in the white spirit, the content of the harmful substances in the white spirit is effectively reduced through the steps of primary distillation separation, gas separation, liquid separation, secondary distillation separation and the like, the content of the harmful substances in the white spirit treated according to the separation method is extremely low, and the content of lead ions and methanol is lower than 0.005mg/mL and greatly lower than the national required standard.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a process flow diagram of a separation process provided in example 1 of the present invention;
FIG. 2 is a walking diagram of the components of the white spirit by the separation method provided in the embodiment 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. 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.
The invention provides a method for separating harmful substances in white spirit, which comprises the following steps:
first distillation separation: controlling the temperature in the distiller to be a first control temperature so as to separate harmful substances with boiling points lower than the first control temperature; then, controlling the temperature in the distiller to be a second control temperature to separate harmful substances with boiling points higher than the second control temperature, and enabling the white spirit to enter a gas separation process in the form of steam;
gas separation: removing harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like from the white spirit steam through a filter material, condensing the white spirit steam into a liquid state, and entering a liquid separation process;
liquid state separation: removing harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like from the liquor liquid through a filter material, and performing a second distillation separation process;
and (3) second distillation separation: controlling the temperature in the distiller to be a first control temperature so as to separate harmful substances with boiling points lower than the first control temperature; then, controlling the temperature in the distiller to be a second control temperature to separate harmful substances with boiling points higher than the second control temperature, and enabling the white spirit to enter a condensing device in the form of steam, and condensing the white spirit steam to obtain white spirit with separated harmful substances;
wherein the first control temperature is below 75 ℃, and the second control temperature is above 80 ℃.
Wherein, in the first distillation separation, the temperature in the distiller is controlled to be a first control temperature (70-75 ℃) firstly, so as to separate harmful substances with boiling points lower than the first control temperature. Because the boiling point of the effective component ethanol of the white spirit is 77 ℃, when the temperature of the distiller is lower than the first control temperature, harmful substances with the boiling point lower than the first control temperature can be separated out in a gas form, and the effective component ethanol of the white spirit can be continuously kept in the distiller. Then, the temperature in the distiller is controlled to be a second control temperature (80-95 ℃) so as to separate harmful substances with boiling points higher than the second control temperature. Because the boiling point of the effective component ethanol of the white spirit is 77 ℃, when the temperature in the distiller is higher than the second control temperature, the ethanol is evaporated into a gaseous state and enters the gaseous state separation process in the form of white spirit steam, and harmful substances in the white spirit, the boiling point of which is higher than the second control temperature, can still remain in the distiller, so that the primary separation of the white spirit is realized.
After the white spirit steam enters a gas separation process, the white spirit steam passes through a filtering material, and the filtering material can remove harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like, so that secondary separation of the white spirit is realized; meanwhile, after the white spirit steam enters the gas separation process, the temperature is reduced, the white spirit can be condensed into liquid, and the white spirit enters the liquid separation process in the form of white spirit liquid.
After the liquor liquid enters the liquid-state separation process, the liquor liquid passes through the filtering material, and the filtering material can remove harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like, so that the liquor can be separated for the third time.
And (3) the liquor after liquid separation enters a second distillation and separation process, and similar to the first distillation and separation process, the temperature in the distiller is controlled to be the first control temperature (70-75 ℃) at first so as to separate harmful substances with the boiling point lower than the first control temperature. Because the boiling point of the effective component ethanol of the white spirit is 77 ℃, when the temperature of the distiller is lower than the first control temperature, harmful substances with the boiling point lower than the first control temperature can be separated out in a gas form, and the effective component ethanol of the white spirit can be continuously kept in the distiller. Then, the temperature in the distiller is controlled to be a second control temperature (80-95 ℃) so as to separate harmful substances with boiling points higher than the second control temperature. Because the boiling point of the effective component ethanol of the white spirit is 77 ℃, when the temperature in the distiller is higher than the second control temperature, the ethanol is evaporated into a gaseous state and enters the condensing device in the form of white spirit steam, harmful substances in the white spirit with the boiling point higher than the second control temperature still remain in the distiller, and the white spirit steam entering the condensing device is condensed into liquid, so that the white spirit final product with the harmful substances effectively removed is obtained.
The second distillation separation combines together with the first distillation separation, can reach the effect of more effective harmful substance separation.
After the separation method provided by the invention is used for treatment, the content of harmful substances such as formaldehyde, methanol, sulfur, plasticizer, lead, free radicals and the like in the white spirit can be greatly reduced.
In a preferred embodiment, the first controlled temperature is 70 ℃ to 75 ℃, and may be, for example, but not limited to, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, or 75 ℃.
In another preferred embodiment, the second controlled temperature is 80 ℃ to 95 ℃, and may be, for example, but not limited to, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃ or 95 ℃.
In another preferred embodiment, the filter material includes minerals that adsorb harmful substances such as methanol, lead, plasticizers, sulfur, zinc, free radicals, and the like.
In another preferred embodiment, the filter material comprises activated carbon, which is capable of adsorbing harmful substances such as methanol, lead, plasticizers, sulfur, zinc, free radicals, and the like.
In another preferred embodiment, the filter material further comprises a quantum energy releasing substance capable of ionizing the inert substance so as to be removed by adsorption to minerals or activated carbon.
In addition, the invention also provides the white spirit, which is the ecological safe and healthy white spirit with harmful substances removed according to the separation method, wherein the content of the harmful substances is low, for example, the content of lead ions and methanol is lower than 0.005 mg/mL.
In order to facilitate a clearer understanding of the disclosure of the present invention, reference will now be made in detail to specific embodiments thereof.
Example 1
The present embodiment provides a method for separating harmful substances in white spirit, fig. 1 is a process flow diagram of the separation method, fig. 2 is a component walking diagram, and the following is specifically explained with reference to fig. 1 and fig. 2:
putting the white spirit to be subjected to harmful substance removal into a first distiller, firstly controlling the temperature of the first distiller to be 70-75 ℃, and separating harmful substances with lower boiling points in a gas form because the boiling point of the effective component ethanol of the white spirit is 77 ℃, and then feeding the harmful substances into a harmful substance collector, wherein the effective component ethanol of the white spirit is continuously retained in the first distiller. And then, controlling the temperature in the first distiller to be 80-95 ℃, wherein the boiling point of ethanol serving as an effective component of the white spirit is 77 ℃, so that the ethanol can be evaporated into a gaseous state and enters a gaseous separation process in the form of white spirit steam, and harmful substances with higher boiling points in the white spirit can still be remained in the distiller, so that the primary separation of the white spirit is realized.
The liquor steam enters a gaseous filter to be subjected to a gaseous separation process, a filter material is arranged in the gaseous filter, and when the liquor steam passes through the filter material, the filter material can remove the content of harmful substances such as formaldehyde, methanol, lead, sulfur, plasticizer, free radicals and the like, so that the second separation of the liquor is realized; meanwhile, after the white spirit steam enters the gas filter, the temperature is reduced, the white spirit can be condensed into liquid, and the liquid enters the liquid filter in the form of white spirit liquid.
The liquor liquid enters the liquid filter to be subjected to a liquid separation process, the liquid filter is provided with a filtering material, and when the liquor liquid passes through the filtering material, the filtering material can remove the content of harmful substances such as formaldehyde, methanol, lead, sulfur, plasticizers, free radicals and the like, so that the liquor can be separated for the third time.
In this embodiment, the filter material in the gas filter and the liquid filter is activated carbon.
And (3) the liquor subjected to liquid separation enters a second distiller, the temperature of the second distiller is controlled to be 70-75 ℃, and because the boiling point of the effective component ethanol of the liquor is 77 ℃, harmful substances with lower boiling points can be separated in a gas form and enter a harmful substance collector, and the effective component ethanol of the liquor can be continuously retained in the second distiller. And then, controlling the temperature in the second distiller to be 80-95 ℃, wherein the boiling point of the effective component ethanol of the white spirit is 77 ℃, so that the ethanol can be evaporated into a gaseous state and enters the condensing device in the form of white spirit steam, the harmful substances with higher boiling points in the white spirit can still remain in the distiller, and the white spirit steam entering the condensing device is condensed into liquid, so that the final white spirit product with the harmful substances effectively removed is obtained.
Example 2
This embodiment is a modification of embodiment 1, and is the same as embodiment 1 except that the filter materials in the gas filter and the liquid filter are minerals.
Example 3
This embodiment is a modification of embodiment 1, and is the same as embodiment 1 except that the filter materials in the gas filter and the liquid filter are activated carbon and minerals.
After the white spirit is filtered by the activated carbon, the harmful substances in the white spirit can be more effectively removed by mineral substance filtration.
Example 4
This example is a modification of example 1, and is the same as example 1 except that the filter materials in the gas filter and the liquid filter are quantum energy releasing beads, activated carbon, and minerals.
After the white spirit passes through the quantum energy release beads, the quantum energy release beads can promote the ionization of inert substances, and harmful substances in the white spirit can be removed more effectively through the filtration of the activated carbon and the mineral substances.
In addition, the inventor also carried out the detection of harmful substances on the white spirits treated by the methods of examples 1 to 4, and the specific contents are as follows.
Determination of methanol content in white spirit
And measuring the content of the methanol in the white spirit by adopting a gas chromatography.
(1) Reagent: methanol standard and absolute ethyl alcohol
(2) Chromatographic conditions are as follows:
a chromatographic column: capillary chromatography column AC20
Carrier gas: nitrogen at a flow rate of 8mL/min
The temperature of the sample inlet is 220 ℃, and the split ratio is 5:1
Temperature programming: maintaining at 35 deg.C for 4min, increasing to 200 deg.C at 4 deg.C/min, and maintaining for 10min
Detector temperature: at 220 ℃, tail blowing is carried out for 30mL/min, hydrogen flow rate is 40mL/min, and air flow rate is 400mL/min
Sample introduction amount: 0.4. mu.L
(3) Drawing of standard curve
The methanol standard was prepared at concentrations of 0.2, 0.5, 1, 2, and 4 μ g/mL, and 0.4 μ L was sequentially injected into a gas chromatograph and measured, and a standard curve was drawn with the concentration as abscissa and the peak area as ordinate.
(4) Sample analysis
And (3) injecting 0.4 mu L of liquor sample to be detected into a gas chromatograph for determination, recording peak area, and calculating the content of methanol in the liquor sample to be detected according to a standard curve.
Determination of lead content in white spirit
And (3) measuring the content of lead in the white spirit by adopting an atomic absorption spectrophotometer method.
(1) Reagent
Lead nitrate standard solution
(2) Detection conditions
The atomic absorption spectrophotometer has a detection wavelength of 283.3nm, a lamp current of 2.0mA, an oil-free air compressor pressure of 0.3MPa, a fuel gas flow of 1600mL/min and a fuel gas height of 5 mm.
(3) Drawing of standard curve
The lead nitrate standard substance is prepared into concentrations of 0.5, 1, 1.5, 2, 2.5 and 3mg/L, and is measured by an atomic absorption spectrophotometer, and a standard curve is drawn by taking the concentration as an abscissa and the absorbance value as an ordinate.
(4) Sample analysis
Sucking 10mL of white spirit sample into a sample dissolving cup, placing the sample in an electric hot plate at 105 ℃ for evaporation and concentration to be nearly dry (1-2 mL), taking down and cooling, transferring the sample into a 10mL volumetric flask by using 0.5mol/L nitric acid, carrying out constant volume shaking uniformly, measuring by using an atomic absorption spectrophotometer, recording the peak area, and calculating the content of lead in the white spirit sample to be measured according to a standard curve.
With reference to the above content measurement methods, the white spirits treated according to the methods of examples 1 to 4 were tested for harmful substances, and the specific results are shown in table 1.
TABLE 1 content of methanol and lead in different samples of white spirit
Group of Methanol (mg/mL) Lead (mg/mL)
Untreated 3.8 1.4
Example 1 0.008* Must not detect (<0.005)
Example 2 0.009* Must not detect (<0.005)
Example 3 Must not detect (<0.005) Must not detect (<0.005)
Example 4 Must not detect (<0.005) Must not detect (<0.005)
Note: represents significant difference compared with untreated group (P <0.05)
Wherein, the untreated sample refers to an original white spirit sample which is not subjected to harmful substance separation treatment. The data in table 1 show that the content of harmful substances such as methanol and lead in the white spirit is greatly reduced after the separation method provided by the invention is used for treatment, and the white spirit meets the national safety standard and is ecologically safe and healthy.
Furthermore, as can be seen from the data in table 1, when activated carbon and minerals are used together as the filter material, there is a better separation effect, and when the quantum energy releasing beads are used together with activated carbon and minerals, the separation effect is significantly improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A method for separating harmful substances in white spirit is characterized by comprising the following steps:
first distillation separation: controlling the temperature in the distiller to be a first control temperature so as to separate harmful substances with boiling points lower than the first control temperature; then, controlling the temperature in the distiller to be a second control temperature to separate harmful substances with boiling points higher than the second control temperature, and enabling the white spirit to enter a gas separation process in the form of steam;
gas separation: removing harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like from the white spirit steam through a filter material, condensing the white spirit steam into a liquid state, and entering a liquid separation process;
liquid state separation: removing harmful substances such as methanol, lead, plasticizer, sulfur, zinc, free radicals and the like from the liquor liquid through a filter material, and performing a second distillation separation process;
and (3) second distillation separation: controlling the temperature in the distiller to be a first control temperature so as to separate harmful substances with boiling points lower than the first control temperature; then, controlling the temperature in the distiller to be a second control temperature to separate harmful substances with boiling points higher than the second control temperature, and enabling the white spirit to enter a condensing device in the form of steam, and condensing the white spirit steam to obtain white spirit with separated harmful substances;
the first control temperature is 70-75 ℃; the second control temperature is 80-95 ℃.
2. The separation method of claim 1, wherein the filter material comprises a mineral.
3. The separation method of claim 1, wherein the filter material comprises activated carbon.
4. The separation method of claim 2, wherein the filter material further comprises a quantum energy releasing substance capable of ionizing an inert substance.
5. The separation method of claim 3, wherein the filter material further comprises a quantum energy releasing substance capable of ionizing an inert substance.
6. A liquor which is free of harmful substances by the separation method according to any one of claims 1 to 5.
7. The white spirit according to claim 6, wherein the content of lead ions in the white spirit is less than 0.005 mg/mL.
8. The white spirit according to claim 6, wherein the content of methanol in the white spirit is less than 0.005 mg/mL.
CN201710250795.5A 2017-04-17 2017-04-17 Method for separating white spirit and harmful substances in white spirit Expired - Fee Related CN106834068B (en)

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CN108614061B (en) * 2018-07-02 2021-04-02 山东师范大学 Method for removing plasticizer from absolute ethyl alcohol and cyclohexane
CN115261179B (en) * 2022-08-23 2023-07-25 劲牌有限公司 Method for reducing formaldehyde content in white spirit
CN116218626B (en) * 2023-03-09 2024-05-31 上海信悉智能技术有限公司 Small-molecular low-deuterium white spirit and preparation process thereof

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CN201501858U (en) * 2009-09-17 2010-06-09 王伟 Methanol removal device for fermentation wine
CN102051307B (en) * 2010-09-30 2013-01-30 山西悦卜林创业投资有限公司 Red date brandy and production process thereof
CN202519233U (en) * 2012-03-03 2012-11-07 深圳市恒宝昌科技有限公司 White wine steam filtration treating plant
CN103087877B (en) * 2013-01-30 2014-07-30 刘绍国 Method for brewing wine by using wild fruits in mountain forest
CN103468561A (en) * 2013-09-19 2013-12-25 郭文辉 Intelligent household brewing machine
CN105567508B (en) * 2016-03-18 2018-08-21 河北唐城红枣酒业有限公司 A kind of Chinese data wine and preparation method thereof of low methanol content
CN105861256B (en) * 2016-05-30 2019-03-26 杜永生 White wine removal of impurities purification system and method

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