CN103409303A - Membrane distillation quality-improved base liquor of strong-flavor distilled liquor and membrane distillation method thereof - Google Patents
Membrane distillation quality-improved base liquor of strong-flavor distilled liquor and membrane distillation method thereof Download PDFInfo
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Abstract
The invention relates to a membrane distillation quality-improved base liquor of strong-flavor distilled liquor and a membrane distillation method thereof, and belongs to the technical field of brewing production. The membrane distilled base liquor of strong-flavor distilled liquor comprises the following components: 0.75-2.5g/L of ethyl hexanoate, 0.3-1.5g/L of ethyl lactate, and 0.24-1.2g/L of ethyl acetate, 0.05-0.25g/L of ethyl butyrate and 0.3-0.5g/L of isoamyl alcohol. The contents and proportions of all components in the base liquor are reasonably coordinated and quality and flavor of the base liquor are good, so that the quality of base liquor which cannot be used for blending pure kernel solid-state brewed liquor can be improved, the difficulty in blending liquor can be reduced, Chinese distilled liquor which is a system comprising complicated components can be optimized, the existing base liquor of strong-flavor distilled liquor, which contains unreasonable components, can be better balanced, the quality can be improved, the flavor can be more mellow and purer.
Description
Technical field
The present invention relates to a kind of base wine and the preparation method in wine brewing is produced thereof of white wine, more particularly, the present invention relates to a kind of base wine and membrane distillation method thereof of the aromatic Chinese spirit through the membrane distillation upgrading, belong to the wine brewing production technical field.
Background technology
White wine claims again liquor, is the distinctive a kind of liquor of China, is by starchy material, adds the sugar-fermenting agent, through solid-state, semi-solid state or liquid state fermentation, distillation, store, blend and make.The temporary work in-process wine to be defined the level of interim warehouse-in that fermented-wine unstrained spirits obtains through distillation, habituation is referred to as " former wine " in the industry.The wine degree of former wine is generally at 60-80%vol.Former wine, after deciding grade and level, classification, will combine the warehouse-in ageing, and the former wine of storehouse ageing is " base wine ".It is the wine (a class wine) with certain organoleptic feature (same rank).
The main component of white wine is the second alcohol and water, accounts for 98% of gross weight, and all the other 2% are only multiple chromatogram framework ingredient and the micro-fragrance matter that forms the white wine individual style.In white wine, flavour ingredient has detected 180 various ingredients at present.Mainly include machine acid, alcohol, ester, carbonyl compound and aromatics etc., although their content is atomic, determining quality and the style of wine.These components the number, quantity relative ratio relationship each other, be the key component that forms the wine body of the plentiful coordination of white wine.
The ester class is the essential substance that presents fragrance in China white wine, and the ordering of various ester classes is followed successively by the measured aromatic Chinese spirit of matter: ethyl hexanoate>ethyl lactate>ethyl acetate>ethyl butyrate.Wherein, the high-content of ethyl hexanoate, determined the main flavor characteristic of aromatic Chinese spirit; Content next be ethyl lactate, due to ethyl lactate be difficult to volatility and can and Multiple components generation affinity interaction, aftertaste to wine plays the cushioning balance effect, so, appropriate ethyl lactate has certain effect to the fragrance style of wine, and the wine body is imperfect at least excessively, crosses main body fragrant at most and does not give prominence to, the wine body is dull, can make wine produce astringent taste.
At present in the aromatic Chinese spirit of China, due to the impact of brewageing former wine and be subjected to the factors such as raw material and production technique, make former wine have larger difference at aspects such as physical and chemical index, sense organ, style and features, the one-level rate is no more than 40% usually, have 60% because of all kinds of indexs are undesirable can not be as one-level wine, in secondary wine, especially with ethyl lactate, exceed standard and the proportion of degradation is larger, this part wine content of ethyl lactate is higher, so that content of ethyl lactate affects vinosity higher than ethyl hexanoate content.Therefore, corresponding technical measures are adopted in research, reduce the content of ethyl lactate in the former wine of this part, make ethyl lactate and ethyl hexanoate ratio reasonable coordination, and the quality that promotes China's aromatic Chinese spirit is had to real meaning.
The base wine of existing aromatic Chinese spirit or the content of former wine main component are: ethyl hexanoate 0.75-2.5g/L, ethyl lactate 3-6g/L, ethyl acetate 0.24-1.2g/L, ethyl butyrate 0.1-0.25g/L, primary isoamyl alcohol 0.4-0.6g/L, its content of ethyl lactate reaches 3-6g/L usually, content of ethyl lactate has surpassed ethyl hexanoate content, ratio is extremely inharmonious, can't use base wine as blending.
In the prior art, the process for purification of former wine is mainly alcohol is carried out to rectifying, namely by rectifying tower, improve the purity of alcohol, but there is following shortcoming in this method:
1, need to repeat distillation by multi-stage column, energy consumption is high;
2, facility investment and battlefield area are large;
3, after rectifying in former wine Hubeiwan also be removed, can not remove for specific component.
Membrane distillation (MD) is the membrane sepn process that membrane technique combines with still-process, and it be take dewatering microporous film and is medium, and under the effect of film both sides draught head, in feed liquid, volatile constituent sees through fenestra with the steam form, thereby realizes the purpose of separating.With other sepn processes commonly used, compare, membrane distillation has that separation efficiency is high, operational condition is gentle, to the advantage such as the mechanical property of film and stock liquid interphase interaction and film is less demanding.
Membrane distillation adopts dewatering microporous film to take the poor process of membrane sepn as the mass transfer motivating force of film both sides atmospheric pressure, can be used for the distillation desalination of water, to aqueous solution removal volatile matter.For example, when the aqueous solution of differing temps is separated by dewatering microporous film, hydrophobicity due to film, the aqueous solution of both sides all can not see through fenestra and enter opposite side, but due to the air pressure of the warm side aqueous solution and membrane interface higher than cold side, water vapour will see through fenestra and enter cold side and condensation from warm side, this is quite similar with evaporation, mass transfer, condensation process in conventional distillation, so be called the membrane distillation process.
Paper document about film distillation technology:
1, Ma Jiutong, Zhang Fengjun, Wu Haoyu, " the membrane distillation method is processed the research of methanol aqueous solution ", " water technology ", 2003(01);
In above-mentioned paper, disclose and utilized tubular fibre membrane distillation assembly to carry out membrane distillation and process research containing methanol aqueous solution, high spot reviews affect the factor of methyl alcohol flux.As feed temperature, concentration, flow velocity, and the carrier fluid flow velocity etc.Found best working conditions.Its method is to impel methyl alcohol to enter absorption liquid by film by the temperature head of film both sides, and its component is only methyl alcohol and distilled water, so this method be not suitable for the processing of the present invention to the former wine of white wine.
2, Zheng Kai, Wang Changjin, Wu Chaoliang, Jin Jiang, " research of the membrane distillation method separating alcohol aqueous solution ", " water technology ", 2009(07);
Above-mentioned paper discloses the ceramic-film tube adopted after modification, the low-concentration ethanol aqueous solution has been carried out membrane distillation the experimental study high spot reviews operating parameters of membrane distillation process.The film that this technical scheme is selected is ceramic membrane; What process is the aqueous ethanolic solution of lower concentration (1-5%), and component is only water and ethanol, can't be to reduction or the removal of some specific components.
3, Sun Wei, the Wang Zhihai ，Nong Shao village, " selection of hollow-fibre membrane optimal performance condition when refining low alcohol white spirit ", " Journal of Dalian Institute of Light ", 1994(04).
Above-mentioned paper discloses the operational condition that a kind of hollow-fibre membrane filters for low alcohol, but the operation scheme of film is not described in detail, and the index before and after filtering is not contrasted, and only the turbidity when the low temperature contrasts to wine.
Patent documentation about film distillation technology:
1, State Intellectual Property Office in 2012.7.11, to disclose an application number be 201210056112.X, name is called the patent of invention of " a kind of membrane distillation technique that adopts the hollow fiber film assembly treatment of dyeing and printing ", this patent provides a kind of membrane distillation technique that adopts the hollow fiber film assembly treatment of dyeing and printing, comprises the following steps: step 1: the pre-treatment of dyeing waste water, step 2: membrane distillation is processed: will pass into Thermostatic water heaters through pretreated waste water, utilize the low-quality thermal source that produces in dyeing and printing process and the heat exchange of Thermostatic water heaters, waste water is heated to 50-60 degree centigrade, then pass in the membrane distillation pond that hollow fiber film assembly is housed, when waste water did not have hollow fiber film assembly, utilize the constant temperature cold water storage cistern to pass into the cold water of 10-15 degree centigrade in the hollow-fibre membrane in hollow fiber film assembly, make the inside and outside formation temperature difference of hollow-fibre membrane, water vapour in waste water is by the inboard migration in tunica fibrosa lateral, entering rear flank in tunica fibrosa is discharged by inboard cold water condensation.Can improve well the ratio of desalinization of wastewater treatment, reduce simultaneously the pre-treatment requirement, simplify treating processes, energy-saving and emission-reduction, reduce operation and maintenance cost.
This patent provides a kind of membrane distillation technique that adopts the hollow fiber film assembly treatment of dyeing and printing, if this process application is filtered to the following problem that mainly exists in the former wine dipper matter of white wine:
1) film immerses and is filtered in liquid, and the impurity in filtered liquid is very easily made the pollution of pair of films;
2) it passes into water coolant in film, after filtering, liquid directly mixes with water coolant, after mixing, liquid flooding could immerse the filtered liquid water tank, if be used to filtering white wine, be first allow after filtering wine with enter again the filtered liquid collection box after water coolant mixes, in fact water coolant has caused secondary pollution to filtering rear white wine, and after filtering, component concentration (as the wine degree) is wayward.
2, State Intellectual Property Office in 2008.2.13, to disclose an application number be 200710058024.2, name is called the patent of invention of " by the membrane distillation dehydration method of the polyatomic alcohol water solution of Maize Production ", this patent discloses a kind of dewatering of the polyatomic alcohol water solution by Maize Production, belongs to the utilisation technology of vacuum membrane distillation.The method adopts distillation device, at first polyatomic alcohol water solution is heated to 61 ℃-65 ℃ of temperature, then adopt feedstock pump that polyatomic alcohol water solution is joined in hollow-fibre membrane, in the film outside, form the vacuum environment of 0.085MPa-0.089MPa, thereby form in the film both sides, transmit steam pressure difference, water in the inboard polyatomic alcohol water solution of film sees through fenestra and enters the hollow-fibre membrane outside under the effect of steam pressure difference with vapor form, again through the cooling condensation Cheng Shui of the condenser system in the membrane module outside, collect water of condensation, thereby realization is concentrated by the dehydration of the polyatomic alcohol water solution of Maize Production.The invention has the advantages that, service temperature is below 65 ℃, and low with existing common distillation method phase specific energy consumption, film used is high to the rejection of polyvalent alcohol, and the polyvalent alcohol rate of loss is low.
It is only concentrated to its dehydration that above-mentioned corn polyatomic alcohol water solution adopts film distillation technology, the composition that needs in can't the former wine for aromatic Chinese spirit to remove or reduce content is removed and reduces content, and then just can't obtain high-quality, the pure positive aromatic Chinese spirit base wine of local flavor.
Summary of the invention
It is inharmonious that the present invention is intended to solve in the base wine of existing aromatic Chinese spirit component proportions, cause that quality is not high, local flavor is just not pure, the film distillation technology of other field is applied to the problem that the quality of China white wine and local flavor exist in controlling, overcome its defect, a kind of base wine of the aromatic Chinese spirit through the membrane distillation upgrading is provided, reach component concentration, ratio reasonable coordination, the purpose that quality and local flavor are good.
In order to realize the foregoing invention purpose, its concrete technical scheme is as follows:
A kind of base wine of the aromatic Chinese spirit through the membrane distillation upgrading is characterized in that: comprise following composition:
Ethyl hexanoate 0.75-2.5g/L
Ethyl lactate 0.3-1.5g/L
Ethyl acetate 0.24-1.2g/L
Ethyl butyrate 0.05-0.25g/L
Primary isoamyl alcohol 0.3-0.5g/L.
The ratio of ethyl hexanoate of the present invention, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.6-0.8:0.5-0.6:0.1.
The ratio of ethyl butyrate of the present invention and ethyl hexanoate<0.1.
A kind of membrane distillation method of base wine of the aromatic Chinese spirit through the membrane distillation upgrading is characterized in that: comprise following processing step:
A, former wine pre-treatment
Get the former wine of the aromatic Chinese spirit of identical alcoholic strength; Perhaps the former wine of the aromatic Chinese spirit of different wine precision is mixed;
B, former wine membrane distillation are processed
To in a side of film, be heated to vapor state through pretreated former wine, described film is hydrophobic hollow-fibre membrane, board-like film or rolled film, at the opposite side of film, controlling vacuum tightness is 0.7-0.95MPa, the former wine that makes to be heated to vapor state migrates to opposite side from a side of film, carries out the cross-film migration;
C, condensation of gas
The device that is heated in step B after the former wine cross-film migration of vapor state be condensed is condensed into liquid, obtains the base wine of membrane distillation aromatic Chinese spirit.
According to Raoult's law, the content of lower boiling component in vapour phase is always than high in liquid phase.When containing the mixed solution boiling of two kinds of compositions, the content A in the steam of certain component is that A/B=K is its volatility coefficient with the ratio of the content B in solution.The volatility coefficient of trace ingredients is rectifying coefficient K ˊ with the ratio of the volatility coefficient of ethanol, if the rectifying coefficient is greater than at 1 o'clock, means that it is volatile than ethanol; And be less than at 1 o'clock, than the difficult volatilization of ethanol.Under a certain wine degree, when the rectifying coefficient K of certain impurity ˊ is less than 1, illustrate that the concentration in the former ethanolic soln of the organic concentration ratio of another part in the ethanolic soln distillated is low.This partial organic substances is fewer than ethanol evaporation, has just reached the purpose of partly removing.
The present invention is in steps A, and the alcoholic strength of the former wine of the mixed aromatic Chinese spirit of former wine of the former wine of the aromatic Chinese spirit of described identical alcoholic strength or the aromatic Chinese spirit of different wine precision is 45-80%vol.
The present invention, in step B, describedly will be heated to vapor state in a side of film through pretreated former wine and refer to former wine is heated to 50-65 ℃.
The present invention is in step B, and described film is hydrophobic hollow-fibre membrane, and is placed in the top on former drinks plane.
The material of above-mentioned hollow-fibre membrane is tetrafluoroethylene, and aperture is 0.01-0.5 μ m, and the film internal diameter is 1-1.5mm, and external diameter is 2-3mm.
The present invention is in step C, and the condensing temperature of described condensation is 5-25 ℃.
The present invention is in step C, and the cooling medium in described condenser is refrigerated water, chilled brine or crosses cold organic medium.
The useful technique effect that the present invention brings:
1, each component concentration, ratio reasonable coordination in the base wine of membrane distillation aromatic Chinese spirit of the present invention, quality and local flavor are good.The base wine of aromatic Chinese spirit in prior art, its content of ethyl lactate reaches 3-6g/L usually, and content of ethyl lactate has surpassed ethyl hexanoate content, and ratio is extremely inharmonious, can't use base wine as blending.The composition that the base wine of membrane distillation aromatic Chinese spirit of the present invention is retained is ethyl hexanoate, ethyl acetate, and the composition that is lowered content is ethyl lactate, reduces the content of ethyl lactate and has avoided the meeting on the high side of its content to make the situation of liquor body style imbalance; Reduce primary isoamyl alcohol, the control primary isoamyl alcohol too much causes bitter taste, the astringent taste of wine.The adjustment of said components makes originally can not to promote be used to the base wine vinosity of blending solid fermentation by pure grains wine, reduce the wine body and hook the difficulty of adjusting, make the processing that is optimized of system that this component of China white wine is extremely complicated, make the base wine of the unreasonable aromatic Chinese spirit of existing component reach better balance, just make its quality improving, the more mellow alcohol of local flavor.
2, except absolute content, the ratio of several main esters also has a significant impact the quality of wine.The present invention is preferred, and the ratio of ethyl hexanoate, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.6-0.8:0.5-0.6:0.1, and the ratio at the enterprising one-step optimization composition in basis of basic content, reach better balance; In addition, the ratio of the preferred ethyl butyrate of the present invention and ethyl hexanoate, below 0.1, can avoid wine to produce the mud stink; Preventing that ethyl acetate fragrance is excessive causes that a presumptuous guest usurps the role of the host, affects the typical style of Luzhou-flavor.
3, on the basis of existing membrane distillation technique, the invention provides a kind of membrane distillation technique of optimization, adopt hydrophobic film, by heating, make the former wine vaporization of film one side, the vacuum tightness of controlling in hollow-fibre membrane is 0.7-0.95MPa, the various gas molecules that evaporate that make to vaporize move with different speed cross-films, make in the former wine of white wine the component tunicle that needs to remove and partly remove hold back, and the component that needs the component retained and part to retain is farthest passed through, obtain membrane distillation base wine through condensation.The method is applicable to the extremely optimization process of complicated system of this component of China white wine, makes the front unreasonable white wine of component of processing reach better balance, just makes its quality improving, the more mellow alcohol of local flavor; Described film is without immersing in former wine, and the membrane material used can not be dissolved in former wine yet, can not pollute film, has reduced the cost of producing and safeguarding; In the present invention, the material of cross-film migration is gas, indirectly with cooling medium in condenser, contacts, and can not pollute by membrane distillation base wine.The present invention adopts the membrane distillation technique technology that is suitable for the former wine of China white wine Luzhou-flavor, removes or reduces specific components in the former wine of white wine to reach, and optimizes the purpose of white wine quality and local flavor.
4,, on the basis of basic technical scheme, preferably in steps A, former wine wine degree is controlled to 45-80%vol.The component that needs part to remove due to the present invention is ethyl lactate, takes into account part and removes potato spirit, makes the balance of these component ratios, and the balance of they and ethyl hexanoate ratio, just can reach quality and the local flavor of white wine the best.Because in white wine, the volatility coefficient of each component (K) has very large relation with alcohol concn, so former wine wine degree is controlled to 45-80%vol, can control the relative rate of volatilization of various components, also just can control the removal amount of various components, further just can obtain best proportionlity, make the membrane distillation finally obtained base wine reach quality and the local flavor be more suitable for.
5, hydrophobic film of the present invention is preferably hydrophobic hollow-fibre membrane, by adopting the hollow-fibre membrane of the type, having selected vacuum pressure, be 0.7-0.95MPa, initial alcoholic strength is 45-80%vol, after Heating temperature is 50-65 ℃ of technique, utilize the ethyl lactate volatility coefficient low, under this kind processing condition, can make ethyl lactate be reduced to 1.5g/L by 5.0g/L, and the material at this pressure and temperature and film, under index, output reaches processing requirements, condensing temperature is 5-25 ℃, coordinate other processing parameters also between energy consumption and efficiency, to find trim point.The hydrophobic hollow fiber film is placed in to the top on former drinks plane, can cause secondary pollution to former wine, again because hollow-fibre membrane is pencil, almost can filling level above space, can increase the area of unit space inner membrance, raise the efficiency.
The accompanying drawing explanation
Fig. 1 is the distillation device structural representation that embodiment 17 is applicable to membrane distillation technique of the present invention;
Fig. 2 is the distillation device structural representation that embodiment 18 is applicable to membrane distillation technique of the present invention;
Fig. 3 is hollow fiber film structure schematic diagram in embodiment 17,18;
Fig. 4 is the membrane distillation device structural representation used in embodiment 18.
In figure, be labeled as: 1 is tank body, 2 is upper cover, 3 is liquid-inlet, 4 is pneumatic outlet, 5 is dividing plate, 6 is hollow-fibre membrane, 7 is heating unit, 8 is vacuum meter, 9 is rinse water entrance I, 10 is the liquidometer I, 11 is the hot blast import, 12 is sewage draining exit, 13 is the transport pipe I, 14 is condenser, 15 is the transport pipe II, 16 is liquid collecting tank, 17 is the liquidometer II, 18 is vacuum pump, 19 is rinse water entrance II, 20 is former wine discharge port, 21 is take away pump, 22 is blow-off pipe, 23 is Controlling System, 24 is sealing cover, 25 is stop part, 26 is sealing member, 61 is end socket, 62 is hollow fiber film tube.
Embodiment
Embodiment 1
A kind of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following composition:
Ethyl hexanoate 0.75g/L
Ethyl lactate 0.3g/L
Ethyl acetate 0.24g/L
Ethyl butyrate 0.05g/L
Primary isoamyl alcohol 0.3g/L.
Embodiment 2
A kind of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following composition:
Ethyl hexanoate 2.5g/L
Ethyl lactate 1.5g/L
Ethyl acetate 1.2g/L
Ethyl butyrate 0.25g/L
Primary isoamyl alcohol 0.5g/L.
Embodiment 3
A kind of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following composition:
Ethyl hexanoate 1.625g/L
Ethyl lactate 0.9g/L
Ethyl acetate 0.72g/L
Ethyl butyrate 0.15g/L
Primary isoamyl alcohol 0.4g/L.
A kind of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following composition:
Ethyl hexanoate 2.1g/L
Ethyl lactate 0.6g/L
Ethyl acetate 1g/L
Ethyl butyrate 0.12g/L
Primary isoamyl alcohol 0.35g/L.
Embodiment 5
On the basis of embodiment 1-4, preferred:
The ratio of described ethyl hexanoate, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.6:0.5:0.1.
Further, the ratio of described ethyl butyrate and ethyl hexanoate<0.1.
On the basis of embodiment 1-4, preferred:
The ratio of described ethyl hexanoate, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.8:0.6:0.1.
Further, the ratio of described ethyl butyrate and ethyl hexanoate<0.1.
Embodiment 7
On the basis of embodiment 1-4, preferred:
The ratio of described ethyl hexanoate, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.7:0.55:0.1.
Further, the ratio of described ethyl butyrate and ethyl hexanoate<0.1.
Embodiment 8
On the basis of embodiment 1-4, preferred:
The ratio of described ethyl hexanoate, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.65:0.52:0.1.
Further, the ratio of described ethyl butyrate and ethyl hexanoate<0.1.
Embodiment 9
A kind of membrane distillation method of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following processing step:
A, former wine pre-treatment
Get the former wine of the aromatic Chinese spirit of identical alcoholic strength; Perhaps the former wine of the aromatic Chinese spirit of different wine precision is mixed;
B, former wine membrane distillation are processed
To in a side of film, be heated to vapor state through pretreated former wine, described film is hydrophobic hollow-fibre membrane, board-like film or rolled film, at the opposite side of film, controlling vacuum tightness is 0.7MPa, the former wine that makes to be heated to vapor state migrates to opposite side from a side of film, carries out the cross-film migration;
C, condensation of gas
The device that is heated in step B after the former wine cross-film migration of vapor state be condensed is condensed into liquid, obtains the base wine of membrane distillation aromatic Chinese spirit.
A kind of membrane distillation method of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following processing step:
A, former wine pre-treatment
Get the former wine of the aromatic Chinese spirit of identical alcoholic strength; Perhaps the former wine of the aromatic Chinese spirit of different wine precision is mixed;
B, former wine membrane distillation are processed
To in a side of film, be heated to vapor state through pretreated former wine, described film is hydrophobic hollow-fibre membrane, board-like film or rolled film, at the opposite side of film, controlling vacuum tightness is 0.95MPa, the former wine that makes to be heated to vapor state migrates to opposite side from a side of film, carries out the cross-film migration;
C, condensation of gas
The device that is heated in step B after the former wine cross-film migration of vapor state be condensed is condensed into liquid, obtains the base wine of membrane distillation aromatic Chinese spirit.
A kind of membrane distillation method of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following processing step:
A, former wine pre-treatment
Get the former wine of the aromatic Chinese spirit of identical alcoholic strength; Perhaps the former wine of the aromatic Chinese spirit of different wine precision is mixed;
B, former wine membrane distillation are processed
To in a side of film, be heated to vapor state through pretreated former wine, described film is hydrophobic hollow-fibre membrane, board-like film or rolled film, at the opposite side of film, controlling vacuum tightness is 0.825MPa, the former wine that makes to be heated to vapor state migrates to opposite side from a side of film, carries out the cross-film migration;
C, condensation of gas
The device that is heated in step B after the former wine cross-film migration of vapor state be condensed is condensed into liquid, obtains the base wine of membrane distillation aromatic Chinese spirit.
A kind of membrane distillation method of base wine of the aromatic Chinese spirit through the membrane distillation upgrading comprises following processing step:
A, former wine pre-treatment
Get the former wine of the aromatic Chinese spirit of identical alcoholic strength; Perhaps the former wine of the aromatic Chinese spirit of different wine precision is mixed;
B, former wine membrane distillation are processed
To in a side of film, be heated to vapor state through pretreated former wine, described film is hydrophobic hollow-fibre membrane, board-like film or rolled film, at the opposite side of film, controlling vacuum tightness is 0.9MPa, the former wine that makes to be heated to vapor state migrates to opposite side from a side of film, carries out the cross-film migration;
C, condensation of gas
The device that is heated in step B after the former wine cross-film migration of vapor state be condensed is condensed into liquid, obtains the base wine of membrane distillation aromatic Chinese spirit.
On the basis of embodiment 9-12, preferred:
In steps A, the alcoholic strength of the former wine of the mixed aromatic Chinese spirit of former wine of the former wine of the aromatic Chinese spirit of described identical alcoholic strength or the aromatic Chinese spirit of different wine precision is 45%vol.
In step B, describedly will in a side of film, be heated to vapor state through pretreated former wine and refer to former wine is heated to 50 ℃.
In step B, described film is hydrophobic hollow-fibre membrane, and is placed in the top on former drinks plane.
The material of hollow-fibre membrane is tetrafluoroethylene, and aperture is 0.01 μ m, and the film internal diameter is 1mm, and external diameter is 2mm.
In step C, the condensing temperature of described condensation is 5 ℃.
In step C, the cooling medium in described condenser is refrigerated water, chilled brine or crosses cold organic medium.
On the basis of embodiment 9-12, preferred:
In steps A, the alcoholic strength of the former wine of the mixed aromatic Chinese spirit of former wine of the former wine of the aromatic Chinese spirit of described identical alcoholic strength or the aromatic Chinese spirit of different wine precision is 80%vol.
In step B, describedly will in a side of film, be heated to vapor state through pretreated former wine and refer to former wine is heated to 65 ℃.
In step B, described film is hydrophobic hollow-fibre membrane, and is placed in the top on former drinks plane.
The material of hollow-fibre membrane is tetrafluoroethylene, and aperture is 0.5 μ m, and the film internal diameter is 1.5mm, and external diameter is 3mm.
In step C, the condensing temperature of described condensation is 25 ℃.
In step C, the cooling medium in described condenser is refrigerated water, chilled brine or crosses cold organic medium.
On the basis of embodiment 9-12, preferred:
In steps A, the alcoholic strength of the former wine of the mixed aromatic Chinese spirit of former wine of the former wine of the aromatic Chinese spirit of described identical alcoholic strength or the aromatic Chinese spirit of different wine precision is 62.5%vol.
In step B, describedly will in a side of film, be heated to vapor state through pretreated former wine and refer to former wine is heated to 57.5 ℃.
In step B, described film is hydrophobic hollow-fibre membrane, and is placed in the top on former drinks plane.
The material of hollow-fibre membrane is tetrafluoroethylene, and aperture is 0.255 μ m, and the film internal diameter is 1.25mm, and external diameter is 2.5mm.
In step C, the condensing temperature of described condensation is 15 ℃.
In step C, the cooling medium in described condenser is refrigerated water, chilled brine or crosses cold organic medium.
On the basis of embodiment 9-12, preferred:
In steps A, the alcoholic strength of the former wine of the mixed aromatic Chinese spirit of former wine of the former wine of the aromatic Chinese spirit of described identical alcoholic strength or the aromatic Chinese spirit of different wine precision is 56%vol.
In step B, describedly will in a side of film, be heated to vapor state through pretreated former wine and refer to former wine is heated to 52 ℃.
In step B, described film is hydrophobic hollow-fibre membrane, and is placed in the top on former drinks plane.
The material of hollow-fibre membrane is tetrafluoroethylene, and aperture is 0.09 μ m, and the film internal diameter is 1.15mm, and external diameter is 2.7mm.
In step C, the condensing temperature of described condensation is 22 ℃.
In step C, the cooling medium in described condenser is refrigerated water, chilled brine or crosses cold organic medium.
Be applicable to the distillation device of membrane distillation technique of the present invention:
A kind of distillation device for former wine dipper matter, comprise membrane distillation device, condenser 14 and liquid collecting tank 16, one end of described condenser 14 is communicated with the output terminal of membrane distillation device, the other end is communicated with the input terminus of liquid collecting tank 16, in described membrane distillation device, be provided with one group of hollow-fibre membrane 6 that is " U " shape, described hollow-fibre membrane 6 is immersed in the former wine that is arranged in the membrane distillation device, and " U " shape opening end of hollow-fibre membrane 6 is communicated with the pneumatic outlet 4 that is positioned at membrane distillation device top.
Described membrane distillation device comprises tank body 1 and upper cover 2, described tank body 1 is provided with liquid-inlet 3, described pneumatic outlet 4 is arranged on upper cover 2, described upper cover 2 is fixed on tank body 1 and forms annular seal space, in described annular seal space, be provided with dividing plate 5, described dividing plate 5 is divided into liquid storehouse and gaseous state storehouse by annular seal space; Described liquid storehouse is communicated with liquid-inlet 3, and the gaseous state storehouse is communicated with pneumatic outlet 4; Described hollow-fibre membrane 6 is immersed in the former wine that is arranged in liquid storehouse, and " U " shape opening end of described hollow-fibre membrane 6 is fixed on dividing plate 5, and described liquid storehouse is communicated with the gaseous state storehouse by hollow-fibre membrane 6.
Described hollow-fibre membrane 6 comprises end socket 61 and is " U " shape hollow fiber film tube 62, and " U " shape opening end of described hollow fiber film tube 62 is fixed on end socket 61, and the residue body portion is suspended in liquid storehouse; Hollow-fibre membrane 6 is fixed on " U " shape opening end of hollow fiber film tube 62 on dividing plate 5 by end socket 61.
Described dividing plate 5 is provided with threaded hole, and described end socket 61 is provided with screw thread, and described hollow-fibre membrane 6 is fixed on dividing plate 5 by screw thread and threaded hole.
Described a kind of distillation device for former wine dipper matter also comprises transport pipe I 13 and transport pipe II 15, one end of described condenser 14 is communicated with the pneumatic outlet 4 of membrane distillation device by transport pipe I 13, and the other end is communicated with the input terminus of liquid collecting tank 16 by transport pipe II 15.
Described liquid-inlet 3 is arranged on membrane distillation device middle part, and membrane distillation device middle part also is provided with vacuum meter 8, rinse water entrance I 9 and liquidometer I 10; Described membrane distillation device bottom is provided with sewage draining exit 12; Described upper cover 5 also is provided with hot blast import 11.
Described a kind of distillation device for former wine dipper matter also comprises Controlling System 23, and described tank body 1 bottom is provided with heating unit 7, and described heating unit 7 is connected with Controlling System 23.
The input terminus of described liquid collecting tank 16 is arranged on the liquid collecting tank middle part, and described liquid collecting tank middle part is provided with liquidometer II 17 and vacuum pump 18, and the top of described liquid collecting tank 16 is provided with rinse water entrance II 19.
The bottom of described liquid collecting tank 16 is provided with former wine discharge port 20.
During use, after the liquid-inlet 3 of the former wine of need purifying by the membrane distillation device enters the membrane distillation device, by heating unit, liquid is heated again, each component volatilization enters gas phase in wine, the film selectivity is held back needs to remove component, after needing retained fraction by hollow-fibre membrane 6, enter the gaseous state storehouse, then enter and in condenser 14, carry out coolingly through transport pipe I 13, by transport pipe II 15, deliver in liquid collecting tank 16 and focus on again after cooling.
Be applicable to the distillation device of membrane distillation technique of the present invention:
A kind of distillation device for former wine dipper matter, comprise membrane distillation device, condenser 14 and liquid collecting tank 16, one end of described condenser 14 is communicated with the output terminal of membrane distillation device, the other end is communicated with the input terminus of liquid collecting tank 16, in described membrane distillation device, be provided with three groups of hollow-fibre membranes 6 that are " U " shape, described hollow-fibre membrane 6 is immersed in the former wine that is arranged in the membrane distillation device, and " U " shape opening end of hollow-fibre membrane 6 is communicated with the pneumatic outlet 4 that is positioned at membrane distillation device top.
Described membrane distillation device comprises tank body 1 and upper cover 2, described tank body 1 is provided with liquid-inlet 3, described pneumatic outlet 4 is arranged on upper cover 2, described upper cover 2 is fixed on tank body 1 and forms annular seal space, in described annular seal space, be provided with dividing plate 5, described dividing plate 5 is divided into liquid storehouse and gaseous state storehouse by annular seal space; Described liquid storehouse is communicated with liquid-inlet 3, and the gaseous state storehouse is communicated with pneumatic outlet 4; Described hollow-fibre membrane 6 is immersed in the former wine that is arranged in liquid storehouse, and " U " shape opening end of described hollow-fibre membrane 6 is fixed on dividing plate 5, and described liquid storehouse is communicated with the gaseous state storehouse by hollow-fibre membrane 6.
Described membrane distillation device also comprises the sealing cover 24 that is provided with stop part 25, and described sealing cover 24 is fixed on tank body 1, and described upper cover 2 is pressed on tank body 1 by stop part 25.
Described tank body 1 is provided with sealing member 26 with the junction of upper cover 2, and described sealing member 26 can be sealing-ring.
Described hollow-fibre membrane 6 comprises end socket 61 and is " U " shape hollow fiber film tube 62, and " U " shape opening end of described hollow fiber film tube 62 is fixed on end socket 61, and the residue body portion is suspended in liquid storehouse; Hollow-fibre membrane 6 is fixed on " U " shape opening end of hollow fiber film tube 62 on dividing plate 5 by end socket 61.
Described dividing plate 5 is provided with threaded hole, and described end socket 61 is provided with screw thread, and described hollow-fibre membrane 6 is fixed on dividing plate 5 by screw thread and threaded hole.
Described a kind of distillation device for former wine dipper matter also comprises transport pipe I 13 and transport pipe II 15, one end of described condenser 14 is communicated with the pneumatic outlet 4 of membrane distillation device by transport pipe I 13, and the other end is communicated with the input terminus of liquid collecting tank 16 by transport pipe II 15.
Described liquid-inlet 3 is arranged on membrane distillation device middle part, and membrane distillation device middle part also is provided with vacuum meter 8, rinse water entrance I 9 and liquidometer I 10; Described membrane distillation device bottom is provided with sewage draining exit 12; Described upper cover 5 also is provided with hot blast import 11.
Described a kind of distillation device for former wine dipper matter also comprises Controlling System 23, and described tank body 1 bottom is provided with heating unit 7, and described heating unit 7 is connected with Controlling System 23.
The input terminus of described liquid collecting tank 16 is arranged on the liquid collecting tank middle part, and described liquid collecting tank middle part is provided with liquidometer II 17 and vacuum pump 18, and the top of described liquid collecting tank 16 is provided with rinse water entrance II 19.
The bottom of described liquid collecting tank 16 is provided with former wine discharge port 20.
Described former wine discharge port 20 is provided with take away pump 21 and blow-off pipe 22.
Claims (10)
1. wine of the base through the aromatic Chinese spirit of membrane distillation upgrading is characterized in that: comprise following composition:
Ethyl hexanoate 0.75-2.5g/L
Ethyl lactate 0.3-1.5g/L
Ethyl acetate 0.24-1.2g/L
Ethyl butyrate 0.05-0.25g/L
Primary isoamyl alcohol 0.3-0.5g/L.
2. the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 1, it is characterized in that: the ratio of described ethyl hexanoate, ethyl lactate, ethyl acetate and ethyl butyrate is 1:0.6-0.8:0.5-0.6:0.1.
3. the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 1 and 2, is characterized in that: the ratio of described ethyl butyrate and ethyl hexanoate<0.1.
4. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 1 is characterized in that: comprise following processing step:
A, former wine pre-treatment
Get the former wine of the aromatic Chinese spirit of identical alcoholic strength; Perhaps the former wine of the aromatic Chinese spirit of different wine precision is mixed;
B, former wine membrane distillation are processed
To in a side of film, be heated to vapor state through pretreated former wine, described film is hydrophobic hollow-fibre membrane, board-like film or rolled film, at the opposite side of film, controlling vacuum tightness is 0.7-0.95MPa, the former wine that makes to be heated to vapor state migrates to opposite side from a side of film, carries out the cross-film migration;
C, condensation of gas
The device that is heated in step B after the former wine cross-film migration of vapor state be condensed is condensed into liquid, obtains the base wine of membrane distillation aromatic Chinese spirit.
5. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 4, it is characterized in that: in steps A, the alcoholic strength of the former wine of the mixed aromatic Chinese spirit of former wine of the former wine of the aromatic Chinese spirit of described identical alcoholic strength or the aromatic Chinese spirit of different wine precision is 45-80%vol.
6. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 4, it is characterized in that: in step B, describedly will in a side of film, be heated to vapor state through pretreated former wine and refer to former wine is heated to 50-65 ℃.
7. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 4, it is characterized in that: in step B, described film is hydrophobic hollow-fibre membrane, and is placed in the top on former drinks plane.
8. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 7, it is characterized in that: the material of described hollow-fibre membrane is tetrafluoroethylene, aperture is 0.01-0.5 μ m, and the film internal diameter is 1-1.5mm, and external diameter is 2-3mm.
9. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 4, it is characterized in that: in step C, the condensing temperature of described condensation is 5-25 ℃.
10. the membrane distillation method of the base wine of a kind of aromatic Chinese spirit through the membrane distillation upgrading according to claim 4 is characterized in that: in step C, the cooling medium in described condenser is refrigerated water, chilled brine or crosses cold organic medium.
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| CN103409303B (en) | 2016-04-06 |
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