CN101186872A - Osmosis evaporation separation recombination white spirit - Google Patents
Osmosis evaporation separation recombination white spirit Download PDFInfo
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- CN101186872A CN101186872A CNA2007100509986A CN200710050998A CN101186872A CN 101186872 A CN101186872 A CN 101186872A CN A2007100509986 A CNA2007100509986 A CN A2007100509986A CN 200710050998 A CN200710050998 A CN 200710050998A CN 101186872 A CN101186872 A CN 101186872A
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Abstract
A process for improving the quality of novel alcohol by permeation, evaporation, separation and reforming relates to application of separation technique with pervaporation membrane in the field of alcohol. The technique of the invention is that raw material alcohol is maintained in constant relatively low temperature, the liquor is transferred to a silastic composite membrane device by a pump and the liquor conducts circular flow in the upper reaches of the membrane, the lower reaches of the membrane is maintained in vacuum state by a vacuum pump, ethanol and volatile flavoring substances are selectively separated by pervaporation and turn into permeation vapor, representative mouth feeling and flavoring substances are reformed or concentrated in vapor, a low temperature condenser is equipped in the lower reaches of the membrane, condensed liquor with different components quantity of mouth feeling and flavoring substances is achieved by time steps of condensing of the permeation vapor, the liquor made by time steps of condensing is reformed and novel alcohol with high quality is blended. The process has the advantages of simple technological process, compact equipment, high maneuverability, short treatment period, which can develop novel alcohol with low cost and poor quality into novel alcohol with high price and good quality.
Description
Technical field
A kind of pervaporation is produced the method for high-quality liquor, relates to the application of pervaporation membrane separation technique at liquor industry, belongs to wine brewing science and membrane science field of engineering technology.
Technical background
White spirit is to adopt edible ethanol to combine with high-quality solid state fermentation base wine, carries out flavour passage or solid-liquid and blends, and carries out the flavouring seasoning with multiple eating spices and various sauce by the quantity relative ratio relationship of trace ingredients in the famous brand of wine or the wine body that designs voluntarily again and forms.China's white spirit develops in the fifties in last century, but gets up until the prosperity of the nineties, and tempo was exceedingly fast in recent years, output, sales volume cumulative year after year, and product covers the whole nation.The white spirit Total sales volume has accounted for more than 60% of national liquor market at present.White spirit has less investment, and consumption grain is low, with short production cycle, and mechanize, level of automation height are easy to expand the scale of production, remarkable in economical benefits, can in time adjust the style of wine according to market demand, continually develop the advantages such as product innovation that adapt to market; Its foreign matter content is low, hygienic safety, and the content of acid wherein, ester, aldehyde, potato spirit only is equivalent to 1/10~1/100 of traditional liquor, has drunk mouth and has not done, and head is not bitterly, and is little to the side effect of human body.The white spirit constant product quality, be easy to control, this is significant to the China white wine market of move towards to internationalize.
Because white spirit and traditional liquor production technique are different, quality also has than big difference, be mainly reflected in: the trace ingredients in the white spirit is complicated unlike other fermented wine, because most of without fermentation, trace ingredients is in kind and quantitatively exist congenital defect; Association in the edible ethanol between ethanol molecule and the water molecules is good not as grain wine, and unboiled water is distinguished the flavor of clearly.Therefore need take certain means to remedy the day after tomorrow, improve the mouthfeel of white spirit, improve its quality.At these problems, some liquor investigators add acetal monomer perfume composition artificially blending when accounting for the white spirit of main ratio with edible ethanol, in the hope of reaching promising result, but have occurred the dry sense of taste of uncomfortable suffering in the wine.People such as Tao Yang (publication number CN1609183) have invented a kind of new nano material, are placed in the liquor storage vessel with behind the former wine storage certain hour effectively to improve the liquor turbidity, remove new vinosity, but the required treatment time of this method are longer.
Have not yet to see the bibliographical information that adopts the pervaporation method to improve the white spirit quality.
Summary of the invention
The purpose of this invention is to provide a kind of novel process of improving the white spirit quality.
Specific embodiments of the present invention is:
Raw material liquor is maintained the constant lesser temps, with pump wine liquid being sent into the composite silicone rubber membrane device circulates in the upstream of film, vacuum state is kept by vacuum pump in the film downstream, ethanol in the wine and volatile flavor compounds are separated by pervaporation optionally becomes infiltration steam, and representational mouthfeel and flavour ingredient obtain reorganization or concentrate in steam; In the film downstream cryogenic condensation device is set,, obtains the condensation wine liquid of the different compositions of mouthfeel with fragrance matter by the infiltration of condensation at times steam; Condensation wine liquid reconfigures at times again, can blend the high-quality liquor that makes new advances.
The composite silicone rubber membrane cortical material that the present invention adopts is a polydimethylsiloxane, can optionally separate the volatile constituent in the liquor.
Raw material liquor is circulation repeatedly in the loop line that is made of raw wine storage tank, fresh feed pump, interchanger and membrane module, main component is separated fully through film in former wine, the condensation at times of film downstream is divided into three sections at least, and the timed interval was good from 0.5~10 hour with 1~3 hour.
The pervaporation operational condition is: 15~40 ℃ of feed temperatures, and feed liquid circulation velocity 0.02~1.0m/s, through the vacuum tightness 10~60mmHg of side, film condensed downstream temperature is-22~-30 ℃.
Beneficial effect of the present invention: by representative mouthfeel and the flavor compound in the separation recombination white spirit, strengthened the association of water and alcohol in the former wine, quickened the acetalation of acetaldehyde, the content of acetal in the former wine is increased, improve acetaldehyde brings in the former wine pungency and pungent sense effectively; Prepared new wine flavour is strong, and it is pure and sweet to distinguish the flavor of, smell coordination, and aftertaste is refreshing only, and outer perfuming and alcohol flavor are not obvious, and the slightly aging sense of acetal flavor is arranged on the smell.
Adopt the quality of the method raising white spirit of pervaporation, flow process is simple, facility compact, workable, and the processing cycle is short, the white spirit of inferior quality with low cost can be developed to the new wine product of high-quality high price.Have good market outlook.
Description of drawings
Accompanying drawing is the schematic flow sheet that pervaporation separates reorganization liquor.
1-raw wine storage tank wherein; The 2-fresh feed pump; The 3-interchanger; The 4-membrane module; The 5-condenser; The 6-transferpump; The 7-vacuum pump; 8,9,10-condensation wine liquid storage tank
Concrete embodiment
Pressing the flow process of accompanying drawing, is 0.024m with a composite silicone rubber membrane area
2Membrane module connect into the testing apparatus that pervaporation separates the liquor of recombinating with other equipment.Get the raw wine 8L of 52 degree, and its temperature maintenance is carried out pervaporation at 30 ℃, the feed liquid circulation velocity is 0.2m/s, and film downstream vacuum tightness is 10mmHg, and condensing temperature is-25 ℃.Raw wine liquid is at film upstream circulation 10h, and every 2h collects a condensation wine liquid.During EO, the most of flavor compound in the former wine is separated fully sees through film.Flavor compound and content thereof are as shown in table 1 in the condensation wine liquid collected of per period.
The separation rate and the rate of recovery can characterize composite silicone rubber membrane to the ability that removes of flavor compound and the recovery ability of system, and its expression formula is as follows respectively: certain flavour substances quality in separation rate=(in the former wine in certain flavour substances quality-seepage remaining liquid certain flavour substances quality)/former wine
Certain flavour substances total mass in the rate of recovery=penetrating fluid/(in the former wine in certain flavour substances quality-seepage remaining liquid certain flavour substances quality)
The local flavor substances content changes and data analysis unit: mg/100mL in 30 ℃ of condensation wine of table 1 liquid
|
1# | 2# | 3# | 4# | 5# | Seepage remaining liquid | Former wine | The upstream separation rate | Down-stream recovery |
Ethanol (wt.%) acetaldehyde methanol ethyl acetate n-propyl alcohol sec-butyl alcohol acetal isopropylcarbinol propyl carbinol | 74.52 16.64 6.85 352.06 23.66 3.1 71.41 18.3 6.48 | 73.13 14.64 6.73 156.84 24.69 2.98 43.84 17.7 6.81 | 72.10 11.13 6.69 54.83 24.29 2.84 25.56 16.42 6.82 | 70.62 8.95 5.83 13.64 23.25 2.86 16.35 15.18 6.5 | 69.16 6.15 7.87 0 21.52 2.25 8.93 13 5.83 | 26.49 3.9 3.75 0 5.61 0 0 2.15 1.15 | 42.61 20.16 4.33 62.82 12.54 1.09 11.88 6.89 3.11 | 58.62% 87.38% 43.49% 100.00% 70.81% 100.00% 100.00% 79.64% 75.87% | 86.10% 20.48% 40.57% 70.97% 65.27% 90.14% 103.78% 82.21% 72.70% |
Ethyl butyrate primary isoamyl alcohol Valeric acid ethylester ethyl lactate n-hexyl alcohol ethyl hexanoate total acid (g/L) | 135.12 35.81 42.38 53.42 4.17 1081.91 0.27 | 74.39 38.89 24.76 64.08 3.92 718.61 0.31 | 34.33 38.59 12.07 78.87 5.07 386.91 0.33 | 13.9 36.35 4.96 85.91 5.3 187.33 0.4 | 5.32 31.73 1.54 99.79 5.57 79.63 0.45 | 0 4.12 0 110.62 0 2.94 1.23 | 21.2 15.13 5.9 111.17 2.18 187.97 0.44 | 100.00% 82.23% 100.00% 35.07% 100.00% 98.98% - | 94.14% 83.59% 99.93% 23.38% 75.63% 97.75% - |
As can be seen from Table 1, the composition of flavour substances is all inequality in the condensation wine liquid collected of per period, and all more former wine of each component (except that acetaldehyde and ethyl lactate) has in various degree concentrated.5 kinds of ester classes (except the ethyl lactate) separation efficiency in the former wine is near 100%, the separation efficiency of other alcohols (removing methyl alcohol) is more than 70%, the overwhelming majority that sees through component is reclaimed in condensation wine liquid, and the new wine that the pervaporation of explanation process thus separation reorganization obtains can keep the flavor characteristic of former wine well.The separation rate of film upstream acetaldehyde is 87.38%, and down-stream recovery only is 20.48%, and promptly acetaldehyde is more in the process of pervaporation loss, and this is because the acetaldehyde boiling point is lower on the one hand, condenser system is not enough to acetaldehyde steam total condensation, and the part acetaldehyde that removes on the other hand transforms for acetal.The reduction of acetaldehyde makes pungent, the stimulation mouthfeel of former wine obviously weaken, and the new wine after the reorganization has the slightly aging sense of acetal flavor on smell.The rate of recovery of methyl alcohol is lower, and this explanation methyl alcohol also loses more in process of pervaporation.The rate of recovery of acetal has surpassed 100%, is because the part acetaldehyde condensation that removes is an acetal.
The aesthetic quality relatively before and after table 2 white spirit was crossed film
Sense organ | Former wine sensory evaluation | New wine sensory evaluation |
The aging sense aftertaste of color, smell and taste | Transparent clarification is aromatic, the flavor is pure and sweet, fragrance is coordinated, cleaner, have obviously to add the fragrance flavor the slightly bitter assorted flavor of living alcohol flavor aftertaste is arranged | Transparent clarification aromatic strongly fragrant, pure and sweet, the smell coordination of flavor, outer perfuming and give birth to the alcohol flavor and reduce greatly and have the aging sense aftertaste of acetal flavor slightly refreshing only on the smell |
Overall merit | Vinosity by white spirit behind this organo-silicone rubber composite membrane improves a lot |
Wine liquid after the expert of brewery separates pervaporation reconfigures, and under the situation of not adding any other flavour ingredient, blends the liquor that makes new advances.The senior of two professional institutions comments the wine expert that new wine has been carried out judging evaluation, as can be seen from Table 2, improves a lot through the more former wine of new wine quality that separates after recombinating.
Adopt the device identical with embodiment 1, get the 52 raw wine 8L that spend, and its temperature maintenance is carried out pervaporation at 35 ℃, the feed liquid circulation velocity is 0.2m/s, and film downstream vacuum tightness is 10mmHg, and condensing temperature is-25 ℃.Raw wine liquid is at film upstream circulation 10h, and every 2h collects a condensation wine liquid.During EO, the most of flavor compound in the former wine is separated fully sees through film.Flavor compound and content thereof are as shown in table 3 in the condensation wine liquid collected of per period.
The local flavor substances content changes and data analysis unit: mg/100mL in 35 ℃ of condensation wine of table 3 liquid
|
1# | 2# | 3# | 4# | 5# | Seepage remaining liquid | Former wine | The upstream separation rate | Down-stream recovery |
Ethanol (wt.%) acetaldehyde methanol ethyl acetate n-propyl alcohol sec-butyl alcohol acetal isopropylcarbinol propyl carbinol ethyl butyrate primary isoamyl alcohol Valeric acid ethylester ethyl lactate n-hexyl alcohol ethyl hexanoate total acid (g/L) | 71.87 23.46 5.46 385.78 24.28 3.19 74.07 18.15 7.01 128.4 40.19 40.08 68.19 5.45 1026.27 0.31 | 72.21 19.46 5.55 157.51 24.96 3.27 45.56 17.33 7.01 59.92 39.94 19.58 80.16 5.9 569.4 0.38 | 70.28 14.67 5.7 44.58 23.48 2.62 27 14.91 6.53 23.53 36.55 7.63 97.75 6.02 253.44 0.46 | 68.82 9.86 6.04 6.13 22.2 2.38 16.12 12.96 5.84 7.96 31.14 2.43 110.16 5.24 102.06 0.58 | 65.41 5.58 5.99 0 18.33 1.73 8.3 9.56 4.42 2.12 22.02 0 125 3.61 32.42 0.62 | 24.66 2.29 3.49 0 3.95 0 0 1.1 0.52 0 0.97 0 104.57 0 0 1.34 | 42.61 20.16 4.33 62.82 12.54 1.09 11.88 6.89 3.11 21.2 15.13 5.9 111.17 2.18 187.97 0.44 | 62.92% 93.13% 51.24% 100.00% 80.94% 100.00% 100.00% 90.34% 89.88% 100.00% 96.12% 100.00% 43.09% 100.00% 100.00% - | 87.53% 30.41% 50.17% 86.06% 72.34% 98.43% 124.38% 86.15% 79.98% 93.86% 91.17% 96.18% 33.17% 96.81% 93.51% - |
As can be seen from Table 3, the composition of flavour substances is all inequality in the condensation wine liquid collected of per period, and all more former wine of each component (except that acetaldehyde and ethyl lactate) has in various degree concentrated.5 kinds of ester classes (except the ethyl lactate) separation efficiency in the former wine is near 100%, the separation efficiency of other alcohols (removing methyl alcohol) is more than 80%, the overwhelming majority that sees through component is reclaimed in condensation wine liquid, and the new wine that the pervaporation of explanation process thus separation reorganization obtains can keep the flavor characteristic of former wine well.The separation rate of film upstream acetaldehyde is 93.13%, and down-stream recovery only is 30.41%, be that acetaldehyde is more in the process of pervaporation loss, this is because the acetaldehyde boiling point is lower on the one hand, condenser system is not enough to acetaldehyde steam total condensation is got off, and the part acetaldehyde that removes on the other hand transforms for acetal.The reduction of acetaldehyde makes pungent, the stimulation mouthfeel of former wine obviously weaken, and the new wine after the reorganization has the slightly aging sense of acetal flavor on smell.The rate of recovery of methyl alcohol is lower, and this explanation methyl alcohol also loses more in process of pervaporation.The rate of recovery of acetal has surpassed 100% up to 124.38%, is because the part acetaldehyde condensation that removes is an acetal.
The aesthetic quality relatively before and after table 4 white spirit was crossed film
Sense organ | Former wine sensory evaluation | New wine sensory evaluation |
The aging sense aftertaste of color, smell and taste | Transparent clarification is aromatic, the flavor is pure and sweet, fragrance is coordinated, cleaner, have obviously to add the fragrance flavor the slightly bitter assorted flavor of living alcohol flavor aftertaste is arranged | Transparent clarification aromatic strongly fragrant, pure and sweet, the smell coordination of flavor, outer perfuming and give birth to the alcohol flavor and reduce greatly and have the aging sense aftertaste of acetal flavor slightly refreshing only on the smell |
Overall merit | Vinosity by white spirit behind this organo-silicone rubber composite membrane improves a lot |
Wine liquid after the expert of brewery separates pervaporation reconfigures, and under the situation of not adding any other flavour ingredient, blends the liquor that makes new advances.The senior of two professional institutions comments the wine expert that new wine has been carried out judging evaluation, as can be seen from Table 4, improves a lot through the more former wine of new wine quality that separates after recombinating.
Adopt the device identical with embodiment 1 and example 2, get the 52 raw wine 8L that spend, and its temperature maintenance is carried out pervaporation at 40 ℃, the feed liquid circulation velocity is 0.2m/s, and film downstream vacuum tightness is 10mmHg, and condensing temperature is-23 ℃.Raw wine liquid is at film upstream circulation 10h, and every 2h collects a condensation wine liquid.During EO, the most of flavor compound in the former wine is separated fully sees through film.Flavor compound and content thereof are as shown in table 5 in the condensation wine liquid collected of per period.
The local flavor substances content changes and data analysis unit: mg/100mL in 40 ℃ of condensation wine of table 5 liquid
|
1# | 2# | 3# | 4# | 5# | Seepage remaining liquid | Former wine | The upstream separation rate | Down-stream recovery |
Ethanol (wt.%) acetaldehyde methanol ethyl acetate n-propyl alcohol sec-butyl alcohol acetal isopropylcarbinol propyl carbinol ethyl butyrate primary isoamyl alcohol Valeric acid ethylester ethyl lactate n-hexyl alcohol ethyl hexanoate total acid (g/L) | 72.21 23.01 5.42 370.29 24.5 3.27 68.05 18.39 7.15 128.14 40.86 40.08 72.8 5.74 1050.88 0.33 | 72.10 16.96 5.59 155.59 24.84 3.2 39.94 17.16 7.12 61.66 39.88 19.84 84.47 6.23 581.4 0.41 | 71.64 11.71 5.2 47.01 22.95 2.81 23.39 14.67 6.53 24.11 36.4 8.03 99.41 5.68 270.98 0.48 | 68.49 7.3 4.02 5.69 21.07 2.24 12.7 12.91 5.53 8.42 31.03 2.03 115.86 4.62 99.24 0.56 | 66.28 5.55 5.34 0 19.22 1.85 7.45 10.15 4.69 2.29 22.98 0 135.26 3.73 33.89 0.68 | 22.82 2.03 2.89 0 3.85 0 0 1.18 0.58 0 1.52 0 96.79 0 0 1.31 | 42.61 20.16 4.33 62.82 12.54 1.09 11.88 6.89 3.11 21.2 15.13 5.9 111.17 2.18 187.97 0.44 | 58.06% 94.20% 61.56% 100% 82.32% 100% 100% 90.14% 89.26% 100% 94.21% 100% 49.85% 100% 100% - | 88.96% 28.44% 50.34% 85.71% 76.90% 99.24% 115.14% 89.19% 85.93% 97.75% 93.79% 99.77% 37.87% 99.92% 99.42% - |
As can be seen from Table 5, the composition of flavour substances is all inequality in the condensation wine liquid collected of per period, and all more former wine of each component (except that acetaldehyde and ethyl lactate) has in various degree concentrated.5 kinds of ester classes (except the ethyl lactate) separation efficiency in the former wine is near 100%, the separation efficiency of other alcohols (removing methyl alcohol) is more than 80%, the overwhelming majority that sees through component is reclaimed in condensation wine liquid, and the new wine that the pervaporation of explanation process thus separation reorganization obtains can keep the flavor characteristic of former wine well.The separation rate of film upstream acetaldehyde is 94.20%, and down-stream recovery only is 28.44%, be that acetaldehyde is more in the process of pervaporation loss, this is because the acetaldehyde boiling point is lower on the one hand, condenser system is not enough to acetaldehyde steam total condensation is got off, and the part acetaldehyde that removes on the other hand transforms for acetal.The reduction of acetaldehyde makes pungent, the stimulation mouthfeel of former wine obviously weaken, and the new wine after the reorganization has the slightly aging sense of acetal flavor on smell.The rate of recovery of methyl alcohol is lower, and this explanation methyl alcohol also loses more in process of pervaporation.The rate of recovery of acetal has surpassed 100%, is because the part acetaldehyde condensation that removes is an acetal.
The aesthetic quality relatively before and after table 6 white spirit was crossed film
Sense organ | Former wine sensory evaluation | New wine sensory evaluation |
The aging sense aftertaste of color, smell and taste | Transparent clarification is aromatic, the flavor is pure and sweet, fragrance is coordinated, cleaner, have obviously to add the fragrance flavor the slightly bitter assorted flavor of living alcohol flavor aftertaste is arranged | Transparent clarification aromatic strongly fragrant, pure and sweet, the smell coordination of flavor, outer perfuming and give birth to the alcohol flavor and reduce greatly and have the aging sense aftertaste of acetal flavor slightly refreshing only on the smell |
Overall merit | Vinosity by white spirit behind this organo-silicone rubber composite membrane improves a lot |
Wine liquid after the expert of brewery separates pervaporation reconfigures, and under the situation of not adding any other flavour ingredient, blends the liquor that makes new advances.The senior of two professional institutions comments the wine expert that new wine has been carried out judging evaluation, as can be seen from Table 6, improves a lot through the more former wine of new wine quality that separates after recombinating.
Claims (5)
1. thereby method that improves its quality by osmosis evaporation separation recombination white spirit, it is characterized in that the present invention adopts following technical process: raw material liquor is maintained the constant lesser temps, with pump wine liquid being sent into the composite silicone rubber membrane device circulates in the upstream of film, vacuum state is kept by vacuum pump in the film downstream, ethanol in the wine and volatile flavor compounds are separated by pervaporation optionally becomes infiltration steam, and representational mouthfeel and flavour ingredient obtain reorganization or concentrate in steam; In the film downstream cryogenic condensation device is set,, obtains the condensation wine liquid of the different compositions of mouthfeel with fragrance matter by the infiltration of condensation at times steam; Condensation wine liquid reconfigures at times again, can blend the high-quality liquor that makes new advances.
2. thereby improve the method for its quality according to claim 1 is described by osmosis evaporation separation recombination white spirit, it is characterized in that described composite silicone rubber membrane cortical material is a polydimethylsiloxane.
3. thereby according to the described method that improves its quality by osmosis evaporation separation recombination white spirit of claim 1, it is characterized in that the circulation repeatedly in the loop line that is made of raw wine storage tank, fresh feed pump, interchanger and membrane module of raw material liquor, main component is separated fully through film in former wine.
4. thereby improve the method for its quality according to claim 1 is described by osmosis evaporation separation recombination white spirit, it is characterized in that described condensation at times is divided into three sections at least, the timed interval was good from 0.5~10 hour with 1~3 hour.
5. thereby according to the described method that improves its quality by osmosis evaporation separation recombination white spirit of claim 1, it is characterized in that described pervaporation operational condition is: 15~40 ℃ of feed temperatures, feed liquid circulation velocity 0.02~1.0m/s, see through the vacuum tightness 10~60mmHg of side, film condensed downstream temperature is-22~-30 ℃.
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CN113295809A (en) * | 2021-05-25 | 2021-08-24 | 北京工商大学 | Analytical method for extracting ester compounds in white spirit based on pervaporation membrane |
CN113214947A (en) * | 2021-06-09 | 2021-08-06 | 江苏久膜高科技股份有限公司 | Device and method for reducing content of higher alcohol in Maotai-flavor liquor |
CN113214948A (en) * | 2021-06-09 | 2021-08-06 | 江苏久膜高科技股份有限公司 | Device and method for reducing content of higher alcohol in strong aromatic Chinese spirits |
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CN113214948B (en) * | 2021-06-09 | 2024-01-16 | 江苏久膜高科技股份有限公司 | Device and method for reducing content of higher alcohol in Luzhou-flavor liquor |
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