CN1003378B - Prodn. of low percentage spirit using maifanshi stone - Google Patents

Prodn. of low percentage spirit using maifanshi stone Download PDF

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Publication number
CN1003378B
CN1003378B CN87100543.3A CN87100543A CN1003378B CN 1003378 B CN1003378 B CN 1003378B CN 87100543 A CN87100543 A CN 87100543A CN 1003378 B CN1003378 B CN 1003378B
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China
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medical stone
low alcohol
spirit
white spirit
technology
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CN87100543.3A
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CN87100543A (en
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魏玉清
只秉文
王雁飞
马锦秋
张经坤
姚风仪
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Nankai University
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Nankai University
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Publication of CN1003378B publication Critical patent/CN1003378B/en
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Abstract

The present invention belongs to the improvement on the technology for preparing and purifying low-alcohol spirits by an adsorption method. In order to overcome the defects of complicated technology and equipment as well as high cost of the existing technologies for preparing low-alcohol spirits by a membrane method and a resin method, a method that selected and processed medical stone is mixed with high-alcohol spirits and drinking water, and the low-alcohol spirits are prepared by standing or oscillation and filtration is adopted. The present invention has the advantages of simple technology and equipment, easy obtainment of raw materials and low cost; the quality of the low-alcohol spirits prepared by the technology is improved, the flavor of the original spirits is maintained, various trace elements necessary for human bodies are added to the spirits, and heavy metal elements harmful to human health are reduced. The technology is suitable for preparing low-alcohol spirits from high-alcohol spirits.

Description

Utilize medical stone to prepare low alcohol white spirit
The present invention relates to purification via adsorption-based process is prepared the improvement of low alcohol technology, particularly relate to the natural mineral medical stone and make sorbent material is prepared low alcohol white spirit by high spirit method.
Liquor is subjected to liking of the people deeply in China.Along with improving constantly of standard of living, people increase day by day to the requirement of high quality liquor, but ethanol content is higher in the high spirit (being generally 55-65 °), drinks in a large number and can be harmful to HUMAN HEALTH.For this reason, the technology of preparing of an urgent demand exploitation high-quality low alcohol white spirit (generally at 40-28 ° or lower) is to satisfy needs of society.
At present, the key issue of low alcohol white spirit production is after the high wine base adds water degree of falling, and can produce immediately with the cotton-shaped muddiness of the indeterminable white of general filter method, loses the original transparency of wine base, seriously influences the quality of wine.By analysis, the main component of white floss is colorless oil, is dissolved in alcohol, water insoluble, high boiling ethyl palmitate, ethyl oleate and ethyl linoleate.The solubleness of these three kinds of materials in alcohol also has much relations with temperature except that outside the Pass having with the wine degree, and temperature reduces, and their solubleness also reduces.
Absorption method is a kind of common method of low alcohol white spirit turbidity removal, and its mechanism of action is to utilize the absorption property of sorbent material that white flocculent turbidity thing is adsorbed on the sorbent material, removes by the method for mechanical filter then.Sorbent material commonly used has gac, starch, wilkinite (carclazyte), sodium alginate (algin), agar etc.Wherein, gac and starch are considered to effective sorbent material.The activated carbon method precipitation is rapid, easy and simple to handle, because gac has huge surface-area, adsorptive power is very strong, therefore, when the control of activated carbon dosage and action time improper, can be in the absorption low alcohol white spirit in the dregs, beneficiating ingredients such as the acid in the sorbing liquor, ester are difficult for keeping former wine taste; Advantage easy and simple to handle, less investment that the starch absorption method also has, but when the starch consumption is excessive, can bring the unpleasant odor of starch into to low alcohol, and adopt this method turbidity removal thorough inadequately, if the temperature drop of filling a wine cup for is low to moderate muddiness can take place again below 3 ℃ or be the loss of gloss phenomenon; Wilkinite has ion exchangeable and adsorptivity, so can be used for the low alcohol white spirit turbidity removal, it is contained the sodium mild alkaline treatment with silicic acid hydrogen sodium etc., can make its clarifying effect better, but the low alcohol white spirit turbidity removal effect that it is used for below 35 ° is better, increases with the wine degree, and clarifying effect weakens; Use sodium alginate or agar as sorbent treatment Luzhou-flavor low alcohol white spirit, the low alcohol mouthfeel is better, but clarifying speed is not ideal enough.
In recent years, adopt preparation that two or more material was mixed in proportion or made definite shape report also to be arranged as the sorbent material of low alcohol white spirit turbidity removal.For example, adopt gac and moisture silicic acid mixture, Weibull and bentonite mixes or they the two and gac blended mixture or the like, these mixed type sorbent materials have overcome the use one matter as sorbent material some deficiency at aspects such as sedimentation speed, clarifying effects, but some is cumbersome in the preparation of mixed preparation, it is more that some then makes the total acid of low alcohol white spirit, total ester descend, and the decline of potato spirit is remarkable etc.In addition, the resin method of using also is a kind of newer low alcohol white spirit manufacturing technology at present, it is to adopt polymeric adsorbent to handle high spirit earlier, and the high spirit with treated mistake mixes (its water yield is decided on the number of degrees of the low alcohol white spirit that need prepare) and promptly makes required low alcohol white spirit with an amount of tap water again.Though the polymeric adsorbent adsorptive power a little less than, but select then property height, adopt the low alcohol white spirit of resin method preparation haze-free, can keep former wine taste, sorbent materials such as specific activity charcoal, starch have incomparable superiority, but shortcoming is the Processes and apparatus more complicated, and technology of preparing is difficult for grasping, and this special resin cost height, thereby limited applying of it.
The purpose of this invention is to provide a kind of absorption method improvement technology for preparing low alcohol white spirit by high spirit, the sorbent material raw material that it adopts is easy to get, production technique and equipment are simple, with low cost, and the low alcohol decapacitation that makes improve former wine quality, keep outside the local flavor of former wine still a kind of nutrient excellent product that contains the various trace elements that is of value to HUMAN HEALTH.
Modern mineralogy thinks that medical stone is that the silicate that belongs to igneous rock forms through weathering.Because of its outward appearance is quite gained the name like the rice dumpling that pearl barley cooks.It is a kind of porousness ore, wherein contains tens kinds of trace elements that are of value to HUMAN HEALTH such as iron, magnesium, potassium, sodium, calcium, manganese, titanium, phosphorus, sulphur, silicon.Have and promote to grow and proteinic synthesizing the ability of raising antifatigue, anti-hypoxia and immunity.As far back as the Ming Dynasty, just have in the Compendium of Material Medica of the big physician's LI Shi-Zhen of China: the record of " nature and flavor of medical stone, sweet temperature is nontoxic, cures mainly swollen, the carbuncle on the back of all carbuncles " etc.In recent years; domestic and international adsorption to medical stone; cleaning action; the sterilization fresh-keeping effect; the effect of release of trace elements; regulating effect of aqueous solution pH etc. has been carried out big quantity research; proved that medical stone can be used as reodorant; the water mineralizer; water conditioner; food preservative; fodder additives; plant growth promoter etc.; developed medical stone in health care; beverage/food; farming, animal husbandry and fishery; environment protection; the series product of aspects such as beauty treatment; be widely used among industrial and agricultural production and the people's lives; the medical stone series products is liking of people extremely, and high-quality low alcohol white spirit of the present invention is one of medical stone beverage series product just.
The invention belongs to the improvement that purification via adsorption-based process prepares low alcohol technology, it is characterized in that used sorbent material is the medical stone of the selected processing of a kind of process, the mixed solution of this medical stone and high spirit and an amount of tap water (its water yield is decided on the concentration of the low alcohol white spirit that will prepare) is mixed, through leaving standstill or the after-filtration that vibrates, promptly make the low alcohol white spirit of desired concn.
In the solution of the present invention, at first the medical stone ore is carried out selected, with yellow-white for well.Then it washed, dries, pulverizes (the most handy stone ball mill pulverize), sieve, disinfection by ultraviolet light, make 8~100 purpose particles, the used best granularity of this technology is 8~16 orders.Next is the mixed solution of preparation high spirit and tap water, is about to a certain amount of high spirit and mixes with an amount of tap water (its water yield is decided on the number of degrees of the low alcohol white spirit of need preparation), and its tap water can be a tap water.After the drinks mixed solution prepares, the selected medical stone that processes can be added in the above-mentioned mixed solution solid-to-liquid ratio>5%(weight of general may command medical stone of the add-on of its medical stone and high spirit), best solid-to-liquid ratio is 5~10%(weight).Then above-mentioned solidliquid mixture is carried out purification process, treating processes can be carried out at normal temperatures and pressures, can adopt standing methods, above-mentioned solidliquid mixture is left standstill got final product in 24 hours, filters then, and the filtrate of gained promptly is the high-quality low alcohol white spirit of making; Also can adopt the method for vibration, vibration only needed get final product in 2 minutes as adopting at a high speed, filtered then, can make high-quality low alcohol white spirit of the present invention equally.Filtration can be used filter paper or filter core.Medical stone granule: can use half a year approximately continuously.The low alcohol white spirit that adopts the present invention to make can make the processing of wine accomplish turbidity removal, removal of impurities, not remove perfume, improves the quality of wine.
When by this processing requirement the solidliquid mixture of medical stone and high spirit and tap water being handled, when temperature, treatment time and solid-to-liquid ratio one timing, the transmittance of product low alcohol white spirit increases with the medical stone particle size reduction, but changes little; The total acid of low alcohol white spirit (with acetometer) is downward trend gradually with the medical stone particle size reduction, but changes not very big; Total ester (in ethyl acetate) of low alcohol white spirit with the medical stone granularity reduce also change not very big.For obtain the fine low alcohol and consider medical stone easy to process etc. to have selected the optimum size scope be 8~16 orders.
When the drinks mixed solution is a wine: water=2: the 1(volume), the solid-to-liquid ratio of medical stone and high wine is a 10%(weight), time of repose is 24 hours, and when service temperature was 22 ℃, the relation of the transmittance of product low alcohol white spirit, total acid and total ester content and medical stone granularity saw Table 1:
Table 1
The blank 8-16 16-28 of medical stone granularity order 28-50>50
Transmittance % 98.0 97.2 97.0 97.3 99.0
Total acid (with acetometer) grams per liter 0.550 0.540 0.455 0.500 0.475
Total ester (in ethyl acetate) grams per liter 3.119 3.127 2.848 3.067 3.159
Selection about solid-to-liquid ratio, temperature, medical stone granularity and treatment time one timing when drinks mixed solution purification process, increase to some extent by the increase of its transmittance of low alcohol of this prepared with solid-to-liquid ratio, but when solid-to-liquid ratio>20%(weight) after, transmittance is constant substantially; The total acid of low alcohol, total ester fluctuate to some extent with the increase of solid-to-liquid ratio, but change also not very big.But when solid-to-liquid ratio is high, the consumption of medical stone increases, and corresponding increase is all wanted in volume of equipment that purification process is used and power consumption etc., and the raising of the quality of low alcohol is not remarkable, for guaranteeing the quality of low alcohol, the best solid-to-liquid ratio that the present invention selects is 5~10%(weight).
In the drinks mixed solution, wine: water=2: the 1(volume), the purification process temperature is 21 ℃, and used medical stone granule: degree is 8~16 orders, and when time of repose was 24 hours, the relation of the transmittance of low alcohol white spirit, total acid, total ester and solid-to-liquid ratio saw Table 2:
Table 2
Solid-to-liquid ratio (medical stone: % 58 10 15 28 25 remarks high spirit)
Transmittance % 52.5 54.0 56.0 55.0 58.0 58.0 unfiltered supernatant liquors
Total acid (with acetometer) grams per liter 0.47 0.45 0.45 0.48 0.47 0.46
Total ester (in ethyl acetate) grams per liter 2.61 2.69 2.45 2.53 2.52 2.59
Selection about this technological temperature, regularly the transmittance of low alcohol rises appreciably with the rising of temperature when the granularity of medical stone, solid-to-liquid ratio, purification process time one, Zong total acid, ester then change not quite, consider from energy-conservation and simple, the easy to operate angle of technology, generally carry out at normal temperatures and pressures.
When the drinks mixed solution is a wine: water=2: the 1(volume), the medical stone granularity is 8~16 orders, and solid-to-liquid ratio is a 10%(weight), time of repose is 24 hours, the relation between the transmittance of low alcohol white spirit, total acid, total ester and the treatment temp sees Table 3:
Table 3
Treatment temp ℃ blank-20-10 20 22 remarks
Transmittance % 55.5 41.0 47.0 60.5 unfiltered supernatant liquors
Total acid (with acetometer) grams per liter 0.32 0.30 0.30 0.31
Total ester (in ethyl acetate) grams per liter 2.35 2.34 2.40 2.30
Annotate: blank assay is not add medical stone, the drinks mixed solution in the time of 20 ℃, wine: water=2: the 1(volume)
In this technology,, depend on treatment process to the treatment time of the solidliquid mixture of medical stone and high spirit and tap water.When one timing of conditions such as medical stone granularity, solid-to-liquid ratio, temperature, if adopt the method that leaves standstill to get final product in 24 hours; If adopt the method for vibration at a high speed, only need vibrate 2 minutes, filter then, can obtain effect same.
When the drinks mixed solution is a wine: water=2: the 1(volume), treatment temp is 26 ℃, and the medical stone granularity is 8~16 orders, and solid-to-liquid ratio is a 10%(weight) time, the relation of the transmittance of time of repose and low alcohol, total acid and total ester sees Table 4:
Table 4
Time of repose hour blank 24 48 72 96 remarks
Transmittance % 55.5 63 73 80 88 unfiltered supernatant liquors
Total acid (with acetometer) grams per liter 0.55 0.54 0.54 0.52 0.53
Total ester (in ethyl acetate) grams per liter 3.119 3.127 2.860 2.920 2.940
The low alcohol white spirit of prepared of the present invention is colourless, limpid transparent, no suspended substance and precipitation.Identify through national wine expert, all be better than former high spirit aspect color, the wind.Technology of the present invention not only makes high spirit, and treated to accomplish that removal of impurities does not remove fragrant, long storage is not muddy, and its maximum characteristics are also because medical stone energy stripping various trace elements in water, absorption reduces the objectionable impuritiess such as heavy metal element, bacterium and chlorine in the water, increased the various trace elements that is of value to HUMAN HEALTH in the low alcohol and make, reduce the content that is harmful to the heavy metal element of HUMAN HEALTH in the wine, and make wine obtain further sterilization functions, thereby increased the health nutrient value of low alcohol white spirit.In addition, technology of the present invention also has following advantage: (1) used treatment agent " medical stone " is a natural mineral, and China's reserves are abundant, thus raw material be easy to get, with low cost; (2) technology of the present invention and equipment are simple, and technology is grasped easily, and is easy to utilize.
Technology of the present invention is applicable to the low alcohol white spirit that high spirit is prepared into arbitrary concentration.
Be embodiments of the invention below, be used for without stint explanation the present invention.
Embodiment 1
Medical stone: pick up from Ji County Ta Yuan.
High spirit: Yuyang Tequ, Ji County bottled wine, 55.8 ° of wine degree.
Water: storehouse tap water on Ji County.
(1) selected medical stone and to prepare granularity be 8~16 purpose medical stone granule :s
From the medical stone that picks up from Ji County Ta Yuan, select about 1000 grams of medical stone of yellow-white, it washed, dries, pulverizes (using the single head shredder), sieve, selecting granularity is about 150 grams of 8~16 purpose medical stones, carries out disinfection 15 minutes with ultraviolet lamp, stand-by then.
(2) mixed solution of preparation high spirit and tap water
500 milliliters of Yuyang Tequ, Ji County bottled liquors are inserted among 1500 milliliters of vial A, getting on 250 milliliters of Ji County the storehouse tap water then pours among the vial A, shake a bottle A gently, make liquor and water uniform mixing, just made the mixed solution of Yuyang Tequ high spirit and tap water.Wherein, high spirit: water=2: the 1(volume), the wine degree is 37.2 °.
(3) utilize medical stone to prepare Yuyang Tequ low alcohol white spirit
The granularity that above-mentioned (1) is prepared is 8~16 purpose medical stones, the 45 grams vial A that places the high spirit that prepared and tap water mixed solution [solid-to-liquid ratio is a 10%(weight)], under normal pressure and temperature (22 ℃), left standstill 24 hours, with its clear liquid filter paper filtering, gained filtrate promptly is 37.2 ° Yuyang Tequ low alcohol white spirit of prepared of the present invention then.
Adopt the technology of the present invention Yuyang Tequ low alcohol white spirit just main physicochemical data close to compare with the wine degree that adopts the resin method preparation.It the results are shown in Table 5:
Table 5
Project name wine degree total acid and ester methyl alcohol fusel lead-and-oil paint
(degree) (grams per liter) (grams per liter) (restraining/100 milliliters) (restraining/100 milliliters) (mg/litre)
Medical stone method 17.20 0.564 2.937 0.01 0.050<1
Resin method 36.30 0.240 1.988 0.01 0.075<1
As seen from Table 5, with the Yuyang Tequ low alcohol white spirit of medical stone method preparation, its total acid, total ester content are apparently higher than resin method, and potato spirit content then is starkly lower than resin method.
In the present embodiment to using the medical stone method, resin method, and Yuyang Tequ bottled wine to add three kinds of liquor of storehouse tap water on Ji County (not treated) preparation wherein contained to human body beneficial's the trace element and the content of harmful element lead, the contrast situation that adopts atomic absorption spectrometry to analyze sees Table 6:
Table 6
Element term medical stone method resin method Yuyang Tequ+water
(37.20 ° of wine degree) (36.30 ° of wine degree) (37.20 ° of wine degree)
(ppm) (ppm) (ppm)
S 4.262 3.008 -
Ca 49.856 18.425 30.525
Cr 0.068 0.035 0.103
Mn 0.350 0.232 0.069
Fe 0.511 0.172 0.550
Ni 0.007 0.015 0.064
Cn 0.615 0.164 0.356
Zn 2.108 0.375 1.162
Se 0.172 0.067 0.073
Sr 0.318 0.064 0.022
V 11.479 8.753 36.830
Pb 0.042 0.151 0.151
As seen from Table 6, adopt the wherein contained trace element to the human body beneficial of low alcohol white spirit of medical stone method preparation general all apparently higher than resin method and not treated drinks mixed solution, harmful lead then is starkly lower than the latter two.
Yuyang Tequ low alcohol white spirit to above-mentioned two kinds of prepared, the meeting of tasting and appraising through the countries concerned's level and city-level wine expert participation, for the color of wine, wind etc. taste, synthetical comparison and assessment, the result consistently thinks that the low alcohol white spirit of medical stone method preparation is better than resin method.Its quality also is better than former commodity wine.
Embodiment 2
Medical stone: pick up from Ta Yuan village, Ji County, the outward appearance Bluish white.
High spirit: it is 60.5 ° that spring bottled wine (Hebei province's quality liquor) wine degree is met in the product happiness of Lu Tai farm, Hebei province brewery.
Water: Lu Tai farm brewery tap water.
(1) selected medical stone and to prepare granularity be 16~100 purpose medical stone granule :s
Will pick up from about 500 grams of medical stone of Bluish white of Ji County Ta Yuan, preparing granularity by the method for (1) among the embodiment 1 is that 16~100 purpose medical stones about 150 restrain.
(2) mixed solution of preparation high spirit and tap water
Get happiness and meet 500 milliliters of spring bottled liquors (60.5 °), 296 milliliters of Lu Tai farm brewery tap water are liked the mixed solution that meets spring high spirit and tap water by the method preparation of (2) among the embodiment 1, place flask B.Wherein, high spirit: water=2: the 1.2(volume), the wine degree is 38 °.
(3) utilize medical stone preparation happiness to meet the spring low alcohol white spirit
The granularity that above-mentioned (1) is prepared is 16~100 purpose medical stone granule :s, 44 grams [solid-to-liquid ratio is a 10%(weight)], inserting above-mentioned (2) is equipped with among the flask B of drinks mixed solution, with iron platform and iron clamp with flask B suspention and the water-bath (normal temperature) that places the ultrasonic oscillator tank, with ultra-sonic oscillation 2 minutes, then flask B was left standstill 1.5 hours under normal pressure and temperature (26 ℃), promptly make happiness of the present invention with the clear liquid among the filter paper filtering flask B and meet the spring low alcohol white spirit.
Meet spring low alcohol white spirit and the happiness of handling without medical stone to meet spring low alcohol white spirit (being wine and water mixed liquid) with the happiness of prepared of the present invention, its physical and chemical index and the contrast situation of the content (employing aas determination) of human body beneficial's trace element and harmful ion, particularly heavy metal ion seen Table 7 and table 8 respectively:
Table 7
Project name wine degree total acid and ester methyl alcohol fusel lead-and-oil paint
(degree) (grams per liter) (grams per liter) (restraining/100 milliliters) (restraining/100 milliliters) (mg/litre)
The preparation of medical stone method
38 1.229 3.117 0.0125 0.0645 <1
The spring low alcohol is met in happiness
Handle without medical stone
38 1.284 3.209 0.0313 0.0666 <1
The spring low alcohol white spirit is met in happiness
Table 8
Element term identity element content remarks
Handle without medical stone through the happiness of medical stone processing
Meet spring low alcohol white spirit (38 °) happiness to meet spring low alcohol white spirit (38 °)
Zn (ppm) 0.39 0.26
Fe (ppm) 0.17 0.14
11.95 10.76 couples of human body beneficials of Ca (ppm)
Se (ppm) 0.017 NF trace element
Si (ppm) 11.920 5.220
Mn (ppm) 0.140 0.011
Co (ppm) 0.030 0.004
Sr (ppm) 0.260 0.090
Pb (ppb) 1.46 0.01
The ion that Cd (ppb) 6.36 9.87 is harmful
Hg (ppb) 3.60 10.08 is heavy metal ion particularly
As (ppb) 15.15 18.53
From table 7 and table 8 as seen, meet the spring low alcohol white spirit through the happiness that medical stone is handled, its total acid, total ester content change little, and methyl alcohol, potato spirit obviously reduce.Simultaneously, contained trace element to the human body beneficial rises appreciably in the low alcohol, and harmful ion, particularly heavy metal ion then have reduction greatly.
Annotate: in (1) technology of the present invention, physics and chemistry reagent is analytical pure.
(2) analytical procedure in the technology of the present invention is measured with reference to the method for " aromatic Chinese spirit and test method thereof " [Ministry of Light Industry of People's Republic of China (PRC) ministerial standard (trying) QB850-83] as total acid, total ester, methyl alcohol, potato spirit, plumbous analysis.
(3) used several key instrument equipment are as follows in the technology of the present invention:
Title model manufacturer purposes
Medical stone grinds in single head shredder XPM type Hubei mine locating machine works
The transmittance of the homemade mensuration wine of spectrophotometer 721 types
Atomic absorption spectrum 180-80 type FDAC is measured the trace element in the wine
Gas chromatograph 160 type FDACs are measured methyl alcohol and the potato spirit in the wine

Claims (5)

1, a kind ofly prepares the technology of low alcohol, it is characterized in that used sorbent material is the medical stone of the selected processing of a kind of process, this medical stone and high spirit are mixed with tap water, promptly make low alcohol white spirit through leaving standstill or vibrating, filter with purification via adsorption-based process.
2, by the described technology of claim 1, it is characterized in that used medical stone is a 8-100 purpose particle, best granularity is the 8-16 order, and its consumption is the solid-to-liquid ratio>5%(weight of medical stone and high spirit), best solid-to-liquid ratio is a 5-10%(weight).
3, by claim 1,2 described technologies, it is characterized in that processing, can adopt standing methods at normal temperatures and pressures, make low alcohol white spirit then after filtration the mixed solution of medical stone and high spirit and tap water.
4, by claim 1,2 described technologies, it is characterized in that processing, can adopt the method for vibration at normal temperatures and pressures, make low alcohol white spirit then after filtration medical stone and high spirit and tap water mixed solution.
5,, it is characterized in that prepared low alcohol white spirit can be the low alcohol white spirit of the arbitrary concentration lower than former high spirit concentration by claim 1,2 described technologies.
CN87100543.3A 1987-02-07 1987-02-07 Prodn. of low percentage spirit using maifanshi stone Expired CN1003378B (en)

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Application Number Priority Date Filing Date Title
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CN1003378B true CN1003378B (en) 1989-02-22

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Publication number Priority date Publication date Assignee Title
IT1396424B1 (en) * 2009-06-05 2012-11-23 Hf Europ Srl FOOD PRODUCTS INCLUDING ZEOLITI
CN102363743A (en) * 2011-10-17 2012-02-29 杜成 Method for processing medical stone distilled spirit
CN107805584A (en) * 2017-12-07 2018-03-16 马鞍山市太白酒厂 A kind of low concentration increases the preparation method of micro- fermentation white wine

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