CN102994295A - Method for recycling vinasse - Google Patents
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- CN102994295A CN102994295A CN2011102758392A CN201110275839A CN102994295A CN 102994295 A CN102994295 A CN 102994295A CN 2011102758392 A CN2011102758392 A CN 2011102758392A CN 201110275839 A CN201110275839 A CN 201110275839A CN 102994295 A CN102994295 A CN 102994295A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
Abstract
The invention relates to a method for recycling vinasse, and belongs to the technical field of resource recovery. The vinasse is washed by water and is soaked in the water to be changed into vinasse suspension liquid in which rice hulls and elution precipitates are suspended; the vinasse suspension liquid is subjected to screening and filtration to obtain the integral rice hulls; after the recycled rice hulls and fresh rice hulls are mixed together uniformly according to the mass rate of 1:1, and the mixture is added during a white spirit fermentation process again to produce white spirit; or mouldy bran is produced according to the mass ratio of mouldy bran to rice hulls being 95:5; filtrate which is obtained after screening and filtration is centrifuged or precipitated, and the obtained precipitate is used for preparing an animal feed; and filtrate which is obtained after screening and filtration is centrifuged or precipitated, and the obtained supernatant is recycled to be used as the water for washing the vinasse of step (1). Compared with various vinasse recycling methods of the prior art, the method has high vinasse utilization value, the liquor can recycle all the components of the treated vinasse most effectively, and the method has a good recycling effect.
Description
Technical field
The present invention relates to a kind of recycling method of vinasse, belong to resource recovery technology field.
Background technology
Vinasse be after the wine unstrained spirits has fermented again through distilling out after drinking residual mixing solid substance, so the compositions such as quite a lot of protein that has not utilized, starch, fat are arranged still in the vinasse, similar to the nutritive ingredient in the wine unstrained spirits, difference is just quantitatively arranged.In addition owing to having produced the biochemical change of various complexity in the whole ferment wine brewing process, so wherein also produced considerable new constituent, such as trace ingredientss useful to microorganism growth such as Yeast Nucleic Acid, purine, pyrimidine and some other secondary metabolites, this has promoted the utility value of vinasse greatly.
In recent years, along with the development of China's liquor technology and alcohol fuel promoting the use of in China, the annual production of liquor and ethanol improves gradually, as produce by product---the output of vinasse is also increasing, and the recycling of vinasse has become the problem that liquor industry is needed solution badly.According to relevant report, the in recent years annual production of China's liquor has reached 500-600 ten thousand t, and the output of distillers ' grains has also reached 2,100 ten thousand t.How to utilize vinasse will directly have influence on the development of liquor-making enterprises, be related to again the popularization of the relevant joint grain policy of country simultaneously with practicable.Therefore vinasse are not processed owing to high-moisture, high acidity in addition, very easily putrid and deteriorated, have so not only wasted valuable resource, also can cause severe contamination to the environment of periphery.Therefore, the recycling of vinasse all has very great meaning to resources development and utilization and the environment protection of China.
At present domestic is raw material or base-material as feedstuff industry to losing the most general processing mode of grain, general drying dehydration in addition directly packing sell, its added value is quite low, and carries out drying treatment and will consume mass energy, added value even be to bear.Because the accumulation of a large amount of materials will need very large transit depot, for the large Liquor-making Enterprises ﹠ of turnout, form very large place and take burden simultaneously, under the situation that current cost of land pressure increases gradually, have fatal denouncing.Therefore, how vinasse are efficiently utilized, it is turned waste into wealth, improve its economic worth, just becoming has very had researching value.
Although because the raw material that adopts, production technique is different, caused in the vinasse that solid state process fermentation liquor produces the nutritive ingredient kind all different with content, containing the nutritive substance that quite enriches in the vinasse is a common recognition.If can rationally be utilized, can not only bring certain economic benefit, can also avoid causing the pollution to environment.Following table 1-1 has just listed the content of various nutritive ingredients in the vinasse in detail to showing 1-4.
Conventional nutritive ingredient (% mass percent) in the table 1-1 vinasse
| Project | Bright grain | Do grain | Corn (contrast) |
| Moisture | 60.0-65.33 | 7-10 | 10-19 |
| Thick starch | 5.71-11.34 | 10-22 | 62-70 |
| Crude protein | 5.40-13.84 | 14.3-21.8 | 8-16 |
| Nitrogen-free extract | 18.20-19.34 | 41.7-45.8 | — |
| Crude fat | 1.31-3.24 | 4.2-6.9 | 2.7-5.3 |
| Robust fibre | 10.05-10.20 | 16.8-21.2 | 1.5-3.5 |
| Ash content | 3.50-10.76 | 3.9-15.1 | 1.5-2.6 |
| Total acid | 2.02-3.0 | 3.0 | — |
Annotate: comprised thick starch in the nitrogen-free extract.
Aminoacids content (% mass percent) in the table 1-2 distillers ' grains
| Title | Content | Title | Content | Title | Content |
| L-glutamic acid | 2.209 | α-amino-isovaleric acid | 0.636 | Tyrosine | 0.332 |
| L-Ala | 0.948 | Methionine(Met) | 0.17 | Phenylalanine | 0.705 |
| Threonine | 0.441 | Aspartic acid | 0.884 | Methionin | 0.4 |
| Serine | 0.518 | Isoleucine | 0.588 | Histidine | 0.328 |
| Tryptophane | 1.530 | Glycine | 0.496 | Arginine | 0.494 |
| Gelucystine | 0.754 | Leucine | 1.252 | Proline(Pro) | 0.961 |
Vitamin contents (mg/100g) in the table 1-3 distillers ' grains
| Title | Vitamin A | Vitamins B | Vitamins C | Vitamin PP | Niacinamide |
| Content | 625.00 | 27.90 | 37.50 | 419.92 | 182.69 |
Inorganic element content (mg/100g) in the table 1-4 distillers ' grains
| Title | Content | Title | Content | Title | Content |
| Phosphorus | 0.5 | Manganese | 0.01 | Chlorine | 0.26 |
| Potassium | 0.7 | Sodium | 0.03 | Chromium | — |
| Calcium | 0.3 | Copper | 0.001 | Plumbous | — |
| Magnesium | 0.3 | Molybdenum | 0.0004 | — | — |
| Iron | 0.1 | Caesium | 0.0005 | — | — |
Can find out that from table 1-1 the content except thick starch is lower than the corn the dried grain, the content of other nutritive substances such as crude protein, crude fat all exceeds corn.To showing 1-4 inorganic nutritive elements such as containing 18 seed amino acids (comprising 7 kinds of indispensable amino acids), multivitamin and the calcium that enriches, phosphorus, potassium the vinasse can be described then from table 1-2.In addition, the product that also contains the fermentations such as quite abundant alcohol, ester and acid in the vinasse.Above data prove absolutely that the nutritive ingredient in the vinasse is extremely abundant, have very high value of exploiting and utilizing.
Liquor production is the traditional fermentation technique of China, and the output of the overwhelming majority at home.At present, the large-scale liquor-making enterprises associating of domestic some colleges and universities strengthen the technological development dynamics at vinasse aspect utilizing, and have also obtained good progress aspect considerable, produce biochemical products such as vinasse, and vinasse are produced feed, and vinasse are made vinegar etc.
Contain abundant fermentation byproduct in the vinasse, such as glycerine, organic acid, amino acid, polymer sugar etc., this is to utilize vinasse generationization in next life product to establish good basic substance.Jiang Ying, yellow the U.S. and Britain (Jiang Ying, yellow the U.S. and Britain etc. from vinasse, extract aminoacids complex and trace element [J]. the foodstuffs industry science, 1991,6:14-16.) be studied utilizing vinasse to extract aminoacids complex, at first use H
2SO
4The protein of hydrolysis in the vinasse is used the lime slurry neutralization hydrolyzed solution again, through behind the centrifugal calcium carbonate and decolorizing with activated carbon of sloughing precipitation, extracts at last aminoacids complex again, finds that by measuring the aminoacids complex yield that extracts can reach 18-23%.
Gan Guangfeng, Liu Qingyun and Gu Hongbang, history build Pei (Gan Guangfeng, Liu Qingyun. to extract the experimental study [J] of Phytin in the paddy vinasse. Jianghan Petroleum College's journal, 1994, (1): 72-74.) etc. the people is studied the technique of extracting Phytin from vinasse; In addition, the people such as Wang Jinhua, Li Dongsheng (Wang Jinhua, Li Dongsheng etc. the extraction of water-soluble piperylene and purifying [J] in the brewer's grains. foodstuffs industry .2003, (4): 10-12.) to extract the research that water-soluble piperylene is correlated with from vinasse, find that vinasse are through hydrolysis, enzymolysis reaches further fermentation and the alcohol precipitation processing can extract 9.79% water-soluble piperylene, can obtain 4.50% purifying product through further purification process again.
Along with the raising of people's living standard, the demand of edible mushrooms is increased gradually, but the edible fungus culturing cost of material rises steadily, cause the cost of producing edible mushrooms to increase substantially.Nitrogen in the vinasse, phosphorus element content are high, contain simultaneously abundant vitamin B group and growth hormone, if regulate pH value (such as flat mushroom fostering requirement pH7, Pleurotus sajor-caju cultivate need pH8～9, Hericium erinaceus (Bull. Ex Fr.) Pers. to cultivate need pH4.5～6.5) after namely directly can cultivate the multiple eating bacterium.
Contain a certain amount of thick starch, crude protein, sugar and organic acid in the Chinese liquor distiller grains, thereby can be used as and make the vinegar raw material, this also is one of approach of utilizing of vinasse.It is to replace partially filled material with vinasse that the solid state fermentation vinasse are made vinegar, saves the raw material of making vinegar from the source; In addition, the protein in the vinasse decomposes by fermentation, has increased the aminoacids content in the vinegar, has improved the quality of vinegar, makes the vinegar of brew more fragrant, better to eat.General vinasse can not be separately as raw material, usually need to add batching in vinasse, such as wheat bran, rice, Semen Maydis powder or flour etc., the vinasse ingredient of each brewery is difference slightly, generally speaking, vinasse and other batchings need to be used behind the ratio mixing in 7:3.
For a long time, vinasse are used to bring into play vital role in farmers''s feed in the development of whole rural area animal husbandry and in the benign cycle of biologic chain always.But in recent years, along with the raising of scientific-technical progress and fodder industry aggregate level, the trophic structure in the fresh grain stillage can not full feeding the requirement of industry scientific feeding and the needs of scale development; The fresh grain stillage water content is up to 60% in addition, and acidity is higher, thus the difficulty of storage, if miscarriage is very easily gone mouldy; And containing rice husk 40%-50% in the vinasse, the viscosity of vinasse is also larger simultaneously, has brought suitable difficulty for whole vinasse processing.Therefore quality and the period of storage of lees feeds to be improved, deep processing must be carried out.
(1) separates rice husk oven dry vinasse and produce powdery or granular fodder
Because the crude fiber content in the rice husk is quite high, if the rice husk in the vinasse is not separated convection drying, although production technique is comparatively simple, but greatly affected the quality of feed, so need to manage to remove the rice husk in the vinasse, further make powdery or granular feed by oven dry again.The most frequently used method is to dry first, sieves out rice husk again, and then pulverizes and make feed.
(2) produce tropina
Utilizing biotechnology development and use vinasse, produce animal feeding-stuff containing somatic protein, is the research direction that improves the vinasse added value, also is the important channel that solves current protein feed critical shortage.Though common test report also has suitable distance from forming the scale production ability in recent years.
Make the vinasse robust fibre be converted into protein fodder, at first need one group of effectively polysaccharose substance such as trans-utilization Mierocrystalline cellulose, xylogen, therefore the microorganism that simultaneously can improve again protein content will carry out the orthoselection aspect two simultaneously when screening protein is produced bacterium.In addition, should screen suitable directly feeding living microorganism as far as possible, to improve the overall nutritive value of vinasse, bring into play the comprehensive value of all kinds of nutrition.The microorganism that is usually used at present producing tropina has rhizopus, candidiasis, aspergillus tubigensis, lactobacillus, streptococcus acidi lactici, subtilis bacterium, Methionin to produce bacterium, endomycopsi.sp, geotrichum candidum etc.Common many bacterial classifications mixed culture effect is comparatively obvious.
At present, brewery also is varied to the recycling method of vinasse in liquor production, gets up to concentrate on the Yield and quality that improves wine and several aspects such as economize in raw materials but sum up.
(1) returns the cellar for storing things fermentation
It is recycling to Fermentable substrate matter such as remaining starch in the vinasse that vinasse return cellar for storing things fermentation, remakes the short-term fermentation in the cellar for storing things as adding saccharifying enzyme and active dry yeast in losing grain, can returning.Different because losing poor remaining starch content and quality, therefore the yield of liquor and vinosity are also different.
(2) the vinasse string steams
It is the aroma component that will remain in the vinasse that the vinasse string steams, and utilizes the alcohol steam distillation again to extract.Because wine unstrained spirits when distillation, pure dissolubility flavour ingredient is difficult to be distilled out of and remains in the poor unstrained spirits when ethanol concn is low, water-soluble aroma component when steaming high wine, also be retained in the vinasse, so vinasse contain a large amount of pure dissolubilities, water-soluble flavour ingredient more.Most of vinasse strings adopt following two kinds of methods when steaming:
Add the unstrained spirits string and steam, so as to the raising vinosity, and increase output.When normal wine unstrained spirits loaded steamer, the space of the 5～10cm vinasse of packing into are stayed on top, add alcohol (or not adding alcohol) in the bottom of a pan and go here and there steaming.In the wine unstrained spirits, admix the alcohol effect as best (when going out rice steamer wine unstrained spirits and vinasse are strictly separated, respectively do it and use).The acid, the ester content that add unstrained spirits string steaming wine obviously improve.The aroma daqu liquor test-results is shown: acid improves 13.6～51.68%; Ester improves 69.91～424.1%.Its extracted amount is different because of distillation capacity for liquor.The vinasse string steams, and does not fill the wine unstrained spirits in the rice steamer, all adopts the grain string to steam.This fado uses common white spirit, and the wine after string steams need to be blent, to adjust the balance of flavour ingredient.
(3) add part vinasse koji
Remaining starch in the vinasse and organic acid etc. can be used as the carbon source of microorganism in the koji; Vinasse also can be regulated the pH value of bent material, make beneficial microorganism vigorous growth under suitable acidity, suppress simultaneously harmful microorganism.Contain abundant B family microorganism and phosphorus in the vinasse, be conducive to promote growth and the metabolism of enzyme and the carrying out of diastatic fermentation effect of thalline in the yeast making process.
Yuan Guang and (Yuan Guanghe, Hong Song. Daqu brewery loses the research report [J] of grain recycling. brewing science and technology, 1991, (03) .) etc. will remove grain slag behind the rice husk and wheat and mix in the ratio of 1:3 after koji, be used for yeast wine production, the result detects and finds that wherein the transformation efficiency of starch improves 3.03%, and the yield of liquor has improved 3.81%, and the content of ethyl hexanoate has improved 40%.
Zhang Baonian, Xia Yuanjin (Zhang Baonian, Xia Yuanjin. the application [J] of vinasse in pure wheat koji. wine brewing, 2010,37(03): 61-62.) tested interpolation part vinasse in pure wheat koji, not only can reduce the cost of koji, can also significantly improve the various physical and chemical indexs of made knee-piece simultaneously.
(4) cellar for storing things mud is Nutrious fermented dose
Luzhou-flavor vinosity and pit mud quality are closely related, during the mud of artificial culture cellar for storing things, add nitrogenous source and the microcosmic salts such as soya-bean cake.Not only the content of nitrogen and phosphorous is high in the vinasse, and contains the necessary micro-nutrient composition of cellar for storing things mud microorganism growth, so vinasse are desirable nutrition agents of cellar for storing things mud fermentation.
In addition, the existing ripe technology and equipment of biogas fermentation is produced biogas with vinasse and has not only been solved energy problem, has also reduced the pollution of water resources; Produce in addition fertilizer, produce the sugar activated carbon, produce amylase and cellulase etc., the utilization that can say vinasse is varied.
Summary of the invention
Technical purpose of the present invention is to provide a kind of vinasse recycling method of mixed economy, so that the method has the vinasse utility value for the described various vinasse recoverying and utilizing methods of prior art high, and after wine is processed vinasse each component can both be utilized in maximum efficiency and reclaimed, and recovering effect is splendid.
In order to realize technical purpose of the present invention, technical scheme of the present invention is as follows.
A kind of recycling method of vinasse is characterized in that may further comprise the steps:
(1) vinasse is washed with water, make the vinasse suspension that becomes rice husk, wash-out throw out suspendible after the vinasse immersions;
(2) the rear filtration of sieving of vinasse suspension obtains complete rice husk; After the ratio of 1:1 mixes the rice husk that reclaims and fresh rice husk in mass ratio, again add in the fermenting process of liquor and produce liquor; Perhaps carry out wheat bran production according to quality than wheat bran: rice husk=95:5;
(3) sieve and filter the centrifugal or sedimentation of the filtrate obtain, the throw out that obtains prepares animal-feed;
(4) sieve and filter the centrifugal or sedimentation of the filtrate obtain, the bath water as step (1) vinasse is reclaimed in the supernatant liquor that obtains circulation.
Further, the method that washes with water of the vinasse of described step (1) is the stirring and washing method.Particularly, be: solid-liquid ratio is mass ratio 1:2, and soak time is 30min, and washing times is 6 times.
The vinasse suspension of described step (2) sieves and filters the method obtain complete rice husk and be: the aperture of sieving is 1mm, and centrifugal rotational speed is 3000r/min, and centrifugation time is 15min.
The production method of the wheat bran of described step (2) is: respectively the white song in Ha Noi, subtilis, ester-producing yeast are carried out being mixed in proportion use after single spawn culture is made wheat bran at last; A. Ha Noi is bent in vain: the ratio of selected combination substratum: water=1:1 adds water, stirs, and in 121 ℃ of autoclaving 1h, is cooled to 35 ℃, plant song according to 2% access, mixing shakeouts, and keeps bent room to ventilate, humidity is 95 %-100 %, 35 ℃ of culture temperature, incubation time 72 h; B. subtilis: the characteristic chicken flavor that can produce typical distilled spirit with sesame flavour through fermentation culture, ratio according to selected combination substratum: water=1:1 adds water, 121 ℃ of autoclavings are cooled to 37 ℃, seed liquor is according to 4% access, mixing shakeouts, and keeps 34-37 ℃ of temperature, humidity 85%, control product temperature is no more than 55 ℃, incubation time 36-48h; C. ester-producing yeast: the ratio of selected combination substratum: water=1:1 adds water, and 121 ℃ of autoclavings are cooled to 30 ℃, and seed liquor is according to 4% access, and mixing shakeouts, maintain the temperature at about 30 ℃, and humidity 85%, control product temperature must not surpass 40 ℃, incubation time 48h.
Beneficial effect of the present invention is:
(1) realizes separating of vinasse suspension by adopting to filter with the centrifugal mode that combines, leach complete rice husk; Rice husk after reclaiming is carried out the research of integrity degree, color and luster, smell and support performance.Its structure of rice husk that research find to be reclaimed is substantially complete, and does not have peculiar smell, can consider it is recycled in the liquor fermentation process or add to produce in the production of wheat bran.
(2) in the ratio of 1:1 the rice husk that reclaims and fresh rice husk are mixed after, again add in the fermenting process of wine.The yield of liquor and local flavor by the wine that produces with the fresh rice husk zythepsary of normal employing compare, and checking is added and reclaimed the impact of rice husk on making wine.50% recovery rice husk wine brewing the yield of liquor is 40.9%, and brand-new bright rice husk wine brewing is 41.2%, is more or less the same; It is also similar that local flavor is judged the result.By gas chromatograph flavor compound is analyzed, the spectrogram result shows that content and kind are all close.As seen reclaim in the fermenting process that rice husk directly uses wine, all do not have what impact for the quality of the yield of liquor and wine, feasibility is high.
(3) by the saccharogenic power of investigating the different culture media combination, the evaluation of measuring biochemical indicator separately of liquefaction power, prove that adding a small amount of rice husk is good for wheat bran, so (wheat bran: rice husk=95:5) carries out enlarged culturing to choose wheat bran.The yield of liquor of the sesame-flavor Daqu wine brewing of contrast self-control wheat bran wine brewing and purchase, the former is 40.0%, the latter is 43.1%, is more or less the same; The rice husk that reclaims is added in the production of wheat bran on a small quantity, obviously is of value to the generation of microbial growth and relevant enzyme.
(4) sieve and filter the centrifugal or sedimentation of the filtrate obtain, the throw out drying that obtains is prepared into animal-feed, the protein content of the inside improves nearly 1 times more than than the protein content in the unprocessed direct preparation animal-feed of vinasse after testing, and therefore the economic worth through the animal-feed of preparation after this processing improves greatly.
(5) sieve and filter the centrifugal or sedimentation of the filtrate obtain, the bath water as vinasse is reclaimed in the supernatant liquor circulation that obtains, can realize efficiency of cycling economy, when the supernatant liquor cyclically utilizing repeatedly after, some aroma-producing substance that elutes from vinasse is a large amount of enrichments in supernatant liquor, can extract key substance in the supernatant liquor by separation means, be used further in the white spirit mixing.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is that the flavor compound content that reclaims rice husk fermentation liquor and fresh rice husk fermentation liquor compares.
Fig. 3 is wheat bran expanding production schema.
Embodiment
Embodiment 1
The present embodiment illustrates the preparation method of vinasse suspension of the present invention and the separation and recovery method of complete rice husk, as shown in Figure 1.
The foundation of vinasse suspension and some processing parameters that separate have been determined by experiment of single factor: when solid-liquid ratio is mass ratio 1:2, soak time is 30min, washing times is 6 times, the aperture of sieving is 1mm, centrifugal rotational speed is 3000r/min, just can finish foundation and the sepn process of vinasse suspension when centrifugation time is 15min.
Rice husk and fresh rice husk that separation obtains are examined under a microscope comparative analysis, find that the rice husk color and luster of recycling is darker, and fresh rice husk is golden yellow, color and luster is comparatively vivid.But the rice husk structure that reclaims is still more complete, that is to say still and can play the support fluffing action, and rice husk supports fluffing action exactly as the Main Function that auxiliary material rises during the fermentation.And fresh rice husk contains furfural, need to steam and just can use, but the rice husk that reclaims sees Table 2-1 with regard to there not being this problem.
Table 2-1 reclaims rice husk and fresh rice husk compares
| Project | Reclaim rice husk | New rice husk |
| The rice husk integrity degree | Structural integrity | Complete |
| Color and luster | Color and luster is darker | Color and luster is brighter |
| Smell | Lighter grain flavor | Different assorted flavor is heavier |
The rice husk and the fresh rice husk that accurately take by weighing respectively the 30g recovery are put in the measuring graduates, measure its volume.The results are shown in following table 2-2.As can be seen from the table, although the rice husk structure of recovery is comparatively complete, its support performance is not as fresh rice husk.
Two kinds of rice husk support performances of table 2-2 relatively
| Project | Reclaim rice husk | Fresh rice husk |
| Volume (mL) | 340 | 380 |
Embodiment 2
The application method of rice husk in liquor fermentation reclaimed in the present embodiment explanation.
After the ratio of 1:1 mixes the rice husk that reclaims and fresh rice husk in mass ratio, again add in the fermenting process of liquor and produce liquor; The rice husk that fermentation raw material has half to come from recovery except rice husk, the condition of other raw materials and fermenting process are all the same with original liquor fermentation condition.
Because kind, quality and the starch content of liquor-making raw material is different, stability and the comparability of the yield of liquor all had a great impact.Therefore, the raw grain the yield of liquor can not be as examination standard, and should examine standard raw grain the yield of liquor.Specific requirement and way are as follows:
(1) standard raw grain: raw grain comprises that mainly wine brewing is with the remaining starch in grain, yeast grain and the used Daqu (not comprising wheat bran) etc.The standard raw grain refers to the whole starch in the above-mentioned raw grain, amounts to into starch-containing 65% standard grain; All starch-containing at the supplementary material more than 5%, such as jowar chaff, maize peel, ravine chaff etc., all should be converted to starch-containing 65% standard grain.With the whole standard grains of converting as starch-containing 65% of the starch-containing amount (being as the criterion take enzymatic hydrolysis) of various materials, be called the standard raw grain.It is calculated as follows:
Liquor is produced the total consumption of starch (kg)=wine brewing raw grain (kg) * starch content (W%)+distiller's yeast grain (kilogram) * starch content (W%)+Daqu (kg) * starch content (W%)
Standard raw grain consumption: mark Huaihe River raw grain consumption (kg)=liquor is produced the total consumption of starch (kg)/65%
(2) standard liquor output: the wine degree of liquor is different, for the output of unified examination liquor, and all liquor that is below or above 65 degree, conversion is the output of 65 degree liquor without exception, is called standard liquor output.Its account form is produced the formula of the total consumption of starch with reference to liquor.
(3) standard raw grain the yield of liquor:
Standard raw grain the yield of liquor (%)=standard liquor output/standard raw grain consumption
Husk is main in the fermenting process of wine, and what rise is to support fluffing action, after therefore can the rice husk that reclaim and fresh rice husk being mixed in the ratio of 1:1, again adds in the fermenting process of wine.The yield of liquor and local flavor by the wine that produces with the fresh rice husk zythepsary of normal employing compare, and checking is added and reclaimed the impact of rice husk on making wine.Relatively see Table 3-1 to reclaiming the data that rice husk is made wine and original production is made wine, can find affects also not quite its yield of liquor after rice husk is reclaimed in interpolation, basically can ignore.It is very little that local flavor is judged gap, can say that the application of reclaiming rice husk is fully efficient feasible.
Table 3-1 reclaims the result that rice husk is made wine
| Project | 50% reclaims the rice husk wine brewing | Brand-new bright rice husk wine brewing |
| Standard the yield of liquor (%) | 40.9 | 41.2 |
| Local flavor is judged | Transparent (little Huang), oolong drink with clear aroma, tail is clean, sesame is aromatic strongly fragrant | Transparent (little Huang), mellow, tail are clean, the lingering fragrance sesame is aromatic strongly fragrant |
After comparing qualitative and interior scalar quantity with the self-built template of Yanghe River brewery technique center GC Room, the typical flavor composition in the wine is listed, seen Table in detail 3-2.By computer graphics relatively, see Fig. 2, can find very clearly that other compositions all approach or are more or less the same except indivedual composition difference are large, this has illustrated that also the use of rice husk in wine brewing of recycling is feasible.
Two kinds of wine typical flavor of table 3-2 component content relatively
Embodiment 3
The method that rice husk is produced wheat bran is reclaimed in the present embodiment explanation.
Wheat bran: rice husk=95:5 (mass ratio) carries out wheat bran production, production method is: need altogether 3 kinds of bacterium in the wheat bran, be respectively the white song in Ha Noi, subtilis bacterium, produce fat yeast (all available from ATCC), respectively it is carried out mixing by a certain percentage use after single spawn culture is made wheat bran at last.A. Ha Noi is bent in vain: the ratio of selected combination substratum: water=1:1 adds water, stirs, and in 121 ℃ of autoclaving 1h, is cooled to 35 ℃, plant song according to 2% access, mixing shakeouts, and keeps bent room to ventilate, humidity is 95 %-100 %, and 35 ℃ of culture temperature are about incubation time 72 h.B. bacterium wheat bran: the characteristic chicken flavor that can produce typical distilled spirit with sesame flavour through fermentation culture.Ratio according to selected combination substratum: water=1:1 adds water, and 121 ℃ of autoclavings are cooled to 37 ℃, and seed liquor is according to 4% access, and mixing shakeouts.Keep 34-37 ℃ of temperature, humidity 85%, control product temperature is no more than 55 ℃, and incubation time generally gets final product at 36-48h.C. yeast wheat bran: ester-producing yeast; The ratio of selected combination substratum: water=1:1 adds water, and 121 ℃ of autoclavings are cooled to 30 ℃, and seed liquor is according to 4% access, and mixing shakeouts, maintain the temperature at about 30 ℃, and humidity 85%, control product temperature must not surpass 40 ℃, and incubation time is generally about 48h.
Wherein the measuring method of various parameters is as follows.
1, diastasimetry:
The unit of activity of saccharifying enzyme is defined as the 1g absolute dried sample, and at 35 ℃, 1h is decomposed into Zulkovsky starch the mg of glucose under the pH4.6 condition, represents with μ/g.
(1) preparation of sample leach liquor
Take by weighing the absolute dried sample that is equivalent to 10g (according to measuring moisture, calculate), place the 250mL beaker, add again water (90-5 * moisture %) mL, acetic acid-sodium-acetate buffer of the pH4.6 of 10mL stirs once in 30 ℃ of every 15min of water-bath lixiviate 1h(), with dried filter paper filtering, discard initial 5mL, filtrate is for examination enzyme liquid.
(2) saccharogenic power test fluid preparation
The saccharification test solution of A song leach liquor: accurately draw in the volumetric flask of 2% Zulkovsky starch solution 50mL and 100mL, after in 35 ℃ of water-baths, being incubated 20min, accurately add enzyme leach liquor 10mL, shake up and begin timing, add immediately the sodium hydroxide of the 1mol/L of 3mL in 35 ℃ of water-baths behind the insulation 1h, shake up and make its stopped reaction.Be settled to scale with distilled water after the cooling.
The blank sample of B: and the saccharification test solution just adds first the sodium hydroxide of the 1mol/L of 3mL, enzyme-added leach liquor 10mL again, and other steps are identical.
(3) sugar is measured
The A saccharified liquid is measured: accurately draw 5mL saccharification reagent in the triangular flask of the 150mL that is added with each 5mL of fehling reagent first, second liquid, add an amount of 0.1% standard glucose solution, shake up, with heating by electric cooker make its boiling after, be titrated to blue the disappearance with 0.1% standard sugar liquid at once, this mensuration needs to finish in 1min.
The B blank solution is measured: substitute saccharified liquid with the 5mL blank solution, other steps are the same.
(4) calculate
Saccharifying enzymic activity=(V0-V) * ρ * 1000/(5 * (10/100))/(5/100)
In the formula: the blank sample of V0-5mL consumes 0.1% standard sugar liquid long-pending (mL);
V-5mL saccharified liquid consumes 0.1% standard sugar liquid long-pending (mL);
ρ-standard glucose concentration (g/mL);
Get 10mL at 100mL after 5 * (10/100)-5g absolute dried sample leaches and carry out mashing test;
5/100-get the fixed sugar of 5mL at 100mL;
1000-be converted into mg.
2, liquefaction power is measured:
The unit of activity of liquefying amylase is defined as the 1g absolute dried sample, and at 60 ℃, 1h liquefaction 1g Zulkovsky starch is called 1 enzyme unit alive under the pH6.0 condition, represents with μ/g.
(1) preparation of sample leach liquor
Take by weighing the absolute dried sample that is equivalent to 10g (according to measuring moisture, calculate), place the 500mL beaker, add again 200mL pH6.0 Sodium phosphate dibasic-citrate buffer solution, stir once in 40 ℃ of every 15min of water-bath lixiviate 1h(), filter with absorbent cotton, discard initial 5mL, filtrate is for examination enzyme liquid.
(2) measure
Draw 20mL 2% Zulkovsky starch solution and 5mL pH6.0 Sodium phosphate dibasic-citric acid solution, insert in 25 * 200mm test tube preheating 10min in 60 ℃ of water-baths.Accurately add 5mL dilution enzyme liquid; Clock immediately, fully shake up, regularly take out approximately 0.5mL reaction solution with dropper, splash in the white plaque hole that fills in advance rare iodine liquid (approximately 1.5mL), color reaction gradually becomes reddish-brown by bluish voilet; Until till identical with the standard colorimetric solution colour, be reaction end, write down the reaction times.
(3) calculate
Liquefying amylase vigor=20 * 2% * 60/10/V/t.
In the formula: 20-2% Zulkovsky starch uptake (mL);
2%-Zulkovsky starch concentration (g/mL);
60—1h；
10/V-1mL sample leach liquor contains song g number;
T-enzyme digestion reaction time (min).
3, acidic protein enzymatic determination
Acid protease activity is defined as: the 1g absolute dried sample is under 40 ℃ and pH 3 conditions, and 1min produces amino acid whose μ g number with casein hydrolysis, represents with μ/g.
(1) enzyme leach liquor preparation
Take by weighing the sample (according to measuring moisture, calculating) of 10g absolute dried sample, it is 200mL that adding pH 3 lactic acid-Sodium.alpha.-hydroxypropionate damping fluid makes cumulative volume, and 30min is leached in water-bath in 40 ℃, then uses filter paper filtering.Reserved filtrate is stand-by.
(2) enzyme liquid colour developing
A sample determination: draw enzyme leach liquor 1mL, join in the 20mL test tube preheating 5min in 40 ℃ of water-baths, accurately add 2% casein solution 1mL, timing insulation 10min adds the 2mL0.4mol/L trichoroacetic acid(TCA) immediately, make unnecessary protein precipitation, stopped reaction.Use filter paper filtering.Draw 1mL filtrate and add in the test tube, add again 5mL 0.4mol/L sodium carbonate solution and 1.00mL Folin reagent, mixing, heating 20min colour developing in 40 ℃ of water-baths.
B blank test: carry out simultaneously with sample, in test tube, behind the adding 1mL enzyme reagent, add first the 0.4mol/L trichoroacetic acid(TCA) of 2mL, add again 2% casein solution 1mL.Other are the same.
(3) drafting of typical curve and sample determination
The A mark is bent to be drawn: preparation tyrosine concentration increases progressively from the standard amino acid solution of 0-80 μ g/mL with 10 μ g/mL, then drawing respectively each concentration solution 1mL is added in 9 test tubes, the yellow soda ash and the 1mL Folin reagent that add again 5mL0.4mol/L, 40 ℃ of water-bath 20min color reactions, under the 680nm wavelength, survey its optical density(OD), take the standard amino acid solution of 0 μ g/mL as contrast, draw the zeroaxial calibration curve of optical density(OD).The optical density(OD) of looking at curve is 1 o'clock tyrosine concentration, is the extinction constant K.
B sample determination: take check sample as contrast, under the 680nm wavelength, survey its optical density(OD).
(4) calculate
Proteinase activity=K * A/m/ (1/200 * 1/4)/10.
In the formula: K-optical density(OD) is 1 o'clock tyrosine μ g number;
E-sample mean optical density(OD);
M-sample quality (g);
1/200 * 1/4-sample extension rate;
10-reaction times.
4, esterification power is measured
(1) esterifying liquid preparation
Get 100mL1% caproic acid ethanolic soln in the matrass of 250mL, add 5 absolute dried samples (according to measuring moisture, calculating), at 30-32 ℃ of lower esterification 100h.Then adding distil water 50mL adds the effluent liquid that 100mL is accepted in thermal distillation.
(2) ethyl hexanoate assay
Draw 50mL distillate fluid, with the 0.1mol/L sodium hydroxide phenolphthalein terminal point that neutralizes.Accurately add again 25mL 0.1mol/L sodium hydroxide, backflow saponification 30min in the boiling water bath.Sulphuric acid soln with 0.05 mol/L after the cooling is titrated to the disappearance of phenolphthalein pink colour.
(3) calculate
Esterification power (mg/g)=(C1V1-C2V2)/(m * 50/100) * 144.
In the formula: C1, C2-the be respectively concentration (mol/L) of sodium hydroxide and sulfuric acid;
V1, V2-the be respectively volume (mL) of sodium hydroxide and sulfuric acid standardized solution;
M-sample quality;
50/100-from distillate 100mL, get 50mL to measure;
The reduction factor of 144-ethyl hexanoate.
5, fermenting power is measured
The fermenting power definition is that 1g or 1mL sample are being cultivated the CO that produces with pol under 25 ℃ in the matrix of 12-13 degree
2Quality.
(1) saccharified liquid preparation
Fructus Hordei Germinatus is pulverized, added the saccharification under 60 ℃ of water-baths of water mixing, reach 13 degree with the saccharometer measurement and namely can be used as the fermented liquid use.
(2) sterilization
Get the 150mL saccharified liquid in the fermentation flask of 250mL, tampon is wrapped oilpaper beyond the Great Wall, and 15min sterilizes under 98kPa.
(3) fermentation, mensuration
After the sterilization cooling, under aseptic condition, add sample 1g, weigh, connect fermentation bung, in fermentation bung, add the sulfuric acid of 10mL 5mol/L, use simultaneously paraffin sealing.25 ℃ of cultivations, the 48h that ferments in the case takes out fermentation flask and removes fermentation bung, rocks carbonic acid gas is all overflowed, and then weighs.
Fermenting power (in the titanium dioxide Quality Fraction of Carbonium, g/100g)=(M1-M2)/M * 100
In the formula: M1, M2-be respectively fermentation front and back fermentation flask to weigh (g);
M-sample quality (g) or volume (mL).
6, seed culture
Needing altogether 3 kinds of bacterium in the wheat bran, is respectively the white song in Ha Noi, subtilis bacterium, ester-producing yeast, respectively it is carried out mixing by a certain percentage use after single spawn culture is made wheat bran at last.
The culturing process in Ha Noi white bent (available from ATCC) is that the large triangular flask solid culture of the little triangular flask solid culture-5L of test tube slant cultivation-500mL-bent room is cultivated.
Subtilis (available from ATCC) culturing process is that the little triangular flask liquid culture of test tube slant cultivation-500mL-bent room is cultivated.
Producing fat yeast (available from ATCC) culturing process is that the little triangular flask liquid culture of test tube slant cultivation-500mL-bent room is cultivated.
(1) seed culture in the white bent triangular flask in Ha Noi
Wheat bran, rice husk, vinasse that table 4-1 different ratios mixes
| Grouping | Wheat bran | Rice husk | Vinasse (doing) |
| 1 | 100 | 0 | —— |
| 2 | 95 | 5 | —— |
| 3 | 90 | 10 | —— |
| 4 | 85 | 15 | —— |
| 5 | 95 | —— | 5 |
| 6 | 90 | —— | 10 |
| 7 | 85 | —— | 15 |
| 8 | 80 | —— | 20 |
| 9 | 75 | —— | 25 |
The 1st step accessed to the white song in Ha Noi according to the different culture media of table among the 4-1: water is in the triangular flask of 500mL of 1:0.8, is placed to the inclined-plane after the sterilization in 35 ℃ constant incubator, and intermediate demand button bottle is cultivated about 72h.Observe its upgrowth situation, measure simultaneously the indexs such as its saccharogenic power, liquefaction power and compare.
The 2nd goes on foot according to the different culture media among the table 2-1: water is that the ratio of 1:0.8 adds water, is added to behind the mixing in the large triangular flask of 5L.121 ℃ of autoclavings are cooled to 35 ℃, and Ha Noi is bent in vain in the access bottle, and mixing shakeouts.Keep about 35 ℃ of temperature, be placed to the inclined-plane, intermediate demand button bottle, incubation time generally gets final product at 72h.Observe its upgrowth situation, measure simultaneously its saccharogenic power, the indexs such as liquefaction power compare.
(2) yeast wheat bran triangular flask seed culture
Liquid nutrient medium is selected malt juice liquid medium, adds approximately the substratum of 250mL and gone out and cultivate 24-48h behind the bacterium in 30 ℃ of constant-temperature tables in the triangular flask of 500mL.
(3) bacterium wheat bran triangular flask seed culture
Liquid nutrient medium is selected the beef extract-peptone liquid nutrient medium, adds approximately 250mL substratum in the triangular flask of 500mL, cultivates 24-48h behind the bacterium of having gone out in 37 ℃ of constant-temperature tables.
(4) bent room expanding production technical process
Bacterium wheat bran: the characteristic chicken flavor that can produce typical distilled spirit with sesame flavour through fermentation culture.Ratio according to selected combination substratum: water=1:1 adds water, and 121 ℃ of autoclavings are cooled to 37 ℃, and seed liquor is according to 4% access, and mixing shakeouts.Keep 34-37 ℃ of temperature, humidity 85%, control product temperature is no more than 55 ℃, and incubation time generally gets final product at 36-48h.
Yeast wheat bran: ester-producing yeast; The ratio of selected combination substratum: water=1:1 adds water, and 121 ℃ of autoclavings are cooled to 30 ℃, and seed liquor is according to 4% access, and mixing shakeouts, maintain the temperature at about 30 ℃, and humidity 85%, control product temperature must not surpass 40 ℃, and incubation time is generally about 48h.
Ha Noi is bent in vain: the ratio of selected combination substratum: water=1:1 adds water, stirs, and in 121 ℃ of autoclaving 1h, is cooled to 35 ℃, plant song according to 2% access, mixing shakeouts, and keeps bent room to ventilate, humidity is 95 %-100 %, and 35 ℃ of culture temperature are about incubation time 72 h.
Respectively the biochemical property of 3 kinds of wheat brans detected.
(5) enter the cellar for storing things and produce checking
To above-mentioned 3 kinds of wheat brans bent 45kg of bacterium in proportion, yeast distiller 30 kg, white bent 150 kg in Ha Noi, bent 75 kg of high temperature add in the cellar for storing things and ferment, and go out the cellar for storing things after 35 days and steam wine.Measure its yield of liquor and wine taste is measured comparison.
The analysis that the wheat bran the yield of liquor that makes and local flavor are judged relatively.
The result that table 4-2 self-control wheat bran is made wine
| Project | The wine brewing of self-control wheat bran | The sesame-flavor Daqu wine brewing of buying |
| Standard the yield of liquor (%) | 40.0 | 43.1 |
| Local flavor is judged | Transparent (little Huang), oolong drink with clear aroma, sesame are aromatic strongly fragrant | Transparent (little Huang), mellow, tail remainder are fragrant, sesame is aromatic strongly fragrant |
The wine brewing of contrast self-control wheat bran relatively sees Table 4-2 with the yield of liquor of the sesame-flavor Daqu wine brewing of buying, and can find: the yield of liquor of comparing wine from koji with the sesame-flavor Daqu of purchase is slightly low, but differs and not quite; Gap is comparatively obvious on the local flavor, does not have the outsourcing song mellow, and tail is clean.
Claims (5)
1. the recycling method of vinasse is characterized in that may further comprise the steps:
(1) vinasse is washed with water, make the vinasse suspension that becomes rice husk, wash-out throw out suspendible after the vinasse immersions;
(2) the rear filtration of sieving of vinasse suspension obtains complete rice husk; After the ratio of 1:1 mixes the rice husk that reclaims and fresh rice husk in mass ratio, again add in the fermenting process of liquor and produce liquor; Perhaps carry out wheat bran production according to quality than wheat bran: rice husk=95:5;
(3) sieve and filter the centrifugal or sedimentation of the filtrate obtain, the throw out that obtains prepares animal-feed;
(4) sieve and filter the centrifugal or sedimentation of the filtrate obtain, the bath water as step (1) vinasse is reclaimed in the supernatant liquor that obtains circulation.
2. the recycling method of vinasse according to claim 1 is characterized in that the method that the vinasse of described step (1) wash with water is the stirring and washing method.
3. the recycling method of vinasse according to claim 2, it is characterized in that described stirring and washing method is: solid-liquid ratio is mass ratio 1:2, and soak time is 30min, and washing times is 6 times.
4. the recycling method of vinasse according to claim 1, the vinasse suspension that it is characterized in that described step (2) sieves and filters the method that obtains complete rice husk and be: the aperture of sieving is 1mm, centrifugal rotational speed is 3000r/min, and centrifugation time is 15min.
5. the recycling method of vinasse according to claim 1 is characterized in that the production method of the wheat bran of described step (2) is: respectively the white song in Ha Noi, subtilis, ester-producing yeast are carried out being mixed in proportion use after single spawn culture is made wheat bran at last; A. Ha Noi is bent in vain: the ratio of selected combination substratum: water=1:1 adds water, stirs, and in 121 ℃ of autoclaving 1h, is cooled to 35 ℃, plant song according to 2% access, mixing shakeouts, and keeps bent room to ventilate, humidity is 95 %-100 %, 35 ℃ of culture temperature, incubation time 72 h; B. subtilis: the characteristic chicken flavor that can produce typical distilled spirit with sesame flavour through fermentation culture, ratio according to selected combination substratum: water=1:1 adds water, 121 ℃ of autoclavings are cooled to 37 ℃, seed liquor is according to 4% access, mixing shakeouts, and keeps 34-37 ℃ of temperature, humidity 85%, control product temperature is no more than 55 ℃, incubation time 36-48h; C. ester-producing yeast: the ratio of selected combination substratum: water=1:1 adds water, and 121 ℃ of autoclavings are cooled to 30 ℃, and seed liquor is according to 4% access, and mixing shakeouts, maintain the temperature at about 30 ℃, and humidity 85%, control product temperature must not surpass 40 ℃, incubation time 48h.
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