CN101407829B - Method for preparing ethanol from molasses - Google Patents
Method for preparing ethanol from molasses Download PDFInfo
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- CN101407829B CN101407829B CN2008101457748A CN200810145774A CN101407829B CN 101407829 B CN101407829 B CN 101407829B CN 2008101457748 A CN2008101457748 A CN 2008101457748A CN 200810145774 A CN200810145774 A CN 200810145774A CN 101407829 B CN101407829 B CN 101407829B
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Abstract
The invention discloses a method for preparing ethanol by gooey; wherein, the method includes the following steps of: mixing a gooey water liquid and water vapor, cooling the obtained mixture to the fermentation temperature and carrying out fermentation; wherein, the temperature for mixing the gooey water liquid and the water vapor is between 105 DEG C and 115 DEG C, the pressure thereof is between 0.2 MPa and 0.5 MPa and the mixing time is between 10 minutes and 50 minutes. The yield rate of the ethanol prepared by the method is higher; besides, the method avoids the using of sulphuric acid and no acid ions enter the waste distilled water of the alcohol, thus extensively reducing the processing difficulty of the waste water after the separation of the ethanol.
Description
Technical field
The invention relates to the alcoholic acid preparation method, more specifically about adopting molasses to prepare the alcoholic acid method.
Background technology
Molasses claim syrup again, be sugarcane or beet in sugar industry, with the syrup liquid that squeezes out, through heating, neutralization, precipitation, filter, concentrate, the remaining dense thick sugar liquors that contains after the operation sugaring such as crystallization.China's year molasses stock number is about 2,500,000 tons, and the South and the North all has distribution.The main component of molasses is a carbohydrate, and cane molasses contains the about 24-36 weight of sucrose %, the about 12-24 weight % of other sugar; The contained carbohydrate of beet sirup almost is sucrose entirely, about 47 weight %.In addition, also contain the solubility colloid of 3-4 weight % in the nitrogen-free extract, be mainly xylan, araban and pectin etc.
Molasses are mainly used in production ethanol, adopt the ethanol yield that is obtained by molasses fermented preparation alcoholic acid method of prior art lower, generally are no more than 49%.
Summary of the invention
The objective of the invention is to overcome existing employing molasses and prepare the lower defective of alcohol yied that the alcoholic acid method obtains, provide the higher employing molasses of a kind of alcohol yied to prepare the alcoholic acid method.
The present inventor finds, molasses are microbiological contamination very easily, therefore, in order to suppress the breeding of acid formers in the molasses fermented preparation alcoholic acid process, guarantee the continuity of fermentation, the employing molasses raw material of prior art prepares in the alcoholic acid method, before fermentation, need carry out acidifying, sterilization to molasses solution, promptly, adding the pH value that a large amount of sulfuric acid is adjusted molasses in molasses solution, is 3.5-5.0 as the pH value, could guarantee that molasses are not easy microbiological contamination under this pH value, but, under the condition of low pH value, the fermentative activity of yeast saccharomyces cerevisiae can be suppressed, and causes alcohol yied to reduce.In addition, in ethanol separation waste liquid, contain a large amount of sulfate ions, thereby in the wastewater treatment process, sulfate ion makes the organism in the waste water be difficult to thorough degraded to substrate competition and the toxic action of methanogen, cause the COD value in the waste water higher, be difficult to accomplish qualified discharge.
The invention provides a kind of employing molasses and prepare the alcoholic acid method, wherein, this method comprises mixes molasses water solution and water vapor, the mixture that obtains is cooled to leavening temperature to ferment, wherein, with molasses water solution and water vapor blended temperature is 105-115 ℃, and pressure is the 0.2-0.5 MPa, and the blended time is 10-50 minute.
In the method for the invention, molasses water solution is being carried out in the blended process with water vapor, assorted bacterium in the molasses is removed, and need not to realize by the method that adds sulfuric acid acidation, adjusting molasses pH value, therefore, according to method of the present invention, in follow-up fermenting process, can guarantee under the optimal pH condition of yeast, to carry out, thereby guarantee ethanol yield.
Unlike the prior art be, employing molasses of the present invention prepare in the alcoholic acid method, need in molasses, not add sulfuric acid adjustment pH value and suppress the molasses microbiological contamination, molasses water solution and water vapor be mixed, utilize the shearing force when mixing that water vapor is sterilized to molasses water solution and adopt.Method of the present invention has been avoided the vitriolic use, therefore, in follow-up fermenting process, can ferment under higher pH, has higher vigor to guarantee yeast, thereby has improved ethanol yield.
In addition,, do not have entering of sulfate ion in the waste water behind follow-up ethanol distillation, alleviated the intractability of waste water after ethanol separates significantly because method of the present invention has avoided using sulfuric acid before fermenting process.According to the present invention, under the preferable case, the sterilization after, the fermentation before, molasses water solution is carried out the secondary steam that flash distillation produced can also secondary steam can be utilized again as the isolating thermal source of ethanol, greatly reduce energy consumption.
Description of drawings
Fig. 1 prepares the alcoholic acid process flow diagram for employing molasses of the present invention.
Embodiment
Prepare the alcoholic acid method according to employing molasses provided by the invention, this method comprises mixes molasses water solution and water vapor, the mixture that obtains is cooled to leavening temperature ferments, wherein, with molasses water solution and water vapor blended temperature is 105-115 ℃, is preferably 108-112 ℃; Pressure is the 0.2-0.5 MPa, is preferably the 0.3-0.4 MPa; The blended time is 10-50 minute, is preferably 10-20 minute.
According to method of the present invention, the mixture of molasses water solution and water vapor is under certain pressure, temperature, shearing force when utilizing water vapor and molasses aqueous solution makes molasses water solution and water vapor uniform mixing for some time, to reach the effect that molasses water solution is sterilized.
According to method of the present invention, the adjustable extent broad of described molasses water solution and the feed weight ratio of water vapor is under the preferable case, in order to take into account good sterilising effect and than less energy-consumption, described molasses water solution is 100:2-6, more preferably 100:3-5 with the feed weight ratio of water vapor.
According to method of the present invention, the mixing of described molasses water solution and water vapor can be carried out in reactor, the mixing of described molasses water solution and water vapor can mix by intermittent mode, also can mix continuously, under the preferable case, molasses water solution and water vapor are added reactor continuously, and mixture is shifted out continuously, the blended time is the residence time of mixture in reactor.
Molasses claim syrup again, be sugarcane or beet in sugar industry, with the syrup liquid that squeezes out, through heating, neutralization, precipitation, filter, concentrate, the remaining dense thick sugar liquors that contains after the operation sugaring such as crystallization.For fear of microbiological contamination, molasses normally pass through the higher state of spissated viscosity in storage process, therefore before alcohol prepared by fermenting, need dilute molasses, and are general, adopt molasses water solution to carry out alcohol prepared by fermenting.Under the preferable case, the concentration of molasses water solution of the present invention is 25-35 weight %, is preferably 25-30 weight %.The method that obtains the molasses water solution of above-mentioned concentration can be for well known to a person skilled in the art the whole bag of tricks, and as directly molasses and water being mixed in reactor, obtaining concentration is 25-35 weight %, is preferably the molasses water solution of 25-30 weight %.For the conserve water resource, the present invention preferably adopts distillation tower still water as dilution molasses water.
The main component of molasses comprises sugar, crude protein, crude fat, robust fibre, coarse ash, phosphorus and water.According to the present invention, the content of molasses is generally represented with sugar hammer degree in the molasses water solution.Described sugar hammer degree is defined as: the percentage composition of the soluble solids in the molasses solution, the soluble solids in the described molasses solution comprise the impurity of sugar and a small amount of solubility, are abbreviated as a ° Bx, and the percentage composition of soluble solids is 1% in the molasses solution, is 1 ° of Bx.The measuring method of described sugar hammer degree can adopt conventional various measuring methods, for example, obtains by measuring refractive index, and the measuring method of described sugar hammer degree is the detection method that sugar industry is generally used.
According to the present invention, the measuring method of described sugar hammer degree can adopt and well known to a person skilled in the art the whole bag of tricks, measures the sugar hammer degree of molasses water solution as adopting brix spindle.
Concrete measuring method comprises: get a suitable volumetrical graduated cylinder, earlier with a small amount of liquid glucose flushing dose tube inwall, wash complete discarding.Fill with liquid glucose then, leave standstill, treat the effusion of sample liquid inner air, behind the floating upward liquid level of foam, foam is removed.With liquid glucose flushing exsiccant concentration meter, insert in the graduated cylinder (, then inserting thermometer separately) then slowly as concentration meter enclosure temperature meter not, when thermometer is correctly represented the temperature of sample, with the real liquid level reading of horizontal line of sight by syrup, write down observation hammer degree, and record temperature reading at that time.Table look-up numerical value when being corrected into 20 ℃.
When using brix spindle, as the liquid glucose temperature is not that 20 ℃ of (standard temperature) measured numerical value are just incorrect, under higher temperature, that is to say that the gained numeric ratio should have reading low when surpassing 20 ℃, otherwise, the gained read-around ratio should have reading height (because not having the thermal expansion reason) when being lower than 20 ℃, so the temperature height is all had a temperature correction number, can all can find on the foodstuffs industry handbook about the temperature correction number.
That is, T〉20 ℃, with recording number+correction;
T＜20 ℃ are with recording number-correction.
The main component of molasses is a sugar, and wherein, the content of sucrose (disaccharides) is higher, and the measuring method of total sugar content can adopt the method that well known to a person skilled in the art to measure in the molasses, as adopts following acid-hydrolysis method:
Take by weighing a certain amount of molasses sample in 250 milliliters of clean triangular flasks, add 20 milliliters of 20 weight %HCl solution, add a certain amount of water (principle of amount of water is to guarantee that the cumulative volume of the solution of participation hydrolysis is 100 milliliters), put in the boiling water bath hydrolysis 30-35 minute, take out Quench then, change in the volumetric flask again, wash triangular flask with less water, wash water is also gone in the volumetric flask, thin up (is diluted to reducing sugar content and is lower than 0.2%, extension rate is determined according to different samples, can directly be measured the sample that reducing sugar content is lower) shake up standby.
Fei Linshi liquid is demarcated:
Fei Linshi first liquid: take by weighing cupric sulfate crystals (CuSO
45H
2O) 35 grams, blue 0.05 gram of methyne, with 1000 milliliters of less water dissolving back constant volumes, standby.
Fei Linshi second liquid: take by weighing Rochelle salt 117 grams, sodium hydroxide 126.4 grams, three water yellow prussiate of potash, 9.4 grams, with 1000 milliliters of less water dissolving back constant volumes, standby.
0.1% glucose standardized solution: smart dextrose anhydrous 1.0000 grams that claim 100-105 ℃ of oven dry, use water dissolution, add 5 milliliters of concentrated hydrochloric acids (massfraction 36.5%), be settled to 1000 milliliters, mixing is standby.
Draw each 5 milliliters of Fei Linshi first, second liquid, place 150 milliliters of triangular flasks, add 10 milliliters of 0.1% glucose reference liquids, after discharge is heated on the stove and boiled 2 minutes, dropwise splash into 0.1% Glucose Liquid (solution must keep boiling) to solution again and become pink, change 2-3 second one speed into and drip to light yellow for terminal point, it is " A0 " that institute consumes the glucose volume.Other gets Fei Linshi first, second liquid and puts in the triangular flask for each 5 milliliters, add 0.1% glucose (A0-0.7) milliliter, heating on the discharge stove (boiling in 1.0-1.5 minute), seethe with excitement after 2 minutes, the speed of dripping second with every 2-3 drip to the yellow that shoals be terminal point (this amount should between the 0.5-1.0 milliliter), so repeat 2-3 time, get its several arithmetical av and be designated as " A " milliliter, be the calibration value of Fei Linshi liquid near value.
Sample is measured:
Different is with demarcating Fei Linshi liquid, 10 milliliter of 0.1% Glucose Liquid that replaces beginning to add in advance with the rare reduction liquid glucose of V milliliter (being generally 10 milliliters), terminal point is yellow, other is identical, if rare sugar concentration too high (surpass 0.2%) can change and adds 5 milliliters of rare sugar solns and 5 ml waters for it.During calculation result, should multiply by 2 on former formula basis, 0.1% the reducing sugar milliliter number that record consumes is B.
The result calculates:
Total reducing sugar: (% or gram/100 milliliter)=extension rate of 0.1% * solution [(A-B) *]/(V * G)
In the formula: the A representative consumes the milliliter number of 0.1% glucose when demarcating Fehling liquid;
B consumes the milliliter number of 0.1% reducing sugar when representing the titration sample;
The milliliter number that adds rare reduction liquid glucose when V represents titration;
The G representative takes by weighing sample size, gram or milliliter.
Because the present invention only relates to the improvement of molasses water solution sterilization mode, therefore other step that adopts molasses to prepare the alcoholic acid method is had no particular limits.
Can make sucrose inversion is that the microorganism of pentose and/or hexose and ferment pentoses and/or hexose may be used to fermenting process of the present invention, and yeast saccharomyces cerevisiae is the microorganism of the zymohexose that ethanol-tolerant, by product are few, alcohol yied is high of widespread usage on the wine industry.In every gram molasses, the employed zymic inoculum size of described fermentation is 10
3-10
8Colony-forming unit, more preferably 10
4-10
6Colony-forming unit.Employed yeast is fermented in the present invention can be for being purchased yeast solids preparation (such as dried yeast powder) or barms (such as the cereuisiae fermentum of ATCC numbering 2601).Described zymic colony-forming unit can be measured by means commonly known in the art, such as the methylene blue staining viable bacteria counting method.The concrete grammar of methylene blue staining viable bacteria counting method is as follows:
1 gram dried yeast powder is dissolved in 10 ml sterile waters, or 1 milliliter of actication of culture liquid is diluted to 10 milliliters with sterilized water, add 0.5 milliliter of 0.1 weight % methylene blue, be incubated 30 minutes down at 35 ℃.Under 10 times of opticmicroscopes,, can get the number of viable bacteria in 1 gram dry yeast or the 1 milliliter of actication of culture liquid, i.e. colony forming single-digit with the number (dead bacterium dyeing, viable bacteria is not dyeed) of viable bacteria in the solution after the blood counting chamber counting insulation.
Described yeast can adopt conventional method inoculation, for example adds the seed liquor of 5-15 volume % in enzymolysis product.Described seed liquor can be the aqueous solution or the culture medium solution of dry yeast, also can or be purchased the activated seed liquid of bacterial classification for dry yeast.The temperature of described fermentation can be any temperature that is suitable for yeast growth, is preferably 30-36 ℃, more preferably 32-35 ℃.The time of described fermentation can be for beginning from inoculation to occur to the decline phase of yeast growth the time of (being that fermentation time is that lag phase, logarithmic phase add stationary phase), and the time of preferred fermentation is 32-48 hour, more preferably 32-40 hour.Fermentation pH value is 5.5-6.Tunning ethanol can be with conventional method, according to requirement (requiring alcoholic acid purity to reach more than 99% such as the fuel alcohol) separation and refining of different Industrial products, such as distilling, concentrate, dewatering.
Under the preferable case, described fermenting process can also comprise the adding additive, think that yeast provides nutrient, the kind of described additive and consumption are conventionally known to one of skill in the art, for example, described additive can be ammoniacal liquor and/or urea, in every gram molasses, the consumption of additive is the 0.0001-0.0005 gram, is preferably the 0.0001-0.0003 gram.
For save energy, reduce energy consumption, method of the present invention can also be included in and molasses solution is cooled to before the leavening temperature step of molasses solution being carried out flash distillation.Flash distillation is meant thermo-coagulating water under certain pressure or feedwater by step-down, the portion water double evaporation-cooling.
It is the 0.01-0.02 MPa that the method for flash distillation of the present invention can be included in vacuum tightness, be preferably the 0.01-0.015 MPa, temperature is under 50-60 ℃, perhaps be 90-95 ℃ and kept 10-30 minute down, obtain secondary steam in normal pressure (being often referred to a normal atmosphere, i.e. 0.1 MPa), temperature.Vacuum tightness of the present invention refers to the absolute value of the difference of absolute pressure (true pressure) and barometric point.
According to a concrete embodiment of the present invention, being blended in the reactor of described molasses water solution and water vapor carried out, molasses water solution and water vapor are added reactor continuously, and mixture is shifted out continuously, the blended time is the residence time of mixture in reactor.As shown in Figure 1, molasses and water feed in the mixing tanks 1 by the pipeline 7 of conveying molasses and the pipeline 8 of fluming water respectively, stir, mix, obtaining concentration is 25-35 weight %, be preferably the molasses water solution of 25-30 weight %, then this molasses water solution is entered in the reactor by the pipeline 10 of first feeding pump 9 through carrying molasses water solution, simultaneously, water vapor feeds in the reactor by the pipeline 11 of fluming water steam, molasses water solution and water vapor are mixed in reactor, described reactor comprises mixing tank 2 and keeps pipe 3, the mixture of molasses water solution and water vapor is the 0.2-0.5 MPa at pressure in mixing tank 2 earlier, temperature is 105-110 ℃ and mixes 1-30 second down, be preferably 3-10 second, this mixture is moved to from mixing tank 2 and keeps in the pipe 3 then, continuation is mixed into further sterilization of row under above-mentioned mixing condition, the length of keeping pipe 3 guarantees that the residence time of mixture in keeping pipe 3 is 10-49 minute, is preferably 10-20 minute.This mixture is pumped in the gas-liquid separator 4 thereupon then, under flash conditions, carry out flash distillation, the vacuum pump of the secondary steam that obtains by gas-liquid separator 4 upper ends pumps and enters the ethanol distillation separating unit, molasses water solution after the sterilization is pumped to decrease temperature and pressure in the remaining tank 5, simultaneously additive is added in the remaining tanks 5 and described molasses aqueous solution 45 minutes-1 hour by additive delivery pipeline 12, then the said mixture material is pumped into through second feeding pump 13 and pump in the fermentor tank 6 by material conveying pipe 15 after being cooled to leavening temperature in the interchanger 14, adding yeast by yeast transport pipe 16 in fermentor tank 10 simultaneously ferments, in every gram molasses, the employed zymic inoculum size of described fermentation is 10
3-10
8Colony-forming unit; The condition of fermentation comprises that temperature is 30-36 ℃, and fermentation pH value is 5.5-6, and fermentation time is 32-48 hour; After the fermentation ends fermenting-ripening liquid pumped to the ethanol distillation separating unit by the 3rd feeding pump 17 and carry out ethanol distillation.
The present invention will be described in more detail below in conjunction with embodiment.
Embodiment 1
Present embodiment is used to illustrate that employing molasses of the present invention prepare the alcoholic acid method.
(1) dilution of molasses
With 1000 kilograms of molasses concentrated solutions, sugar hammer degree is that 70 ° of Bx (adopt Abbe refractometer to measure, Shanghai is triumphant comes experimental installation company limited to produce, measuring temperature is 20 ℃) (record according to the above-mentioned acid-hydrolysis method of the present invention total sugar content is 66 weight % in the molasses concentrated solution), the pH value is 6.0, mix in thinning tank with the waste water 1200 kilograms (pH5.0) of discharging at the bottom of the alcohol distillation tower, obtain molasses water solution.
(2) sterilization
The molasses water solution and the water vapor (weight ratio of molasses water solution and water vapor is 100:3) of step (1) are pumped into water heater (the long chemical industry equipment in sky, Nantong company limited respectively simultaneously, model PS-III) mixes in, the mixture of molasses water solution and water vapor is 108 ℃ in temperature, pressure is to mix 5 seconds in water heater under 0.4 MPa, then this mixture is shifted out from water heater and pumps into and keep in the pipe, the pressure of keeping in the pipe is 0.3 MPa, temperature is 108 ℃, continue to mix 30 minutes, then, shift out and pump into said mixture in the gas-liquid separator, at 60 ℃, vacuum tightness is to keep 10 minutes under 0.01 MPa, and the secondary steam that obtains after the flash distillation enters the ethanol distillation separate part, recycles waste heat.
(3) fermentation
Material after the vacuum flashing is cooled the temperature to 33 ℃ by interchanger,, add urea 0.0003 gram in the weight of every gram molasses, and in the weight of every gram molasses, inoculation 10
6The distillery yeast of colony-forming unit (the super highly active dry yeast in Angel, Hubei Angel Yeast stock company produces), with gained mixture stir culture 32 hours in fermentor tank, the heat that zymamsis produces is exchanged by the water coolant in the outer board-like water cooler of jar, to keep leavening temperature at 33 ℃.
At 100 ℃ of distillation gained tunnings, the gained distillation fraction can get 331.3 kilograms of ethanol at 78.3 ℃ of following second distillations, and calculates ethanol yield according to following formula, and calculation result sees Table 1.
Total sugar content in alcohol yied=100% * ethanol weight/molasses
Karusen after the fermentation is totally 2071 grams, get the mash of 100 grams behind the distilled spirits and filter, get 10 milliliters of filtrates and carry out sugared assay, record and calculate and contain reducing sugar 4.95 grams in the karusen altogether according to above-mentioned acid-hydrolysis method with B, and according to following formula calculating residual sugar rate, calculation result sees Table 1.
Total sugar content in reducing sugar amount/molasses in residual sugar rate=100% * karusen
Comparative Examples 1
The explanation of this Comparative Examples adopts molasses to prepare alcoholic acid reference method.
(1) dilution of molasses
With 1000 kilograms of molasses concentrated solutions, sugar hammer degree is that 70 ° of Bx (adopt Abbe refractometer to measure, Shanghai is triumphant comes experimental installation company limited to produce, measuring temperature is 20 ℃) (record according to the above-mentioned acid-hydrolysis method of the present invention total sugar content is 66 weight % in the molasses), the pH value is 6.0, mix in thinning tank with the waste water 1200 kilograms (pH5.0) of discharging at the bottom of the alcohol distillation tower, obtain molasses water solution.
(2) acidifying of molasses
Adding sulfuric acid adjusting molasses pH value of aqueous solution in the molasses water solution of step (1) is 3.5.
(3) fermentation
With the material after the acidifying, according to the method alcohol prepared by fermenting of embodiment 1, at 100 ℃ of distillation gained tunnings, the gained distillation fraction can get ethanol 322.1 grams at 78.3 ℃ of following second distillations.And calculate ethanol yield according to the formula of embodiment 1, calculation result sees Table 1.
Karusen after the fermentation is totally 2039 grams, getting the mash of 100 grams behind the distilled spirits filters with B, get 10 milliliters of filtrates and carry out sugared assay according to above-mentioned acid-hydrolysis method, record and calculate and contain reducing sugar 7.92 grams in the karusen altogether, and according to the calculating of the formula among the embodiment 1 residual sugar rate, calculation result sees Table 1.
Embodiment 2
Present embodiment is used to illustrate that employing molasses of the present invention prepare the alcoholic acid method.
(1) dilution of molasses
With 1000 kilograms of molasses concentrated solutions, sugar hammer degree is that 65 ° of Bx (adopt Abbe refractometer to measure, Shanghai is triumphant comes experimental installation company limited to produce, measuring temperature is 20 ℃) (record according to the above-mentioned acid-hydrolysis method of the present invention total sugar content is 62 weight % in the molasses), the pH value is 6.0, mix in thinning tank with the waste water 1200 kilograms (pH5.3) of discharging at the bottom of the alcohol distillation tower, obtain molasses water solution.
(2) sterilization
The molasses water solution and the water vapor (weight ratio of molasses water solution and water vapor is 100:4) of step (1) are pumped into water heater (the long chemical industry equipment in sky, Nantong company limited simultaneously, model PS-III) mixes in, the mixture of molasses water solution and water vapor is 110 ℃ in temperature, pressure is under 0.4 MPa, in water heater, mixed 3 seconds, then this mixture is shifted out to pump into and keep in the pipe, the pressure of keeping in the pipe is 0.3 MPa, temperature is 105 ℃, mixing time is 40 minutes, then, said mixture is shifted out and pumps in the gas-liquid separator, and at 60 ℃, vacuum tightness is to keep 20 minutes under 0.015 MPa, the secondary steam that obtains after the flash distillation enters the alcohol distillation separate part, recycles waste heat.
(3) fermentation
Material after the vacuum flashing is cooled the temperature to 33 ℃ by interchanger,, add urea 0.0003 gram in the weight of every gram molasses, and in the weight of every gram molasses, inoculation 10
6The distillery yeast of colony-forming unit (the super highly active dry yeast in Angel, Hubei Angel Yeast stock company produces), with gained mixture stir culture 32 hours in fermentor tank, the heat that zymamsis produces is exchanged by the water coolant in the outer board-like water cooler of jar, to keep leavening temperature at 33 ℃.
After the fermentation ends, at 100 ℃ of distillation gained tunnings, the gained distillation fraction can get ethanol 308.8 grams at 78.3 ℃ of following second distillations, and calculates ethanol yield according to the formula among the embodiment 1, and calculation result sees Table 1.
Karusen after the fermentation is totally 2052 grams, getting the mash of 100 grams behind the distilled spirits filters with B, get 10 milliliters of filtrates and carry out sugared assay according to above-mentioned acid-hydrolysis method, record and calculate and contain reducing sugar 4.96 grams in the karusen altogether, and according to the calculating of the formula among the embodiment 1 residual sugar rate, calculation result sees Table 1.
Embodiment 3
Present embodiment is used to illustrate that employing molasses of the present invention prepare the alcoholic acid method.
Method according to embodiment 1 prepares ethanol, different is, in step (2), the molasses water solution and the water vapor (weight ratio of molasses water solution and water vapor is 100:2) of step (1) are pumped into water heater (the long chemical industry equipment in sky, Nantong company limited respectively, model PS-III) mixes in, the mixture of molasses water solution and water vapor is 105 ℃ in temperature, pressure is under 0.2 MPa, mixed 5 seconds in water heater, this mixture is pumped into keep in the pipe then, the pressure of keeping in the pipe is 0.2 MPa, temperature is 105 ℃, mixing time is 40 minutes, then, said mixture is pumped in the gas-liquid separator, at 90 ℃, pressure is to keep 15 minutes under 0.1 MPa, and the secondary steam that obtains after the flash distillation enters the alcohol distillation separate part, recycles waste heat.
Fermentation obtains ethanol 325.4 grams, and the karusen after the fermentation is totally 2040 grams, records and calculates to contain reducing sugar 6.27 grams in the karusen altogether, and calculate alcohol yied and residual sugar rate according to the formula of embodiment 1.
Embodiment 4
Present embodiment is used to illustrate that employing molasses of the present invention prepare the alcoholic acid method.
Method according to embodiment 1 prepares ethanol, different is, in step (2), the molasses water solution and the water vapor (weight ratio of molasses water solution and water vapor is 100:3) of step (1) are pumped into water heater (the long chemical industry equipment in sky, Nantong company limited respectively, model PS-III) mixes in, it is 115 ℃ in temperature that the input speed of molasses water solution and water vapor makes this mixture, pressure is under 0.5 MPa, mixed 10 seconds in water heater, this mixture is pumped into keep in the pipe then, the pressure of keeping in the pipe is 0.4 MPa, temperature is 110 ℃, mixing time is 25 minutes, then, said mixture is pumped in the gas-liquid separator, at 60 ℃, vacuum tightness is to keep 30 minutes under 0.01 MPa, and the secondary steam that obtains after the flash distillation enters the alcohol distillation separate part, recycles waste heat.
Fermentation obtains ethanol 326.7 grams, and the karusen after the fermentation is totally 2045 grams, records and calculates to contain reducing sugar 5.30 grams in the karusen altogether, and calculate alcohol yied and residual sugar rate according to the formula of embodiment 1.
Embodiment 5
Present embodiment is used to illustrate that employing molasses of the present invention prepare the alcoholic acid method.
Method according to embodiment 1 prepares ethanol, different is, in step (2), the molasses water solution and the water vapor of step (1) is pumped into water heater (the long chemical industry equipment in sky, Nantong company limited respectively, model PS-III) mix in, the weight ratio of molasses water solution and water vapor is 100:1.
Fermentation obtains ethanol 326.7 grams, and the karusen after the fermentation is totally 2040 grams, records and calculates to contain reducing sugar 5.30 grams in the karusen altogether, and calculate alcohol yied and residual sugar rate according to the formula of embodiment 1.
Table 1
| Embodiment or Comparative Examples | Embodiment 1 | Comparative Examples 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Alcohol yied (%) | 50.2 | 48.8 | 49.8 | 49.3 | 49.5 | 49.5 |
| Residual sugar rate (%) | 0.75 | 1.2 | 0.8 | 0.95 | 0.8 | 0.8 |
Data from last table 1 compared with prior art, adopt molasses provided by the invention to prepare alcohol yied that the alcoholic acid method obtains apparently higher than the reference method as can be seen, and simultaneously, the residual sugar rate also decreases.
In addition, adopt method of the present invention to prepare ethanol after because ethanol separates the existence that does not have sulfate ion in the waste liquid, the waste water that the ethanol distillation sepn process produces is easy to be utilized by methane-producing bacteria and degrade, thereby greatly reduces the processing pressure of waste water.
Claims (9)
1. one kind is adopted molasses to prepare the alcoholic acid method, it is characterized in that, this method comprises mixes molasses water solution and water vapor, the mixture that obtains is cooled to leavening temperature to ferment, wherein, with molasses water solution and water vapor blended temperature is 105-115 ℃, and pressure is the 0.2-0.5 MPa, and the blended time is 10-50 minute; Described molasses water solution is 100 with the feed weight ratio of water vapor: 2-6.
2. method according to claim 1 wherein, is 108-112 ℃ with molasses water solution and water vapor blended temperature, and pressure is the 0.3-0.4 MPa, and the blended time is 10-20 minute.
3. method according to claim 1, wherein, being blended in the reactor of molasses water solution and water vapor carried out, and molasses water solution and water vapor are added reactor continuously, and mixture shifted out continuously, the blended time is the residence time of mixture in reactor.
4. method according to claim 1, wherein, described molasses water solution is 100 with the feed weight ratio of water vapor: 3-4.
5. according to claim 1,2 or 3 described methods, wherein, the concentration of described molasses water solution is 25-35 weight %.
6. method according to claim 1, wherein, this method also is included in and is cooled to the step that leavening temperature carries out flash distillation with mixture before.
7. method according to claim 6, wherein, it is that 0.01-0.02 MPa, temperature are under 50-60 ℃ that the step of flash distillation is included in vacuum tightness, is under 90-95 ℃ in normal pressure, temperature perhaps, keeps 10-30 minute.
8. method according to claim 1, wherein, the employed yeast of described fermentation is a yeast saccharomyces cerevisiae; In every gram molasses, the employed zymic inoculum size of described fermentation is 10
3-10
8Colony-forming unit, the temperature of described fermentation are 30-36 ℃, and the time of fermentation is 32-48 hour, and the pH value is 5.5-6.
9. according to claim 1 or 8 described methods, wherein, fermenting process also comprises the adding additive, and described additive is ammoniacal liquor and/or urea, and in every gram molasses, the consumption of additive is the 0.0001-0.0005 gram.
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| CN110702846A (en) * | 2019-10-17 | 2020-01-17 | 四川鑫统领新材料有限公司 | Method for determining total sugar in Fehling solution and molasses |
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| Title |
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| 王锋等.磁场流化床反应器大规模糖蜜酒精发酵可行性的研究.《酿酒科技》.2006,(第6期),32-34. * |
| 邓忠海.提高糖蜜酒精生产技术的途径.《广西轻工业》.2006,(第6期),52-53. * |
| 陈世忠等.醪液中亚硫酸对酒精发酵的影响.《酿酒》.2000,(第3期),82-83. * |
| 陈旭.同步糖化浓醪发酵影响因素的探析.《酿酒》.2008,第35卷(第4期),60-62. * |
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