CN109182393A - A kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol - Google Patents
A kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol Download PDFInfo
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- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
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- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
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Abstract
The invention discloses a kind of methods of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, belong to wastewater treatment and technical field of ethanol fermentation industry.The present invention is by anaerobic effluent through the filtered membrane filtration liquid of film, smart tower raffinate, other spice water and smashed cereal materials mix, it is 1 by ingredient material-water ratio: (2~3.5), then through liquefying, saccharification, fermentation, the processes such as distillation obtain ethyl alcohol, wherein, membrane filtration liquid accounts for the 10-90% of total ingredient water quality, smart tower raffinate accounts for the 1-30% of total ingredient water quality, other spice water account for the 0-60% of total ingredient water quality, by adjusting membrane filtration liquid, the ratio of smart tower raffinate and other spice water, or addition acetic acid, the volatile acid concentration of ingredient water is controlled at 100-1200mg/L (with Acetometer).The method of the present invention drastically reduces ethanol production wastewater discharge, has saved water resource, while significant raising Rate of producing alcohol, raw material availability improve 1-5%, reduce ethyl alcohol production energy consumption and cost.
Description
Technical field
The present invention relates to a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, belong to wastewater treatment and
Technical field of ethanol fermentation industry.
Background technique
Ethyl alcohol is that a kind of ethyl alcohol is a kind of important raw material of industry, is widely used in the industry neck such as food, medicine, chemical industry
Domain, while being also a kind of important renewable bioenergy (alcohol fuel), the great attention by countries in the world government.
While ethanol industry fast development, it is also faced with realistic problem very outstanding.I.e. production process needs to consume
A large amount of starchy material and water resource, and generate a large amount of high concentrated organic wastewater (slops).According to statistics, at present I
The ethyl alcohol raw materials for production of 60% or more state are corn, wheat and ageing paddy, brown rice, and every one ton of ethyl alcohol of production consumes 3 tons or so
Raw material and 15-20 tons of process waters, while generating considerable amount of waste water.These problems bring huge economical negative to enterprise
Load.Therefore, the discharge of wastewater of unit product how is reduced, water resources consumption is reduced, reduces cost for wastewater treatment, is improved simultaneously
Raw material availability just becomes current ethanol industry outstanding problem urgently to be solved.
When producing ethyl alcohol as raw material using corn, wheat, paddy and brown rice, common process is raw material through crushing, ingredient, liquid
Change, be saccharified, fermenting and the processes such as distillation obtain ethyl alcohol, remaining slops (full vinasse) obtains by solid-liquid separation treatment
Distiller's grains liquor and wet vinasse slag.Ingredient be tap water or purified treatment with water after a water such as surface water, the pH of liquefaction process
Value is between 5-6, and 85-105 DEG C of temperature, liquefying time 80-200 minutes, α-amylase additive amount was 8-20U/g raw material；Be saccharified work
Sequence pH value is between 4.2-5.6, and 58-62 DEG C of temperature, saccharificatinn period 5-60 minutes, carbohydrase additive amount was 120-200U/g former
Material；Fermentation uses natural ph, and 28-36 DEG C of temperature, yeast-inoculated amount is 10-30% (v/v)；Distillation mainly include slightly evaporate and
Two step of rectifying can increase the equipment such as dealdehyder tower, eparating methanol tower according to ethyl alcohol quality requirement, can be divided according to operating pressure difference
For differential distillation or air-distillation etc..
Distiller's grains liquor obtains concentrate (syrup) and evaporation and condensation water through being concentrated by evaporation, wherein syrup and the mixing of wet vinasse slag
Drying is made vinasse albumen feed (DDGS), and evaporation and condensation water is then and after other waste water mixing in smart tower raffinate, production process
Into anaerobic digestion, anaerobic effluent enters three-level sewage after the processes such as aerobic biochemical, Fenton oxidation are further processed again
Pipe network or qualified discharge.The separation of solid and liquid of slops mainly uses plate compression or centrifuge separation two ways.To reduce wine
The steam consumption that grains liquor is concentrated by evaporation, generallys use three-quadruple effect multiple-effect evaporation modes.
The waste water produced in the production process of ethyl alcohol using cereal as raw material mainly has: (1) slops: being ethanol distillation mistake
The waste liquid that topping still discharges in journey, the waste liquid have the characteristic of high solid content, high COD, low pH；(2) smart tower raffinate: being ethyl alcohol
The waste liquid that rectifying column discharges in distillation process, the waste liquid have as clear as crystal, low COD, high temperature, the characteristic without miscellaneous bacteria；(3) it steams
Send out condensed water: distiller's grains liquor is concentrated by evaporation the secondary steam condensed water generated during production DDGS, which equally has clearly
Clear transparent, low COD, the characteristic without miscellaneous bacteria；(4) other waste water: being in ethanol production process because flushing device, ground are formed
Waste water, sanitary sewage etc. also include that water vapour condensed water, pump cooling water etc. assist waste water.In order to reduce waste discharge and drop
Low waste water treatment cost, can be part distiller's grains liquor direct reuse in ethyl alcohol burden process in production, but research shows that vinasse are clear
The reuse ratio of liquid is usually no more than 30%, and otherwise the substances such as solid content, acetic acid, lactic acid and sodium salt can accumulate in distiller's grains liquor
And alcohol fermentation yeast is poisoned, cause raw material availability to reduce.There are two disadvantages for distiller's grains liquor direct reuse ingredient: first is that wine
Grains liquor contains miscellaneous bacteria, and reuse ingredient is easy to cause the raw acid of alcohol fermentation, raw material availability is reduced, second is that after distiller's grains liquor ingredient
Slurry pH is relatively low, needs to add alkali or ammonium hydroxide adjustment pH value to α-amylase optimal pH range, increases operation and cost.
The COD of evaporation and condensation water is generally lower, about 1500mg/L or so, and is free of miscellaneous bacteria, and theoretically evaporation and condensation water returns
With the risk of no microbiological contamination, but evaporation and condensation water contains the impurity such as volatile alcohol, aldehyde, acid, ester.In spite of a large amount of evaporation and condensations
The report of water reuse ingredient, but it was verified that only add 10% evaporation and condensation water ingredient in tap water, ferment will be inhibited
Female proliferation and fermentation reduces alcohol yied, improves the consumption of raw materials of unit product.
Smart tower raffinate is the waste liquid of rectifying column discharge during ethanol distillation, and the waste liquid is as clear as crystal, but containing a certain amount of
Volatile acid, and volatile acid concentration depend on alcohol fermentation.The volatile acid of essence tower raffinate is in 200- when alcohol fermentation is normal
800mg/L (with Acetometer), volatile acid when alcohol fermentation exception in essence tower raffinate can reach 3000mg/L.Since smart tower is residual
The temperature of liquid is generally at 90 DEG C or so, and commonly used to production equipments such as cleaning and sterilizing fermentors in production, waste water is used as after cleaning
Anaerobic digester system is discharged into be further processed.
In existing distiller's grains liquor or evaporation and condensation water reuse technology scheme, only pass through part from the angle of environmental protection
Reuse achievees the purpose that reduce wastewater discharge, and has ignored distiller's grains liquor, evaporation and condensation water reuse to the light of alcohol fermentation
Lithographic is rung.By taking the alcohol fermentation of conventional spice concentration as an example, the concentration of alcohol of maturing fermentation wine with dregs is in 11-13% after fermentation
(v/v) left and right, if because distiller's grains liquor, evaporation and condensation water reuse cause ethyl alcohol absolute concentration to reduce 0.1-0.2% (v/v),
It is inconspicuous in production, but for the ethyl alcohol manufacturing enterprise for producing 100000 tons of scales per year, this minimal effect causes
Economic loss be exactly 5,000,000 RMB or so.
Summary of the invention
It is an object of the invention to overcome the shortcoming of above-mentioned prior art, realize emission reduction, it is water-saving while, improve second
Alcohol yield, cuts down the consumption of raw materials, and reaches the two-win of environmental benefit and economic benefit.
The present invention provides a kind of methods of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, it may be assumed that ethyl alcohol production
In the process, using anaerobic effluent through the filtered membrane filtration liquid of film and smart tower raffinate as ingredient water, wherein membrane filtration liquid, which accounts for, matches
Expect that the 10-90% of water gross mass, smart tower raffinate account for the 1-30% of ingredient water gross mass；The anaerobic effluent is raw for ethyl alcohol
Other waste water are obtained by anaerobic digestion in evaporation and condensation water in production or the evaporation and condensation water in ethyl alcohol production and production process
, smart tower raffinate refers to the waste liquid of distillation workshop section's rectifying tower bottom discharge.
In one embodiment of the invention, evaporation and condensation water includes that the slops in ethyl alcohol production divides by solid-liquid
From the water obtained with evaporating concentration process；Other waste water include equipment flushing water, ground flushing water, machine in the production process
The one or more of cooling water, sanitary sewage, smart tower raffinate or other technique waste waters are pumped, the slops refers to distillation work
The waste liquid of section topping still tower bottom discharge.
In one embodiment of the invention, the separation of solid and liquid operation is plate compression or centrifuge separation.
In one embodiment of the invention, the ingredient water further includes other spice water.
In one embodiment of the invention, other described spice water are tap water, cleaning surface water, water recovery
One or more of water, cleaning of evaporator water, cooling water.
In one embodiment of the invention, by adjusting the ratio of membrane filtration liquid, smart tower raffinate and other spice water, control
The volatile acid concentration of ingredient water processed is 100-1200mg/L (with Acetometer).
In one embodiment of the invention, when volatile acid concentration is less than 100mg/L in ingredient water, acetic acid can be added
Adjust volatile acid concentration.
In one embodiment of the invention, it is preferred that the membrane filtration liquid accounts for the 85-90% of ingredient water gross mass, essence
Tower raffinate accounts for the 10-15% of ingredient water gross mass.
In one embodiment of the invention, it is preferred that the preferred 300-600mg/ of the volatile acid concentration of the ingredient water
L。
In one embodiment of the invention, it the described method comprises the following steps:
(1) anaerobic effluent is divided through the filtered membrane filtration liquid of film, smart tower raffinate, other spice water according to mass fraction
It Wei not 10-90%, 1-30%, 0-60% and smashed cereal materials mix；
(2) ethyl alcohol and slops and smart tower raffinate are obtained through liquefaction, saccharification, fermentation, distillation process；
(3) by being separated by solid-liquid separation, being concentrated by evaporation, obtained wet vinasse slag and syrup is dried to obtain DDGS, obtains slops
To evaporation and condensation water enter anaerobic digestion process together with other waste water in production process, obtain anaerobic effluent；
(4) anaerobic effluent part is handled by aerobic sigestion system, and membrane filtration liquid partially is obtained by filtration by film；
(5) by the smart tower raffinate that step (2) obtains and the membrane filtration liquid that step (4) obtains together as ingredient water, with crushing
Cereal materials mix afterwards is mixed when ingredient water is insufficient or ingredient water volatile acid concentration is greater than 1200mg/L with other
Material water is supplied or is adjusted；
It is circuited sequentially according still further to step (1)-(5), in cyclic process, membrane filtration is adjusted according to volatile acid concentration in ingredient water
The ratio of liquid, smart tower raffinate and other spice water, or addition acetic acid, so that the volatile acid concentration of ingredient water is 100-
1200mg/L (with Acetometer).
In one embodiment of the invention, the material-water ratio (w/v) of cereal materials and ingredient water is 1 in the ingredient:
(2~3.5).
In one embodiment of the invention, other waste water in the production process be sanitary sewage, distiller's grains liquor,
Smart tower raffinate or other technique waste waters.
In one embodiment of the invention, the cereal materials be one of corn, wheat, paddy and brown rice or
It is several.
In one embodiment of the invention, the film is filtered into one or more of micro-filtration, ultrafiltration or nanofiltration.
In one embodiment of the invention, the volatile acid refers to the volatile organic acids such as acetic acid, propionic acid, butyric acid,
It is measured with the way of distillation, and is calculated with acetic acid concentration.
In one embodiment of the invention, the crushing, ingredient, liquefaction, saccharification, fermentation, distillation, separation of solid and liquid,
It is concentrated by evaporation and anaerobic digestion process is ethanol production industry routine techniques.
In one embodiment of the invention, it is preferred that the pH value of the liquefaction process is 5-6, temperature 85-105
DEG C, liquefying time is 80-200 minutes, and α-amylase additive amount is 8-20U/g raw material；The saccharification process pH value is 4.2-5.6,
Temperature is 58-62 DEG C, and saccharificatinn period is 5-60 minutes, and carbohydrase additive amount is 100-200U/g raw material；The fermentation temperature is
28-38 DEG C, yeast-inoculated amount is 10-30% (v/v)；The distillation process includes slightly evaporating and rectifying.
The invention patent has following advantage:
(1) waste water recycling ratio can be increased substantially as ingredient water using membrane filtration liquid, realizes ingredient station fresh water
" zero consumption ", ton ethyl alcohol reduces wastewater discharge 6-8 tons and saves the water resource of equivalent: and direct reuse distiller's grains liquor, evaporation
Condensed water compares, after Anaerobic Digestion, largely to the virose organic matter of ethanol yeast by anaerobic methane in waste water
Flora decomposition is more advantageous to alcohol fermentation processes.
(2) the raw sour problem of alcohol fermentation can utmostly be avoided: through membrane separation as ingredient water using membrane filtration liquid
After further reduce to the virose organic matter of alcohol fermentation yeast in anaerobic effluent, while filtering off in addition to detesting
Miscellaneous bacteria in oxygen digestion water outlet, it is possible to prevente effectively from the raw sour problem of alcohol fermentation.
(3) smart tower raffinate is supplemented on the basis of membrane filtration liquid as ingredient water, can significantly improve Rate of producing alcohol, raw material utilizes
Rate improves 1-5%, can under the premise of identical raw and auxiliary material total amount consumed for producing 100000 tons of ethyl alcohol manufacturing enterprises per year
To increase by 1000 tons of alcohol yied or more: membrane filtration liquid usually contains the volatile acid no more than 100mg/L, supplement portion in membrane filtration liquid
Volatile acid concentration is in reasonable concentration in point smart adjustable spice water of tower raffinate, so as to improve alcohol fermentation performance.
(4) smart tower raffinate is supplemented on the basis of membrane filtration liquid as ingredient water, can recycle the heat of smart tower raffinate, raising is matched
Slurry temperature after material, to reduce the steam consumption of liquefaction process；Simultaneously because smart tower raffinate is free of miscellaneous bacteria, ethyl alcohol hair is improved
The craft sanitary of ferment reduces the risk of the raw acid of alcohol fermentation.
(5) pollutant (COD) of other waste water is lower in evaporation and condensation water and production process, detesting after anaerobic digestion
Oxygen digestion water outlet has the low (≤1000mgCaCO of basicity3/ L), ammonia nitrogen concentration low (≤100mg/L) the advantages that, therefore when ingredient
Without adding sulfuric acid to adjust slurry pH value, cost is minimum.
(6) membrane filtration liquid and smart tower raffinate are free of miscellaneous bacteria, and liquefaction process can use low temperature (86-88 DEG C) digesting technoloy,
High-temperature cooking process with 95 DEG C of routine or more compares, and can reduce ethyl alcohol production energy consumption, ton ethyl alcohol liquefaction process steam consumption
10kg or more can be reduced.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention will be further described technical solution of the present invention using embodiment in conjunction with Fig. 1 below.
Method for determining concentration of alcohol: karusen 100mL is accurately measured with 100mL volumetric flask, injects 500mL distilling flask
In, it with 100mL moisture time washing capacity bottle and injects in distilling flask, heating distillation, distillate is collected in the capacity of 100mL
In bottle, when band distillate is close to scale, removes, add water to scale, shake up.It pours into the graduated cylinder that 100mL is clean, dry, with wine
Essence meter and thermometer survey its alcoholic strength and temperature simultaneously, look into conversion table according to the concentration of alcohol and temperature measured, are scaled 20 DEG C
Concentration of alcohol (%, v/v).
Total volatile acid measuring method: by waste water with phosphoric acid after, therefrom evaporate volatile fatty acid, then be with phenolphthalein
Indicator titrates distillate with NaOH solution.Ammoniacal nitrogen in waste water may form interference to measurement, therefore should be first in alkali
Ammoniacal nitrogen is evaporated under the conditions of property.
Reagent: 10%NaOH solution；NaOH standard solution, 0.1000mol/L；10% phosphoric acid solution takes 70mL density
1.7g/cm3Phosphoric acid be diluted with water to 1L；Phenolphthalein indicator.
Determination step:
50-200mL waste water to be measured is put into cucurbit, volatile acid content is no more than 30mmol.Not such as volume of water sample
Sufficient 100mL can be diluted to 100mL with distilled water.A few drop phenolphthalein indicators are added.10%NaOH solution is added, makes solution
In alkalinity, and make the NaOH amount of skipping over.Start to distill, until into cucurbit, remaining liquid is 50~60mL.It will with distilled water
Cucurbit remaining liq is diluted to original volume, and with the phosphoric acid of 10mL 10%, 10mL distillation is put into receiving bottle
Water simultaneously connect receiving bottle with the condenser pipe on cucurbit, and the liquid level of receiving bottle or less should be immersed by pouring into pipe.Distillation liquid into bottle
Until body is 15-20mL.After bottle to be distilled is cooling, 50mL distilled water is added and distills herein, until residue 10~20mL liquid is
Only.10 drop phenolphthalein are added into distillate, are titrated to until pale pink do not disappear with NaOH standard solution.
It calculates:
In formula:
VNaOH--- the volume of the NaOH standard solution of titration consumption, mL；
C --- the actual concentrations of the NaOH standard solution of titration consumption, mol/L；
Vs--- the volume of tested waste water water sample, mL.
Converted mash, karusen acidity assaying method: being instruction with phenolphthalein with 10mL coarse filtration liquid according to acid-base neutralization principle
Agent is titrated with 0.1mol/L NaOH standard solution, and consumption 1mL 0.1mol/LNaOH standard solution is 1 degree.
Converted mash or filtering fermentation liquor liquid 1mL are drawn, is placed in 250mL triangular flask, adds water 50mL, add phenolphthalein indicator 2
Drop is titrated with 0.1mol/LNaOH standard solution, and it is in blush and colour-fast for terminal in 30s to be titrated to solution.
In formula:
The concentration of c-NaOH standard solution, mol/L；
v1The volume of-absorption sample, mL；
The volume of the NaOH standard solution consumed when v-titration, mL.
Embodiment 1
A kind of reuse anaerobic effluent of the present invention and the method for smart tower raffinate production ethyl alcohol use following processing step:
Membrane filtration liquid and smart tower raffinate are mixed according to 85: 15 ratio, volatile acid concentration 600mg/L；It takes smashed
Corn flour 100Kg adds 310L mixed liquor ingredient, is added Thermostable α-Amylase (10U/g starch), is heated to after mixing evenly
86 DEG C and maintain 200min；60 DEG C are cooled to, is added carbohydrase (180U/g starch), after mixing evenly heat preservation saccharification 15min.
30 DEG C are cooled to after saccharification, access 15% (v/v) yeast starter liquid starting fermentation.After fermentation, second is obtained through distillation
Alcohol, slops and smart tower raffinate.Slops obtains wet vinasse slag and distiller's grains liquor, distiller's grains liquor with 60 mesh filter-cloth filterings
Syrup and evaporation and condensation water are obtained through being concentrated by evaporation again.Wet vinasse slag and syrup combination drying obtain DDGS, evaporation and condensation water and
Other waste water enter the processing of anaerobic digestion workshop section.The ultrafiltration membrance filter of 300,000 molecular cut offs of anaerobic effluent, membrane filtration liquid
The smart tower raffinate obtained with distillation workshop section is back to next batch alcohol fermentation after mixing in proportion.Continuous circulation by this method
10 batches, the proportion of membrane filtration liquid and smart tower raffinate is adjusted when different batches ingredient according to acetic acid concentration, controls the volatile acid of ingredient water
Concentration is in 600mg/L or so.The fermentation period average out to 48h of 10 batches of alcohol fermentations, average ethanol concentration 11.24% (v/v),
Karusen average acidity 3.2, and the fermentation period of the alcohol fermentation of control group tap water ingredient is 56h, concentration of alcohol average out to
11.11% (v/v), karusen average acidity 3.5.
The natural ph of slurry is between 5.3-5.7 after the present embodiment membrane filtration liquid, smart tower raffinate and corn flour mix,
Therefore liquefaction process is without adding sulfuric acid adjustment pH value.Karusen average acidity reduces 0.3 simultaneously, and concentration of alcohol improves
0.13% (v/v), is equivalent to raw material availability and improves 1.2%.
Embodiment 2
A kind of reuse anaerobic effluent of the present invention and the method for smart tower raffinate production ethyl alcohol use following processing step:
Membrane filtration liquid and smart tower raffinate are mixed according to 90: 10 ratio, volatile acid concentration 400mg/L；It takes smashed
260L mixed liquor ingredient is added in coarse rice powder 100Kg, is added Thermostable α-Amylase (8U/g starch), is heated to after mixing evenly
90 DEG C and maintain 100min；58 DEG C are cooled to, is added carbohydrase (150U/g starch), after mixing evenly heat preservation saccharification 30min.
30 DEG C are cooled to after saccharification, access 10% (v/v) yeast starter liquid starting fermentation.After fermentation, second is obtained through distillation
Alcohol, slops and smart tower raffinate.Slops obtains wet vinasse slag and distiller's grains liquor, distiller's grains liquor with 60 mesh filter-cloth filterings
Syrup and evaporation and condensation water are obtained through being concentrated by evaporation again.Wet vinasse slag and syrup combination drying obtain DDGS, evaporation and condensation water and
Other waste water enter the processing of anaerobic digestion workshop section.The ultrafiltration membrance filter of 500,000 molecular cut offs of anaerobic effluent, membrane filtration liquid
The smart tower raffinate obtained with distillation workshop section is back to next batch alcohol fermentation after mixing in proportion.Continuous circulation by this method
10 batches, the proportion of membrane filtration liquid and smart tower raffinate is adjusted when different batches ingredient according to acetic acid concentration, controls the volatile acid of ingredient water
Concentration is in 300mg/L or so.The fermentation period average out to 48h of 10 batches of alcohol fermentations, average ethanol concentration 12.15% (v/v),
Karusen average acidity 3.2, and the fermentation period of the alcohol fermentation of control group tap water ingredient is 56h, concentration of alcohol average out to
12.03% (v/v), karusen average acidity 3.5.
The natural ph of slurry is between 5.5-5.8 after the present embodiment membrane filtration liquid, smart tower raffinate and corn flour mix,
Therefore liquefaction process is without adding sulfuric acid adjustment pH value.Karusen average acidity reduces 0.3 simultaneously, and concentration of alcohol improves
0.12% (v/v), is equivalent to raw material availability and improves 1.0%.
Embodiment 3
A kind of reuse anaerobic effluent of the present invention and the method for smart tower raffinate production ethyl alcohol use following processing step:
Membrane filtration liquid and smart tower raffinate are mixed according to 99: 1 ratio, volatile acid concentration 100mg/L；It takes smashed rough
2600L mixed liquor ingredient is added in rice flour 1000Kg, is added Thermostable α-Amylase (15U/g starch), is heated to after mixing evenly
95 DEG C and maintain 100min；60 DEG C are cooled to, is added carbohydrase (160U/g starch), after mixing evenly heat preservation saccharification 30min.
30 DEG C are cooled to after saccharification, access 12% (v/v) yeast starter liquid starting fermentation.After fermentation, second is obtained through distillation
Alcohol, slops and smart tower raffinate.Slops obtains wet vinasse slag and distiller's grains liquor, distiller's grains liquor with 60 mesh filter-cloth filterings
Syrup and evaporation and condensation water are obtained through being concentrated by evaporation again.Wet vinasse slag and syrup combination drying obtain DDGS, evaporation and condensation water and
Other waste water enter the processing of anaerobic digestion workshop section.The ultrafiltration membrance filter of 800,000 molecular cut offs of anaerobic effluent, membrane filtration liquid
The smart tower raffinate obtained with distillation workshop section is back to next batch alcohol fermentation after mixing in proportion.Continuous circulation by this method
10 batches, the proportion of membrane filtration liquid and smart tower raffinate is adjusted when different batches ingredient according to acetic acid concentration, controls the volatile acid of ingredient water
Concentration is in 300mg/L or so.The fermentation period average out to 48h of 10 batches of alcohol fermentations, average ethanol concentration 12.06% (v/v),
Karusen average acidity 3.2, and the fermentation period of the alcohol fermentation of control group tap water ingredient is 56h, concentration of alcohol average out to
12.03% (v/v), karusen average acidity 3.5.
The natural ph of slurry is between 5.5-5.9 after the present embodiment membrane filtration liquid, smart tower raffinate and corn flour mix,
Therefore liquefaction process is without adding sulfuric acid adjustment pH value.Karusen average acidity reduces 0.3 simultaneously, and concentration of alcohol improves
0.03% (v/v), is equivalent to raw material availability and improves 0.2%.
Embodiment 4
A kind of reuse anaerobic effluent of the present invention and the method for smart tower raffinate production ethyl alcohol use following processing step:
Membrane filtration liquid, smart tower raffinate and tap water are mixed according to 40: 30: 30 ratio, and add acetic acid to make ingredient water
Volatile acid concentration reaches 1200mg/L；It takes the smashed coarse rice powder of 1000Kg that 2600L mixed liquor ingredient is added, high temperature resistant is added
α-amylase (10U/g starch), is heated to 90 DEG C after mixing evenly and maintains 100min；60 DEG C are cooled to, carbohydrase is added
(180 U/g starch) keeps the temperature saccharification 30min after mixing evenly.It is cooled to 30 DEG C after saccharification, accesses 15% (v/v) yeast
Seed liquor starting fermentation.After fermentation, ethyl alcohol, slops and smart tower raffinate are obtained through distillation.Slops is filtered with 60 mesh
Wet vinasse slag and distiller's grains liquor is obtained by filtration in cloth, and distiller's grains liquor obtains syrup and evaporation and condensation water through being concentrated by evaporation again.Wet vinasse
Slag and syrup combination drying obtain DDGS, and evaporation and condensation water and other waste water enter the processing of anaerobic digestion workshop section.Anaerobic digestion goes out
The smart tower raffinate that the ultrafiltration membrance filter of 100,000 molecular cut offs of water, membrane filtration liquid and distillation workshop section obtain returns after mixing in proportion
For next batch alcohol fermentation.Continuous circulation 10 batches by this method adjusts membrane filtration according to acetic acid concentration when different batches ingredient
The proportion of liquid and smart tower raffinate, controls the volatile acid concentration of ingredient water in 300mg/L or so.The fermentation week of 10 batches of alcohol fermentations
Phase average out to 52h, average ethanol concentration 12.03% (v/v), karusen average acidity 3.2, and control group tap water ingredient
The fermentation period of alcohol fermentation is 56h, concentration of alcohol average out to 12.03% (v/v), karusen average acidity 3.5.
The natural ph of slurry is between 5.2-5.7 after the present embodiment membrane filtration liquid, smart tower raffinate and corn flour mix,
Therefore liquefaction process is without adding sulfuric acid adjustment pH value.Karusen average acidity reduces 0.3 simultaneously, concentration of alcohol and originally
Water phase is worked as.
Embodiment 5
A kind of reuse anaerobic effluent of the present invention and the method for smart tower raffinate production ethyl alcohol use following processing step:
In spice water pot, membrane filtration liquid and smart tower raffinate are continuously mixed according to 85: 15 ratio, use pump will in mixing
Mixed liquor is continuously introduced into material-compound tank, and the flow of mixed liquor is 105m3/ h, mixed liquor volatile acid concentration is between 300-800mg/L
Fluctuation；Continuously add smashed corn flour simultaneously in material-compound tank, corn flour mass flow is 37.5t/h, while according to
The concentration unit of 16U/g raw material is continuously added to Thermostable α-Amylase；Slurry after ingredient is heated to 88 continuously across heater
It DEG C liquefies, liquefied pot continuous feed continuous discharge, liquefied fermented glutinous rice residence time in liquefied pot is 120min；Liquefaction terminates
Liquefied fermented glutinous rice is cooled to 60 DEG C into saccharifying tank, according to the dense of 160U/g raw material in saccharifying tank by heat exchanger continuous coo1ing afterwards
Degree unit is continuously added to carbohydrase, the same continuous feed continuous discharge of saccharifying tank, and converted mash residence time in saccharifying tank is
30min；Converted mash pump is continuously introduced into heat exchanger and is cooled to 30 DEG C, is then fed into fermentor, while accessing 25% (v/v's)
Yeast starter liquid, fermentor total volume 1200m3, charge 1000m3, converted mash is sent into after filling by switch valve by fermentor
Another fermentor repeats aforesaid operations, with heat exchanger control temperature at 30-36 DEG C in fermentation process, the hair of single fermentor
The ferment time is 50-62 hours.After fermentation, ethyl alcohol, slops and smart tower raffinate are obtained through two tower differential distillations.Distillation
Waste liquid obtains wet vinasse slag with 60 mesh filter cloth plate-frame filterings and distiller's grains liquor, distiller's grains liquor obtain sugar through three-effect evaporation and condensation again
Slurry and evaporation and condensation water.Wet vinasse slag and syrup combination drying obtain DDGS, and evaporation and condensation water and other waste water enter anaerobism and disappear
The processing of chemical industry section.The ultrafiltration membrance filter of 800,000 molecular cut offs of anaerobic effluent, flow 89.25m3/ h membrane filtration liquid and steaming
Evaporate the 15.75m that workshop section obtains3The smart tower raffinate of/h is back to next batch alcohol fermentation after mixing in proportion.Connect by this method
Continuous circulation 10 batches, when different batches ingredient, adjust the proportion of membrane filtration liquid and smart tower raffinate according to acetic acid concentration, control ingredient water
Volatile acid concentration is in 300mg/L or so.The fermentation period average out to 48h of 10 batches of alcohol fermentations, average ethanol concentration 11.46%
(v/v), karusen average acidity 3.2, and the fermentation period of the alcohol fermentation of control group tap water ingredient is 56h, concentration of alcohol
Average out to 11.34% (v/v), karusen average acidity 3.5.
The natural ph of slurry is between 5.5-5.9 after the present embodiment membrane filtration liquid, smart tower raffinate and corn flour mix,
Therefore liquefaction process is without adding sulfuric acid adjustment pH value.Karusen average acidity reduces 0.3 simultaneously, and concentration of alcohol improves
0.12% (v/v), is equivalent to raw material availability and improves 1.0%.
Embodiment 6: influence of the ingredient water of the volatile acid containing various concentration to alcohol fermentation
On the basis of embodiment 3, using volatile acid concentration in the method adjustment ingredient water of addition acetic acid and ethyl alcohol is carried out
Fermentation, the results are shown in Table 1 and tap water compares, when volatile acid concentration is no more than 1000mg/L in ingredient water, Ke Yiming
It is aobvious to improve concentration of alcohol, and when volatile acid concentration is more than 1200mg/L, distillery yeast proliferation is suppressed, concentration of alcohol decline.
The different volatile acid concentration ingredient waters of table 1 and originally the water by fermentation table of comparisons
| Volatile acid mg/L | 0 (tap water) | 100 | 300 | 400 | 600 | 800 | 1000 | 1200 | 1400 |
| Ethyl alcohol % (v/v) | 12.03 | 12.06 | 12.13 | 12.15 | 12.18 | 12.11 | 12.05 | 12.03 | 11.26 |
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection of the invention without departing from the spirit and scope of the present invention
Range should subject to the definition of the claims.
Claims (10)
1. a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, which is characterized in that the method are as follows: ethyl alcohol
In production process, using anaerobic effluent through the filtered membrane filtration liquid of film and smart tower raffinate as ingredient water, wherein membrane filtration liquid accounts for
The 10-90% of ingredient water gross mass, smart tower raffinate account for the 1-30% of ingredient water gross mass；The anaerobic effluent is raw for ethyl alcohol
Other waste water are obtained by anaerobic digestion in evaporation and condensation water in production or the evaporation and condensation water in ethyl alcohol production and production process
, smart tower raffinate refers to the waste liquid of distillation workshop section's rectifying tower bottom discharge.
2. a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, feature exist according to claim 1
In evaporation and condensation water includes the water that the slops in ethyl alcohol production is obtained by separation of solid and liquid and evaporating concentration process；It is described
In production process other waste water include equipment flushing water, ground flushing water, pump cooling water, sanitary sewage, remaining smart tower raffinate,
One or more of remaining distiller's grains liquor or other technique waste waters；Wherein, the slops refers to distillation workshop section's topping still
The waste liquid of tower bottom discharge.
3. the method for a kind of reuse anaerobic effluent according to claim 1 or claim 2 and smart tower raffinate production ethyl alcohol, feature
It is, the ingredient water further includes other spice water.
4. a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, feature exist according to claim 3
In other described spice water are one of tap water, cleaning surface water, water recovery water, cleaning of evaporator water, cooling water or several
Kind.
5. -4 any a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol according to claim 1,
It is characterized in that, the method controls the volatile acid of ingredient water by adjusting the ratio of membrane filtration liquid, smart tower raffinate and other spice water
Concentration is 100-1200mg/L.
6. -5 any a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol according to claim 1,
It is characterized in that, when volatile acid concentration is less than 100mg/L in the ingredient water, addition acetic acid adjusts volatile acid concentration.
7. -6 any a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol according to claim 1,
It is characterized in that, the membrane filtration liquid accounts for the 85-90% of ingredient water gross mass, and smart tower raffinate accounts for the 10-15% of ingredient water gross mass.
8. -7 any a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol according to claim 1,
It is characterized in that, the described method comprises the following steps:
(1) it is respectively according to mass fraction through the filtered membrane filtration liquid of film, smart tower raffinate, other spice water by anaerobic effluent
10-90%, 1-30%, 0-60% and smashed cereal materials mix；
(2) ethyl alcohol and slops and smart tower raffinate are obtained through liquefaction, saccharification, fermentation, distillation process；
(3) by being separated by solid-liquid separation, being concentrated by evaporation, obtained wet vinasse slag and concentrate is dried to obtain DDGS, obtains slops
Evaporation and condensation water enter anaerobic digestion process together with other waste water in production process, obtain anaerobic effluent；
(4) membrane filtration liquid is obtained by filtration by film in anaerobic effluent part, and remainder enters aerobic sigestion system and further locates
Reason；
(5) and smashed by the smart tower raffinate that step (2) obtains and the membrane filtration liquid that step (4) obtains together as ingredient water
Cereal materials mix, when ingredient water is insufficient or ingredient water volatile acid concentration is greater than 1200mg/L, with other spice water
It supplies or adjusts；
It is circuited sequentially according still further to step (1)-(5), in cyclic process, membrane filtration liquid, essence is adjusted according to volatile acid concentration in ingredient water
The ratio of tower raffinate and other spice water, or addition acetic acid, so that the volatile acid concentration of ingredient water is 100-1200mg/L.
9. a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol, feature exist according to claim 8
In the material-water ratio g/mL of cereal materials and ingredient water is 1 in the ingredient: (2~3.5), wherein the cereal materials are jade
One or more of rice, wheat, paddy and brown rice.
10. a kind of method of reuse anaerobic effluent and smart tower raffinate production ethyl alcohol according to claim 8 or claim 9, special
Sign is that the pH value of the liquefaction process is 5-6, and temperature is 85-105 DEG C, and liquefying time is 80-200 minutes, α-amylase addition
Amount is 8-20U/g raw material；The saccharification process pH value is 4.2-5.6, and temperature is 58-62 DEG C, and saccharificatinn period is 5-60 minutes, sugar
Change enzyme additive amount is 100-200U/g raw material；The fermentation temperature is 28-38 DEG C, and yeast-inoculated amount is 10-30% (v/v)；Institute
Stating distillation process includes slightly evaporating and rectifying.
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