CN104498533A - Method for preparing ethyl alcohol - Google Patents

Method for preparing ethyl alcohol Download PDF

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CN104498533A
CN104498533A CN201410662601.9A CN201410662601A CN104498533A CN 104498533 A CN104498533 A CN 104498533A CN 201410662601 A CN201410662601 A CN 201410662601A CN 104498533 A CN104498533 A CN 104498533A
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mash
macrobead
raw material
starch
broken
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CN104498533B (en
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岳国海
刘克
张木兰
魏斯钊
刘锦旗
曹孟君
杨素珍
杨晓光
刘贵忠
庞法拥
张波
李鹏
苑颖
高合龙
孙成志
李建
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PetroChina Jilin Chemical Engineering Co., Ltd.
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Jilin Design Institute
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00Preparation of oxygen-containing organic compounds
    • C12P7/02Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06Ethanol, i.e. non-beverage
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Health & Medical Sciences (AREA)
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  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention provides a method for preparing ethyl alcohol. The method is characterized by including the steps that starch raw materials are smashed to form large-particle starchiness raw materials; water and thermostable amylase are added into the large-particle starchiness raw materials to be mixed and stirred to form a first mash; gelatinization processing is carried out on the first mash to form a second mash; liquefaction processing is carried out; saccharification processing is carried out on the liquefied second mash to form a third mash; and the third mash is fermented. According to the method, under the condition that the large-particle starchiness raw materials can be used, the viscosity of the mashes of the starchiness raw materials is controlled to be within the technology acceptable range. Meanwhile, as the viscosity and the liquefied saccharification effect of the mashes of the starchiness raw materials are well controlled, the problems of difficult conveying and incomplete liquefied saccharification in the prior art when the mashes of the starchiness raw materials are used for producing the ethyl alcohol are solved, and the energy consumption in the production technology is further reduced.

Description

A kind of method preparing ethanol
Technical field
The present invention relates in general to ethanol preparation field, more specifically, relates to a kind of method preparing ethanol.
Background technology
In ethanol production process, the energy-saving and cost-reducing theme having become promotion industry development.Wherein thick mash fermentation technique is the most obvious to the effect that alcohol production is energy-saving and cost-reducing.Realize one of prerequisite of thick mash fermentation technology for improving the content of the fermentable sugar in fermentation liquid, namely the concentration of starch content in mash after the starchy material of pulverizing and water spice is improved, and controlled by certain technological operation with this, prepare the mellow solution of saccharification of high-content of starch, thus when not changing zymotechnique operation, the concentration of fermentable sugar in fermentation liquid is effectively improved, the fermentation liquid metabolic conversion of same volume can be made like this to produce more alcohol product, and then reach the water consumption significantly reduced in production process, energy consumption and production cost, reduce wastewater treatment burden, improve the object that equipment efficiency of usage etc. is saved energy and reduce the cost.
At present, for thick mash ethanol fermentation most study is add fire resistant alpha-diastase in the activity of raising α-amylase and saccharifying enzyme, the acid resistance improving saccharifying enzyme, the resistance to height sugar improving fermented bacterium and the performance of resistance to high alcohol concn, the granularity of improvement raw material pulverizing and pulverizing raw material spice process to promote the aspects such as starchy material pre liquefied.And the existing method preparing ethanol comprises the following steps: adopt beater disintegrating machine by the pulverizing of starchy material; General size controlling is at below 1.2mm; Mixed with water by raw material after powder, general material-water ratio is more than 1:2.8; The mash that formed after mixing is inputted in pre liquefied tank, adds appropriate α-amylase, mix and rear intensification liquefaction processing is carried out to mash; Carry out saccharification process again; Cool the mash after saccharification, enters fermentation procedure to form ethanol.
And for how to prepare the qualified mellow solution of saccharification of high density by macrobead dry starch raw material mash, and then the research of the ethanol of preparation high density is little, not yet meets relevant report so far.
In the prior art, alcohol concn in alcohol production enterprise fermenting-ripening wine with dregs is generally 11% (v) left and right, the ratio of amounting to into pulverizing raw material and spice water is about 1:2.8, do not reach the processing requirement (ratio of amounting to into pulverizing raw material and spice water is about 1:2) that fermenting-ripening wine with dregs alcohol concn is 14% (v) or higher thick mash ethanol fermentation, improve and to pulverize after raw material spice starch content in mash, when the particle diameter of usual raw material pulverizing is below 1.2mm, the simplest way is exactly reduce the addition of spice water, but can there is following problem in the addition only by reducing spice water: owing to pulverizing the increase of material quantity in mash, although the starch content in mash can be impelled to increase, but along with the intensification of mash, the viscosity of mash can increase considerably, difficulty can be brought to the conveying of mash, also the power consumption in course of conveying can be increased, sometimes also the conveying of mash can be affected because the viscosity of mash increases, even produce the difficulty that mash is difficult to carry, directly have influence on the normal operation of production.
In order to effectively solve an above difficult problem, pulverizing under the certain condition of raw material spice water, the method of the granularity improving raw material pulverizing can be taked, namely 3.0mm to 3.5mm is brought up to by the dry starch raw material pulverized particles diameter of normal employing at present by below 1.2mm, like this, greatly can reduce the feed particles of pulverizing and the contact area of spice water on the one hand, while raw material spice mash concentration is pulverized in raising, improve the ratio of free-water in mash as far as possible, thus the mobility of mash can be improved, be conducive to the conveying of mash.But, there is again new problem, due to the raising of starchy material pulverized particles degree, after mixing with spice water, the absorption speed of macrobead starch can be slack-off, directly will have influence on the effect of liquefaction and saccharification, and then affect the effect of ethanol fermentation and the utilizing status of raw material.Therefore, how when ensureing that starchy material pulverized particles degree is larger, reducing the viscosity of mash, improve and ensure liquefaction and saccharification result, and the concentration effectively increasing the ethanol that fermentation produces further being present stage urgent problem.
Summary of the invention
In order to solve problems of the prior art, according to an aspect of the present invention, provide a kind of method preparing ethanol, it is characterized in that, comprising: starch material is pulverized to form macrobead starchy material; Add water in macrobead starchy material and fire resistant alpha-diastase mix and blend to form the first mash; Gelatinization process is carried out to form the second mash to the first mash; Liquefaction isothermal holding; Saccharification process is carried out to form the 3rd mash to the second mash after liquefaction isothermal holding; 3rd mash is fermented.
In the above-mentioned methods, carry out gelatinization process to the first mash to comprise further with the step forming the second mash: implement one-level and spray broken refinement; Macrobead starchy material is degraded; And implement the broken refinement of two-stage injection.
In the above-mentioned methods, the broken refining device of injection is used to carry out gelatinization process to form the second mash to the first mash.
In the above-mentioned methods, it is characterized in that, the viscosity number of the second mash is in the scope of 60mPa.s to 100mPa.s.
In the above-mentioned methods, starch material is being pulverized to be formed in the step of macrobead starchy material, after pulverising step, the granularity of macrobead starchy material is 3.0mm to 3.5mm, the viscosity number of the first mash is in the scope of 80mPa.s to 150mPa.s, and starch material comprises corn and/or cassava;
In the above-mentioned methods, the add-on of fire resistant alpha-diastase is 8u/g to 12u/g.
In the above-mentioned methods, in after-ripening device, liquefaction isothermal holding is implemented; Lower the temperature in vacuum cooling system; Saccharification process is implemented in saccharifying tank.
In the above-mentioned methods, in after-ripening device, liquefaction isothermal holding is implemented; Lower the temperature in vacuum cooling system; Saccharification process is implemented in saccharifying tank.The temperature of carrying out being incubated in after-ripening device, in the scope of 90 DEG C to 100 DEG C, is cooled in the scope of 55 DEG C to 65 DEG C in vacuum cooling system.
In the above-mentioned methods, in after-ripening device, liquefaction isothermal holding is implemented; Lower the temperature in vacuum cooling system; Saccharification process is implemented in saccharifying tank.The time of liquefaction processing is in the scope of 80 minutes to 100 minutes.
In the above-mentioned methods, in after-ripening device, liquefaction isothermal holding is implemented; Lower the temperature in vacuum cooling system; Saccharification process is implemented in saccharifying tank.When the DE value of mash is in the scope of 14 to 18, stop saccharification step.
According to method of the present invention, can when the starchy material utilizing granularity larger, by the viscosity controller of starchy material mash in the acceptable scope of technique.Simultaneously, owing to controlling viscosity and the thinning effect of macrobead starchiness mash well, therefore efficiently solve in prior art the difficulty of transportation and the incomplete problem of thinning that occur when using macrobead macrobead starchiness mash to carry out alcohol production, reduce the energy consumption in production technique further.In addition, owing to employing macrobead starchiness mash, therefore effectively the ratio pulverizing raw material and spice water is improved to about 1:2, thus the alcohol concn of generation is increased to more than 14%.
Accompanying drawing explanation
Embodiment for a more complete understanding of the present invention and advantage thereof, now by following description carried out by reference to the accompanying drawings as a reference, wherein:
Fig. 1 is the schema of the method for the preparation of ethanol according to some embodiments of the present invention.
Embodiment
Below, preparation and the use of various embodiments of the present invention is discussed in detail.But, should be appreciated that, the invention provides many applicable inventive concepts that can realize in various specific environment.The specific embodiment discussed illustrate only preparation and uses the concrete mode of present subject matter, and is not used in the scope limiting different embodiment.
As shown in Figure 1, in step S101, starch material is pulverized to form macrobead starchy material.Starch can be corn, cassava or other dry starch raw material.In certain embodiments, beater grinder can be adopted to carry out dry ground to starch material.The granularity size of the starchy material obtained after can controlling pulverizing by selecting the hole diameter of sieve (perforated) plate size of pulverizer.In the prior art, alcohol production enterprise adopts aperture to be that the sieve plate of about 1.2mm to 1.5mm is pulverized mostly, and the granularity of the starchy material obtained after pulverizing is generally at below 1.2mm, and fine powder is more.In some embodiments of the invention, in order to the level making the pulverized particles degree of starchy material reach about 3.0mm to about 3.5mm, can select and there is the sieve plate of about 4.0mm to about 8.0mm sieve aperture, and the smashing capability of pulverizer is improved, make the pulverized particles degree of starchy material reach the level of about 3.0mm to about 3.5mm.Simultaneously, the granularity of the macrobead starchy material after pulverizing can reach more uniform level, such as, the particle that can reach about 3.0mm to about 3.5mm has accounted for more than 85% of sum, the particle being less than about 1.2mm only accounts for less than 5% of sum, and the particle being greater than 3.5mm only accounts for less than 3% of sum.Pulverize through one-level and can reach the requirement of raw material pulverizing degree, like this can the power consumption of conservation pulverizing process.The macrobead raw material powder that raw starch obtains after pulverizing sends into feed bin storage.
As shown in Figure 1 in step s 103, add water in macrobead starchy material and fire resistant alpha-diastase mix and blend to form macrobead starchy material mash, i.e. the first mash.In certain embodiments, to join in macrobead starchy material after the recycle-water of distillation workshop section being cooled to 75 DEG C and carry out spice.After spice, the temperature of macrobead starchy material mash needs to reach 65 DEG C, if the temperature of macrobead starchy material mash after spice is lower than 65 DEG C, can adopt indirect steam heating method that macrobead starchy material mash is heated to this temperature.The fire resistant alpha-diastase raw material powder of about 8u/g to about 12u/g is added in spice process.After being uniformly mixed, sampling detects the viscosity number of macrobead starchy material mash in the scope of about 80mPa.s to about 150mPa.s.When above-mentioned viscosity number, the conveying of mash is not had an impact.Mash transferpump is adopted to be sent in the broken refining device of novel injection.
As shown in Figure 1, in step S105, gelatinization process is carried out to form the second mash to the first mash.In some embodiments of the invention, use the broken refining device enforcement of macrobead starch mash to the gelatinization of macrobead starchy material mash and Operation for liquefaction.Adopt the mode of transferpump to deliver to the macrobead starch mash in above-mentioned temporary storage tank to spray in broken refining device.Nozzle place before mash being delivered into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash and sprays in broken refining device.N number of first order jet nozzle structure design be arranged on same pitch circle that liquidates is adopted owing to spraying broken refining device, therefore the steam mash mixing liquid sprayed from the nozzle of symmetry first under the influence of centrifugal force, overcome viscous force and the surface tension of mash itself, the macrobead starch in mash is made to obtain centrifugal and distensibility fragmentation, then the form ejection at a high speed of the granulated drop of taper shape at an angle is sentenced from jet hole, wherein, water component in mash forms vaporific little water droplet, macrobead starch wherein carries out liquidating high-speed impact with the form of the membrane-enclosed particle droplet of water in the impingement region sprayed, friction, broken, macrobead starch is made to obtain effectively broken and refinement.Then, water membrane-enclosed macrobead starch fall into below the one-level spray jet spraying broken refining device cavity together with water smoke in turbulence flow flied solution form liquid level.Now, the macrobead starch of the incomplete broken refinement in mash in effects such as the raw intergranular turbulent dispersion of turbulence flow flied relaying supervention, concussion, friction, water-swelling, dissolving and degradeds, thus makes the particle diameter of remaining macrobead starch be reduced further.
Then, mash from the ejection at a high speed of one-level reducing and expansion mouth, enters in the cavity of secondary contracting flared upper part under the effect of equipment internal pressure, and this process can make mash produce pressure release, and make the starch granules in mash produce Swelling Functions, be more conducive to starch granules and absorb moisture and make starch granules soluble in water.Meanwhile, because fire resistant alpha-diastase is to the Degradation of starch, thus the viscosity of mash is reduced.
In certain embodiments, enter mash in secondary reducing and expansion mouth upper chamber again through being arranged on cavity wall with the steam that oliquely downward form equally distributed secondary nozzle in inclination angle sprays into carry out directly moment Hybrid Heating.Mash after heating is from the ejection at a high speed of secondary reducing and expansion mouth, produce the pressure release of mash, to make in mash residual not in step before starch granules that is broken and refinement again produce Swelling Functions, impel it to heat up further, water suction, expanded, dissolve and degrade.Like this, the starch granules in mash just can reach whole dissolved states.In certain embodiments, the mash flowed out from the injection reducing and expansion mouth sprayed below broken refining device is sent into after-ripening device under pressure and carry out Operation for liquefaction.In whole operating process, macrobead starch in mash achieves complicated physics fragmentation refinement and the biochemical degradation processes such as expanded, broken, the refinement of water suction, dissolving, decomposition and intensification at short notice substantially, wherein, fire resistant alpha-diastase is all playing the effect of degraded starch in whole operating process, the viscosity of mash is effectively reduced, thus effectively raises the ability of the conveying of mash.
Wherein, the liquid level of the broken refining device inside of this injection, mash flow, steam flow, mash temperature all adopts robot control system(RCS) to control, simultaneously, also tensimeter is installed at the top of the broken refining device of this novel injection and bottom, thermometer, the devices such as vision slit visor and thief hole, control in the scope of about 90 DEG C to about 95 DEG C for the mash temperature after one-level is sprayed broken refinement, to control in the scope of about 105 DEG C to about 110 DEG C from spraying the mash temperature that below broken refining device, two-stage injection reducing and expansion mouth ejects, then after decompression evaporator, the temperature of mash is made to be reduced in the scope of about 90 DEG C and about 100 DEG C, and send in after-ripening device and carry out Operation for liquefaction, the viscosity number of now mash is detected in the scope of 60mPa.s to 100mPa.s through sampling.
As shown in Figure 1, in step s 107, liquefaction processing is carried out to the second mash, and in step S109, saccharification process is carried out to form the 3rd mash to the second mash after liquefaction processing subsequently.The mash spraying the discharge of broken refining device bottom pressure relief reducing and expansion mouth is sent in after-ripening device and liquefies, control liquefaction temperature at about 90 DEG C in the scope of 100 DEG C, liquefying time 90min, sampling detects the viscosity number fluctuation of mash within the scope of 30 ~ 50mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds the saccharifying enzyme of about 100u/g to about 130u/g raw material, the saccharification regular hour after stirring, when the DE value of detection mash is between 14 to 18, be saccharification to terminate.
As shown in Figure 1, in step S111, the 3rd mash is fermented.In certain embodiments, mash obtained in step S109 is cooled to ethanol fermentation temperature and send into fermentation workshop section.Because the operation of this step is with to use mash to prepare the technique of ethanol in prior art identical, therefore in order to simply with clearly object, will not repeat at this.The concentration of the ethanol prepared by the present invention is 16% ~ 18% (volume).
Although employ the broken refining device of novel injection to carry out gelatinization and liquefaction processing to macrobead starchy material mash in description herein, this is only an example.It will be understood by those skilled in the art that and any other machinery can be used to implement gelatinization and liquefaction processing., should be appreciated that meanwhile, other can be used to comprise and method or the technique that one-level sprays the broken refinement of broken refinement, degraded and two-stage injection is carried out to macrobead starchy material mash, to reach the effect identical with using the broken refining device of novel injection.It will be understood by those skilled in the art that and above-mentionedly can carry out the machinery of gelatinization and liquefaction processing, technological process control all within protection scope of the present invention to macrobead starchy material mash.
By the starchy material that method of the present invention can effectively utilize granularity larger, the starchy material that granularity can only be used to be about about 1.2mm in prior art is promoted to the starchy material utilizing about 3.0mm to about 3.5mm.Meanwhile, owing to employing macrobead starchy material, therefore, effectively material-water ratio is brought up to about 1:2.0 by about 1:2.8.Macrobead starch in mash can be made in high shear power by method of the present invention, mutual impact force, frictional force, under the effect of the power such as bulging force and the continuous Degradation of fire resistant alpha-diastase to obtain moment effective broken, refinement and dissolving, under the condition not adopting high temperature long time treatment, achieve the moment of macrobead starch in mash fluid broken, refinement, expanded, water-swelling, dissolve, the moment temperature-rise period of degraded and mash, for ensuing liquefaction and saccharifying carry out smoothly create favourable condition, and effectively raise the concentration of the final ethanol produced further.
Embodiment 1
1, raw material pulverizing: adopt the dry raw material of cassava to send into pulverizer feed(raw material)inlet from feed bin through rotary conveyor or chapelet, the hole diameter of sieve (perforated) plate of pulverizer is selected to be 4mm, after crushed the raw material powder pulverized is sieved, accounting for raw material powder total amount by the fine powder content of 1.2mm sieve aperture is 3.5%, accounting for raw material powder total amount by the fine powder content of 3.0mm sieve aperture is 11.8%, accounting for raw material powder total amount more than the macrobead content of 3.5mm sieve aperture is 1.5%, and wherein the macrobead of 3.0mm to 3.5mm particle diameter accounts for raw material powder total amount is 86.7%; Then material powder is sent into feed bin to keep in.
2, spice is pulverized: the recycle-water adopting distillation workshop section, carry out spice after cooling to 75 DEG C, the temperature after spice needs to reach 65 DEG C.Add fire resistant alpha-diastase 12u/g raw material powder in spice process, after being uniformly mixed, the viscosity that sampling detects mash is 120mPa.s, does not have an impact to the conveying of mash.Adopt mash transferpump to be sent into spray in broken refining device.
3, in the broken refining device of injection, fragmentation, refinement, instantaneously warming liquid chemical industry sequence are sprayed to macrobead starch mash.Adopting transferpump to send into macrobead starch mash in above-mentioned temporary storage tank sprays in broken refining device, and the nozzle place before mash delivers into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash sprays in broken refining device, this is the operation of one-level spray technology, spray broken refining device adopt 4 to liquidate the nozzle be arranged on same pitch circle sprays steam mash mixed solution, by experiment the mash sampling analysis after injection is obtained, the particle diameter of macrobead starch significantly reduces, wherein most of starch granules all obtains running through of moisture and dissolves, only have the starch granules less than 5% also not obtain moisture to run through, now by controlling the flow of mash and the flow of steam, the temperature of mash is controlled at 90 DEG C.
The steam of this mash again through spraying the jet orifice place bottom broken refining device sprays into, by mash together from the jet orifice sprayed bottom broken refining device ejection at a high speed, it is decompression diffuser tube below jet orifice, obtain from the mash of decompression diffusion mouth of pipe ejection through sampling analysis, the granular starch in mash all refinement dissolves, now, by controlling the flow of mash and the flow of steam, make the temperature of mash control at 105 DEG C, now, the viscosity that sampling detects mash is 90mPa.s.
4, the liquefaction of mash, saccharification: send in after-ripening device liquefy spraying mash that broken refining device bottom pressure relief diffuser tube discharges, controlling liquefaction temperature is 95 DEG C, liquefying time 90min, the viscosity that sampling detects mash is 45mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds saccharifying enzyme 120u/g raw material, the saccharification regular hour after stirring, detect the DE value of mash 14 time, terminate saccharification.
5, the fermentation of mash: the mash after saccharification is delivered to feeding fermentation workshop section and ferment, the alcohol concn obtained after having fermented is 16% (volume).
Embodiment 2
1, raw material pulverizing: send into pulverizer feed(raw material)inlet from feed bin through rotary conveyor or chapelet as adopted the dry raw material of cassava, the hole diameter of sieve (perforated) plate of pulverizer is selected to be 4mm, after crushed the raw material powder pulverized is sieved, accounting for raw material powder total amount by the fine powder content of 1.2mm sieve aperture is 3.5%, accounting for raw material powder total amount by the fine powder content of 3.0mm sieve aperture is 11.8%, accounting for raw material powder total amount more than the macrobead content of 3.5mm sieve aperture is 1.5%, and wherein the macrobead of 3.0mm to 3.5mm particle diameter accounts for raw material powder total amount is 86.7%; Then material powder is sent into feed bin to keep in.
2, spice is pulverized: the recycle-water adopting distillation workshop section, carry out spice after cooling to 75 DEG C, the temperature after spice needs to reach 65 DEG C, if the mash temperature after spice is lower than 65 DEG C, can adopt indirect steam heating method that mash is heated to this temperature.Add fire resistant alpha-diastase 8u/g raw material powder in spice process, after being uniformly mixed, the viscosity number that sampling detects mash is 150mPa.s, does not have an impact to the conveying of mash.Mash transferpump is adopted to be sent in the broken refining device of novel injection.
3, spraying broken refining device sprays broken to macrobead starch mash, refinement, warming liquid chemical industry sequence instantaneously: adopt transferpump to send into macrobead starch mash in above-mentioned temporary storage tank and spray in broken refining device, and the nozzle place before mash delivers into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash sprays in broken refining device, this is the operation of one-level spray technology, spray broken refining device adopt 2 to liquidate the nozzle be arranged on same pitch circle sprays steam mash mixed solution, by experiment the mash sampling analysis after injection is obtained, the particle diameter of macrobead starch significantly reduces, wherein most of starch granules all obtains running through of moisture and dissolves, only have the starch granules less than 15% also not obtain moisture to run through, now by controlling the flow of mash and the flow of steam, the temperature of mash is controlled at 95 DEG C.
The steam of this mash again through spraying the jet orifice place bottom broken refining device sprays into, by mash together from the jet orifice sprayed bottom broken refining device ejection at a high speed, it is decompression diffuser tube below jet orifice, obtain from the mash of decompression diffusion mouth of pipe ejection through sampling analysis, granular starch in mash all refinement dissolves, now, by controlling the flow of mash and the flow of steam, the temperature of mash is made to control at 110 DEG C, the viscosity that sampling detects mash is about 100mPa.s, and mash conveying is very smooth.
4, the liquefaction of mash, saccharification: the mash spraying the discharge of broken refining device bottom pressure relief diffuser tube is sent in after-ripening device and liquefies, controlling liquefaction temperature is 95 DEG C, liquefying time 90min, the viscosity number that sampling detects mash is 50mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds saccharifying enzyme 120u/g raw material, the saccharification regular hour after stirring, detect the DE value of mash 16 time, be saccharification to terminate, then mash is cooled to ethanol fermentation temperature and send into fermentation workshop section.
5, the fermentation of mash: the mash after saccharification is delivered to feeding fermentation workshop section and ferment, the alcohol concn obtained after having fermented is 17% (volume).
Embodiment 3
1, raw material pulverizing: send into pulverizer feed(raw material)inlet from feed bin through rotary conveyor or chapelet as adopted the dry raw material of cassava, the hole diameter of sieve (perforated) plate of pulverizer is selected to be 6mm, after crushed the raw material powder pulverized is sieved, accounting for raw material powder total amount by the fine powder content of 1.2mm sieve aperture is 2.5%, accounting for raw material powder total amount by the fine powder content of 3.0mm sieve aperture is 10.8%, accounting for raw material powder total amount more than the macrobead content of 3.5mm sieve aperture is 2.0%, and wherein the macrobead of 3.0 ~ 3.5mm particle diameter accounts for raw material powder total amount is 87.2%; Then material powder is sent into feed bin to keep in.
2, spice is pulverized: the recycle-water adopting distillation workshop section, carry out spice after cooling to 75 DEG C, the temperature after spice needs to reach 65 DEG C, if the mash temperature after spice is lower than 65 DEG C, can adopt indirect steam heating method that mash is heated to this temperature.Add fire resistant alpha-diastase 10u/g raw material powder in spice process, after being uniformly mixed, the viscosity that sampling detects mash is about 120mPa.s, does not have an impact to the conveying of mash.Mash transferpump is adopted to be sent in the broken refining device of novel injection.
3, spraying broken refining device sprays broken to macrobead starch mash, refinement, warming liquid chemical industry sequence instantaneously: adopt transferpump to send into macrobead starch mash in above-mentioned temporary storage tank and spray in broken refining device, and the nozzle place before mash delivers into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash sprays in broken refining device, this is the operation of one-level spray technology, spray broken refining device adopt 6 to liquidate the nozzle be arranged on same pitch circle sprays steam mash mixed solution, by experiment the mash sampling analysis after injection is obtained, the particle diameter of macrobead starch significantly reduces, wherein most of starch granules all obtains running through of moisture and dissolves, only have the starch granules less than 1.5% also not obtain moisture to run through, now by controlling the flow of mash and the flow of steam, the temperature of mash is controlled at 95 DEG C.
The steam of this mash again through spraying the jet orifice place bottom broken refining device sprays into, by mash together from the jet orifice sprayed bottom broken refining device ejection at a high speed, it is decompression diffuser tube below jet orifice, obtain from the mash of decompression diffusion mouth of pipe ejection through sampling analysis, the granular starch in mash all refinement dissolves, now, by controlling the flow of mash and the flow of steam, make the temperature of mash control at 110 DEG C, the viscosity that sampling detects mash is about 80mPa.s, and mash conveying is very smooth.
4, the liquefaction of mash, saccharification: the mash spraying the discharge of broken refining device bottom pressure relief diffuser tube is sent in after-ripening device and liquefies, controlling liquefaction temperature is 95 DEG C, liquefying time 90min, the viscosity number that sampling detects mash is 35mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds saccharifying enzyme 120u/g raw material, the saccharification regular hour after stirring, detect the DE value of mash 17 time, be saccharification to terminate, then mash is cooled to ethanol fermentation temperature and send into fermentation workshop section.
5, the fermentation of mash: the mash after saccharification is delivered to feeding fermentation workshop section and ferment, the alcohol concn obtained after having fermented is 18% (volume).
Embodiment 4
1, raw material pulverizing: send into pulverizer feed(raw material)inlet from feed bin through rotary conveyor or chapelet as adopted the dry raw material of cassava, the hole diameter of sieve (perforated) plate of pulverizer is selected to be 8mm, after crushed the raw material powder pulverized is sieved, accounting for raw material powder total amount by the fine powder content of 1.2mm sieve aperture is 2.0%, accounting for raw material powder total amount by the fine powder content of 3.0mm sieve aperture is 8.5%, accounting for raw material powder total amount more than the macrobead content of 3.5mm sieve aperture is 2.5%, and wherein the macrobead of 3.0 ~ 3.5mm particle diameter accounts for raw material powder total amount is 89.0%; Then material powder is sent into feed bin to keep in.
2, spice is pulverized: the recycle-water adopting distillation workshop section, carry out spice after cooling to 75 DEG C, the temperature after spice needs to reach 65 DEG C, if the mash temperature after spice is lower than 65 DEG C, can adopt indirect steam heating method that mash is heated to this temperature.Add fire resistant alpha-diastase 8u/g raw material powder in spice process, after being uniformly mixed, sampling detects the viscosity fluctuation of mash at about 100mPa.s, does not have an impact to the conveying of mash.Mash transferpump is adopted to be sent in the broken refining device of novel injection.
3, spraying broken refining device sprays broken to macrobead starch mash, refinement, warming liquid chemical industry sequence instantaneously: adopt transferpump to send into macrobead starch mash in above-mentioned temporary storage tank and spray in broken refining device, and the nozzle place before mash delivers into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash sprays in broken refining device, this is the operation of one-level spray technology, spray broken refining device adopt 2 to liquidate the nozzle be arranged on same pitch circle sprays steam mash mixed solution, by experiment the mash sampling analysis after injection is obtained, the particle diameter of macrobead starch significantly reduces, wherein most of starch granules all obtains running through of moisture and dissolves, only have the starch granules less than 12% also not obtain moisture to run through, now by controlling the flow of mash and the flow of steam, the temperature of mash is controlled at 95 DEG C.
The steam of this mash again through spraying the jet orifice place bottom broken refining device sprays into, by mash together from the jet orifice sprayed bottom broken refining device ejection at a high speed, it is decompression diffuser tube below jet orifice, obtain from the mash of decompression diffusion mouth of pipe ejection through sampling analysis, the granular starch in mash all refinement dissolves, now, by controlling the flow of mash and the flow of steam, make the temperature of mash control at 110 DEG C, the viscosity that sampling detects mash is about 90mPa.s, and mash conveying is very smooth.
4, the liquefaction of mash, saccharification: the mash spraying the discharge of broken refining device bottom pressure relief diffuser tube is sent in after-ripening device and liquefies, controlling liquefaction temperature is 95 DEG C, liquefying time 90min, the viscosity number that sampling detects mash is 45mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds saccharifying enzyme 120u/g raw material, the saccharification regular hour after stirring, detect the DE value of mash 18 time, be saccharification to terminate, then mash is cooled to ethanol fermentation temperature and send into fermentation workshop section.
5, the fermentation of mash: the mash after saccharification is delivered to feeding fermentation workshop section and ferment, the alcohol concn obtained after having fermented is 16% (volume).
Embodiment 5
1, raw material pulverizing: send into pulverizer feed(raw material)inlet from feed bin through rotary conveyor or chapelet as adopted the dry raw material of cassava, the hole diameter of sieve (perforated) plate of pulverizer is selected to be 6mm, after crushed the raw material powder pulverized is sieved, accounting for raw material powder total amount by the fine powder content of 1.2mm sieve aperture is 2.5%, accounting for raw material powder total amount by the fine powder content of 3.0mm sieve aperture is 10.8%, accounting for raw material powder total amount more than the macrobead content of 3.5mm sieve aperture is 2.0%, and wherein the macrobead of 3.0 ~ 3.5mm particle diameter accounts for raw material powder total amount is 87.2%; Then material powder is sent into feed bin to keep in.
2, spice is pulverized: the recycle-water adopting distillation workshop section, carry out spice after cooling to 75 DEG C, the temperature after spice needs to reach 65 DEG C, if the mash temperature after spice is lower than 65 DEG C, can adopt indirect steam heating method that mash is heated to this temperature.Add fire resistant alpha-diastase 12u/g raw material powder in spice process, after being uniformly mixed, the viscosity that sampling detects mash is about 90mPa.s, does not have an impact to the conveying of mash.Mash transferpump is adopted to be sent in the broken refining device of novel injection.
3, spraying broken refining device sprays broken to macrobead starch mash, refinement, warming liquid chemical industry sequence instantaneously: adopt transferpump to send into macrobead starch mash in above-mentioned temporary storage tank and spray in broken refining device, and the nozzle place before mash delivers into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash sprays in broken refining device, this is the operation of one-level spray technology, spray broken refining device adopt 2 to liquidate the nozzle be arranged on same pitch circle sprays steam mash mixed solution, by experiment the mash sampling analysis after injection is obtained, the particle diameter of macrobead starch significantly reduces, wherein most of starch granules all obtains running through of moisture and dissolves, only have the starch granules less than 12.5% also not obtain moisture to run through, now by controlling the flow of mash and the flow of steam, the temperature of mash is controlled at 95 DEG C.
The steam of this mash again through spraying the jet orifice place bottom broken refining device sprays into, by mash together from the jet orifice sprayed bottom broken refining device ejection at a high speed, it is decompression diffuser tube below jet orifice, obtain from the mash of decompression diffusion mouth of pipe ejection through sampling analysis, the granular starch in mash all refinement dissolves, now, by controlling the flow of mash and the flow of steam, make the temperature of mash control at 110 DEG C, the viscosity that sampling detects mash is about 70mPa.s, and mash conveying is very smooth.
4, the liquefaction of mash, saccharification: the mash spraying the discharge of broken refining device bottom pressure relief diffuser tube is sent in after-ripening device and liquefies, controlling liquefaction temperature is 95 DEG C, liquefying time 90min, the viscosity number that sampling detects mash is 48mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds saccharifying enzyme 120u/g raw material, the saccharification regular hour after stirring, detect the DE value of mash 14 time, be saccharification to terminate, then mash is cooled to ethanol fermentation temperature and send into fermentation workshop section.
5, the fermentation of mash: the mash after saccharification is delivered to feeding fermentation workshop section and ferment, the alcohol concn obtained after having fermented is 18% (volume).
Embodiment 6
1, raw material pulverizing: send into pulverizer feed(raw material)inlet from feed bin through rotary conveyor or chapelet as adopted the dry raw material of cassava, the hole diameter of sieve (perforated) plate of pulverizer is selected to be 8mm, after crushed the raw material powder pulverized is sieved, accounting for raw material powder total amount by the fine powder content of 1.2mm sieve aperture is 2.0%, accounting for raw material powder total amount by the fine powder content of 3.0mm sieve aperture is 8.5%, accounting for raw material powder total amount more than the macrobead content of 3.5mm sieve aperture is 2.5%, and wherein the macrobead of 3.0 ~ 3.5mm particle diameter accounts for raw material powder total amount is 89.0%; Then material powder is sent into feed bin to keep in.
2, spice is pulverized: the recycle-water adopting distillation workshop section, carry out spice after cooling to 75 DEG C, the temperature after spice needs to reach 65 DEG C, if the mash temperature after spice is lower than 65 DEG C, can adopt indirect steam heating method that mash is heated to this temperature.Add fire resistant alpha-diastase 12u/g raw material powder in spice process, after being uniformly mixed, sampling detects the viscosity fluctuation of mash at about 80mPa.s, does not have an impact to the conveying of mash.Mash transferpump is adopted to be sent in the broken refining device of novel injection.
3, spraying broken refining device sprays broken to macrobead starch mash, refinement, warming liquid chemical industry sequence instantaneously: adopt transferpump to send into macrobead starch mash in above-mentioned temporary storage tank and spray in broken refining device, and the nozzle place before mash delivers into the broken refining device of injection passes into steam-jet siphon, heating steam is sprayed into together with mash sprays in broken refining device, this is the operation of one-level spray technology, spray broken refining device adopt 2 to liquidate the nozzle be arranged on same pitch circle sprays steam mash mixed solution, by experiment the mash sampling analysis after injection is obtained, the particle diameter of macrobead starch significantly reduces, wherein most of starch granules all obtains running through of moisture and dissolves, only have the starch granules less than 10% also not obtain moisture to run through, now by controlling the flow of mash and the flow of steam, the temperature of mash is controlled at 90 DEG C.
The steam of this mash again through spraying the jet orifice place bottom broken refining device sprays into, by mash together from the jet orifice sprayed bottom broken refining device ejection at a high speed, it is decompression diffuser tube below jet orifice, obtain from the mash of decompression diffusion mouth of pipe ejection through sampling analysis, the granular starch in mash all refinement dissolves, now, by controlling the flow of mash and the flow of steam, make the temperature of mash control at 105 DEG C, the viscosity that sampling detects mash is about 60mPa.s, and mash conveying is very smooth.
4, the liquefaction of mash, saccharification: the mash spraying the discharge of broken refining device bottom pressure relief diffuser tube is sent in after-ripening device and liquefies, controlling liquefaction temperature is 95 DEG C, liquefying time 90min, the viscosity number that sampling detects mash is 45mPa.s, after liquefaction terminates, adopting the method for vacuum cooling mash to be cooled to 62 DEG C sends in saccharifying tank, stream adds the pH value that the vitriol oil regulates mash, stream adds saccharifying enzyme 120u/g raw material, the saccharification regular hour after stirring, detect the DE value of mash 18 time, be saccharification to terminate, then mash is cooled to ethanol fermentation temperature and send into fermentation workshop section.
5, the fermentation of mash: the mash after saccharification is delivered to feeding fermentation workshop section and ferment, the alcohol concn obtained after having fermented is 18% (volume).
Although describe in detail embodiments of the invention and advantage thereof, should be appreciated that, when not deviating from the spirit and scope of the present invention that claims limit, various change, replacement and change can have been made to the present invention.And, the specific embodiment of the technique that the expection of the scope of the application is not limited to describe in this specification sheets, machine, preparation, material component, instrument, method and step.To understand easily as those of ordinary skill in the art, according to the present invention, can utilize existing or from now on by exploitation, the corresponding embodiment that is used for describing with the present invention performs substantially identical function or obtains the technique of basic identical result, machine, preparation, material component, instrument, method or step.Correspondingly, claims are intended to these technique, machine, preparation, material component, instrument, method or step to be included in their scope.

Claims (10)

1. prepare a method for ethanol, it is characterized in that, comprising:
Starch material is pulverized to form macrobead starchy material;
Add water in described macrobead starchy material and fire resistant alpha-diastase mix and blend to form the first mash;
Gelatinization process is carried out to form the second mash to described first mash;
Liquefaction isothermal holding;
Saccharification process is carried out to form the 3rd mash to described second mash after liquefaction isothermal holding;
Described 3rd mash is fermented.
2. method according to claim 1, is characterized in that, carries out gelatinization process comprise further with the step forming the second mash described first mash:
Implement one-level and spray broken refinement;
Described macrobead starchy material is degraded; And
Implement the broken refinement of two-stage injection.
3. method according to claim 1, is characterized in that, uses the broken refining device of injection to carry out gelatinization process to form the second mash to described first mash.
4. according to the method in any one of claims 1 to 3, it is characterized in that, the viscosity number of described second mash is in the scope of 60mPa.s to 100mPa.s.
5. method according to claim 1, it is characterized in that, starch material is being pulverized to be formed in the step of macrobead starchy material, after described pulverising step, the granularity of described macrobead starchy material is 3.0mm to 3.5mm, the viscosity number of described first mash is in the scope of 80mPa.s to 150mPa.s, and described starch material comprises corn and/or cassava.
6. method according to claim 1, is characterized in that, the add-on of described fire resistant alpha-diastase is 8u/g to 12u/g.
7. method according to claim 1, is characterized in that:
Described liquefaction isothermal holding is implemented in after-ripening device;
Lower the temperature in vacuum cooling system;
Described saccharification process is implemented in saccharifying tank.
8. method according to claim 7, is characterized in that, the temperature of carrying out in ripe device being in the rear incubated, in the scope of 90 DEG C to 100 DEG C, is cooled in the scope of 55 DEG C to 65 DEG C in described vacuum cooling system.
9. method according to claim 7, is characterized in that, the time of described liquefaction processing is in the scope of 80 minutes to 100 minutes.
10. method according to claim 7, is characterized in that, when the DE value of described mash is in the scope of 14 to 18, stops described saccharification step.
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CN109528956A (en) * 2018-12-27 2019-03-29 郑州大学第附属医院 It is a kind of to reduce Steroid-resistant nephrotic syndrome patient to the drug of Hormone refractory

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CN108103112A (en) * 2018-02-09 2018-06-01 广东中科天元新能源科技有限公司 A kind of technique that alcohol fuel is produced as raw material using cornstarch matter
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