CN114250251B - Method for producing ethanol - Google Patents
Method for producing ethanol Download PDFInfo
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- CN114250251B CN114250251B CN202011010785.2A CN202011010785A CN114250251B CN 114250251 B CN114250251 B CN 114250251B CN 202011010785 A CN202011010785 A CN 202011010785A CN 114250251 B CN114250251 B CN 114250251B
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 210
- 238000004519 manufacturing process Methods 0.000 title description 11
- 235000013312 flour Nutrition 0.000 claims abstract description 116
- 241000209140 Triticum Species 0.000 claims abstract description 86
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- 229920002472 Starch Polymers 0.000 claims abstract description 58
- 239000008107 starch Substances 0.000 claims abstract description 56
- 235000019698 starch Nutrition 0.000 claims abstract description 56
- 238000000855 fermentation Methods 0.000 claims abstract description 54
- 230000004151 fermentation Effects 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 54
- 235000021329 brown rice Nutrition 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 235000013336 milk Nutrition 0.000 claims abstract description 23
- 239000008267 milk Substances 0.000 claims abstract description 23
- 210000004080 milk Anatomy 0.000 claims abstract description 23
- 238000004821 distillation Methods 0.000 claims abstract description 17
- 235000007164 Oryza sativa Nutrition 0.000 claims description 65
- 235000009566 rice Nutrition 0.000 claims description 65
- 239000007788 liquid Substances 0.000 claims description 46
- 238000003825 pressing Methods 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 18
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- 230000008901 benefit Effects 0.000 abstract description 5
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- 238000002791 soaking Methods 0.000 description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
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- 229920000945 Amylopectin Polymers 0.000 description 3
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 3
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 2
- 102000013142 Amylases Human genes 0.000 description 2
- 108010065511 Amylases Proteins 0.000 description 2
- 229920000856 Amylose Polymers 0.000 description 2
- 241000228245 Aspergillus niger Species 0.000 description 2
- 108010028688 Isoamylase Proteins 0.000 description 2
- 241000235527 Rhizopus Species 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
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- 244000063299 Bacillus subtilis Species 0.000 description 1
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- 229920000742 Cotton Polymers 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
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- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 101001052076 Homo sapiens Maltase-glucoamylase Proteins 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
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- 102100024295 Maltase-glucoamylase Human genes 0.000 description 1
- 244000113306 Monascus purpureus Species 0.000 description 1
- 235000002322 Monascus purpureus Nutrition 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 241000303962 Rhizopus delemar Species 0.000 description 1
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- 244000138286 Sorghum saccharatum Species 0.000 description 1
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
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- 239000000295 fuel oil Substances 0.000 description 1
- 229930182830 galactose Natural products 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
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- 229940057059 monascus purpureus Drugs 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
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- 230000035899 viability Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/06—Ethanol, i.e. non-beverage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
- B01D3/003—Rectification of spirit
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Biotechnology (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- 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 relates to the field of microbial fermentation, and discloses a method for preparing ethanol, which comprises the following steps: sequentially carrying out enzymolysis, fermentation and distillation on starch milk containing a starchy raw material, wherein the starchy raw material is at least partially derived from brown rice and flour, the grain size of the flour is less than or equal to 0.9mm, and the weight of the flour with the grain size of 0.25-0.42mm accounts for 60-80% of the total weight of the flour. The method does not involve a process for extracting wheat gluten, can effectively improve the starch wine yield and reduce the alcohol grain consumption; the liquefied product obtained by the method has the advantages of low viscosity, low content of total sugar and reducing sugar in the fermentation product, good color and high yield; while preventing clogging and wear of the equipment.
Description
Technical Field
The invention relates to the field of microbial fermentation, in particular to a method for preparing ethanol.
Background
Fuel ethanol is a clean burning high octane fuel, and is a renewable energy source. Ethanol is not only an excellent fuel, but also an excellent fuel improver. Ethanol is an oxygenation agent of fuel oil, so that the internal oxygen of gasoline is increased, and the gasoline is fully combusted, thereby achieving the purposes of energy conservation and environmental protection.
Fuel ethanol is ethanol which is obtained from biomass as a raw material through biological fermentation and other ways and can be used as fuel. Fuel ethanol production technology is divided into two types, namely a first generation and a second generation, according to the difference of the raw materials used. The first generation fuel ethanol technology is to produce fuel ethanol by taking sugar and starch crops as raw materials, wherein the main raw materials are aged grains, cassava, corn, sweet sorghum, sweet potatoes and other starch; the second generation fuel ethanol technology is to produce ethanol by taking lignocellulose as a raw material. The high cost of producing ethanol by lignocellulose restricts the main raw materials of the fuel ethanol in China to be corn, cassava, aged grain and the like at present.
The stock quantity of the aged rice and wheat in China is huge, and a large amount of aged grains are needed to be treated. In the industry, the aged rice is generally used for producing fuel ethanol, and the aged rice full-crushing process has the defects of greatly reduced productivity, large equipment abrasion, poor fermentation index, easy blockage of a distillation tower, limited feed yield and the like. The main process engineering for producing fuel ethanol by using aged wheat in the industry is to mix wheat gluten extracted from wheat with cassava and other cereal raw materials to produce fuel ethanol, and distillers waste mash is subjected to full-grain high-temperature anaerobic process treatment without co-production of feed. A small part of edible alcohol production factories take wheat as raw materials, and after wheat bran and wheat gluten are extracted, wheat starch milk is utilized for alcohol production. There are also some plants that utilize the wheat starch byproduct B starch for alcoholic fermentation. But all of this process is based on extraction of wheat bran and gluten. Because the technological process for extracting bran and wheat gluten is complex, if new technological lines are invested, the investment limit is huge, and when the super standard wheat is processed, the equipment and devices are idle. And lack of economic viability.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a method for preparing ethanol, which does not relate to a process for extracting wheat gluten, and has the advantages of higher starch wine yield, lower alcohol grain consumption, lower viscosity of liquefied products, lower content of total sugar and reducing sugar of fermentation residues, good DDGS color, higher yield and equipment blockage and abrasion prevention.
In order to achieve the above object, the present invention provides a method for preparing ethanol, comprising: sequentially carrying out enzymolysis, fermentation and distillation on starch milk containing a starchy raw material, wherein the starchy raw material is at least partially derived from brown rice and flour, the grain size of the flour is less than or equal to 0.9mm, and the weight of the flour with the grain size of 0.25-0.42mm accounts for 60-80% of the total weight of the flour.
By adopting the technical scheme of the invention, the process of extracting wheat gluten is not involved, the viscosity of liquefied products, the water content of filter residues, the total sugar content of fermentation residues, the reducing sugar content of fermentation residues and the alcohol grain consumption can be effectively reduced, the blockage of distillation equipment and the abrasion of the equipment in the distillation process can be effectively prevented, and the starch liquor yield (ethanol yield) and the DDGS yield are effectively improved; the technical scheme of the invention can reasonably utilize the wheat and the rice, and improves the utilization value of grains and the enterprise benefit. By adopting the most preferred embodiment of the invention, the wine yield of the starch can reach 51.1 percent, and the consumption of the alcohol grain can be as low as 3.33g/g.
The invention is favorable for solving the problems in the production of fuel ethanol by aged rice and aged wheat, is a breakthrough progress, solves the limitations in equipment, technology, quality, productivity and the like in the production process of fuel ethanol, and is an important means for stabilizing and improving the quality of products and improving the yield. The method has important significance for relieving the pressure of the aging grain depot, solving the shortage of raw materials, reducing the production cost, improving the enterprise benefit and being popularized in the fuel ethanol industry.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The invention provides a method for preparing ethanol, which comprises the following steps: sequentially carrying out enzymolysis, fermentation and distillation on starch milk containing a starchy raw material, wherein the starchy raw material is at least partially derived from brown rice and flour, the grain size of the flour is less than or equal to 0.9mm, and the weight of the flour with the grain size of 0.25-0.42mm accounts for 60-80% of the total weight of the flour.
In the present invention, it is understood that brown rice is whole grain rice obtained by husking rice without processing or with less processing, and is composed of rice bran, embryo and endosperm. Flour refers to a powder obtained by removing bran from wheat.
In the present invention, preferably, the enzymolysis method includes liquefying starch milk containing starchiness raw material to obtain liquefied product, and saccharifying the liquefied product.
In the present invention, the quality of the brown rice is not particularly limited, and for example, the brown rice may be new or old, which does not affect the effect of the present invention. The quality of the flour is not particularly limited, and for example, can be a flour prepared from fresh grains or a flour prepared from aged grains, which does not affect the effect of the present invention. The method of the invention uses the aged grains to prepare the starchy raw material, which can reasonably utilize the aged grains and lead the aged grains to generate higher added value. The storage time of the aged grain can be within a wide range, such as aged grain stored for more than 3 years (especially 3-5 years).
In the invention, because the protein content of the wheat is higher, the viscosity of the liquefied product obtained by liquefaction is higher and is unfavorable for fermentation and ethanol purification, in order to control the viscosity of materials to be at a lower level, the viscosity of the liquefied product is preferably not higher than 120mPa.s, more preferably 85-110mPa.s, a higher amount of enzyme is needed, and one preferable amount is as follows: the amount of enzyme used for the liquefaction is 6 to 30U (enzyme activity unit) relative to 1g of the starchy material. The definition of the enzyme activity unit of the enzyme is as follows: the amount of enzyme required to convert 1 mg of starch to reducing sugar in 1 minute at a pH of 6 and a temperature of 70℃is one enzyme activity unit.
In the present invention, the type of the enzyme used for the liquefaction is not particularly limited, and may be an enzyme conventionally used in the art, and in order to enhance the effect of the liquefaction, the enzyme used for the liquefaction is preferably an amylase. Amylases typically include alpha-amylase, beta-amylase and isoamylase, more preferably alpha-amylase.
Alpha-amylase, also known as starch 1, 4-dextrinase, liquefying enzyme, is capable of randomly and irregularly cleaving alpha-1, 4-glycosidic bonds within the starch chain, hydrolyzing starch into maltose, oligosaccharides containing 6 glucose units and branched oligosaccharides. The microorganisms producing the enzyme mainly include bacillus subtilis, aspergillus niger, aspergillus oryzae, rhizopus and the like.
Beta-amylase is also called starch 1, 4-maltosidase, and can cleave 1, 4-glycosidic bonds from the non-reducing end of starch molecules to produce maltose. The products of this enzyme action on starch are maltose and limiting dextrins.
The isoamylase is also called starch alpha-1, 6-glucosidase and branching enzyme, and acts on alpha-1, 6-glycosidic bond at branching point of amylopectin molecule to cut the whole side chain of amylopectin into amylose.
In the present invention, the liquefaction method is not particularly limited, and in order to further enhance the effect of the liquefaction, the liquefaction is preferably jet liquefaction.
In the present invention, in order to further enhance the liquefaction effect, the temperature of the jet liquefaction is preferably 90 to 110 ℃ (for example, 90 ℃, 92 ℃, 94 ℃, 96 ℃, 98 ℃, 100 ℃, 102 ℃, 104 ℃, 106 ℃, 108 ℃, 110 ℃, or any value between the above values), more preferably 90 to 95 ℃.
In the present invention, in order to further enhance the liquefaction effect, the pH of the jet liquefaction is preferably 5 to 6.5 (for example, may be 5, 5.3, 5.5, 5.7, 5.9, 6.1, 6.3, 6.5, or any value between the above values), more preferably 5.5 to 6.
In the present invention, in order to further enhance the liquefaction effect, the jet liquefaction time is preferably 90 to 130min (for example, may be 90min, 95min, 100min, 105min, 110min, 115min, 120min, 125min, 130min, or any value between the above values), and more preferably 110 to 125min.
In the present invention, the saccharification method is not particularly limited, and may be performed by a conventionally used method as long as the saccharification liquid obtained by saccharification can be allowed to ferment normally after being inoculated with a fermentation strain, for example, the saccharification enzyme used for saccharification is directly added to the liquefied product for saccharification.
In the present invention, the amount of the saccharifying enzyme may be selected within a wide range, and in order to enhance the effect of saccharification, it is preferable that the amount of the saccharifying enzyme used for saccharification is 80 to 150U, more preferably 100 to 130U, relative to 1g of the starchy material. The source of the saccharifying enzyme is not particularly limited, and for example, the saccharifying enzyme can be commercially available, and may be, for example, a complex saccharifying enzyme purchased from jeidae, su Hong 474 saccharifying enzyme of novelin, su Hong 475 saccharifying enzyme, saccharifying enzyme of vinca-coronarism, or the like. The definition of the enzyme activity unit of the enzyme is as follows: 1ml of enzyme solution or 1g of enzyme powder is hydrolyzed for 1h to generate 1mg of glucose under the conditions of 40 ℃ and pH4.6, namely the unit of enzyme activity is shown as the following symbol: U/mL (or U/g).
The saccharifying enzyme is also called starch alpha-1, 4-glucosidase, and acts on the non-reducing end of starch molecule, and sequentially acts on alpha-1, 4-glycosidic bond in the starch molecule by taking glucose as a unit to generate glucose. Products after the saccharifying enzyme acts on the amylopectin include glucose and oligosaccharides with alpha-1, 6-glycosidic bonds; the product after the action on amylose is almost entirely glucose. The enzyme producing strain is mainly Aspergillus niger (Aspergillus left and Aspergillus awamori), rhizopus (Rhizopus niveus and Rhizopus delemar), endomycete, monascus purpureus, etc.
In the present invention, the pH of the saccharification may be selected within a wide range, and in order to enhance the saccharification effect, it is preferable that the pH of the saccharification is 4 to 5 (for example, may be 4, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, 4.9, 5, or any value between the above values), and more preferably 4.2 to 4.4.
In the present invention, the saccharification temperature may be selected within a wide range, and in order to enhance the saccharification effect, the saccharification temperature is preferably 55 to 65 ℃ (for example, 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, or any value between the above values), more preferably 59 to 61 ℃.
In the present invention, the saccharification time may be selected within a wide range, and in order to enhance the saccharification effect, the saccharification time is preferably 40 to 60 minutes.
In the present invention, in order to enhance the saccharification effect, the method preferably further comprises subjecting the liquefied product to solid-liquid separation prior to saccharification. The liquid phase obtained by solid-liquid separation is used for saccharification in the next step, and filter residues can be used for preparing vinasse protein feed.
In the present invention, the method of solid-liquid separation is not particularly limited, and may be a separation method conventionally used in the art, such as plate-and-frame filtration separation, press filtration separation, centrifugal separation, and the like.
In a particularly preferred embodiment of the present invention, the liquefied product to be subjected to solid-liquid separation further contains rice hulls in an amount of 2.5 to 21 wt% (for example, may be 2.5 wt%, 5 wt%, 7.5 wt%, 10 wt%, 12.5 wt%, 15 wt%, 17.5 wt%, 20 wt%, 21 wt%, or any value between any two groups) based on the total weight of the brown rice and the flour, more preferably 10 to 13.5 wt%. By adopting the particularly preferred embodiment, the solid-liquid separation is carried out by using the filter pressing, in the filter pressing process, the rice hulls can form a filter pressing filtering layer on the surface of the filter cloth, the filtering efficiency is improved, the water content of filter residues is reduced, substances such as rice hulls and proteins in the liquefied product are effectively removed, the influence of the rice hulls on equipment abrasion, blockage of distillation tower plates and heat exchange efficiency of a heat exchanger is effectively reduced or avoided, and the influence of substances with high viscosity such as proteins in wheat and rice on heat exchange and yeast metabolism is effectively reduced or avoided.
In the present invention, the hulls may be added alone or may be carried over from the addition of unhulled and/or partially dehulled rice. In the embodiment in which the rice hulls are added separately, the rice hulls may be added during the process of preparing the starch milk or may be added directly to the liquefied product obtained by the liquefaction.
Rice refers to the fruiting body of rice husk that has not been removed. The paddy in the present invention refers to rice.
In the present invention, the quality of the rice is not particularly limited, and for example, the rice may be new grain or old grain, which does not affect the effect of the present invention. The method of the invention uses the rice old grains to prepare the starchy raw materials, which can reasonably utilize the old grains and lead the old grains to generate higher added value. The storage time of the aged grain can be within a wide range, such as aged grain stored for more than 3 years (especially 3-5 years).
In the present invention, the particle size of the rice hulls is not particularly limited and may be selected within a wide range, and in order to enhance the effect of solid-liquid separation, it is preferable that the rice hulls are present in the liquefied product in a pulverized form, and the pulverized rice hulls pass through a sieve having a pore size of 1 to 2.5mm, preferably 1 to 1.5 mm.
In the present invention, in order to further enhance the effect of the press filtration, preferably, the conditions of the press filtration include: the working pressure is 0.4-0.65MPa, preferably 0.55-0.6MPa; the filter pressing time is 2-4h, preferably 3-4h.
It will be appreciated that in the case of filter pressing using a filter press apparatus, the initial feed flow rate, initial feed time and initial feed pressure are generally controlled first, and a filter layer is formed on the filter cloth of the filter press apparatus to further enhance the effect of the filter pressing, preferably the filter layer thickness of the filter pressing is 15 to 80mm, more preferably 33 to 39mm.
In the present invention, there is no particular limitation on the initial feed flow rate, the initial feed time and the initial feed pressure, as long as a uniform filter layer can be formed, for example, the initial feed flow rate is 5 to 80m 3 Preferably 25-35m 3 /h; the initial feeding time is 0.5-2.5h, preferably 1.8-2h; the initial feed pressure filtration pressure is 0.05-0.4MPa, preferably 0.08-0.2MPa.
In the present invention, in order to further enhance the effect of the press filtration, it is preferable that the filter membrane used for the press filtration has a pore size of 60 to 200 mesh, more preferably 80 to 120 mesh.
More preferably, the filter cloth is made of at least one material selected from nylon, polypropylene, terylene and cotton.
In the present invention, in order to further enhance the effect of the pressure filtration, the solid content of the liquefied product is preferably 15 to 30% by weight, more preferably 25 to 27% by weight.
In the present invention, the apparatus used for the press filtration is not particularly limited, and may be a press filtration apparatus conventionally used in the art, such as a plate and frame filter or a chamber filter press, preferably a chamber filter press.
In the present invention, preferably, the brown rice and the flour are used in such an amount that the weight ratio of the brown rice to the flour is 20 to 100:15, more preferably 40-90:15.
in a particularly preferred embodiment of the invention, the weight of the flour having a particle size in the range of 0.25-0.42mm is 65-75% of the total weight of the flour. With the preferred embodiment, the wheat bran removing effect can be more effectively improved.
In the present invention, in order to enhance the effects of solid-liquid separation, fermentation and ethanol purification, it is preferable that the starchy raw material is at least partially derived from rice, brown rice and flour, and more preferably, the starchy raw material is entirely derived from rice, brown rice and flour.
In the present invention, the rice may be rice from various places, for example, from the places of Hubei province, hunan province, jiangxi province, northeast province, guangxi province, anhui province, and the like.
In the present invention, in order to further improve the effects of solid-liquid and fermentation and ethanol purification, preferably, the rice, brown rice and flour are used in such amounts that the weight ratio of the rice, brown rice and flour is 10 to 60:25-75:15, more preferably 25-45:40-60:15, further preferably 30-35:50-55:15.
in the present invention, in order to enhance the effect of solid-liquid separation, the rice is preferably present in a pulverized form in starch milk. The rice may be pulverized by a conventional pulverizing method in the art, and the present invention is not particularly limited as long as the desired particle size of the present invention can be obtained.
In the present invention, in order to further enhance the effect of solid-liquid separation, it is preferable that the crushed rice pass through a sieve having a pore diameter of 1 to 2.5mm, preferably 1 to 1.5 mm.
In the present invention, the rice, brown rice and flour are preferably derived from aged grains, preferably aged grains stored for 3 years or more.
In the present invention, in order to enhance the liquefying effect, the starch milk preferably has a Baume of 12 to 15 DEG Bes, more preferably 13.5 to 14.5 DEG Bes. Wherein Baume is a method of representing the concentration of a solution: the Baume is immersed in the measured solution to obtain the Baume degree, which is expressed in terms of Bes.
In the present invention, the fermentation may be accomplished by methods conventional in the art. Among them, a microorganism capable of fermenting with monosaccharides (e.g., glucose and/or fructose) and/or oligosaccharides (e.g., sucrose and/or galactose) to produce ethanol may be used in the fermentation process of the present invention, and preferably, the microorganism used for the fermentation is yeast in order to further increase the ethanol yield and reduce the production of byproducts in the fermentation process. Preferably, the yeast is Saccharomyces cerevisiae because of its high ethanol tolerance.
In the present invention, in order to enhance the effect of fermentation, it is preferable that the yeast is inoculated in an amount such that the number of colonies per gram of the saccharified liquid is 1X 10 8 -1×10 9 cfu, more preferably 1X 10 8 -3×10 8 cfu。
In the present invention, the source of the yeast is not particularly limited, and for example, the yeast may be a commercially available yeast solid preparation such as dry yeast powder or a yeast strain such as Angel super Saccharomyces cerevisiae high activity dry yeast, las 12 (Rasse XII) yeast, K-type yeast, nanyang five-type yeast (1300) and Nanyang hybrid yeast (1308).
In the present invention, the method for inoculating the yeast is not particularly limited, and the yeast may be inoculated by a method conventional in the art, for example, 10 to 50% by volume of a yeast seed solution is added to the saccharifying solution based on the volume of the saccharifying solution, and in order to enhance the fermentation effect, the colony count in the yeast seed solution is preferably such that the colony count in the saccharifying solution after inoculation is 1X 10 colonies per gram of saccharifying solution 8 -1×10 9 cfu. The yeast seed liquid can be an aqueous solution or a culture medium solution of dry yeast, or can be an activated seed liquid of dry yeast or an activated seed liquid of commercial yeast strains. The preparation method of the yeast seed solution can be a method conventionally used in the field, and is not described in detail herein.
In the present invention, the temperature of the fermentation may be any temperature suitable for yeast growth metabolism, and in order to enhance the effect of the fermentation, it is preferable that the temperature of the fermentation is 30 to 36 ℃, more preferably 30 to 33 ℃.
In the present invention, the pH of the fermentation may be any pH suitable for yeast growth metabolism, and in order to enhance the effect of the fermentation, the pH of the fermentation is preferably 3 to 6, more preferably 4 to 4.5.
In the present invention, the fermentation time may be selected within a wide range, for example, the fermentation time may be a period from the start of inoculation to the growth of yeast into the decay period (i.e., the fermentation time is the sum of the lag phase, the log phase and the stationary phase), and in order to enhance the effect of fermentation, the fermentation time is preferably 50 to 75 hours, more preferably 60 to 70 hours.
In the invention, the ethanol can be separated and purified from the fermented mash obtained by fermentation by selecting a proper method from the conventional methods for separating and purifying the ethanol according to the requirements of different industrial products (such as fuel alcohol requires ethanol with the purity of more than 99 percent), for example, the methods of distillation, concentration, water removal and the like are used.
In the invention, the distillation can adopt a three-tower (i.e. a crude tower, a combined tower and a refined tower) distillation process to obtain ethanol liquid and waste mash liquid. The conditions for the distillation are not particularly limited and may be those conventionally used in the art, and in order to improve the yield and purity of ethanol, the crude column bottoms temperature is preferably 80 to 85℃and the pressure is preferably from-45 kPa to-50 kPa.
Preferably, the temperature of the tower bottom of the combined tower is 110-130 ℃ and the pressure is 75-80kPa.
Preferably, the temperature of the tower kettle of the rectifying tower is 155-160 ℃ and the pressure is 380-400kPa.
In the invention, waste mash is generated in the process of distilling the fermented mash, and the obtained waste mash can be used for preparing DDGS (distillers' grains protein feed) after concentration treatment. Wherein the conditions for concentration may be those conventionally used in the art, such as concentrating the spent mash to 8-12% of the original volume at 60-95 ℃.
In the present invention, preferably, the method further comprises the steps of removing bran from wheat to obtain the flour and the bran, concentrating the distilled fermented waste mash, and mixing the concentrated product with the bran to obtain the distillers' grains protein feed. By adopting the method, the bran can be reasonably utilized, and the yield and quality (such as color, yield and the like) of the vinasse protein feed can be effectively improved.
In the present invention, more preferably, the concentrated product is used with bran in such an amount that the weight ratio of the concentrated product to bran is 1 to 8 on a dry matter basis: 1, more preferably 3-5:1.
in the present invention, preferably, the wheat debranning method comprises the steps of:
1) Soaking wheat;
2) Performing skin milling on the infiltrated wheat to obtain coarse bran and endosperm grains with flour; performing heart grinding on the obtained endosperm grains to obtain flour and bran;
3) Scraping (skin grinding) the coarse bran containing the flour to obtain secondary flour and bran, wherein the primary flour and the secondary flour are mixed to obtain the wheat flour. The primary powder and the secondary powder are not ground.
In the present invention, in order to further enhance the effect of the skin grinding, it is preferable that the skin grinding of step 1) is performed for 2 to 4 times.
More preferably, the conditions of the skin grinding include: the rotation speed of the grinding roller is 500-620 r.min -1 Grinding roll tooth number is 3-9 teeth cm -1 The tooth angle of the grinding roller is 25-40 degrees/60-70 degrees, and the inclination of the grinding roller is 1:10-16.
More preferably, the conditions of the heart-fire include: the rotation speed of the grinding roller is 500-620 r.min -1 Grinding roll tooth number 5-11 tooth cm -1 The tooth angle of the grinding roller is 25-40 degrees/60-70 degrees, and the inclination of the grinding roller is 1:10-16.
According to the present invention, the wheat may be wheat from various places, for example, northeast, henan, hebei, anhui, shanxi, etc.
In the present invention, the immersion liquid used for immersing the wheat is not particularly limited, and may be any immersion liquid conventionally used in the art, such as water and/or steam.
In the present invention, the equipment used for the infiltration is not particularly required as long as the wheat can be sufficiently infiltrated to facilitate separation of the wheat flour and the bran, for example, the wheat can be infiltrated in a water-wetting bin, preferably so that the water content of the infiltrated wheat satisfies the requirements.
In the present invention, the moisture content of the infiltrated wheat may be selected within a wide range, and in order to enhance the debranning effect, the moisture content of the infiltrated wheat is preferably 13 to 20 wt%, more preferably 14 to 17 wt%.
In the present invention, in order to make the wheat bran having the moisture content after the soaking have better flexibility and to make the endosperm portion of the wheat have a certain toughness so as to improve the effect of removing bran from the wheat, a particularly preferred embodiment is that the soaking temperature is 40-90 ℃, more preferably 48-55 ℃.
In the present invention, in order to further enhance the effect of wheat debranning, preferably, the amount of water used for the infiltration is 10-80Kg per 1000Kg dry weight of wheat; more preferably 20-50Kg.
The inventors of the present invention have found through studies that in order to further increase the bran flexibility of the wheat after infiltration and to allow the endosperm fraction of wheat to still have a better crispness, it is preferred that the time of infiltration is 3-10 hours, more preferred that the time of infiltration is 5-7 hours. In the preferred soaking time of the invention, the wheat bran can fully absorb water to achieve proper flexibility, and endosperm contained in the wheat can not lose brittleness due to excessive water absorption, so that a better bran removing effect can be achieved, the wheat flour after bran removal has a certain granularity, the amount of fine powder is reduced, and the bran removing effect is improved.
In the present invention, the apparatus and control conditions used in the wheat debranning method are not particularly limited, and may be those conventionally used in the art, as long as the wheat flour and the bran can be effectively separated by the wheat debranning, preferably such that the weight of the flour having a particle size in the range of 0.25 to 0.42mm is 60 to 80%, preferably 65 to 75% of the total weight of the flour. The granularity of the wheat flour meets the requirements, the solid-liquid separation effect can be further improved, the obtained wheat flour is used for preparing starch milk which is used for ethanol fermentation raw materials, the ethanol yield can be higher, the obtained wheat bran is used for preparing DDGS with higher quality, the wheat is reasonably utilized, and the added value of the wheat is improved.
The present invention will be described in detail by examples. In the following examples of the present invention,
the viscosity of the liquefied product is obtained by a viscometer;
the total sugar of the fermentation residue is measured according to the direct titration method of the total sugar of GB/T15038-2006;
the fermented residual reducing sugar is measured by a reducing sugar tester (for the principle of reducing sugar measurement see GB 5009.7-2016);
starch wine yield = 100% x mass of ethanol per mass of starch of the feedstock; the method for measuring the starch quality refers to GB/T5006-1985;
Consumption of alcohol grain: raw material mass (in g/g) required for producing ethanol per unit mass;
DDGS yield = 100% ×ddgs mass per grade/total mass of DDGS;
DDGS grade: the first grade product is defined as golden yellow without variegation and uniform in particle size; the secondary product is defined as golden yellow with variegated color and uniform particle size; tertiary is defined as light brown and less uniform particles; the fourth grade is defined as brown particle size non-uniformity; five-stage product is defined as dark brown and has very non-uniform particle size; DDDGS color refers to the color of DDGS feed, and is generally compared by a color chart;
yield of DDGS = DDGS mass/ethanol product mass (99.5% v/v);
alpha-amylase is purchased from commercial product with Alpha of the company of Jiegeraceae (China) bioengineering, and the enzyme activity is 130000U/g;
saccharifying enzyme is purchased from NoveXin company as Su Hong 475, and the enzyme activity is 150000U/g;
the yeasts are purchased from Angel super-brewing high activity dry yeasts, from Angel Yeast, inc., hubei Angel;
wheat is a aged grain stored for 3 years;
brown rice is aged grain stored for 3 years;
the rice is aged grains stored for 3 years, and is crushed and used, and the rice hull content is 25 wt%;
the filter press equipment was purchased from commercial products available under the trademark XAZF500-1500 from Jingjin environmental protection Co.
Preparation example 1
The specific process for preparing the yeast seed liquid comprises the following steps: relative to 25m 3 170 kg of yeast is added into sugar solution with the concentration of 3 weight percent, after the mixture is stirred uniformly, the mixture is activated for 20 minutes under the condition of 37 ℃ with the temperature being kept, and the activated yeast solution is added into the mixture with the volume of 400m 3 Is cultured in a mother liquor culture tank at 30deg.C until the colony number is 8×10 8 cfu/mL。
Example 1
(1) Wheat bran removal: soaking 100 parts by weight of wheat in dry weight at 50 ℃ for 6 hours with 3.5 parts by weight of water, wherein the water content of the soaked wheat is 15% by weight;
performing skin milling on the obtained infiltrated wheat to obtain coarse bran and endosperm grains with flour, wherein the skin milling adopts 3 milling steps, and the skin milling conditions are as follows: the rotation speed of the grinding roller is 550 r.min -1 Grinding roll tooth number (one grinding 3 teeth cm) -1 Two-pass grinding 5 teeth cm -1 Three grinding 7 teeth cm -1 ) Grinding roll tooth angle is 30 degrees/65 degrees, and grinding roll inclination is 1:10; carrying out heart grinding on the obtained endosperm grains to obtain flour and bran, wherein the heart grinding adopts 3-pass grinding, and the heart grinding conditions are as follows: the rotation speed of the grinding roller is 550 r.min -1 Grinding roll tooth number (one grinding 5 teeth cm) -1 Two-pass grinding 7 teeth cm -1 Three grinding 11 teeth cm -1 ) Grinding roll tooth angle is 30 degrees/65 degrees, and grinding roll inclination is 1:16; the coarse bran containing flour is subjected to 3 times of scraping treatment (skin grinding) to obtain secondary flour and bran, wherein the conditions of the 3 times of scraping treatment are as follows: the rotation speed of the grinding roller is 550 r.min -1 Grinding roll tooth number (one grinding 3 teeth cm) -1 Two-pass grinding 5 teeth cm -1 Three grinding 7 teeth cm -1 ) The tooth angle of the grinding roller is 30 degrees/65 degrees, and the inclination of the grinding roller is 1:10. Mixing the flour and flour two, sieving to obtain wheat flour with particle size less than or equal to 0.9mm and particle size of 0.25-0.42mm, wherein the weight of the flour is 70% of the total weight of the flour.
(2) Mixing 31 parts by weight of rice, 54 parts by weight of brown rice and 15 parts by weight of wheat flour to obtain a starchy raw material, wherein the granularity of the rice is less than or equal to 1.2mm, and the rice hull accounts for 11.2% by weight of the total weight of the brown rice and the wheat flour; the starch milk is prepared by mixing the obtained starchy material with water, wherein the Baume degree of the prepared starch milk is 13.7 DEG Be.
(3) Uniformly mixing the starch milk obtained in the step (2) with alpha-amylase, and then performing jet liquefaction to obtain a liquefied product, wherein the viscosity of the liquefied product is shown in Table 1; the amount of alpha-amylase used was 20U, the temperature of liquefaction was 92℃and the liquefaction time was 120 minutes, relative to 1g of starchy material, the pH of the jet liquefaction was 5.68; carrying out filter pressing on the obtained liquefied product to obtain filter residues and clear liquid, wherein the filter pressing conditions are as follows: the working pressure is 0.58MPa, and the press filtration time is 3.5h. The filter cloth used for the filter pressing is a nylon silk screen with 100 meshes, and the thickness of the filter layer for the filter pressing is 36mm. Regulating the pH value of the clear liquid to 4.35, uniformly mixing the clear liquid with saccharifying enzyme, and saccharifying to obtain saccharified liquid with the pH value of 4.22; the amount of saccharifying enzyme used was 125U relative to 1g of starchy material, and the conditions for saccharification were: the saccharification temperature was 60℃and the saccharification time was 50 minutes. The water content of the obtained filter residue is shown in Table 1.
(4) Stirring is started, the obtained saccharification liquid is inoculated with the seed liquid of preparation example 1, and fermentation is carried out for 68 hours at the temperature of 31.5 ℃ to obtain a fermentation product; wherein the yeast seed solution is inoculated in an amount such that the number of colonies in the saccharification solution is 2X 10 based on 1 g of the saccharification solution 8 cfu, the stirring speed in the yeast culture stage is such that the dissolved oxygen value in the fermentation system is 7ppm. The residual total sugar content, residual reducing sugar content, and calculated starch wine yield and alcohol consumption in the obtained fermentation product are shown in Table 1.
(5) Distilling the ethanol from the obtained fermentation product by adopting a three-tower (i.e. a crude tower, a combined tower and a refined tower) distillation process flow to obtain ethanol liquid and waste mash; the temperature of the crude tower kettle is 82 ℃, the pressure is-48 kPa, the temperature of the combined tower kettle is 120 ℃, the pressure is 78kPa, the temperature of the refined tower kettle is 157 ℃, and the pressure is 392kPa; the ethanol solution obtained was dehydrated by molecular sieve to obtain an ethanol product (concentration 99.6 vol%).
(6) Concentrating the obtained waste mash at 65 ℃ to 30% of the original volume of the waste mash, thereby obtaining thick slurry; uniformly mixing the obtained concentrated slurry, bran and filter residues, and drying at 95 ℃ until the water content of the mixed materials is 10 wt%, thereby obtaining DDGS, wherein the weight ratio of the concentrated slurry to the bran is 4 based on dry weight; the yield and yield of DDGS are shown in Table 1.
Example 2
(1) Wheat bran removal: soaking 100 parts by weight of wheat in terms of dry weight with 2 parts by weight of water at 48 ℃ for 5 hours, wherein the water content of the soaked wheat is 14% by weight;
performing skin milling on the obtained infiltrated wheat to obtain coarse bran and endosperm grains with flour, wherein the skin milling adopts 3 milling steps, and the skin milling conditions are as follows: grinding roller rotating speed 620 r.min -1 Grinding roll tooth number (one grinding 3 teeth cm) -1 Two-pass grinding 5 teeth cm -1 Three grinding 7 teeth cm -1 ) Grinding roll tooth angle is 30 degrees/65 degrees, and grinding roll inclination is 1:16; carrying out heart grinding on the obtained endosperm grains to obtain flour and bran, wherein the heart grinding adopts 3-pass grinding, and the heart grinding conditions are as follows: grinding roller rotating speed 620 r.min -1 Grinding roll tooth number (one grinding 5 teeth cm) -1 Two-pass grinding 7 teeth cm -1 Three grinding 11 teeth cm -1 ) Grinding roll tooth angle is 30 degrees/65 degrees, and grinding roll inclination is 1:16; the coarse bran containing flour is subjected to 3 times of scraping treatment (skin grinding) to obtain secondary flour and bran, wherein the conditions of the 3 times of scraping treatment are as follows: grinding roller rotating speed 620 r.min -1 Grinding roll tooth number (one grinding 5 teeth cm) -1 Two-pass grinding 7 teeth cm -1 Three grinding 11 teeth cm -1 ) The tooth angle of the grinding roller is 30 degrees/65 degrees, and the inclination of the grinding roller is 1:16. Mixing the flour with the flour to obtain wheat flour, wherein the grain diameter of the obtained wheat flour is less than or equal to 0.9mm, and the weight of the flour with the grain diameter in the range of 0.25-0.42mm accounts for 75% of the total weight of the flour.
(2) Mixing 35 parts by weight of rice, 50 parts by weight of brown rice and 15 parts by weight of wheat flour to obtain a starchy raw material, wherein the granularity of the rice is less than or equal to 1mm, and the rice hull accounts for 13.5% by weight of the total weight of the brown rice and the wheat flour; the starch milk is prepared by mixing the obtained starchy material with water, wherein the Baume degree of the prepared starch milk is 13.5 DEG Be.
(3) Uniformly mixing the starch milk obtained in the step (2) with alpha-amylase, and then performing jet liquefaction to obtain a liquefied product, wherein the viscosity of the liquefied product is shown in Table 1; the amount of alpha-amylase used was 30U, the temperature of liquefaction was 95℃and the liquefaction time was 110 minutes, relative to 1g of starchy material, the pH of the jet liquefaction was 5.5;
carrying out filter pressing on the obtained liquefied product to obtain filter residues and clear liquid, wherein the filter pressing conditions are as follows: the working pressure is 0.55MPa, and the press filtration time is 3 hours. The filter cloth used for the filter pressing is an 80-mesh nylon silk screen, and the thickness of the filter layer for the filter pressing is 33mm. Regulating the pH value of the clear liquid to 4.2, uniformly mixing the clear liquid with saccharifying enzyme, and saccharifying to obtain saccharified liquid with the pH value of 4.2; the amount of saccharifying enzyme used was 130U relative to 1g of starchy material, and the conditions for saccharification were: the saccharification temperature was 59℃and the saccharification time was 40 minutes. The water content of the obtained filter residue is shown in Table 1.
(4) Stirring is started, the obtained saccharification liquid is inoculated with the seed liquid of preparation example 1, and fermentation is carried out for 70 hours at the temperature of 30 ℃ to obtain a fermentation product; wherein the yeast seed solution is inoculated in an amount such that the number of colonies in the saccharification solution is 2X 10 based on 1 g of the saccharification solution 8 cfu, the speed of stirring during yeast cultivation was such that the dissolved oxygen value in the fermentation system was 8ppm. The residual total sugar content, residual reducing sugar content, and calculated starch wine yield and alcohol consumption in the obtained fermentation product are shown in Table 1.
(5) Distilling the obtained fermentation product by adopting a three-tower (i.e. a crude tower, a combined tower and a refined tower) distillation process flow to obtain ethanol liquid and waste mash; the temperature of the crude tower kettle is 80 ℃, the pressure is-50 kPa, the temperature of the combined tower kettle is 110 ℃, the pressure is 71kPa, the temperature of the refined tower kettle is 160 ℃, and the pressure is 398kPa; the ethanol solution obtained was dehydrated by molecular sieve to obtain an ethanol product (concentration 99.6 vol%).
(6) Concentrating the obtained waste mash at 60 ℃ to 20% of the original volume of the waste mash, thereby obtaining thick slurry; uniformly mixing the obtained concentrated slurry, bran and filter residues, and then drying at 90 ℃ until the water content of the mixed materials is 10 wt%, thereby obtaining DDGS, wherein the weight ratio of the concentrated slurry to the bran is 4 based on dry weight: 1, a step of; the yield and yield of DDGS are shown in Table 1.
Example 3
(1) Wheat bran removal: soaking 100 parts by weight of wheat in terms of dry weight with 5 parts by weight of water at 55 ℃ for 7 hours, wherein the water content of the soaked wheat is 17 percent;
performing skin milling on the obtained infiltrated wheat to obtain coarse bran and endosperm grains with flour, wherein the skin milling adopts 3 milling steps, and the skin milling conditions are as follows: grinding roller rotation speed 500 r.min -1 Grinding roll tooth number (one grinding 3 teeth cm) -1 Two-pass grinding 5 teeth cm -1 Three grinding 7 teeth cm -1 ) Grinding roll tooth angle is 30 degrees/65 degrees, and grinding roll inclination is 1:10; carrying out heart grinding on the obtained endosperm grains to obtain flour and bran, wherein the heart grinding adopts 3-pass grinding, and the heart grinding conditions are as follows: grinding roller rotation speed 500 r.min -1 Grinding roll tooth number (one grinding 5 teeth cm) -1 Two-pass grinding 7 teeth cm -1 Three grinding 11 teeth cm -1 ) Grinding roll tooth angle is 30 degrees/65 degrees, and grinding roll inclination is 1:16; the coarse bran containing flour is subjected to 3 times of scraping treatment (skin grinding) to obtain secondary flour and bran, wherein the conditions of the 3 times of scraping treatment are as follows: grinding roller rotation speed 500 r.min -1 Grinding roll tooth number (one grinding 5 teeth cm) -1 Two-pass grinding 7 teeth cm -1 Three grinding 11 teeth cm -1 ) The tooth angle of the grinding roller is 30 degrees/65 degrees, and the inclination of the grinding roller is 1:10. Mixing the flour with the flour to obtain wheat flour, wherein the grain diameter of the obtained wheat flour is less than or equal to 0.9mm, and the weight of the flour with the grain diameter in the range of 0.25-0.42mm accounts for 65% of the total weight of the flour.
(2) Mixing 30 parts by weight of rice, 55 parts by weight of brown rice and 15 parts by weight of wheat flour to obtain a starchy raw material, wherein the granularity of the rice is less than or equal to 1.5mm, and the rice hull accounts for 10.7% by weight of the total weight of the brown rice and the wheat flour; the starch milk is prepared by mixing the obtained starchy material with water, wherein the Baume degree of the prepared starch milk is 14.5 DEG Be.
(3) Uniformly mixing the starch milk obtained in the step (2) with alpha-amylase, and then performing jet liquefaction to obtain a liquefied product, wherein the viscosity of the liquefied product is shown in Table 1; the amount of alpha-amylase used was 6U, the temperature of liquefaction was 90℃and the liquefaction time was 125 minutes, the pH of the jet liquefaction was 6, relative to 1g of starchy material;
carrying out filter pressing on the obtained liquefied product to obtain filter residues and clear liquid, wherein the filter pressing conditions are as follows: the working pressure is 0.6MPa, and the filter pressing time is 4 hours. The filter cloth used for the filter pressing is a 120-mesh nylon silk screen, and the thickness of the filter layer for the filter pressing is 39mm. Regulating the pH value of the clear liquid to 4.4, uniformly mixing the clear liquid with saccharifying enzyme, and saccharifying to obtain saccharified liquid with the pH value of 4.4; the amount of saccharifying enzyme used was 130U relative to 1g of starchy material, and the conditions for saccharification were: the saccharification temperature was 61℃and the saccharification time was 60 minutes. The water content of the obtained filter residue is shown in Table 1.
(4) Stirring is started, the obtained saccharification liquid is inoculated with the seed liquid of preparation example 1, and fermentation is carried out for 60 hours at the temperature of 33 ℃ to obtain a fermentation product; wherein the yeast seed solution is inoculated in an amount such that the number of colonies in the saccharification solution is 2X 10 based on 1 g of the saccharification solution 8 cfu, the speed of stirring during yeast cultivation was such that the dissolved oxygen value in the fermentation system was 6ppm. The residual total sugar content, residual reducing sugar content, and calculated starch wine yield and alcohol consumption in the obtained fermentation product are shown in Table 1.
(5) Distilling the obtained fermentation product by adopting a three-tower (i.e. a crude tower, a combined tower and a refined tower) distillation process flow to obtain ethanol liquid and waste mash; the temperature of the crude tower kettle is 85 ℃, the pressure is-40 kPa, the temperature of the combined tower kettle is 130 ℃, the pressure is 84kPa, the temperature of the refined tower kettle is 155 ℃, and the pressure is 388kPa; the ethanol solution obtained was dehydrated by molecular sieve to obtain an ethanol product (concentration 99.6 vol%).
(6) Concentrating the obtained waste mash at 70 ℃ to 40% of the original volume of the waste mash, thereby obtaining thick slurry; uniformly mixing the obtained concentrated slurry, bran and filter residues, and then drying at a drying temperature of 100 ℃ until the water content of the mixed materials is 10 weight percent to obtain DDGS, wherein the weight ratio of the concentrated slurry to the bran is 4 in terms of dry weight: 1, a step of; the yield and yield of DDGS are shown in Table 1.
Example 4
Ethanol was prepared as in example 1, except that the particle size of the rice in step (2) was 1.5mm < 2.5mm or less.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 1.
Example 5
Ethanol was prepared as in example 1, except that 28 parts by weight of rice, 57 parts by weight of brown rice and 15 parts by weight of wheat flour were blended in step (2) to obtain a starchy material.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 1.
Example 6
Ethanol was prepared as in example 1, except that 37 parts by weight of rice, 48 parts by weight of brown rice and 15 parts by weight of wheat flour were blended in step (2) to obtain a starchy material.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 1.
Example 7
Ethanol was prepared as in example 1, except that rice was replaced with equal amounts of brown rice and rice hulls (crushed rice hulls were able to pass through a 1.5mm screen) such that the resulting starchy material had 2.5% by weight of rice hulls relative to the total weight of brown rice and wheat flour.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 2.
Example 8
Ethanol was prepared as in example 1, except that the liquefied product obtained in step (3) was not subjected to pressure filtration; in the step (6), the obtained waste mash is subjected to pressure filtration, and then the obtained clear liquid (filtrate) is subjected to concentration treatment, wherein the pressure filtration conditions and concentration conditions are the same as those in the example 1.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 2.
Comparative example 1
Ethanol was prepared according to the method of example 1, except that wheat was not subjected to a debranning treatment, the wheat was directly ground into particles, and the resulting particles had a particle size of 0.9mm or less and a particle size in the range of 0.25 to 0.42mm, the weight of the flour accounting for 70% of the total weight of the flour.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 2.
Comparative example 2
Ethanol was prepared as in example 1, except that brown rice was replaced with an equal amount of wheat flour.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 2.
Comparative example 3
Ethanol was prepared as in example 1, except that in step (1), 100 parts by weight of wheat, calculated as dry weight, was infiltrated with 7% by weight of water at 40 ℃ for 8 hours, and the water content of the infiltrated wheat was 18% by weight;
performing skin milling on the obtained infiltrated wheat to obtain coarse bran and endosperm grains with flour, wherein the skin milling adopts 2 milling steps, and the skin milling conditions are as follows: grinding roller rotation speed 500 r.min -1 Grinding roll tooth number (one grinding 4 teeth cm) -1 Two-pass mill 10 teeth cm -1 ) Grinding roll tooth angle 21 degrees/67 degrees, grinding roll inclination 1:8; carrying out heart grinding on the obtained endosperm grains to obtain flour and bran, wherein the heart grinding adopts 3-pass grinding, and the heart grinding conditions are as follows: grinding roller rotation speed 500 r.min -1 Grinding roll tooth number (one grinding 8)Teeth cm -1 Two-grinding 12 teeth cm -1 Three grinding 16 teeth cm -1 ) Grinding roll tooth angle 40 degrees/70 degrees, grinding roll inclination 1:8; 2 times of scraping treatment (skin grinding) are carried out on the coarse bran containing the flour to obtain two times of flour and bran, wherein the conditions of the 2 times of scraping treatment are as follows: grinding roller rotation speed 500 r.min -1 Grinding roll tooth number (one grinding 4 teeth cm) -1 Two-pass mill 10 teeth cm -1 ) The tooth angle of the grinding roller is 21 degrees/67 degrees, and the inclination of the grinding roller is 1:8. Mixing the flour with the flour to obtain wheat flour, wherein the grain diameter of the obtained wheat flour is less than or equal to 0.9mm, and the weight of the flour with the grain diameter in the range of 0.25-0.42mm accounts for 40% of the total weight of the flour. The grain size of the obtained wheat flour is more than 0.9mm and less than 1.2mm.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 2.
Comparative example 4
Ethanol was prepared as in example 1, except that in step (1), 100 parts by weight of wheat, calculated as dry weight, was infiltrated with 6% by weight of water at 55 ℃ for 6 hours, and the water content of the infiltrated wheat was 18% by weight;
performing skin milling on the obtained infiltrated wheat to obtain coarse bran and endosperm grains with flour, wherein the skin milling adopts 2 milling steps, and the skin milling conditions are as follows: grinding roller rotating speed 620 r.min -1 Grinding roll tooth number (one grinding 4 teeth cm) -1 Two-pass grinding 9 teeth cm -1 ) Grinding roll tooth angle 40 degrees/70 degrees, grinding roll inclination 1:16; carrying out heart grinding on the obtained endosperm grains to obtain flour and bran, wherein the heart grinding adopts 3-pass grinding, and the heart grinding conditions are as follows: grinding roller rotating speed 620 r.min -1 Grinding roll tooth number (one grinding 9 teeth cm) -1 Two-pass mill 9.5 teeth cm -1 Three-pass mill 10.5 teeth cm -1 ) Grinding roll tooth angle 40 degrees/70 degrees, grinding roll inclination 1:8; 2 times of scraping treatment (skin grinding) are carried out on the coarse bran containing the flour to obtain two times of flour and bran, wherein the conditions of the 2 times of scraping treatment are as follows: grinding roller rotating speed 620 r.min -1 Grinding roll tooth number (one grinding 4 teeth cm) -1 Two-pass grinding 9 teeth cm -1 ) Grinding roller tooth angle 40 DEG-70 DEG, and the grinding roll inclination is 1:16. Mixing the flour with the flour to obtain wheat flour, wherein the grain diameter of the obtained wheat flour is less than or equal to 0.9mm, and the weight of the flour with the grain diameter in the range of 0.25-0.42mm accounts for 40% of the total weight of the flour.
The viscosity of the obtained liquefied product, the water content of the filter residue, the residual total sugar content and the residual reducing sugar content in the fermented product, and the calculated starch wine yield and alcohol consumption, and the yield of DDGS are shown in Table 2.
TABLE 1
TABLE 2
From the results, the method for preparing the ethanol does not relate to a process for extracting the wheat gluten, can effectively reduce the viscosity of liquefied products, the water content of filter residues, the total sugar content of fermentation residues, the reducing sugar content of fermentation residues and the consumption of alcohol grains, can effectively prevent blockage of distillation equipment and abrasion to the equipment in the distillation process, and has higher starch wine yield (ethanol yield) and DDGS yield; the technical scheme of the invention can reasonably utilize the wheat and the rice, and improves the utilization value of grains and the enterprise benefit. Significantly better results are obtained with examples 1-3 of the most preferred embodiment of the invention.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (12)
1. A method of producing ethanol, the method comprising: sequentially carrying out enzymolysis, fermentation and distillation on starch milk containing a starchy raw material, wherein the starchy raw material is at least partially derived from rice, brown rice and flour, and the rice exists in the starch milk in a crushed form; the grain diameter of the flour is less than or equal to 0.9mm, and the weight of the flour with the grain diameter in the range of 0.25-0.42mm accounts for 60-80% of the total weight of the flour; the rice, the brown rice and the flour are used in an amount such that the weight ratio of the rice, the brown rice and the flour is 30-35:50-55:15;
the enzymolysis mode comprises the steps of liquefying starch milk containing starchiness raw materials to obtain liquefied products, and saccharifying the liquefied products; and before saccharification of the liquefied product, carrying out solid-liquid separation on the liquefied product.
2. The method of claim 1, wherein the liquefied product to be subjected to solid-liquid separation further comprises rice hulls, the rice hulls are used in an amount of 2.5-21 wt% based on the total weight of the brown rice and the flour, and the solid-liquid separation is performed by press filtration.
3. The process of claim 2 wherein the rice hulls are used in an amount of 10-13.5% by weight based on the total weight of the brown rice and flour.
4. A process according to claim 2 or 3, wherein the conditions of the press filtration comprise: the working pressure is 0.4-0.65MPa, and the filter pressing time is 2-4h;
and/or the aperture of the filter cloth used for filter pressing is 60-200 meshes;
and/or the thickness of the filter layer of the filter pressing is 15-80mm.
5. The process of claim 4 wherein the press conditions comprise: the working pressure is 0.55-0.6MPa; the filter pressing time is 3-4 hours;
and/or the aperture of the filter cloth used for filter pressing is 80-120 meshes;
and/or the thickness of the filter layer of the filter pressing is 33-39mm.
6. The method of claim 1, wherein the flour having a particle size in the range of 0.25-0.42mm comprises 65-75% by weight of the total weight of the flour.
7. A method according to any one of claims 1 to 3 and 6 wherein the crushed rice is passed through a screen having a pore size of 1 to 2.5 mm;
And/or, the rice, brown rice and flour are derived from aged grains.
8. A method according to claim 7 wherein the crushed rice is passed through a screen having a pore size of 1-1.5 mm;
and/or, the rice, brown rice and flour are derived from aged grains stored for more than 3 years.
9. The method of claim 1, wherein the starch milk has a baume of 12-15 °be.
10. The method of claim 9, wherein the starch milk has a baume of 13.5-14.5 °be.
11. The method of claim 1, further comprising debranning wheat to obtain the flour and bran, concentrating the distilled fermented waste mash, and mixing the concentrated product with bran to obtain a distillers grain protein feed.
12. The method of claim 11, wherein the concentrated product is used with the bran in an amount such that the weight ratio of concentrated product to bran is 3-5 on a dry matter basis: 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590553A (en) * | 2003-09-03 | 2005-03-09 | 郑州凯乐生物能有限公司 | Alcohol cleaning production technology using wheat as raw material |
| CN109762851A (en) * | 2018-12-27 | 2019-05-17 | 吉林中粮生化有限公司 | A kind of method of paddy processing production alcohol fuel and by-product rice DDGS |
| CN110468161A (en) * | 2019-08-08 | 2019-11-19 | 国投生物科技投资有限公司 | The application of corn and rice in wheat alcohol fermentation processes and the method using mixed raw material progress raw material fermentation production ethyl alcohol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590553A (en) * | 2003-09-03 | 2005-03-09 | 郑州凯乐生物能有限公司 | Alcohol cleaning production technology using wheat as raw material |
| CN109762851A (en) * | 2018-12-27 | 2019-05-17 | 吉林中粮生化有限公司 | A kind of method of paddy processing production alcohol fuel and by-product rice DDGS |
| CN110468161A (en) * | 2019-08-08 | 2019-11-19 | 国投生物科技投资有限公司 | The application of corn and rice in wheat alcohol fermentation processes and the method using mixed raw material progress raw material fermentation production ethyl alcohol |
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