CN109762851B - Method for producing fuel ethanol and byproduct rice DDGS by processing rice - Google Patents
Method for producing fuel ethanol and byproduct rice DDGS by processing rice Download PDFInfo
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- CN109762851B CN109762851B CN201811607687.XA CN201811607687A CN109762851B CN 109762851 B CN109762851 B CN 109762851B CN 201811607687 A CN201811607687 A CN 201811607687A CN 109762851 B CN109762851 B CN 109762851B
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Abstract
The invention relates to a method for processing and producing fuel ethanol and byproduct rice DDGS by taking paddy as a raw material, which comprises the following steps: (1) rice crushing pretreatment; (2) preparing liquefied mash; (3) preparing yeast mash; (4) preparing fermented mature mash; (5) preparing fuel ethanol; (6) preparing rice DDGS. The product fuel ethanol obtained by the method has high volume fraction of ethanol, and the quality of the product fuel ethanol meets the national standard GB18350-2013 denatured fuel ethanol; in addition, the detection result of the mycotoxin in the rice DDGS byproduct is lower than the limit standard, and the protein content is high. Therefore, the invention realizes the industrial production of the rice processing fuel ethanol and the byproduct rice DDGS, avoids the risk of over standard mycotoxin in the DDGS caused by harmful mycotoxin entering a food chain system, improves the protein content in the DDGS, and greatly improves the comprehensive utilization value of the rice.
Description
Technical Field
The invention relates to the field of fuel ethanol production, in particular to a method for producing fuel ethanol by processing rice, by-product Dried rice wine lees and soluble substances (DDGS for short) thereof.
Background
In recent years, with the increase of energy crisis, the demand of ethanol is increasing as one of the alternative fuels in the future. If the fuel ethanol is mixed with gasoline to form the ethanol gasoline for the vehicle according to the addition of 10 percent as a renewable green clean energy source, the fuel ethanol plays an important role in relieving the shortage of fossil energy, effectively reducing carbon emission, greatly reducing the pollution of harmful substances in the tail gas of the vehicle, protecting the environment and the like. Currently, the fuel ethanol yield in China is about 260 ten thousand tons per year, which accounts for only 3% of the global fuel ethanol yield, and the third rank has a significant difference from the yields of the first two ranked U.S. and Brazil. The fuel ethanol consumption of China only accounts for 2.1 percent of the gasoline consumption, so the development space for producing the fuel ethanol is huge.
At present, grains, potatoes and molasses are mainly used as raw materials for producing fuel ethanol, wherein the grains are usually corn, wheat, rice and the like. Among these cereal starchy feedstocks, corn is often the primary source of fuel ethanol, since corn is only about 15-20% of what is actually consumed by humans, and thus the fuel ethanol produced from corn is about 48% of the national annual fuel ethanol production. DDGS refers to distillers dried grains with soluble solids as a byproduct of fuel ethanol production. Because the protein content of DDGS is high (generally over 26 wt%), DDGS becomes a novel protein feed raw material widely applied by feed production enterprises at home and abroad. In recent years, the import of DDGS has increased dramatically in China, and the DDGS is the first major country for export from the United states in 2010. Along with the popularization of the method for producing fuel ethanol by using corn as a raw material in China, the yield of DDGS in China is correspondingly increased. For example, patent document CN 108374024a discloses a method for co-producing ethanol, fructose and various byproducts from sweet sorghum stalks and corn. However, the problem of DDGS in the process of producing fuel ethanol when using corn as a raw material, particularly the problem of high content of mycotoxin in corn, is the biggest obstacle to the use of DDGS produced by China as a feed raw material. In addition, in the above patent documents, the method of preparing biogas residues and biogas slurry from the vinasse with excessive mycotoxins as organic fertilizer, and the mycotoxins return to the crops after a series of treatment processes, which causes secondary pollution. Thus, it is not in fact effective in controlling mycotoxin levels in corn DDGS, but rather uses the over-graded stillage for conversion to other byproducts.
The southern China mainly plants paddy. Among the rice, middle-season rice and late-season rice provide grain and food markets, and early-season rice is frequently used as reserve grain due to the characteristics of low water content and storage durability. According to statistics of relevant data, the total yield of the rice in 2017 nationwide is 2 hundred million tons, the expected balance is 0.2 hundred million tons, and the balance in the stock is still high. In addition, the starch content in rice is between 70 and 80 wt%, and the starch content in corn is about 73.2 wt%, which shows that the starch content in rice is also sufficient for producing fuel ethanol. Therefore, the method for producing the fuel ethanol by processing the rice is a scientific and reasonable solution, and has great development significance.
The rice is the seed of rice, and is the grain made from rice through the processes of hulling, cleaning, hulling, milling and finishing. Although rice can be used for producing fuel ethanol and can produce high-quality DDGS as a byproduct, the rice produced from rice still needs multiple processes, which not only increases the process cost, but also causes waste of food resources and the like. In addition, because the outer layer of rice grain has a higher protein content than the inner layer, the protein content of rice is 7-8 wt%, whereas the protein content of rice is about 9.5 wt%, and the protein content of corn, which is commonly used for fuel ethanol production, is about 8.5 wt%. Thus, the protein content of DDGS produced by rice and corn is far less than that of rice. Therefore, the method for producing the fuel ethanol and the byproduct rice DDGS by using the rice as the raw material has obvious advantages.
Disclosure of Invention
The invention provides a method for producing fuel ethanol and byproduct rice DDGS by processing rice, which can overcome the technical problems of corn DDGS while efficiently producing the fuel ethanol. The method for producing fuel ethanol and by-product rice DDGS by processing rice comprises the following steps:
(1) rice crushing pretreatment: removing impurities from rice, and pulverizing with a pulverizer to obtain rice powder passing through a 25-mesh screen;
(2) preparing liquefied mash: uniformly mixing rice powder and water to form powder slurry, adjusting the pH value to 5.2-5.5, adding high-temperature amylase, preheating the powder slurry to 53-55 ℃ in a powder slurry tank, injecting high-temperature steam for liquefaction, then feeding the liquefied powder slurry into a cooking maintaining tank, keeping the temperature in the cooking maintaining tank to be 95-97 ℃, reducing the temperature to 85-87 ℃ after negative pressure flash evaporation, feeding the liquefied powder slurry into a liquefaction tank for liquefaction, reducing the temperature to 65-75 ℃ through negative pressure flash evaporation after the liquefaction is finished, and reducing the temperature to 31-32 ℃ through a heat exchanger to obtain liquefied mash;
(3) preparing yeast mash: adding liquefied mash, water and yeast wine into an activation tank, introducing sterile air, maintaining the activation temperature at 34-36 ℃ through an external heat exchanger, and hydrating and activating the yeast wine to form activation liquid; introducing the activation liquid into a yeast tank filled with liquefied mash, introducing sterile air, maintaining propagation temperature of 28-30 ℃ through an external heat exchanger, and rapidly propagating yeast under aerobic condition until the yeast number reaches more than 2.5 hundred million/mL to obtain yeast mash;
(4) preparing fermented mature mash: adding the rest of the liquefied mash into a fermentation tank, adjusting the pH value to 4.2-4.4, and simultaneously adding high-efficiency saccharifying enzyme and urea; adding yeast mash into the fermentation tank with an inoculation amount of 15-20% (v/v), and fermenting in the fermentation tank under oxygen-free condition to obtain fermented mash;
(5) preparing fuel ethanol: preheating fermented mash, then feeding the preheated fermented mash into a distillation system, feeding alcohol steam extracted from the distillation system into a molecular sieve system after passing through a superheater, and dehydrating and cooling to obtain anhydrous fuel ethanol;
(6) preparing rice DDGS: and filtering and separating waste mash of the distillation system to obtain clear liquid and wet grains, evaporating and concentrating the clear liquid to obtain clear liquid concentrate, drying the wet grains, mixing the wet grains with the clear liquid concentrate, and drying the mixture in a dryer to obtain the rice DDGS.
Advantageous effects
The method for producing the fuel ethanol and the byproduct rice DDGS by processing the rice adopts the rice as the raw material to produce the fuel ethanol and the rice DDGS, and has a plurality of beneficial technical effects:
1. the aged grain is adopted as the raw material, so that on one hand, the problem of food safety caused by the fact that the aged grain flows into a grain market is avoided, the utilization rate of the aged grain is obviously increased, and the waste is reduced; on the other hand, under the condition of ensuring the purity of ethanol in the produced fuel ethanol, the aged grain is used as a raw material, so that the price advantage is very obvious compared with that of corn, the production cost is reduced by about 17 percent compared with that of corn, and the economic benefit and profit of enterprises are improved.
2. The produced by-product rice DDGS has a protein content higher than that of corn DDGS and contains high-quality complete protein which is a mixture of rice protein and yeast protein and is high-quality protein without allergen.
3. The steam jet liquefaction technology is adopted when the liquefied mash is prepared, and the technical means such as flash evaporation cooling and the like are combined, so that energy optimization is realized, the effects of liquefaction and synchronous saccharification and fermentation of starch in aged grains are ensured, and the energy consumption and equipment investment cost are reduced.
4. The pulverizer is adopted to pulverize the paddy into small-particle paddy powder, so that the problems of pipeline and equipment abrasion, pipeline blockage and the like caused by large-particle materials (particularly incompletely pulverized paddy hulls) are avoided, and the utilization rate of the paddy hulls is improved.
Drawings
FIG. 1 is a process flow diagram of one embodiment of the method for producing fuel ethanol and byproduct rice DDGS by rice processing according to the present invention.
Detailed Description
The invention aims to provide a method for producing fuel ethanol and a byproduct rice DDGS by processing rice, which can produce high-quality rice DDGS while ensuring high-efficiency production of the fuel ethanol and improve the utilization rate of aged grains.
The rice is generally classified into fresh grain, aged grain and aged grain. Generally, the rice produced in the same year is new grain, the rice stored for more than one year for the first time is aged grain, and the rice stored for more than 3 years is aged grain. The rice which is deteriorated after being stored is aged grain. During the storage process of the rice, under the influence of microorganisms and storage conditions, a series of physiological changes occur to the rice, and the rice often generates heat, mildew and buds. The aged grain can not be eaten as the grain for oral administration because the nutrition and the edible value are obviously reduced.
In the invention, the rice is used as the raw material for producing fuel ethanol and rice DDGS, and fresh grain, aged grain and aged grain can be used as the raw material. Generally, the shorter the storage time of rice, the lower the mycotoxin level, and the higher the quality of the resultant rice DDGS (i.e., the lower the mycotoxin level), however, the use of short-term stored rice tends to result in wasted food. Therefore, it is preferable to use aged grains that cannot be directly used as a ration in the present invention. Furthermore, the inventors have found that even when aged grain is used in the process of the present invention, the rice DDGS produced therefrom is generally of a higher quality than corn DDGS produced from corn.
In the present invention, the quality of DDGS is determined by its protein content and mycotoxin content. The higher the protein content and the lower the mycotoxin content, the quality of DDGSThe higher. The most predominant mycotoxins in DDGS include vomitoxin, zearalenone, aflatoxin B1And ochratoxin, and the like. Compared with other mycotoxins, the content of vomitoxin and zearalenone is higher, and the toxicity is stronger. Zearalenone is widely present in some cereal crops, such as corn, sorghum, wheat and the like, and particularly in corn and its by-products, in relatively high amounts. The DDGS feed can cause strong pollution to DDGS so as to cause serious harm to animal organisms, mainly because the DDGS feed has strong reproductive toxicity and teratogenic toxicity, the DDGS feed can affect the reproductive performance of animals, reduce the growth performance, cause immunosuppression, cause cell damage and the like, so that the animal health is harmed, and huge economic loss is brought to animal husbandry, so the DDGS feed should avoid the pollution of the DDGS feed for the first time. Vomitoxin is a very common mycotoxin, has lower toxicity than zearalenone, but has strong toxicity to human and animals, and can cause vomiting reactions of many animals, and even death can be caused. In addition, vomitoxin is stable in chemical property, generally cannot be damaged in the processes of processing, storage and cooking, can be stored for a long time under laboratory conditions, keeps toxicity unchanged, has strong heat resistance, and is easy to accumulate in animals, and further accumulates in human bodies at the tail ends of food chains to cause various food poisoning phenomena.
In one embodiment, the method of the present invention uses aged grains as a raw material for production, preferably aged grains with a storage life of 3 to 5 years, and more preferably aged grains with a storage life of 3 to 4 years. The aged grain with the above age cannot be used as a food for a long time, and the content of mycotoxin (especially zearalenone) is relatively low, so that the harm caused by the fact that the mycotoxin enters a food chain is avoided from the source.
In a preferred embodiment, the method of the present invention may further comprise the step of testing and screening the rice raw material before the rice milling pretreatment to ensure that the mycotoxin level is strictly controlled within a limited standard. Further, the method for detecting the rice material is not particularly limited, and for example, high performance liquid chromatography or other feasible detection means may be used. Generally, the longer the storage time of rice under the same storage conditions, the higher the mycotoxin content. Therefore, in the invention, whether to detect and screen the raw material of the rice is selected according to the storage life of the aged grain, and preferably, the aged grain with 3-4 years can be directly used as the raw material without detection and screening; for aged grains of 5 years or more, preferably, the grains are detected and screened before the rice is crushed and pretreated.
The method of removing impurities from the rice in the step (1) is not particularly limited as long as impurities in the rice can be removed, and different removal methods may be employed for different impurities. Impurities in rice can vary depending on the source of the rice, and generally these impurities do not have any benefit for the production of fuel ethanol and DDGS and can affect production. In the present invention, the impurities are, for example, hard materials (such as sand, ironware and/or other unidentified materials) which easily wear out the equipment or the pipeline, and woven fabrics which are not easily crushed. In one embodiment, in step (1), the rice is preferably subjected to a specific gravity stone remover to remove impurities such as sand, iron and the like, an electromagnetic iron remover to remove impurities such as iron and the like, and a roller classifying screen to remove impurities such as woven fabric and the like. The rice screened by the roller grading sieve can be directly used as rice powder. And crushing the oversize rice serving as a roller grading sieve to obtain rice powder. Further, the method of pulverizing the rice is not particularly limited as long as the rice on the screen can be pulverized to a desired particle size, and for example, a hammer mill capable of adjusting the pulverizing particle size can be used. The grain diameter of the undersize rice and the oversize crushed rice powder of the roller classifying screen is preferably 25 meshes. The rice flour and the rice hull with the particle sizes are fully crushed, so that the abrasion of large particle materials to pipelines and equipment is avoided, and the pipeline cannot be blocked.
In one embodiment, in the step (1), the rice flour may be further separated from impurities such as dust having a small particle size by a separator, and a method of the separation is not particularly limited, for example, it may be separated by a cyclone separator.
In one embodiment, in step (2), the ratio of the mixture of rice flour and water is 1:1.9 to 1:2.1, preferably 1:2. After the rice flour is mixed with water to form a slurry, the pH is adjusted to 5.2-5.5, preferably to 5.3, with sulfuric acid; the dry matter concentration of the powder slurry is controlled between 27 and 29 weight percent, and is preferably controlled to be 28 weight percent; the amount of the high-temperature amylase added was 0.3kg/t based on the mass of the rice material. Subsequently, the slip is preheated to 53-55 ℃, preferably 55 ℃ in a slip tank.
In the invention, in the step (2), a steam jet liquefaction process is adopted, and high-temperature steam is fully contacted with the rice starch granules, so that the structure of the rice starch granules is loose, the starch molecules are thoroughly expanded, the gelatinization is full, and the hydrolysis of amylase is facilitated.
In the present invention, in step (2), the negative pressure flash evaporation is performed 2 times. After the first negative pressure flash evaporation, the temperature is reduced by 6-8 ℃, and the starch molecules are further expanded and broken into small particles by the rapid change of the temperature and the pressure, so that the enzyme is more fully contacted with the starch particles. After liquefaction, secondary negative pressure flash evaporation is carried out, so that the use of a heat exchanger and cooling water is reduced, and the energy consumption is saved.
In the present invention, in the step (2), the liquefaction time in the liquefaction tank is not particularly limited as long as the starch in the rice can be liquefied. In one embodiment, the liquefaction time in the liquefaction tank is 140-.
In one embodiment, in step (3), the activation temperature of the yeast in the activation tank is 34 to 36 ℃, preferably 35 ℃. After the activation liquid is introduced into the yeast tank, the yeast is rapidly propagated in a large amount to generate heat, the heat is carried by an external heat exchanger, and the propagation temperature of the yeast is maintained at 28-30 ℃, preferably 29 ℃.
In the present invention, in the step (3), the propagation time of the yeast in the yeast tank is not particularly limited as long as the yeast can be propagated to a concentration of 2.5 hundred million/mL or more. In one embodiment, in step (3), the propagation time of the yeast in the yeast tank is 12-18h, preferably 15 h.
In one embodiment, in step (4), the remaining liquefied mash is adjusted to a pH of 4.2-4.4, preferably 4.3, using sulfuric acid.
In one embodiment, in step (4), the beer is inoculated into the fermentor at an inoculum size of 15-20% (v/v), preferably 15% (v/v).
In the present invention, in the step (4), the fermentation process and time of the yeast are not particularly limited. In one embodiment, the fermentation process is a simultaneous saccharification and fermentation process, and the simultaneous saccharification and fermentation process is a batch operation. Specifically, in the intermittent fermentation process, the fermentation temperature is controlled to be 28-31.5 ℃ and preferably 30 ℃ within the first 8 h; after 8h, controlling the fermentation temperature at 32.5-33.5 ℃, preferably 33 ℃, and ending the fermentation for 60 h.
In a preferred embodiment, an inorganic nitrogen source is added to the yeast tank in step (3) and the fermentor in step (4) to increase the propagation efficiency and wine production capacity of the yeast. The type of inorganic nitrogen source to be added is not particularly limited, but generally one of ammonium salts, and examples thereof include ammonium sulfate, ammonium nitrate, ammonium chloride, and the like.
In one embodiment, the carbon dioxide gas produced in the alcohol tank in step (3) and the fermentation tank in step (4) is washed in a washing tower and then vented to the atmosphere, and the washing liquid is recovered and then sent to the distillation system in step (5) for separation to separate ethanol contained therein.
In the present invention, in the step (5), the distillation system is not particularly limited as long as the fuel ethanol can be separated from the fermented mash. According to the solid-liquid composition of fermented mash, the preferred distillation system comprises a coarse distillation tower and a rectification tower in turn, and the combination mode and the number of tower plates of the coarse distillation tower and the rectification tower can be adjusted at will according to actual conditions. Wherein the coarse distillation tower is used for separating the fuel ethanol in the fermented mature mash in the form of alcohol steam from the fermented mature mash, and the rectification tower is used for further reducing the water vapor content in the alcohol steam. In one embodiment, the distillation system comprises, in order, a crude distillation column, a first rectification column and a second rectification column. In addition, the distillation system adopts thermal coupling, wherein fresh direct steam is used as a heat source for the first rectifying tower, overhead gas of the first rectifying tower is used as a heat source for the second rectifying tower, and overhead gas of the second rectifying tower is used as a heat source for the rough distillation tower, so that the steam consumption is low, and the energy consumption is reduced. The fermented mash enters a coarse distillation tower after being preheated to 60 ℃ in three stages, wherein the heat source for preheating in the first stage is the top gas of the coarse distillation tower, the heat source for preheating in the second stage is the side gas of the coarse distillation tower, and the heat source for preheating in the third stage is the finished product wine gas of a molecular sieve system, so that additional steam consumption is not needed. In addition, the bottom liquid of the first rectifying tower and the bottom liquid of the second rectifying tower hardly contain fuel ethanol, and can be independently used as stirring water or cleaning water of powder slurry or mixed with the bottom liquid of the rough distillation tower to form waste mash of a distillation system, so that the consumption of water is saved.
In one embodiment, the distillation system preferably produces an alcohol vapor having a volume fraction of fuel ethanol vapor of 92-95%.
In one embodiment, the molecular sieve system in step (5) is composed of an adsorption tower and a desorption tower, and the adsorption tower and the desorption tower can be automatically controlled and switched. Alcohol vapor extracted by the distillation system enters an adsorption tower after passing through a superheater, finished product alcohol gas is obtained after dehydration in the adsorption tower, and anhydrous fuel ethanol is obtained after the finished product alcohol gas is cooled. Meanwhile, the desorption tower is subjected to back washing and vacuumizing regeneration, and the two towers work alternately. The light wine which is back flushed to contain a small amount of fuel ethanol enters a light wine recovery tank and is circulated to a distillation system, so that the waste of the fuel ethanol is avoided, and the yield of the fuel ethanol are improved.
In the present invention, the waste mash of the distillation system in the step (6) means a liquid phase mixture obtained by fractionating fermented matured mash by the distillation system. In embodiments where the distillation system comprises a coarse distillation column and a rectification column, the mash of the distillation system consists of the coarse distillation column bottoms and a portion of the rectification column bottoms. Wherein the solid content in the bottom liquid of the coarse distillation tower is high, and the bottom liquid contains the solid content of the rice DDGS; the solid content in the bottom liquid of the rectifying tower is extremely low, and the rectifying tower is mainly used for diluting the bottom liquid of the coarse distillation tower.
In step (6), as long as the waste mash of the distillation system can be separated into a clear liquid and a wet tank, the separation method is not particularly limited, and examples thereof include a plate and frame filter press and a horizontal screw separator. In one embodiment, in step (6), the separated wet tank has a solids content of 36-38 wt% and a clear liquid solids content of 4-5 wt%. Evaporating and concentrating the clear liquid to obtain clear liquid concentrate with solid content of 32-35 wt%.
In the step (6), as long as the wet tank and the mixture of the wet tank and the clear liquid concentrate can be dried, the manner of drying is not particularly limited, and for example, a drum dryer, a tube bundle dryer, or the like can be used. In one embodiment, the wet grains are conveyed to a drum dryer by a screw conveyor, and the dry grains produced by the drum dryer are conveyed to a tube bundle dryer by the screw conveyor, and the clear liquid concentrate is added and dried by the tube bundle dryer to obtain the rice DDGS with the moisture content of less than 10 wt%.
In the present invention, the type of the external heat exchanger is not particularly limited as long as the liquefaction tank, the activation tank, and the yeast tank can maintain their respective temperatures. In the present invention, the external heat exchanger is preferably an external plate heat exchanger.
In the invention, in order to avoid the problems of abrasion of pipelines and equipment, pipeline blockage and the like caused by large-particle materials, the materials of the screen mesh, the pipelines, the plate heat exchanger, the tower plate and the like of the vibrating screen used in the invention are low-alloy structural steel with higher toughness and wear resistance to replace carbon steel and stainless steel 316L, thereby prolonging the service life of the equipment and reducing the maintenance cost.
Examples
The following describes exemplary embodiments of the present invention, and it should be understood by those skilled in the art that the following embodiments do not limit specific embodiments of the present invention, and should be interpreted to include all modifications, equivalents, and alternatives falling within the spirit and scope of the present invention. Many modifications and other embodiments are within the ability of one of ordinary skill in the art and are contemplated as falling within the scope of the invention.
Reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Detection and screening of rice raw material
In the process of the present invention, rice is used as a feedstock to produce fuel ethanol and rice DDGS. In order to ensure the quality and yield of rice DDGS, a certain amount of aged grain samples are extracted, and high performance liquid chromatography (Agilent1200) is adopted to detect mycotoxins in aged grains and corns with different storage years. Table 1 shows the mycotoxin levels in corn and aged grains of different storage years and four mycotoxin limit standards, wherein the vomitoxin limit standard is from GB 2761-2011 and the other mycotoxin limit standards are from GB/T25866-2010.
TABLE 1 mycotoxin content in corn and aged grains
*: the total content refers to the total content of four mycotoxins
As can be seen from Table 1, the total content of the four mycotoxins in corn was 916ppb, while the total content of the four mycotoxins in aged grains stored for 3-5 years was 450-959 ppb. In addition, corn has relatively high zearalenone content, and thus, the present invention preferably uses aged grains with a storage life of 3-5 years, more preferably aged grains with a storage life of 3-4 years.
Example 1
(1) Rice crushing pretreatment: aged grains with the storage life of 3 years are sequentially passed through a specific gravity stoner (model: TQSF200), an electromagnetic iron remover (model: RCDB) and a roller grading sieve (model: GS1530) to remove impurities such as sand, ironware, braided fabrics and the like. The rice under the screen of the roller grading screen passes through a sand-water separator to be used as a part of rice powder, the rice on the screen is further crushed by a hammer mill (model: PC-0604), the particle diameter of the rice powder particles after the rice under the screen and the rice on the screen are crushed is 25 meshes of screen mesh, the materials are separated from impurities such as dust by a CZT type cyclone separator after being mixed, and the rice powder passing through the 25 meshes of screen mesh is obtained.
(2) Preparing liquefied mash: uniformly mixing rice flour and water to form a flour slurry, wherein the material-water ratio of the rice flour is 1:2, adjusting the pH to 5.3 by using sulfuric acid, controlling the dry matter concentration of the flour slurry to be 28%, and adding 0.3kg/t of high-temperature amylase (from Novitin) relative to the mass of the rice raw material. Preheating to 55 deg.C in a slurry tank, feeding into a steam liquefaction ejector (HYW-D) at a feeding speed of 100t/h, injecting the slurry into a cooking maintaining tank with a temperature of 95 deg.C after liquefaction by the steam liquefaction ejector. Then the temperature is reduced to 86 ℃ after negative pressure flash evaporation, the mixture enters a liquefaction tank for liquefaction for 150min, and after the liquefaction is finished, the temperature is reduced to 70 ℃ through negative pressure flash evaporation, and then the temperature is reduced to 32 ℃ through a plate heat exchanger, so that liquefied mash is obtained.
(3) Preparing yeast mash: adding the liquefied mash, water and yeast wine into an activation tank, wherein the mass ratio of the liquefied mash to the water to the yeast wine is 10:5:1, introducing sterile air, maintaining the activation temperature at 35 ℃ through an external plate heat exchanger, and hydrating and activating the yeast wine to form activation liquid. And (3) introducing the activation liquid into a yeast tank filled with liquefied mash, wherein the mass ratio of the activation liquid to the liquefied mash is 1:9, introducing sterile air, and adding 3kg/t of ammonium sulfate into the yeast tank to serve as an inorganic nitrogen source. Under the aerobic condition, the yeast is rapidly propagated in large quantities and generates heat, the heat is taken away through external circulation of the external plate heat exchanger, and the propagation temperature is maintained at 29 ℃. After culturing for 15h, the number of yeast is more than 2.5 hundred million/mL to obtain yeast mash.
(4) Preparing fermented mature mash: the remaining liquefied mash was added to a fermentation tank, and sulfuric acid was added to adjust the pH to 4.3, and 2.14kg/t of a high-efficiency saccharifying enzyme (Novoxil), 1.02kg/t of urea, and 8kg/t of ammonium sulfate were added to the mass of the rice raw material. In the fermentation tank, the yeast mash is added with the inoculation amount of 15% (v/v), and the fermentation is carried out by adopting a synchronous saccharification and fermentation process of intermittent operation. During the fermentation process, the fermentation temperature is controlled to be 30 ℃ in the first 8h, the fermentation temperature is controlled to be 33 ℃ after 8h, and the fermentation is finished after 60h to obtain fermented mash.
(5) Preparing fuel ethanol: the distillation system consists of a crude distillation tower, a first rectifying tower and a second rectifying tower. The fermented mature mash is preheated by three stages (the fermented mature mash is preheated by three stages)The heat source of the first-stage preheating is the top gas of the crude distillation tower, the heat source of the second-stage preheating is the side gas of the crude distillation tower, and the heat source of the third-stage preheating is the finished product wine gas of a molecular sieve system) reaches 60 ℃, and then 100m is used3The feed amount per hour sequentially enters a rough distillation tower, a first rectifying tower and a second rectifying tower, wherein the number of the plates of the rough distillation tower, the first rectifying tower and the second rectifying tower is 32, 9 and 32 respectively. Fresh direct steam is adopted as a heat source in the first rectifying tower, the gas at the top of the first rectifying tower is used as a heat source in the second rectifying tower, and the gas at the top of the second rectifying tower is used as a heat source in the rough rectifying tower. And (3) using the bottom liquid of the first rectifying tower as the stirring water in the step (2). And 93% (v/v) alcohol steam is extracted from the top of the second rectifying tower, and enters a molecular sieve system consisting of an adsorption tower and a desorption tower after passing through a superheater. Dehydrating the alcohol vapor in an adsorption tower to obtain finished product liquor gas, and cooling to obtain 14m3And h, the desorption tower is subjected to back washing and vacuumizing regeneration, and the two towers work alternately. And (4) backwashing the desorption tower to wash out the light wine containing a small amount of fuel ethanol, feeding the light wine into a light wine recovery tank, and circulating the light wine to the first rectifying tower.
(6) Preparing rice DDGS: and mixing the bottom kettle liquid of the coarse distillation tower and the bottom kettle liquid of the second rectification tower to form waste mash of the distillation system, and separating clear liquid and wet grains from the waste mash by a plate-and-frame filter press. Wherein the solid content of the wet grains is 36 wt%, and the solid content of the clear liquid is 4 wt%. Evaporating and concentrating the clear liquid to obtain clear liquid concentrate with the solid content of 32 wt%. And (3) feeding the wet grains into a drum dryer through a screw conveyor, feeding the dry grains generated by the drum dryer into a tube bundle dryer through the screw conveyor, simultaneously adding clear liquid concentrate, and drying through the tube bundle dryer to obtain the rice DDGS with the water content of 8 wt%.
Example 2
(1) Rice crushing pretreatment: aged grains with the storage life of 4 years are sequentially passed through a specific gravity stoner (model: TQSF200), an electromagnetic iron remover (model: RCDB) and a roller grading sieve (model: GS1530) to remove impurities such as sand, iron ware, braided fabrics and the like. The rice under the screen of the roller grading screen passes through a sand-water separator to be used as a part of rice powder, the rice on the screen is further crushed by a hammer mill (model: PC-0604), the particle diameter of the rice powder particles after the rice under the screen and the rice on the screen are crushed is 25 meshes of screen mesh, the materials are separated from impurities such as dust by a CZT type cyclone separator after being mixed, and the rice powder passing through the 25 meshes of screen mesh is obtained.
(2) Preparing liquefied mash: uniformly mixing rice flour and water to form a flour slurry, wherein the material-water ratio of the rice flour is 1:2, adjusting the pH to 5.3 by using sulfuric acid, controlling the dry matter concentration of the flour slurry to be 28 wt%, and adding 0.3kg/t of high-temperature amylase (from Novitin) relative to the mass of the flour slurry. Preheating to 55 deg.C in a slurry tank, feeding into a steam liquefaction ejector (HYW-D) at a feeding speed of 100t/h, injecting the slurry into a cooking maintaining tank with a temperature of 95 deg.C after liquefaction by the steam liquefaction ejector. Then the temperature is reduced to 86 ℃ after the liquefaction and negative pressure flash evaporation, the mixture enters a liquefaction tank for liquefaction for 150min, and after the liquefaction is finished, the temperature is reduced to 70 ℃ through flash evaporation, and then the temperature is reduced to 32 ℃ through a plate heat exchanger, so that liquefied mash is obtained.
(3) Preparing yeast mash: adding the liquefied mash, water and yeast wine into an activation tank, wherein the mass ratio of the liquefied mash to the water to the yeast wine is 10:5:1, introducing sterile air, maintaining the activation temperature of 35 ℃ through an external plate heat exchanger, and hydrating and activating the yeast wine to form an activation solution. And (3) introducing the activation liquid into a yeast tank filled with liquefied mash, wherein the mass ratio of the activation liquid to the liquefied mash is 1:9, introducing sterile air, and adding 3kg/t of ammonium sulfate into the yeast tank to serve as an inorganic nitrogen source. Under the aerobic condition, the yeast is rapidly propagated in large quantities and generates heat, the heat is taken away through external circulation of the external plate heat exchanger, and the propagation temperature is maintained at 29 ℃. After culturing for 15h, the number of yeast is more than 2.5 hundred million/mL to obtain yeast mash.
(4) Preparing fermented mature mash: the remaining liquefied mash was added to a fermentation tank, and sulfuric acid was added to adjust the pH to 4.3, and 2.14kg/t of a high-efficiency saccharifying enzyme (Novoxil), 1.02kg/t of urea, and 8kg/t of ammonium sulfate were added to the mass of the remaining liquefied mash. In the fermentation tank, the yeast mash is added with the inoculation amount of 15% (v/v), and the fermentation is carried out by adopting a synchronous saccharification and fermentation process of intermittent operation. During the fermentation process, the fermentation temperature is controlled to be 30 ℃ in the first 8h, the fermentation temperature is controlled to be 33 ℃ after 8h, and the fermentation is finished after 60h to obtain fermented mash.
(5) Preparing fuel ethanol: the distillation system consists of a crude distillation tower, a first rectifying tower and a second rectifying tower. After the mature fermented mash reaches 60 ℃ through three-stage preheating (wherein the heat source of the first-stage preheating is crude distillation tower top gas, the heat source of the second-stage preheating is crude distillation tower side gas, and the heat source of the third-stage preheating is finished product wine gas of a molecular sieve system), 100m of mature fermented mash is used3The feed amount per hour sequentially enters a rough distillation tower, a first rectifying tower and a second rectifying tower, wherein the number of the plates of the rough distillation tower, the first rectifying tower and the second rectifying tower is 32, 9 and 32 respectively. Fresh direct steam is adopted as a heat source in the first rectifying tower, the gas at the top of the first rectifying tower is used as a heat source in the second rectifying tower, and the gas at the top of the second rectifying tower is used as a heat source in the rough rectifying tower. And (3) using the bottom liquid of the first rectifying tower as water for stirring in the step (2). And 93% (v/v) alcohol steam is extracted from the top of the second rectifying tower, and enters a molecular sieve system consisting of an adsorption tower and a desorption tower after passing through a superheater. Dehydrating the alcohol vapor in an adsorption tower to obtain finished product liquor gas, and cooling to obtain 14m3And h, the desorption tower is subjected to back washing and vacuumizing regeneration, and the two towers work alternately. And (4) backwashing the desorption tower to wash out the light wine containing a small amount of fuel ethanol, feeding the light wine into a light wine recovery tank, and circulating the light wine to the first rectifying tower.
(6) Preparing rice DDGS: and mixing the bottom kettle liquid of the coarse distillation tower and the bottom kettle liquid of the second rectification tower to form waste mash of the distillation system, and separating clear liquid and wet grains from the waste mash by a plate-and-frame filter. Wherein the solid content of the wet grains is 37 wt%, and the solid content of the clear liquid is 5 wt%. Evaporating and concentrating the clear liquid to obtain clear liquid concentrate with the solid content of 34 wt%. Feeding wet grains into a drum dryer through a screw conveyor, feeding dry grains generated by the drum dryer into a tube bundle dryer through the screw conveyor, simultaneously adding clear liquid concentrate, and drying through the tube bundle dryer to obtain rice DDGS with the water content of 9 wt%
Example 3
(1) Rice crushing pretreatment: the aged grains with the storage life of 5 years are sequentially passed through a specific gravity stoner (model: TQSF200), an electromagnetic iron remover (model: RCDB) and a roller grading sieve (model: GS1530) to remove impurities such as sand, iron ware, braided fabrics and the like. The rice under the screen of the roller grading screen passes through a sand-water separator to be used as a part of rice powder, the rice on the screen is further crushed by a hammer mill (model: PC-0604), the particle diameter of the rice powder particles after the rice under the screen and the rice on the screen are crushed is 25 meshes of screen mesh, the materials are separated from impurities such as dust by a CZT type cyclone separator after being mixed, and the rice powder passing through the 25 meshes of screen mesh is obtained.
(2) Preparing liquefied mash: uniformly mixing rice flour and water to form a flour slurry, wherein the material-water ratio of the rice flour is 1:2, adjusting the pH to 5.3 by using sulfuric acid, controlling the dry matter concentration of the flour slurry to be 28 wt%, and adding 0.3kg/t of high-temperature amylase (from Novitin) relative to the mass of the flour slurry. Preheating to 55 deg.C in a slurry tank, feeding into a steam liquefaction ejector (HYW-D) at a feeding speed of 100t/h, injecting the slurry into a cooking maintaining tank with a temperature of 95 deg.C after liquefaction by the steam liquefaction ejector. Then the temperature is reduced to 86 ℃ after the liquefaction and negative pressure flash evaporation, the liquefied mash enters a liquefaction tank for liquefaction for 150min, the temperature is reduced to 70 ℃ after the liquefaction, and the temperature is reduced to 32 ℃ through a plate heat exchanger, so that the liquefied mash is obtained.
(3) Preparing yeast mash: adding the liquefied mash, water and yeast wine into an activation tank, wherein the mass ratio of the liquefied mash to the water to the yeast wine is 10:5:1, introducing sterile air, maintaining the activation temperature of 35 ℃ through an external plate heat exchanger, and hydrating and activating the yeast wine to form an activation solution. And (3) introducing the activation liquid into a yeast tank filled with liquefied mash, wherein the mass ratio of the activation liquid to the liquefied mash is 1:9, introducing sterile air, and adding 3kg/t of ammonium sulfate into the yeast tank to serve as an inorganic nitrogen source. Under the aerobic condition, the yeast is rapidly propagated in large quantities and generates heat, the heat is taken away through external circulation of the external plate heat exchanger, and the propagation temperature is maintained at 29 ℃. After culturing for 15h, the number of yeast is more than 2.5 hundred million/mL to obtain yeast mash.
(4) Preparing fermented mature mash: the remaining liquefied mash was added to a fermentation tank, and sulfuric acid was added to adjust the pH to 4.3, and 2.14kg/t of a high-efficiency saccharifying enzyme (Novoxil), 1.02kg/t of urea, and 8kg/t of ammonium sulfate were added to the mass of the remaining liquefied mash. In the fermentation tank, the yeast mash is added with the inoculation amount of 15% (v/v), and the fermentation is carried out by adopting a synchronous saccharification and fermentation process of intermittent operation. During the fermentation process, the fermentation temperature is controlled to be 30 ℃ in the first 8h, the temperature is controlled to be 33 ℃ after 8h, and the fermentation is finished after 60h to obtain fermented mash.
(5) Preparing fuel ethanol: the distillation system consists of a crude distillation tower, a first rectifying tower and a second rectifying tower. After the mature fermented mash reaches 60 ℃ through three-stage preheating (wherein the heat source of the first-stage preheating is crude distillation tower top gas, the heat source of the second-stage preheating is crude distillation tower side gas, and the heat source of the third-stage preheating is finished product wine gas of a molecular sieve system), 100m of mature fermented mash is used3The feed amount per hour sequentially enters a rough distillation tower, a first rectifying tower and a second rectifying tower, wherein the number of the plates of the rough distillation tower, the first rectifying tower and the second rectifying tower is 32, 9 and 32 respectively. Fresh direct steam is adopted as a heat source in the first rectifying tower, the gas at the top of the first rectifying tower is used as a heat source in the second rectifying tower, and the gas at the top of the second rectifying tower is used as a heat source in the rough rectifying tower. And (3) using the bottom liquid of the first rectifying tower as the stirring water in the step (2). 94% (v/v) alcohol steam is extracted from the top of the second rectifying tower, and enters a molecular sieve system consisting of an adsorption tower and a desorption tower after passing through a superheater. Dehydrating the alcohol vapor in an adsorption tower to obtain finished product liquor gas, and cooling to obtain 14m3And h, the desorption tower is subjected to back washing and vacuumizing regeneration, and the two towers work alternately. And (4) backwashing the desorption tower to wash out the light wine containing a small amount of fuel ethanol, feeding the light wine into a light wine recovery tank, and circulating the light wine to the first rectifying tower.
(6) Preparing rice DDGS: and mixing the bottom kettle liquid of the coarse distillation tower and the bottom kettle liquid of the second rectification tower to form waste mash of the distillation system, and separating clear liquid and wet grains from the waste mash by a plate-and-frame filter press. Wherein, the solid content of the wet grains is 38wt percent, and the solid content of the clear liquid is 5wt percent. Evaporating and concentrating the clear liquid to obtain clear liquid concentrate with the solid content of 34 wt%. And (3) feeding the wet grains into a drum dryer through a screw conveyor, feeding the dry grains generated by the drum dryer into a tube bundle dryer through the screw conveyor, simultaneously adding clear liquid concentrate, and drying through the tube bundle dryer to obtain the rice DDGS with the water content of 7 wt%.
The ethanol volume fractions and the component contents of the ethanol as an anhydrous fuel obtained in examples 1 to 3 are shown in table 2. As can be seen from Table 2, the absolute fuel ethanol produced in the examples 1 to 3 meets the national standard GB18350-2013, and the absolute ethanol fuel obtained by the method disclosed by the invention has high ethanol volume fraction and low content of other corresponding impurities, so that the absolute fuel ethanol is an extremely environment-friendly green clean energy.
Table 2 comparison of fuel ethanol produced in examples 1-3 with national standards
Comparative example 1
The procedure of comparative example 1 was the same as in example 1 except that the aged grain was replaced with corn, to obtain ethanol as an anhydrous fuel and corn DDGS. Through calculation, the cost price of producing each ton of fuel ethanol by taking the aged grain as the raw material is 3603 yuan/t, and the cost price of taking the corn as the raw material is 4355 yuan/t, so that the aged grain has more economic advantages when being taken as the raw material.
Table 3 below shows the protein and mycotoxin contents of the DDGS produced in examples 1 to 3 and comparative example 1, wherein the protein content in the DDGS was measured by Kjeldahl method and the mycotoxin content was measured by high performance liquid chromatography.
TABLE 3 comparison of protein and mycotoxin levels of DDGS produced in examples 1-3 and comparative example 1
*: the total content refers to the total content of four mycotoxins
As can be seen from Table 3, the zearalenone content in the rice DDGS produced in examples 1-3 was lower than that in the corn DDGS in comparative example 1. Zearalenone is known to have estrogen-like action, can cause acute and chronic poisoning of animals, cause abnormal and even death of animal reproductive functions, and can cause huge economic loss to animal farms when the content of zearalenone in DDGS is too high. In addition, zearalenone is not easy to be destroyed because it is residual, and if animal takes DDGS feed with high content of zearalenone for a long time, zearalenone will accumulate in animal body for a long time, and once human takes such animal, it will also possibly cause human body lesion. Further, the total content of four mycotoxins in the DDGS produced in examples 1-3 was also lower compared to comparative example 1. It can be seen that the rice DDGS produced by the method of the present invention is safer, especially when aged grains with a storage life of 3-4 years are used, the rice DDGS produced by the method has four mycotoxin contents (especially zearalenone) which are far lower than the corn DDGS produced by corn.
In addition, the protein content in the rice DDGS produced in examples 1 to 3 was also much higher than that in the corn DDGS produced in comparative example 1, and the protein in the rice DDGS was a high-quality complete protein without allergen, which included rice protein and yeast protein. The rice DDGS obtained by the method of the present invention is also much higher in nutritional value than corn DDGS obtained by corn production.
Claims (11)
1. A method of processing rice to produce fuel ethanol and byproduct rice DDGS, the method comprising the steps of:
(1) rice crushing pretreatment: removing impurities from the rice, and crushing the rice by a crusher to obtain rice powder passing through a 25-mesh screen, wherein the rice is aged grain;
(2) preparing liquefied mash: uniformly mixing rice powder and water to form powder slurry, adjusting the pH value to 5.2-5.5, adding high-temperature amylase, preheating the powder slurry to 55 ℃ in a powder slurry tank, injecting high-temperature steam for liquefaction, then entering a cooking maintaining tank, keeping the temperature in the cooking maintaining tank to be 95 ℃, reducing the temperature to 86 ℃ after negative pressure flash evaporation, entering a liquefaction tank for liquefaction, reducing the temperature to 70 ℃ through negative pressure flash evaporation after liquefaction, and reducing the temperature to 31-32 ℃ through a heat exchanger to obtain liquefied mash;
(3) preparing yeast mash: adding liquefied mash, water and yeast wine into an activation tank, introducing sterile air, maintaining the activation temperature at 34-36 ℃ through an external heat exchanger, and hydrating and activating the yeast wine to form activation liquid; introducing the activation liquid into a yeast tank filled with liquefied mash, introducing sterile air, maintaining propagation temperature of 28-30 ℃ through an external heat exchanger, and rapidly propagating yeast under aerobic condition until the yeast number reaches more than 2.5 hundred million/mL to obtain yeast mash;
(4) preparing fermented mature mash: adding the rest of the liquefied mash into a fermentation tank, adjusting pH to 4.2-4.4, and simultaneously adding saccharifying enzyme and urea; adding yeast mash into a fermentation tank by 15 volume percent of inoculation amount, and fermenting in the fermentation tank under the anaerobic condition to obtain fermented mature mash, wherein the fermentation is synchronous diastatic fermentation, the synchronous diastatic fermentation is intermittent operation, and the fermentation temperature is controlled to be 30 ℃ within the first 8h in the fermentation process of the intermittent operation; after 8h, controlling the fermentation temperature to be 32.5-33.5 ℃;
(5) preparing fuel ethanol: preheating fermented mash, then feeding the preheated fermented mash into a distillation system, feeding alcohol steam extracted from the distillation system into a molecular sieve system after passing through a superheater, and dehydrating and cooling to obtain anhydrous fuel ethanol;
(6) preparing rice DDGS: and filtering and separating waste mash of the distillation system to obtain clear liquid and wet grains, evaporating and concentrating the clear liquid to obtain clear liquid concentrate, drying the wet grains, mixing the wet grains with the clear liquid concentrate, and drying the mixture in a dryer to obtain the rice DDGS.
2. The method according to claim 1, wherein before step (1), the method further comprises the steps of performing mycotoxin detection and screening on the rice.
3. The method according to claim 2, wherein the rice is subjected to mycotoxin detection and screening by using high performance liquid chromatography.
4. The method according to claim 1 or 2, wherein the rice is aged grain having a storage life of 3 to 5 years.
5. The method according to claim 1 or 2, wherein the rice is aged grain having a storage life of 3 to 4 years.
6. The method as claimed in any one of claims 1 to 3, wherein, in the step (2), the mixing ratio of the rice flour to the water is 1:1.9-1: 2.1; the dry matter concentration of the powder slurry is controlled to be 27-29 wt%; the addition amount of the high-temperature amylase is 0.3kg/t relative to the mass of the rice; the liquefaction time in the liquefaction tank is 140-160 min.
7. The method according to any one of claims 1 to 3, wherein in step (3) the propagation time of the yeast in the yeast tank is 12 to 18 h.
8. A process according to any one of claims 1 to 3, wherein an inorganic nitrogen source selected from one or more of ammonium sulphate, ammonium nitrate and ammonium chloride is added to the wine mother tank in step (3) and the fermentor in step (4).
9. The method of claim 8, wherein the inorganic nitrogen source is ammonium sulfate.
10. The method of any one of claims 1-3, wherein in step (5), the distillation system is thermally coupled and comprises a crude distillation column and a rectification column; the molecular sieve system comprises an adsorption tower and a desorption tower.
11. The method of any one of claims 1-3, wherein the rice DDGS has a moisture content of less than 10 wt% in step (6).
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| CN111100881A (en) * | 2020-02-10 | 2020-05-05 | 吉林中粮生化有限公司 | Method for producing ethanol by fermenting starch raw material |
| CN111187790B (en) * | 2020-04-09 | 2020-07-14 | 中粮营养健康研究院有限公司 | Method for preparing ethanol by using rice raw material |
| CN111304261B (en) * | 2020-04-09 | 2023-08-08 | 吉林中粮生化有限公司 | Method for producing ethanol by fermentation |
| CN114250251B (en) * | 2020-09-23 | 2024-02-23 | 中粮生物科技股份有限公司 | Method for producing ethanol |
| CN114685246B (en) * | 2020-12-29 | 2023-07-11 | 国投生物科技投资有限公司 | System and method for co-production of fuel ethanol and alcohol |
| CN115029388A (en) * | 2021-03-05 | 2022-09-09 | 国投生物科技投资有限公司 | Method for co-producing ethanol and DDGS (distillers dried grains with soluble) by fermenting raw materials with wheat |
| CN113061627B (en) * | 2021-03-23 | 2022-03-22 | 中建安装集团有限公司 | Energy-saving process for producing fuel ethanol by using starch-based raw materials |
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