Analysis of Heat Transfer Fouling by Dry‐Grind Maize Thin Stillage Using an Annular Fouling Apparatus

In dry‐grind processing to produce ethanol from corn, unfermented solids are removed from ethanol by distillation and dried to produce distillers dried grains with solubles (DDGS), an animal food. Fouling of thin stillage evaporators has been identified as an important energy consumption issue in dry‐grind facilities. Using an annular fouling apparatus, four batches of thin stillage were analyzed to determine repeatability of fouling rate and induction period measurements. Dry solids, protein and ash concentrations, and pH were correlated to fouling rate and induction period to determine how variation in thin stillage from the same dry‐grind facility affects these fouling parameters. Effects of increasing Reynolds number (Re) in the laminar region on fouling rate, induction period, and fouling deposit protein and ash concentrations were also determined. Repeatability of fouling rate measurements was similar to other studies (CV < 7.0%) but repeatability of induction period measurements was high relative to other studies (CV < 88.7%). Fouling rate increased with increasing dry solids concentration. Thin stillage at Re = 440 had shorter induction periods and greater fouling rates than at Re = 880. Fouling deposits collected from Re = 440 tests had similar protein concentrations and lower ash concentrations compared with deposits from Re = 880 tests.     

Economics of Germ Preseparation for Dry-Grind Ethanol Facilities

A detailed economic analysis of a 914 tonnes/day (36,000 bu/day) “Quick Germ” ethanol process was performed. The Quick Germ ethanol process is a combination of a dry-grind and a wet-milling ethanol process. The Quick Germ ethanol process increases the coproduct value in the dry-grind ethanol process by recovering germ before fermentation. Germ is recovered using the conventional wet-milling degermination process. Economic assessment of the Quick Germ process proved profitable. The savings achieved by recovering germ as a coproduct and by increasing the fermentor capacity due to removal of nonfermentables from the corn mash will reduce the manufacturing cost of ethanol by 2.69 ¢/L (10.19 ¢/gal or $0.265/bu) when compared to the conventional dry-grind ethanol process.     

Effect of pH on Fouling Characteristics and Deposit Compositions in Dry‐Grind Thin Stillage

Dry‐grind corn processing facilities produce ethanol, carbon dioxide, and distillers dried grains with solubles (DDGS). To produce DDGS, dry‐grind corn processors concentrate thin stillage in multieffect evaporators. Concentration of thin stillage uses large amounts of energy, and efficient operation is important for long‐term economic stability of the industry. Little data are available on fouling of evaporators during thin stillage concentration. We evaluated how thin stillage pH and acid type used during pH adjustment affected fouling as measured by induction period, fouling rate, and deposit composition. Using an annular fouling apparatus, fouling tests were conducted at pH 3.5, 4.0, and 4.5. In a second experiment, we used two types of acid, HCl or H₂SO₄, to adjust thin stillage to pH 3.5. Induction periods were shorter at pH 3.5 than at pH 4.0 or 4.5. As pH increased, fouling deposit protein decreased and ash increased. Concentrations of most elements, including P, Ca, Mg, Mn, and K, increased with an increase in pH. Phosphorus was the most abundant mineral element in fouling deposits. Induction periods were similar for the two acids. Thin stillage pH has an influence on deposit concentration, fouling rate, and induction period.     

Effect of the corn breaking method on oil distribution between stillage phases of dry-grind corn ethanol production

The majority of fuel ethanol in the United States is produced by using the dry-grind corn ethanol process. The corn oil that is contained in the coproduct, distillers' dried grains with solubles (DDGS), can be recovered for use as a biodiesel feedstock. Oil removal will also improve the feed quality of DDGS. The most economical way to remove oil is considered to be at the centrifugation step for separating thin stillage (liquid) from coarse solids after distilling the ethanol. The more oil there is in the liquid, the more it can be recovered by centrifugation. Therefore, we studied the effects of corn preparation and grinding methods on oil distribution between liquid and solid phases. Grinding the corn to three different particle sizes, flaking, flaking and grinding, and flaking and extruding were used to break up the corn kernel before fermentation, and their effects on oil distribution between the liquid and solid phases were examined by simulating an industrial decanter centrifuge. Total oil contents were measured in the liquid and solids after centrifugation. Dry matter yield and oil partitioning in the thin stillage were highly positively correlated. Flaking slightly reduced bound fat. The flaked and then extruded corn meal released the highest amount of free oil, about 25% compared to 7% for the average of the other treatments. The freed oil from flaking, however, became nonextractable after the flaked corn was ground. Fine grinding alone had little effect on oil partitioning.     

Effects of Ground Corn Particle Size on Ethanol Yield and Thin Stillage Soluble Solids

The effects of ground corn particle size on ethanol yield and soluble solids in thin stillage was evaluated using a 2‐L laboratory dry‐grind procedure. The procedure was optimized for grinding, liquefaction, sacchari‐fication, and fermentation parameters. The optimized procedure was reproducible with a coefficient of variation of 3.6% in ethanol yield. Five particle size distributions of ground corn were obtained using a cross‐beater mill equipped with five screens (0.5, 2, 3, 4, and 5 mm). Particle size had an effect on ethanol yield and on soluble solids concentration in thin stillage. The highest ethanol yield of 12.6 mL/100 mL of beer was achieved using a 0.5‐mm screen in the cross‐beater mill. Treatment using the 0.5‐mm mill screen resulted in soluble solids concentration of 25.1 g/L and was higher than soluble solids concentrations obtained with other screens. No differences in soluble solid concentrations were observed in samples of thin stillage obtained from 2, 3, 4, and 5‐mm screens which had a mean yield of 16.2 g/L. By optimizing particle size for maximum ethanol yield and minimum solids in thin stillage, dry‐grind corn plants could realize reduced capital and operating costs.     

Laboratory Yields and Process Stream Compositions from E‐Mill and Dry‐Grind Corn Processes Using a Granular Starch Hydrolyzing Enzyme

In dry‐grind corn processing, the whole kernel is fermented to produce ethanol and distillers dried grains with solubles (DDGS); the E‐Mill process was developed to generate coproducts in addition to DDGS. Compositions of thin stillage and wet grains obtained from the E‐Mill process will be different from the dry‐grind process. Knowledge of thin stillage compositions will provide information to improve coproducts from both processes. Laboratory dry‐grind and E‐Mill processes that used granular starch hydrolyzing enzymes (GSHE) were compared and process yields determined. Two methods, centrifugation and screening, were used to produce thin stillage and wet grains from the laboratory processes. Compositions of process streams were determined. In the dry‐grind process using GSHE, solids contents of beer, whole stillage, and wet grains were higher compared to the same fractions from the E‐Mill process using GSHE. Solids contents of mash for both processes were similar. Total solids, soluble solids, and ash contents of thin stillage were similar for the two processes. Fat content of thin stillage from E‐Mill was lower than that from the dry‐grind process; protein content of E‐Mill thin stillage was higher than that from dry‐grind thin stillage. Removal of germ and fiber before fermentation changed composition of thin stillage from the E‐Mill process. The screening method produced higher thin stillage and lower wet grains yields than using a centrifugation method. The screening method was less time consuming but resulted in limited wet grains material for additional analyses or processing. The centrifugation method of thin stillage separation removed more solids from thin stillage than the screening method.     

Recovery of Fiber in the Corn Dry-Grind Ethanol Process: A Feedstock for Valuable Coproducts

A new process was developed to recover corn fiber from the mash before fermentation in dry-grind ethanol production. In this process, corn is soaked in water (no chemicals) for a short period of time and then degermed using conventional degermination mills. In the remaining slurry, corn coarse fiber is floated by increasing the density of the slurry and then separated using density differences. The fiber recovered is called quick fiber to distinguish it from the conventional wet-milled fiber. This study evaluated the percent of quick fiber recovery for a normal yellow dent and high oil corn hybrid. The quick fiber was analyzed for levels of corn fiber oil, levels of ferulate phytosterol esters (FPE) and other valuable phytosterol components in the oil and compared with conventional wet-milled corn coarse and fine fiber samples. Fiber samples were also analyzed and compared for yields of potentially valuable corn fiber gum (CFG, hemicellulose B). Comparisons were made between the quick fiber samples obtained with and without chemicals in the soakwater. An average quick fiber yield of 6–7% was recovered from the two hybrids and represented 46–60% of the total fiber (fine and coarse) that could be recovered by wet-milling these hybrids. Adding steep chemicals (SO₂ and lactic acid) to the soakwater increased the quick fiber yields, percent of FPE recoveries, and total percent of phytosterol components to levels either comparable to (for the dent corn hybrid) or higher than (for the high oil corn hybrid) those recovered from the total conventional wet-milled fiber samples. CFG yields in the quick fiber samples were comparable to those from the wet-milled fiber samples. CFG yields in the quick fiber samples were not significantly affected by the addition of chemicals (SO₂ and lactic acid) to the soakwater.     

Rapid NMR method for the quantification of organic compounds in thin stillage

Thin stillage contains organic and inorganic compounds, some of which may be valuable fermentation coproducts. This study describes a thorough analysis of the major solutes present in thin stillage as revealed by NMR and HPLC. The concentration of charged and neutral organic compounds in thin stillage was determined by excitation sculpting NMR methods (double pulse field gradient spin echo). Compounds identified by NMR included isopropanol, ethanol, lactic acid, 1,3-propanediol, acetic acid, succinic acid, glycerophosphorylcholine, betaine, glycerol, and 2-phenylethanol. The concentrations of lactic and acetic acid determined with NMR were comparable to those determined using HPLC. HPLC and NMR were complementary, as more compounds were identified using both methods. NMR analysis revealed that stillage contained the nitrogenous organic compounds betaine and glycerophosphorylcholine, which contributed as much as 24% of the nitrogen present in the stillage. These compounds were not observed by HPLC analysis.     

Fiber Separated from Distillers Dried Grains with Solubles as a Feedstock for Ethanol Production

In the dry-grind process, corn starch is converted into sugars that are fermented into ethanol. The remaining corn components (protein, fiber, fat, and ash) form a coproduct, distillers dried grains with solubles (DDGS). In a previous study, the combination of sieving and elutriation (air classification), known as the elusieve process, was effective in separating fiber from DDGS. In this study, elusieve fiber was evaluated for ethanol production and results were compared with those reported in other studies for fiber from different corn processing techniques. Fiber samples were pretreated using acid hydrolysis followed by enzymatic treatment. The hydrolyzate was fermented using Escherichia coli FBR5 strain. Efficiency of ethanol production from elusieve fiber was 89–91%, similar to that for pericarp fiber from wet-milling and quick fiber processes (86–90%). Ethanol yields from elusieve fiber were 0.23–0.25 L/kg (0.027–0.030 gal/lb); similar to ethanol yields from wet-milling pericarp fiber and quick fiber. Fermentations were completed within 50 hr. Elusieve fiber conversion could result in 1.2–2.7% increase in ethanol production from dry-grind plants. It could be economically feasible to use elusieve fiber along with other feedstock in a plant producing ethanol from cellulosic feedstocks. Due to the small scale of operation and the stage of technology development for cellulosic conversion to ethanol, implementation of elusieve fiber conversion to ethanol within a dry-grind plant may not be currently economically feasible.     

Quantification of Physical and Chemical Properties,and Identification of Potentially Valuable Components from Fuel Ethanol Process Streams

Wider exploration of ethanol coproduct uses is necessary as the ethanol industry continues to face challenges. Currently, process streams such as thin stillage and condensed distillers solubles (CDS) are processed into distillers dried grains with solubles and used as animal feeds, but other higher value opportunities may exist. The objective of this study was to identify chemical components and quantify physical properties of CDS and thin stillage. Protein, organic acid, and sugar profiles were determined. Zein protein was identified, and glycerol was determined to have a concentration of 18.8 g/L in thin stillage and 63.2 g/L in CDS. Physical properties including density, thermal conductivity, thermal diffusivity, and rheological behaviors were also examined. Thermal conductivity of thin stillage and CDS was approximately 0.54 and 0.45 W/m°C, respectively. Quantification of the physical properties and identification of the chemical constituents pave the way for exploration of new value‐added uses for thin stillage and CDS.     

Effect of Aflatoxin B1 on Dry‐Grind Ethanol Process

Aflatoxins, like all mycotoxins, are toxic fungal metabolites that can have adverse health effects on animals and human beings. Aflatoxins are a major concern for the dry‐grind corn processing industry as it is believed that aflatoxins affect yeast and reduce its efficacy in producing ethanol. In the present study, aflatoxin B1 (100, 200, 350, or 775 ppb) was added to mycotoxin‐free corn and laboratory‐scale fermentations were conducted. No effect of aflatoxin B1 was observed on the fermentation rates or final ethanol concentrations. Mean ethanol concentration in the fermenter was 14.01–14.51% (v/v) at 60 hr for all the treatments. In the dry‐grind ethanol process, 55% of aflatoxin B1 was detected in wet grains and 45% in thin stillage.     

Technique to Measure Surface‐Fouling Tendencies of Steepwater from Corn Wet Milling

Surface‐fouling tendencies of raw light steepwater (LSW) and membrane‐filtered light steepwater (FSW) from corn wet‐milling were studied using an annular fouling probe. The probe contained a heated surface to simulate the surface temperature of an evaporator. The heated region caused a fraction of solids in the steepwater to adhere to the surface, thus fouling the probe over time. FSW samples were prepared by filtering LSW using a microfiltration membrane with a nominal pore size of 0.1 μm. Fouling tendencies of both samples were established at an initial probe wall temperature of 99°C. Batches (30 L) were circulated through the fouling probe until the inner surface temperature of the probe reached 200°C. Temperature and power supplied to the probe were measured over time and used to calculate fouling resistance and rate of fouling. Measurement of maximum fouling resistance and fouling rate had a coefficient of variation (COV) of 5.1 and 7.4%, respectively. Maximum fouling resistances attained over a 12‐hr period were 0.36 and 0.049 m² °C/kW for LSW and FSW, respectively. Average rates of fouling were 4.53 × 10^‐4 and 0.82 × 10^‐4 m² °C/kW/min for LSW and FSW, respectively, showing an 80% decrease in fouling rate using microfiltration to remove 19% of solids.     

EFFECT OF SOIL AMENDMENT WITH THIN STILLAGE AND GLYCEROL ON PLANT GROWTH AND SOIL PROPERTIES

Controlled environment experiments were set up in 2007 and 2008 to evaluate the potential of using by-products of the biofuel industry as soil amendments to improve fertility and plant growth in Saskatchewan soils. Trials were run with thin stillage (a by-product of ethanol production) and glycerol (by-product of biodiesel production). Canola (B. napus L.) and wheat (T. aestivum) were grown as the test crop in amended pots. Plant yield, composition, and soil properties were measured after five weeks. The stillage was found to be an effective soil amendment for increasing plant biomass yield. Per unit of nitrogen (N) added, canola yields were less than that of urea when nitrogen was the only limitation, due to only a portion of the nitrogen in the thin stillage becoming available over the five week period. However, when nutrients other than nitrogen were limiting, canola dry matter yields with thin stillage amendment approached or exceeded that of urea, due to the ability of the amendments to supply other nutrients such as phosphorus in addition to nitrogen. Glycerol, an amendment that only contains carbon, hydrogen and oxygen, was effective in increasing soil organic carbon content, but required supplemental fertilizer to account for nutrient tie-up by microorganisms during decomposition in the soil. The amendments did not have any biologically significant effects on other soil chemical parameters measured, including soluble metals, pH or salinity.     

Enzymatic Process for Corn Dry‐Grind High‐Solids Fermentation

A modified dry‐grind process that combined the use of conventional amylases (glucoamylase [GA]), phytase, and granular starch hydrolyzing enzymes (GSHE) to achieve low liquefaction viscosities and low glucose concentrations during simultaneous saccharification and fermentation (SSF) with a high slurry solids content (>33% w/w) was developed. Doses of GSHE and GA were optimized for the modified process. At 35% solids content, the modified process had 80% lower slurry viscosity, 24% lower peak glucose concentration, 7.5% higher final ethanol concentration, and 51% higher fermentation rate compared with the conventional dry‐grind process. At 40% solids content, the modified process had lower viscosities, lower peak and residual glucose concentrations, and higher ethanol concentrations than the conventional process; however, the results were in contrast to those for 35% solids content. At 40% solids content, SSF did not run to completion for conventional or modified processes, and more than 2.5% w/v of residual glucose was left in the fermentation broth. Final ethanol concentration achieved with the modified process at 40% solids content was 19.5% v/v, similar to the ethanol concentration achieved with the modified process at 35% solids content. At 35% slurry solids content, a GSHE level of 1.25 μL/g db of corn and a GA level of 0.25 μL/g db of corn were selected as optimum enzyme doses for the modified process.     

Optimization of Fermentation Temperature and Mash Specific Gravity for Fuel Alcohol Production

The effects of fermentation temperature and dissolved solids concentration adjusted by changing mashing water-to-grain ratios on wheat fermentation efficiencies, fermentation times, final ethanol concentrations, and ethanol production rates were studied by using response surface methodology. Final ethanol concentrations in fermentors depended primarily on mash specific gravities. Predictably, increases in fermentation temperatures dramatically reduced fermentation times and thereby shortened fermentation cycles. The highest ethanol production rates were achieved with a high fermentation temperature of 30°C and a low water-to-grain ratio of 2.0. At these settings, an ethanol concentration of 13.6% (v/v) was attained with a fermentation time of 54 hr and an ethanol production rate of 2.45 mL of ethanol/L/hr. Optimization of operating conditions suggested in the current study will provide existing fuel alcohol plants with increased productivity without alteration of plant equipment or process flow.     

Quick Fiber Process: Effect of Mash Temperature,Dry Solids,and Residual Germ on Fiber Yield and Purity

Preliminary calculations showed that recovery of fiber before fermentation in the dry grind ethanol facilities known as the Quick Fiber process increases fermenter capacity and reduces ethanol production cost by as much as 4 ¢/gal. The objective of the current research was to evaluate the effect of mash temperature, dry solids, and residual germ on fiber yield and purity when using the quick fiber process. Fiber was recovered by flotation and skimming, while maintaining a specified temperature, dry solids, and residual germ in the mash. Varying temperature and dry solids in the mash resulted in a statistically significant effect on the fiber yield, neutral detergent fiber (NDF) content, and weight of NDF/100 g of dry corn. Varying residual germ in the mash resulted in statistically significant differences for NDF through dilution and the weight of NDF/100 g of dry corn. The highest fiber yield was 10.9% at 45°C, 23% dry solids, and 15% residual germ; the highest NDF was 50.9% at 30°C, 21% dry solids, and 0% residual germ. The highest weight of NDF/100 g of dry corn was observed at 45°C, 23% dry solids, and 0% residual germ.     

Ethanol Production from Modified and Conventional Dry‐Grind Processes Using Different Corn Types

Different corn types were used to compare ethanol production from the conventional dry‐grind process to wet or dry fractionation processes. High oil, dent corn with high starch extractability, dent corn with low starch extractability and waxy corn were selected. In the conventional process, corn was ground using a hammer mill; water was added to produce slurry which was fermented. In the wet fractionation process, corn was soaked in water; germ and pericarp fiber were removed before fermentation. In the dry fractionation process, corn was tempered, degerminated, and passed through a roller mill. Germ and pericarp fiber were separated from the endosperm. Due to removal of germ and pericarp fiber in the fractionation methods, more corn was used in the wet (10%) and dry (15%) fractionation processes than in the conventional process. Water was added to endosperm and the resulting slurry was fermented. Oil, protein, and residual starch in germ were analyzed. Pericarp fiber was analyzed for residual starch and neutral detergent fiber (NDF) content. Analysis of variance and Fisher's least significant difference test were used to compare means of final ethanol concentrations as well as germ and pericarp fiber yields. The wet fractionation process had the highest final ethanol concentrations (15.7% v/v) compared with dry fractionation (15.0% v/v) and conventional process (14.1% v/v). Higher ethanol concentrations were observed in fractionation processes compared to the conventional process due to higher fermentable substrate per batch available as a result of germ and pericarp fiber removal. Germ and pericarp yields were 7.47 and 6.03% for the wet fractionation process and 7.19 and 6.22% for the dry fractionation process, respectively. Germ obtained from the wet fractionation process had higher oil content (34% db) compared with the dry fractionation method (11% db). Residual starch content in the germ fraction was 16% for wet fractionation and 44% for dry fractionation. Residual starch in the pericarp fiber fraction was lower for the wet fractionation process (19.9%) compared with dry fractionation (23.7%).     

Factors Impacting Ethanol Production from Grain Sorghum in the Dry-Grind Process

The goal of this research is to understand the key factors affecting ethanol production from grain sorghum. Seventy genotypes and elite hybrids with a range of chemical compositions and physical properties selected from ≈1,200 sorghum lines were evaluated for ethanol production and were used to study the relationships of composition, grain structure, and physical features that affect ethanol yield and fermentation efficiency. Variations of 22% in ethanol yield and 9% in fermentation efficiency were observed among the 70 sorghum samples. Genotypes with high and low conversion efficiencies were associated with attributes that may be manipulated to improve fermentation efficiency. Major characteristics of the elite sorghum genotypes for ethanol production by the dry-grind method include high starch content, rapid liquefaction, low viscosity during liquefaction, high fermentation speed, and high fermentation efficiency. Major factors adversely affecting the bioconversion process are tannin content, low protein digestibility, high mash viscosity, and an elevated concentration of amylose-lipid complex in the mash.     

Chemical composition of distillers grains, a review

In recent years, increasing demand for ethanol as a fuel additive and decreasing dependency on fossil fuels have resulted in a dramatic increase in the amount of grains used for ethanol production. Dry-grind is the major process, resulting in distillers dried grains with solubles (DDGS) as a major coproduct. Like fuel ethanol, DDGS has quickly become a global commodity. However, high compositional variation has been the main problem hindering its use as a feed ingredient. This review provides updated information on the chemical composition of distillers grains in terms of nutrient levels, changes during dry-grind processing, and causes for large variation. The occurrence in grain feedstock and the fate of mycotoxins during processing are also covered. During processing, starch is converted to glucose and then to ethanol and carbon dioxide. Most other components are relatively unchanged but concentrated in DDGS about 3-fold over the original feedstock. Mycotoxins, if present in the original feedstock, are also concentrated. Higher fold of increases in S, Na, and Ca are mostly due to exogenous addition during processing, whereas unusual changes in inorganic phosphorus (P) and phytate P indicate phytate hydrolysis by yeast phytase. Fermentation causes major changes, but other processing steps are also responsible. The causes for varying DDGS composition are multiple, including differences in feedstock species and composition, process methods and parameters, the amount of condensed solubles added to distiller wet grains, the effect of fermentation yeast, and analytical methodology. Most of them can be attributed to the complexity of the dry-grind process itself. It is hoped that information provided in this review will improve the understanding of the dry-grind process and aid in the development of strategies to control the compositional variation in DDGS.     

Solvent Extraction of Zein from Dry‐Milled Corn

Batch extraction of zein from dry‐milled whole corn with ethanol was optimum with 70% ethanol in water, an extraction time of 30–40 min, and temperature of 50°C. High yields (60% of the zein in corn) and high zein contents in the extracted solids (50%) were obtained at a solvent‐to‐solids ratio of 8 mL of 70% ethanol/g of corn. However, zein concentration in the extract was higher at lower ratios. Multiple extraction of the same corn with fresh ethanol resulted in a yield of 85% after four extractions, whereas multiple extractions of fresh corn with the same ethanol resulted in high (15 g/L) zein concentration in the extract. Optimum conditions for batch extraction of zein were 45°C, with 68% ethanol at a solvent‐to‐solids ratio of 7.8 mL/g for an extraction time of 55 min. Column extractions were also best at 50°C and 70% ethanol; a solvent ratio of 1 mL/g resulted in high zein concentrations in the extract (17 g/L) but yields were low (20%).