• New & Renewable Energy
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• v.6 no.4
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• pp.6-14
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• 2010

Pretreatment of cellulosic biomass is necessary before enzymatic saccharification and fermentation. Extrusion is a well established process in food industries and it can be used as a physicochemical treatment method for cellulosic biomass. Aqueous ammonia soaking treatment at mild temperatures ranging from 60 to $80^{\circ}C$ for longer reaction times has been used to preserve most of the cellulose and hemicellulose in the biomass. The objective of this study was to evaluate the effect of extrusion treatment on aqueous ammonia soaking method. Extrusion was performed with miscanthus sample conditioned to 2mm of particle size and 20% of moisture content at $200^{\circ}C$ of barrel temperature and 175rpm of screw speed. And then aqueous ammonia soaking was performed with 15%(w/w) ammonia solution at $60^{\circ}C$ for 1, 2, 4, 8, 12 hours on the extruded and raw miscanthus samples respectively. In the combined extrusion-soaking treatment, most compositions removal occurred within 1~2 hours and on a basis of 1 hour soaking treatment values, cellulose was recovered about 85% and other compositions, including hemicellulose, are removed about 50% from extruded miscanthus sample. The combined extrusion-soaking treated and soaking only treated samples were subjected to enzymatic hydrolysis using cellulase and ${\beta}$-glucosidase. The enzymatic digestibility value of combined extrusion-2 hours soaking treated sample was comparable to 12 hours soaking only treated sample. It means that extrusion treatment can shorten the conventional long reaction time of aqueous ammonia soaking. The findings suggest that the combination of extrusion and soaking is a promising pretreatment method to solve both problems for no lignin removal of extrusion and long reaction time of aqueous ammonia soaking.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.41 no.5
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• pp.15-19
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• 2009

Ammonia soaking treatment was introduced for hemp woody core pretreatment to increase enzymatic saccharification of polysaccharides. Portions of the xylan, cellulose, and lignin were removed by aqueous ammonia soaking, which improved the enzymatic saccharification of cellulose and xylan. Following ammonia soaking, 37% ($50^{\circ}C$-6 day treatment) to 61% ($90^{\circ}C$-16 h treatment) of the cellulose was converted to glucose and 33% ($50^{\circ}C$-6 day treatment) to 48% ($90^{\circ}C$-16 h treatment) of the xylan to xylose. Cellulose responded better to enzymatic saccharification than did xylan after the ammonia soaking treatment. Aqueous ammonia soaking pretreatment was more effective than electron beam irradiation for increasing enzymatic saccharification of xylan and cellulose in hemp woody core.

• Korean Chemical Engineering Research
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• v.49 no.3
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• pp.292-296
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• 2011

Liberation of fermentable sugars from lignocellulosic biomass is one of the key challenges in production of cellulosic ethanol. Aqueous ammonia cleaves ether and ester bonds in lignin carbohydrate complexes. It is an effective swelling reagent for lignocellulosic biomass. The aqueous ammonia pretreatment selectively reduces the lignin content of biomass. However, at high temperatures, this process solubilizes more than 50% of the hemicellulose in the biomass. Here we conducted a SAA(Soaking in Aqueous Ammonia) process by moderate reaction temperatures at atmospheric pressure using various lignocellulosicbiomass. The optimum condition of this process was 15 wt% of aqueous ammonia at 50 of reaction time during 72 hr. The delignification was up to 60% basis on initial biomass and the enzymatic digestibility was 60-90% for agricultural biomass, respectively.

• 한국신재생에너지학회:학술대회논문집
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• 2009.06a
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• pp.418-421
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• 2009

Effects of aqueous ammonia soaking to three annual plants (hemp woody core, tobacco stalk and corn stover) awere investigated to focus on the enzymatic saccharification characteristics change by this treatment. At two different levels of treatment ($90^{\circ}C$-16 h and $45^{\circ}C$-6 days), higher temperature treatment led to more enzymatic saccharification of cellulose to glucose by commercial cellulase mixtures (Celluclast 1.5L and Novozym 342 from Novozyme Korea). Difference among annual plants were significant. corn stover was the best response to enzymatic saccharification of cellulose and xylan by comercial enzymes all treatment conditions but tobacco stalk was the worst response to all of them. chemical composition or physical structure difference may brought this difference.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.41 no.1
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• pp.61-66
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• 2009

Effects of aqueous ammonia soaking treatments to yellow poplar (Liriodendron tulipifera L.) were investigated to focus on chemical compositional changes and enzymatic hydrolysis characteristics changes by this treatment. Treatment temperature and time were main variables. At 3 different levels of aqueous ammonia soaking temperature and time ($145^{\circ}C$ -1 h, $90^{\circ}C$ -16 h and $45^{\circ}C$ - 6 days), lower temperature and longer soaking time led to more xylan removal based on carbohydrate compositional analysis. However, at higher temperature treatment led to more enzymatic saccharification of cellulose to glucose by commercial cellulose mixtures (Celluclast 1.5L and Novozym 342 from Novozyme, Denmark). Cellulose hydrolysis was gradually increased with increasing enzymatic hydrolysis time but xylan hydrolysis was leveled out at early stage (less than 10 h) of enzymatic hydrolysis.

• 한국신재생에너지학회:학술대회논문집
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• 2011.11a
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• pp.114.1-114.1
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• 2011

Bioenergy production from lignocellulosic biomass and agriculture wastes have been attracted because of its sustainable and non-edible source. Especially, canola is considered as one of the best feedstock for renewable fuel production. Oil extracted canola and its agriculture residues are reuseable for bioethanol production. However, a pretreatment step is required before enzymatic hydrolysis to disrupt recalcitrant lignocellulosic matrix. To increase the sugar conversion, more efficient pretreatment process was necessary for removal of saccharification barriers such as lignin. Alkaline pretreatment makes the lignocellulose swollen through solvation and induces more porous structure for enzyme access. In our previous work, aqueous ammonia (1~20%) was utilized for alkaline reagent to increase the crystallinity of canola residues pretreatment. In this study, significant factors for efficient soaking in aqueous ammonia pretreatment on canola residues was optimized by using the response surface method (RSM). Based on the fundamental experiments, the real values of factors at the center (0) were determined as follows; $70^{\circ}C$ of temperature, 17.5% of ammonia concentration and 18 h of reaction time in the experiment design using central composition design (CCD). A statistical model predicted that the highest removal yield of lignin was 54% at the following optimized reaction conditions: $72.68^{\circ}C$ of temperature, 18.30% of ammonia concentration and 18.30 h of reaction time. Finally, maximum theoretical yields of soaking in aqueous ammonia pretreatment were 42.23% of glucose and 22.68% of xylose.

• Journal of the Korean Wood Science and Technology
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• v.37 no.4
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• pp.381-387
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• 2009

Enhancing enzymatic saccharification of corn stover by aqueous ammonia soaking pretreatment was investigated on chemical compositional changes and enzymatic hydrolysis characteristics. At three different levels of aqueous ammonia soaking temperature and time ($140^{\circ}C$-1 h, $90^{\circ}C$-16 h and $50^{\circ}C$-6 days), higher temperature and shorter treatment time led to more xylan and lignin removal based on overall composition analysis and carbohydrate compositional analysis. More xylan and lignin removal in higher temperature treatment led to higher enzymatic saccharification of cellulose and xylan to monosaccharide by commercial cellulase mixtures (Celluclast 1.5L and Novozym 342 from Novozyme, Denmark).

• 한국신재생에너지학회:학술대회논문집
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• 2010.06a
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• pp.253-253
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• 2010

Rice straw was pretreated with aqueous ammonia in order to enhance enzyme digestibility. Soaking in ammonia aqueous (SAA) was conducted with 15% ammonia, at $60^{\circ}C$. for 24 h. Optimization of both saccharification conditions and enzyme loading of SAA rice straw was carried out. Especially enzyme loading test was performed using statistical method. Moreover proton beam irradiation (PBI) was also performed to overcome the problem which inhibit the enzyme digestibility at 1-25 kGy doses with 45 MeV of beam energy. Optimal condition for enzymatic saccharification was follows; pH 4.8, $50^{\circ}C$, 60 FPU of enzyme activity, 1:4 ratio of celluase and ${\beta}$-glucosidase. Also, optimal doses of PBI on rice straw and SAA-treated rice straw for efficient sugar recovery were found to be 3 kGy, respectively. When saccharification was performed with optimal condition, glucose conversion yield was 89% of theocratical maximum in 48 h, and 3 kGy of PBI was applied to SAA-treated rice straw, approximately 90% of the theoretical glucose yield was obtained in 12 h. The results of X-ray diffractometry (XRD) support the effect of both SAA and PBI on sugar recovery, and scanning electron microscopy (SEM) images unveiled the physical change of the rice straw surface since rugged rice straw surface was observed.

• Korean Chemical Engineering Research
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• v.51 no.3
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• pp.303-307
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• 2013

This study compares the efficacy of soaking and percolation pretreatments with alkaline solutions for lignocellulosic biomass. Various biomass such as rice straw and barley were pretreated by soaking processes in various alkaline solutions including sodium hydroxide, potassium hydroxide, aqueous ammonia and sodium carbonate. The enzymatic digestibility of rice straw and barley that had been pretreated by soaking in aqueous ammonia was over 80%. Eucalyptus residue, Larix leptolepis and Pinus rigida exhibited relatively low enzymatic digestibility. Nevertheless, the enzymatic digestibility of pretreated eucalyptus residue was increased by five times compared to that of the initial biomass. And, the enzymatic digestibility of the percolation pretreated eucalyptus residue was increased 12 times.

• Korean Chemical Engineering Research
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• v.53 no.6
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• pp.682-689
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• 2015

A two-step process was investigated for pretreatment and fractionation of rice straw. The two-step fractionation process involves first, soaking rice straw in aqueous ammonia (SAA) in a batch reactor to recover lignin-rich hydrolysate. This is followed by a second-step treatment in a fixed-bed flow-through column reactor to recover xylo-oligomer-rich hydrolysate. The remaining glucan-rich solid cake is then subjected to an enzymatic process. In the first variant, SAA treatment in the first step dissolves lignin at moderate temperature (60 and $80^{\circ}C$), while in the second step, hot-water treatment is used for xylan removal at higher temperatures ($150{\sim}210^{\circ}C$). Under optimal conditions ($190^{\circ}C$ reaction temperature, 30 min reaction time, 5.0 ml/min flow rate, and 2.3 MPa reaction pressure), the SAA-hot-water fractionation removed 79.2% of the lignin and 63.4% of the xylan. In the second variant, SAA was followed by treatment with dilute sulfuric acid. With this process, optimal treatment conditions for effective fractionation of xylo-oligomer were found to be $80^{\circ}C$, 12 h reaction time, solid-to-liquid ratio of 1:12 in the first step; and 5.0 ml $H_2SO_4/min$, $170^{\circ}C$, and 2.3 MPa in the second step. After this two-step fractionation process, 85.4% lignin removal and 78.9% xylan removal (26.8% xylan recovery) were achieved. Use of the optimized second variant of the two-step fractionation process (SAA and $H_2SO_4$) resulted in enhanced enzymatic digestibility of the treated solid (99% glucan digestibility) with 15 FPU (filter paper unit) of CTec2 (cellulase)/g-glucan of enzyme loading, which was higher than 92% in the two-step fractionation process (SAA and hot-water).