Name: pretreatment of lignocellulosic biomass with low-cost ionic liquids
Uploaded: 2016-08-10T13:00:00
Description: Watch this Scientific Journal Video about Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids at JoVE.com

The authors acknowledge the Grantham Institute for Climate Change and the Environment, Climate-KIC and EPSRC (EP/K038648/1 and EP/K014676/1) for funding and Pierre Bouvier for providing experimental data for pine pretreatments.

Note: The protic ionic liquids used in the process are synthesized in our laboratory, although some might be or become commercially available. The resulting ionic liquids are acidic and corrosive and probably skin/eye irritants (depending on the amine used), and must therefore be handled with care wearing appropriate PPE (lab coat, safety specs, resistant gloves).
1. Preparation
<ol>
	<li>Preparing and storing the lignocellulosic biomass
	<ol>
		<li>Obtain the lignocellulosi...

<ol>
	<li>Lewis, N. S., Nocera, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Powering+the+planet:+chemical+challenges+in+solar+energy+utilization.">Powering the planet: chemical challenges in solar energy utilization.</a> Proc.Natl.Acad.Sci.U.S.A. 103 (43), 15729-15735 (2006).</li><li>Dincer, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Renewable+energy+and+sustainable+development:+a+crucial+review.">Renewable energy and sustainable development: a crucial review.</a> Renewable and Sustainable Energy Reviews. 4 (2), 157-175 (2000).</li><li>Zweibel, K., Mason, J., Fthenakis, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+solar+grand+plan.">A solar grand plan.</a> Sci. Am. 298 (1), 64-73 (2008).</li><li>Lee, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Biological+conversion+of+lignocellulosic+biomass+to+ethanol.">Biological conversion of lignocellulosic biomass to ethanol.</a> J. Biotechnol. 56 (1), 1-24 (1997).</li><li>Carrott, P., Ribeiro Carrott, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lignin-from+natural+adsorbent+to+activated+carbon:+A+review.">Lignin-from natural adsorbent to activated carbon: A review.</a> Bioresour.Technol. 98 (12), 2301-2312 (2007).</li><li>Cardona Alzate, C., S&#225;nchez Toro, O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Energy+consumption+analysis+of+integrated+flowsheets+for+production+of+fuel+ethanol+from+lignocellulosic+biomass.">Energy consumption analysis of integrated flowsheets for production of fuel ethanol from lignocellulosic biomass.</a> Energy. 31 (13), 2447-2459 (2006).</li><li>Field, C. B., Campbell, J. E., Lobell, D. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Biomass+energy:+the+scale+of+the+potential+resource.">Biomass energy: the scale of the potential resource.</a> Trends Biochem Sci. 23 (2), 65-72 (2008).</li><li>Hoogwijk, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Exploration+of+the+ranges+of+the+global+potential+of+biomass+for+energy.">Exploration of the ranges of the global potential of biomass for energy.</a> Biomass Bioenergy. 25 (2), 119-133 (2003).</li><li>Goldemberg, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ethanol+for+a+sustainable+energy+future.">Ethanol for a sustainable energy future.</a> Science. 315 (5813), 808-810 (2007).</li><li>Himmel, M. E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Biomass+recalcitrance:+engineering+plants+and+enzymes+for+biofuels+production.">Biomass recalcitrance: engineering plants and enzymes for biofuels production.</a> Science. 315 (5813), 804-807 (2007).</li><li>Mosier, N., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Features+of+promising+technologies+for+pretreatment+of+lignocellulosic+biomass.">Features of promising technologies for pretreatment of lignocellulosic biomass.</a> Bioresour.Technol. 96 (6), 673-686 (2005).</li><li>Kumar, P., Barrett, D. M., Delwiche, M. J., Stroeve, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Methods+for+pretreatment+of+lignocellulosic+biomass+for+efficient+hydrolysis+and+biofuel+production.">Methods for pretreatment of lignocellulosic biomass for efficient hydrolysis and biofuel production.</a> Ind Eng Chem Res. 48 (8), 3713-3729 (2009).</li><li>Hu, F., Ragauskas, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Suppression+of+pseudo-lignin+formation+under+dilute+acid+pretreatment+conditions.">Suppression of pseudo-lignin formation under dilute acid pretreatment conditions.</a> RSC Advances. 4 (9), 4317-4323 (2014).</li><li>Chakar, F. S., Ragauskas, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Review+of+current+and+future+softwood+kraft+lignin+process+chemistry.">Review of current and future softwood kraft lignin process chemistry.</a> Ind Crop Prod. 20 (2), 131-141 (2004).</li><li>Mutj&#233;, P., Pelach, M., Vilaseca, F., Garc&#237;a, J., Jim&#233;nez, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+comparative+study+of+the+effect+of+refining+on+organosolv+pulp+from+olive+trimmings+and+kraft+pulp+from+eucalyptus+wood.">A comparative study of the effect of refining on organosolv pulp from olive trimmings and kraft pulp from eucalyptus wood.</a> Bioresour.Technol. 96 (10), 1125-1129 (2005).</li><li>Zhao, X., Cheng, K., Liu, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Organosolv+pretreatment+of+lignocellulosic+biomass+for+enzymatic+hydrolysis.">Organosolv pretreatment of lignocellulosic biomass for enzymatic hydrolysis.</a> Appl. Microbiol. Biotechnol. 82 (5), 815-827 (2009).</li><li>Brandt, A., Gr&#228;svik, J., Hallett, J. P., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deconstruction+of+lignocellulosic+biomass+with+ionic+liquids.">Deconstruction of lignocellulosic biomass with ionic liquids.</a> Green Chem. 15, 550 (2012).</li><li>Chen, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inexpensive+ionic+liquids:[HSO+4]&#8722;-based+solvent+production+at+bulk+scale).">Inexpensive ionic liquids:[HSO 4]&#8722;-based solvent production at bulk scale).</a> Green Chem. 16 (6), 3098-3106 (2014).</li><li>Brandt, A., Chen, L., van Dongen, B. E., Welton, T., Hallett, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+changes+in+lignins+isolated+using+an+acidic+ionic+liquid+water+mixture.">Structural changes in lignins isolated using an acidic ionic liquid water mixture.</a> Green Chem. 17, 5019-5034 (2015).</li><li>Sluiter, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NREL/TP-510-42621.">NREL/TP-510-42621.</a> Determination of Total Solids in Biomass and Total Dissolved Solids in Liquid Process Samples. , (2008).</li><li>Sluiter, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NREL/+TP+-+510+-+42618Determination+of+Structural+Carbohydrates+and+Lignin+in+Biomass.">NREL/ TP - 510 - 42618Determination of Structural Carbohydrates and Lignin in Biomass.</a> Determination of Structural Carbohydrates and Lignin in Biomass. , (2011).</li><li>Resch, M. G., Baker, S. R., Decker, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NREL/TP-5100-63351.">NREL/TP-5100-63351.</a> Low Solids Enzymatic Saccharificatin of Lignocellulosic Biomass. , (2015).</li><li>Brandt, A., Ray, M. J., To, T. Q., Leak, D. J., Murphy, R. J., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquid+pretreatment+of+lignocellulosic+biomass+with+ionic+liquid-water+mixtures.">Ionic liquid pretreatment of lignocellulosic biomass with ionic liquid-water mixtures.</a> Green Chem. 13 (9), 2489-2499 (2011).</li><li>Aver, K., Scortegagna, A., Fontana, R., Camassola, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Saccharification+of+ionic-liquid-pretreated+sugar+cane+bagasse+using+Penicillium+echinulatum+enzymes.">Saccharification of ionic-liquid-pretreated sugar cane bagasse using Penicillium echinulatum enzymes.</a> J Taiwan Inst Chem Eng. 45 (5), 2060-2067 (2014).</li><li>George, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Design+of+low-cost+ionic+liquids+for+lignocellulosic+biomass+pretreatment.">Design of low-cost ionic liquids for lignocellulosic biomass pretreatment.</a> Green Chem. 17 (3), 1728 (2015).</li><li>Verd&#237;a, P., Brandt, A., Hallett, J. P., Ray, M. J., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fractionation+of+lignocellulosic+biomass+with+the+ionic+liquid+1-butylimidazolium+hydrogen+sulfate.">Fractionation of lignocellulosic biomass with the ionic liquid 1-butylimidazolium hydrogen sulfate.</a> Green Chem. 16 (3), 1617-1627 (2014).</li><li>Brandt, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquid+pretreatment+of+lignocellulosic+biomass+with+ionic+liquid-water+mixtures.">Ionic liquid pretreatment of lignocellulosic biomass with ionic liquid-water mixtures.</a> Green Chem. 13 (9), 2489-2499 (2011).</li></ol>

The technique for the fractionation of lignocellulosic biomass presented here produces a cellulose-rich pulp and a lignin. Most of the hemicelluloses are dissolved into the ionic liquid and hydrolyzed, but not recovered. If hemicellulose sugars are desired, a hemicellulose pre-extraction step prior to the Ionosolv delignification may be necessary. It has so far been impossible to fully close the mass balance for the biomass, as it is not possible to identify and quantify all degradation products found in the ionic liquid...

Meeting humanity&#39;s energy demand sustainably is one of the greatest challenges that our civilization faces. Energy use is predicted to double in the next 50 years, putting greater strain on fossil fuel resources. 1 The buildup of greenhouse gases (GHG) in the atmosphere through wide-spread fossil fuel use is particularly problematic, as CO2 generated from combustion of fossil fuels is responsible for 50% of the anthropogenic greenhouse effect. 2 Therefore, large-scale application of renewable and carbon neutral technologies is essential for meeting the increased energy and material needs of future generations. 1, 3
Plant biomass is the most versatile renewable resource, as it can be used to produce heat, electricity as well as carbon-based chemicals, materials and fuels. Primary advantages of lignocellulosic biomass over other biomass types are its abundance, potential for high yields per area of land and often much higher CO2 emission savings, which includes high retention of carbon in the soil. 4, 5 Additional benefits of using biomass include local availability, low capital requirements to convert biomass to energy, and soil erosion prevention. 8
Major producers of lignocellulosic feedstocks are the forestry industry and the agricultural sector as well as municipal waste management. 6 Lignocellulose production has the potential to be expanded, with a mind to limiting deforestation and avoiding the replacement of food crops and release of potential pollutants. 7 For renewable biomass to become a viable widespread source of liquid transportation fuels and chemicals, its processing must become economically competitive with fossil fuel conversion technologies. 9, 10 A key to achieving this is to boost the yield and quality of biomass-derived intermediates while reducing cost.
Lignocellulose contains a high proportion of sugars which can be converted to fuels and chemicals via catalytic and microbial conversions. 11 These sugars are present in lignocellulose in polymeric form as cellulose and hemicellulose. They can be hydrolyzed into glucose and other sugar monomers and then used for producing bioethanol and other bio-derived chemicals and solvents. 12
In order to access the cellulosic sugars, pretreatment of the biomass is necessary through physical, chemical, or combined processes. 4 The pretreatment is arguably the most costly step in the valorization of lignocellulosic biomass. Hence research into improved pretreatment processes is imperative.
Various pretreatment technologies are available. Of particular interest are those that separate the lignin from cellulose (fractionative pretreatment). Lignin, the third major component in lignocellulose, limits access of hydrolyzing agents to cellulose and hemicellulose and reduces the sugar yield per ton of feedstock. 11 The separated lignin can be utilized as an additional biorefinery intermediate if it is isolated in suitable quality. 13 One fractionative process is the Kraft process which is the most common pretreatment for paper/cellulose production. In Kraft pulping, wood chips are placed in a mixture of sodium hydroxide and sodium sulfide and heated at elevated temperatures of around 170 &#176;C under high pressure. 14 The alkaline reactions remove hemicellulose and lignin by breaking the polymers down to short fragments via nucleophilic and base catalysis, and by dissolving the lignin fragments via de-protonation of phenolic hydroxyl/alcohol groups. Another common delignification process is the Organosolv process which also fragments and dissolves the lignin and hemicellulose. Rather than using an alkaline aqueous solution, organic solvents such as ethanol and acetic acid are used at high temperatures ranging between 160-200 &#176;C and pressures from 5-30 bar. Organosolv pretreatment has some advantages over Kraft pulping in that it produces less air and water pollution. 15 Both processes possess some economic challenges, if used for production of chemicals and fuels rather than cellulose. 16 The Ionosolv pretreatment uses ionic liquids, which are salts that have melting points below 100 &#176;C and, as a result of their powerful Coulombic interactions, very low vapor pressures. 17 This eliminates air pollution in the pretreatment process, and enables processing at or near atmospheric pressure.
While most ILs are created in laborious, multi-step syntheses, protic ILs can be synthesized in a one-step process from commodity chemicals, which makes them less expensive; it is estimated that some ILs could be produced at bulk scale for a price of $1.24 per kg which is comparable to common organic solvents such as acetone and toluene. 18 The ability to recycle and reuse these customizable ILs in a process that operates at comparatively lower temperatures and pressures makes this a more benign alternative and an economically attractive candidate for biorefining.
This detailed video protocol demonstrates a lab-scale version of the Ionosolv process for the delignification of lignocellulosic biomass and the eventual enzymatic saccharification of the cellulose-rich pulp as well as the recovery of a high-purity odor-free lignin.19

<table border="0" cellpadding="0" cellspacing="0" width="851">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">IL synthesis</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td style="width:267px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Round bottom flask, with standard ground joint 24/29 NS, 1000 ml</td>
			<td style="width:116px;">Lenz</td>
			<td style="width:131px;">3 0024 70</td>
			<td>VWR product code 271-1309&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">250mL Addition Funnel, Graduated, 29/26 Joint Size, 0-4mm PTFE Valve</td>
			<td style="width:116px;">GPE</td>
			<td style="width:131px;">CG-1714-16</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Dish-shaped dewar flask, SCH 31 CAL&#160;</td>
			<td style="width:116px;">KGW-Isotherm</td>
			<td style="width:131px;">1197</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Volumetric flask, 200 ml</td>
			<td style="width:116px;">VWR</td>
			<td style="width:131px;">612-3745&#160;</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Cork rings, pasteur pipettes and teet, wash bottle with deionised water, large magentic stir bar</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Biomass size reduction</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Heavy Duty Cutting Mill SM2000&#160;</td>
			<td style="width:116px;">Retsch&#160;</td>
			<td>Discontinued</td>
			<td style="width:267px;">Replaced with Cutting Mill SM 200 (20.728.0001)&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Bottom sieves (10 mesh square holes, for particle size &#60;2 mm)</td>
			<td style="width:116px;">Retsch&#160;</td>
			<td style="width:131px;">03.647.0318</td>
			<td style="width:267px;">Part of cutting mill</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Analytical Sieve Shaker AS 200</td>
			<td style="width:116px;">Retsch&#160;</td>
			<td>30.018.0001</td>
			<td>Part of sieving machine</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Test Sieve 200 mm &#216; x 50 mm height ISO 3310/1 (180 &#181;m)</td>
			<td style="width:116px;">Retsch&#160;</td>
			<td>60.131.000180</td>
			<td>Part of sieving machine</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Test Sieve 200 mm &#216; x 50 mm height ISO 3310/1 (850 &#181;m)</td>
			<td style="width:116px;">Retsch&#160;</td>
			<td style="width:131px;">60.131.000850</td>
			<td align="left">Part of sieving machine</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Collecting pan, stainless steel, 200 mm &#216;, height 50 mm&#160;</td>
			<td style="width:116px;">Retsch&#160;</td>
			<td style="width:131px;">69.720.0050</td>
			<td>Part of sieving machine</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Rotary evaporator:</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Rotary evaporator (Rotavapor R-210)</td>
			<td style="width:116px;">Buchi&#160;</td>
			<td>Discontinued</td>
			<td>Replaced with Rotavapor R-300</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Water bath (Heating bath B-491)</td>
			<td style="width:116px;">Buchi&#160;</td>
			<td>48201</td>
			<td>Part of rotary evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Recirculator&#160;</td>
			<td style="width:116px;">Julabo</td>
			<td style="width:131px;">F25</td>
			<td>Part of rotary evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum pump (MPC 101 Z)</td>
			<td style="width:116px;">Ilmvac GmbH</td>
			<td style="width:131px;">412522</td>
			<td>Part of rotary evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum controller (Vacuum Control Box VCB 521)</td>
			<td style="width:116px;">Ilmvac GmbH</td>
			<td style="width:131px;">600053</td>
			<td>Part of rotary evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Parallel evaporator:</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">StarFish Base Plate 135mm (for Radleys &#38; IKA)&#160;</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95010</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Monoblock for 5 x 250ml Flasks</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95130&#160;</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Telescopic 5-way Clamp with Velcro</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95400</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Gas/Vacuum Manifold with connectors</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95510&#160;</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">650mm Rod</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95665&#160;</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Quick Release Male, R/A Barbed 6.4mm + Shut-off (3.2mm ID)&#160;</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95520</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Stirrer/hot plate</td>
			<td>Radleys</td>
			<td>RR98072</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Temperature controller</td>
			<td style="width:116px;">Radleys</td>
			<td>RR98073</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Elliptical Stirring Bar 15mm Rare Earth</td>
			<td style="width:116px;">Radleys</td>
			<td>RR98097&#160;</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum cold trap, plastic coated, PTFE stopcock</td>
			<td style="width:116px;">Chemglass</td>
			<td style="width:131px;">CG-4519-01</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum pump (MPC 101 Z)</td>
			<td style="width:116px;">Ilmvac GmbH</td>
			<td style="width:131px;">412522</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Tygon tubing E-3603, 6,40 mm (internal) 12,80 mm (external)&#160;&#160;</td>
			<td style="width:116px;">Saint-Gobain/VWR</td>
			<td style="width:131px;">228-1292&#160;</td>
			<td>Part of parallel evaporator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Parallel Soxhlet extractor:</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">StarFish Base Plate 135mm (for Radleys &#38; IKA)</td>
			<td>Radleys</td>
			<td>RR95010&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Monoblock for 5 x 250ml Flasks</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95130&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Telescopic 5-way Clamp with Velcro</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95400&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Telescopic 5-way Clamp with Silicone Strap and Long Handle</td>
			<td>Radleys</td>
			<td>RR95410&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Water Manifold with connectors</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95500&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">650mm Rod</td>
			<td style="width:116px;">Radleys</td>
			<td>RR95665&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Quick Release Male, R/A Barbed 6.4mm + Shut-off (3.2mm ID)</td>
			<td>Radleys</td>
			<td>RR95520&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Coil condensers with standard ground joints 29/32 NS</td>
			<td>Lenz</td>
			<td>5.2503.04&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Extractor Soxhlet 40mL borosilicate glass 29/32 socket 24/29 cone</td>
			<td>Quickfit</td>
			<td>EX5/43&#160;</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Stirrer/hot plate</td>
			<td>Radleys</td>
			<td>RR98072</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Temperature controller</td>
			<td style="width:116px;">Radleys</td>
			<td>RR98073</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Recirculator</td>
			<td>Grant</td>
			<td>LTC1</td>
			<td>Part of soxhlet extractor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Cellulose extraction thimble</td>
			<td>Whatman</td>
			<td>2280-228</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Tweezers</td>
			<td>Excelta</td>
			<td>20A-S-SE</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum drying oven:</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum drying oven</td>
			<td>Binder</td>
			<td>VD 23</td>
			<td>Part of vacuum oven</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Dewar vessel 2L 100x290mm with handle</td>
			<td>KGW-Isotherm</td>
			<td>10613</td>
			<td>Part of vacuum oven</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Vacuum Trap</td>
			<td>GPE</td>
			<td>CG-4532-01&#160;</td>
			<td>Part of vacuum oven</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Other equipment:</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Analytical balance</td>
			<td style="width:116px;">A&#38;D</td>
			<td style="width:131px;">GH-252</td>
			<td>accuracy to &#177; 0.1 mg</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Volumetric Karl Fischer titrator</td>
			<td style="width:116px;">Mettler Toledo</td>
			<td style="width:131px;">V20</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">10 mL disposable pipette</td>
			<td style="width:116px;">Corning Inc</td>
			<td style="width:131px;">Costar 4101 10 mL Stripette</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Eppendorf&#160;Research&#160;plus pipette, variable volume, volume 100-1000&#160;&#956;L</td>
			<td style="width:116px;">Eppendorf</td>
			<td>3120000062</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Desiccator</td>
			<td style="width:116px;">Jencons</td>
			<td style="width:131px;">JENC250-028BOM</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Ace pressure tube bushing type, Front seal, volume 15&#160;mL&#160;</td>
			<td style="width:116px;">Ace Glass</td>
			<td>8648-04&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Ace O-rings, silicone, 2.6&#160;mm, I.D. 9.2&#160;mm&#160;</td>
			<td style="width:116px;">Ace Glass</td>
			<td>7855216</td>
			<td>O-ring for pressure tube</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Vortex shaker</td>
			<td style="width:116px;">VWR International</td>
			<td style="width:131px;">444-1378 (UK)</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Fan-assisted convection oven</td>
			<td style="width:116px;">ThermoScientific</td>
			<td style="width:131px;">HeraTherm OMH60</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Oven glove (Crusader Flex)</td>
			<td style="width:116px;">Ansel Edmont</td>
			<td>42-325</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">250 mL Round bottom flask single neck ground joint 24/29 (Pyrex)</td>
			<td style="width:116px;">Quickfit&#160;</td>
			<td style="width:131px;">FR250/3S</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Rotaflo stopcock adapter with cone 24/29</td>
			<td style="width:116px;">Rotaflo England</td>
			<td style="width:131px;">MF11/2/SC</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">50 mL Falcon&#160; tube</td>
			<td style="width:116px;">Heraeus/Kendro</td>
			<td style="width:131px;">HERA 76002844</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Centrifuge (Mega Star 3.0)</td>
			<td style="width:116px;">VWR&#160;</td>
			<td style="width:131px;">521-1751</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Reagents:</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Ethanol absolute</td>
			<td style="width:116px;">VWR</td>
			<td style="width:131px;">20820.464</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Triethylamine</td>
			<td style="width:116px;">Sigma-Aldrich</td>
			<td style="width:131px;">T0886</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:339px;">Sulfuric acid 5 mol/l (10N) AVS TITRINORM volumetric solution Safe-break bottle 2,5L</td>
			<td>VWR</td>
			<td>191665V</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Purified water (15 M&#937; ressitance)</td>
			<td style="width:116px;">Elga</td>
			<td style="width:131px;">CENTRA R200</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Lignocellulosic biomass:</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Miscanthus X gigantheus</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:339px;">Pinus sylvestris</td>
			<td style="width:116px;"></td>
			<td style="width:131px;"></td>
			<td></td>
		</tr>
	</tbody>
</table>

pretreatment of lignocellulosic biomass with low-cost ionic liquids

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of a variety of lignocellulosic feedstocks. Here we demonstrate the use of these low-cost protic ILs in the deconstruction of lignocellulosic biomass (Ionosolv pretreatment), yielding cellulose and a purified lignin. In the most generic process, the protic ionic liquid is synthesized by accurate combination of aqueous acid and amine base. The water content is adjusted subsequently. For the delignification, the biomass is placed into a vessel with IL solution at elevated temperatures to dissolve the lignin and hemicellulose, leaving a cellulose-rich pulp ready for saccharification (hydrolysis to fermentable sugars). The lignin is later precipitated from the IL by the addition of water and recovered as a solid. The removal of the added water regenerates the ionic liquid, which can be reused multiple times. This protocol is useful to investigate the significant potential of protic ILs for use in commercial biomass pretreatment/lignin fractionation for producing biofuels or renewable chemicals and materials.

The exact amount of lignin removal and lignin precipitation, recovered pulp and glucose yield depend on the type of biomass used, the temperature at which the treatment is run and the duration of the treatment. Short pretreatment times and low temperatures lead to incomplete pretreatment while at higher temperatures the cellulose becomes unstable in the ionic liquid, leading to hydrolysis and degradation. The selected ionic liquid also plays an important role in the outcome of the fractio...

Watch this Scientific Journal Video about Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids at JoVE.com

Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids

The pretreatment of lignocellulosic biomass with protic low-cost ionic liquids is shown, resulting in a delignified cellulose-rich pulp and a purified lignin. The pulp gives rise to high glucose yields after enzymatic saccharification.

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of ...

Research

JoVE Journal

Environment

High-throughput Screening of Recalcitrance Variations in Lignocellulosic Biomass: Total Lignin, Lignin Monomers, and Enzymatic Sugar Release

The conversion of lignocellulosic biomass to fuels, chemicals, and other commodities has been explored as one possible pathway toward reductions in the ...

Experimental Protocol for Biodiesel Production with Isolation of Alkenones as Coproducts from Commercial Isochrysis Algal Biomass

Experimental Protocol for Biodiesel Production with Isolation of Alkenones as Coproducts from Commercial Isochrysis Algal Biomass

The need to replace petroleum fuels with alternatives from renewable and more environmentally sustainable sources is of growing importance. ...

Measuring the Flight Ability of the Ambrosia Beetle, Platypus Quercivorus (Murayama), Using a Low-Cost, Small, and Easily Constructed Flight Mill

Measuring the Flight Ability of the Ambrosia Beetle, Platypus Quercivorus Murayama, Using a Low-Cost, Small, and Easily Constructed Flight Mill

The ambrosia beetle, Platypus quercivorus (Murayama), is the vector of a fungal pathogen that causes mass mortality of Fagaceae trees (Japanese oak wilt). ...

Ammonia Fiber Expansion (AFEX) Pretreatment of Lignocellulosic Biomass

Ammonia Fiber Expansion AFEX Pretreatment of Lignocellulosic Biomass

Lignocellulosic materials are plant-derived feedstocks, such as crop residues (e.g., corn stover, rice straw, and sugar cane bagasse) and purpose-grown ...

A Novel Method for the Pentosan Analysis Present in Jute Biomass and Its Conversion into Sugar Monomers Using Acidic Ionic Liquid

Recently, ionic liquids (ILs) are used for biomass valorization into valuable chemicals because of their remarkable properties such as thermal stability, ...

A Flexible Low Cost Hydroponic System for Assessing Plant Responses to Small Molecules in Sterile Conditions

A wide range of studies in plant biology are performed using hydroponic cultures. In this work, an in vitro hydroponic growth system designed for ...

Construction of a Compact Low-Cost Radiation Shield for Air-Temperature Sensors in Ecological Field Studies

Low cost temperature sensors are increasingly used by ecologists to assess climatic variation and change on ecologically relevant scales. Although ...

Construction of a Low-cost Mobile Incubator for Field and Laboratory Use

Incubators are essential for a range of culture-based microbial methods, such as membrane filtration followed by cultivation for assessing drinking water ...

BtM, a Low-cost Open-source Datalogger to Estimate the Water Content of Nonvascular Cryptogams

Communities of nonvascular cryptogams, such as mosses or lichens, are an important part of the Earth's biodiversity, contributing to the regulation of the ...

Visualization of Low-Level Gamma Radiation Sources Using a Low-Cost, High-Sensitivity, Omnidirectional Compton Camera

We present experimental protocols for visualizing various low-level gamma radiation sources in the ambient environment. Experiments were conducted by ...