Name: preparation of biomass-based mesoporous carbon with higher nitrogen-/oxygen-chelating adsorption for cu(ii) through microwave pre-pyrolysis
Uploaded: 2019-02-12T12:30:00.000+00:00
Duration: 10 min 44 s
Description: Watch this Scientific Journal Video about Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for CuII Through Microwave Pre-Pyrolysis at JoVE.com

The authors acknowledge the Fundamental Research Funds for the Central Universities of China (No.KYZ201562), China Postdoctoral Science Fund (No. 2014M560429) and the Key research and development plan of Jiangsu Province (No. BE2018708).

1. Preparation of Bagasse-based Activated Carbon
<ol>
	<li>Preparation of the precursor for bagasse-based activated carbon
	<ol>
		<li>Rinse the bagasse (obtained from a farm in Jiangsu, China) with deionized water and put the samples in a drying oven at 100 &#176;C for 10&#160;h.</li>
		<li>Crush the dried bagasse with a grinder and sieve the powder through a 50-mesh sieve.</li>
		<li>Place 30 g of fine bagasse powder into a 15 wt% phosphoric acid (H3PO4) solution in a 1:1 weight ratio for 24 h. Dry the mixture in an oven at 105 &#176;C for 6 h. Collect the resulting product as the precursor for bagasse-based activated carbon (BAC).</li>
	</ol>
	</li>
	<li>Conventional electric-heating pyrolysis of the precursor
	<ol>
		<li>Put 15 g of the precursor into a quartz boat and then insert the quartz boat into a quartz glass tube of an electric furnace.</li>
		<li>Set the heating rate of the furnace at 5 &#176;C min-1 to carbonize the sample. When the temperature reaches 500 &#176;C, keep the temperature for 90 min and then allow the resulting activated-carbon sample to cool to room temperature in nitrogen. Ensure a nitrogen flow of 80 mL min-1 with a rotor flowmeter during the overall process.</li>
		<li>Triturate and collect the electrical-furnace-pyrolyzed bagasse-based activated carbon (EBAC) in a beaker and then heat it in a vacuum drying oven at 105 &#176;C for 24 h.</li>
	</ol>
	</li>
	<li>Microwave pyrolysis of the precursor
	<ol>
		<li>Put 15 g of the precursor in a microwave oven (with a 2.45 GHz frequency).</li>
		<li>Set the power of the microwave oven at 900 W to pyrolyze the sample for 22 min, and ensure the nitrogen flow rate at 20 mL min-1 with a rotor flowmeter. The air inlet of the rotor flowmeter is connected to a nitrogen cylinder using a hose, while the outlet is connected to the air inlet of the microwave oven.</li>
		<li>Allow the resultant carbon to cool to room temperature in nitrogen. Triturate and collect the carbon sample in a beaker and then add 300 mL of hydrochloric acid (0.1 M). Stir the mixture using a magnetic stirrer (at 200 rpm) for more than 12 h at room temperature.</li>
		<li>Filter the carbon by filter paper with vacuum filtration and rinse the sample with deionized water until the pH value of the wash water is &#62; 6. Dry the microwave-pyrolyzed bagasse-based activated carbon (MBAC) in a vacuum drying oven at 105 &#176;C for 24 h.</li>
	</ol>
	</li>
</ol>
2. Modification of Electrical-furnace-pyrolyzed Bagasse-based Activated Carbon and Microwave-pyrolyzed Bagasse-based Activated Carbon
Note: The modification of the two samples was conducted according to the literature29.
<ol>
	<li>Nitrification
	<ol>
		<li>Mix 50 mL of concentrated sulfuric and 50 mL of concentrated nitric acids in a beaker at 0 &#176;C (in an ice bath). 
		CAUTION: When the mixture of concentrated sulfuric acid and concentrated nitric acid is mixed, the concentrated sulfuric acid should be slowly added to the concentrated nitric acid and stirred with a glass rod and cooled in time.</li>
		<li>Add 10 g of EBAC/MBAC to the mixed solution. Use a magnetic stirrer to stir the mixture for 120 min (at 200 rpm).</li>
		<li>Filter the nitrified EBAC/MBAC by filter paper with vacuum filtration. Wash the carbon with deionized water until the wash water reaches pH 6, and then dry it in a drying oven at 90 &#176;C for 24 h.</li>
	</ol>
	</li>
	<li>Reductive modification
	<ol>
		<li>In a three-necked flask, add the 5.05 g of resulting product, 50 mL of deionized water, and 20 mL of ammonia solution (15 M). Stir this mixture for 15 min with a magnetic stirrer (at 200 rpm), then add 28 g of Na2S2O4, and leave the mixture stirring at room temperature for 20 h.</li>
		<li>Fit a reflux condenser to the flask and warm the mixture up to 100 &#176;C using an oil bath. Add 120 mL of CH3COOH (2.9 M) to the flask and allow the mixture to stir for 5 h with a magnetic stirrer (at 200 rpm) under reflux.</li>
		<li>Remove the oil bath to allow the solution to cool down to room temperature. Filter the carbon sample and wash it with deionized water until the solution pH &#62; 6. Dry the modified EBAC/MBAC at 90 &#176;C and denote it as &#8220;EBAC-N/MBAC-N&#8221;.</li>
	</ol>
	</li>
</ol>
3. Adsorbent Characterization
<ol>
	<li>Structural characterization&#8212;Nitrogen adsorption/desorption isotherms 
	<ol>
		<li>Weigh an empty sample tube. Add a carbon sample (~0.15 g) to the sample tube.</li>
		<li>Degas the sample at 110 &#176;C for 5 h in a vacuum. Weigh the sample tube containing carbon. Calculate the weight of the carbon sample.</li>
		<li>Install the sample tube into the test area of the surface-area and porosimetry analyzer using liquid nitrogen to measure it at -196 &#176;C30.</li>
	</ol>
	</li>
	<li>Chemical characterization&#8212;Fourier transform infrared spectroscopy
	<ol>
		<li>Check the temperature and hygrometer and observe whether the environment meets the requirements: the temperature should be 16 - 25 &#176;C and the relative humidity 20% - 50%.</li>
		<li>Remove the desiccant and dust cover in the sample storehouse.</li>
		<li>Dry the carbon sample and potassium bromide at 110 &#176;C for 4 h to avoid the effect of water on the spectrum. Mix the carbon sample with potassium bromide and then use a press mechanism to prepare the test sample.</li>
		<li>Put the sample in the test area and set the parameters of the software.</li>
		<li>Save the spectra and take out the sample. Perform a required data processing for the spectra31.</li>
	</ol>
	</li>
</ol>
4. Cu(II)-adsorption Experiments
<ol>
	<li>Adsorption isotherm
	<ol>
		<li>Place 0.05 g of adsorbent in each of the conical flasks, which contain 25 mL of a CuSO4 solution (pH 5) with a selected initial concentration (10, 20, 30, 40, 50, 60, 80, and 100 mg L-1). Use a 0.1 M HNO3 and 0.1 M NaOH solution to adjust the pH of each copper solution. 
		Note: A solution with the selected initial concentration is diluted by a 1 g L-1 CuSO4 solution, which is made up of a dissolved 3.90625 g of blue vitriol solid using the vase with a 1,000 mL volume.</li>
		<li>Fit lids on the conical flasks and put them in a thermostatic orbital shaker (with a stirring rate of 150 rpm) at 5 &#176;C/25 &#176;C/45 &#176;C for 240&#160;min.</li>
		<li>Use 0.22 &#956;m membrane filters to separate the adsorbents from the solution.</li>
		<li>Use a flame atomic absorption spectrophotometry to determine the copper concentration of the filtrate. 
		Note: All experiments were carried out in triplicate and the data were averaged. The adsorption capacity for Cu(II), qe, was calculated as follows: 
		<img alt="Equation" src="/files/ftp_upload/58161/58161eq1v2.jpg" />&#160;(1) 
		Here, 
		C0 = the initial copper concentration (mg L-1), 
		Ce = the final concentration (mg L-1), 
		V = the solution volume, and 
		m = the weight of each adsorbent (g).</li>
	</ol>
	</li>
	<li>Influence of pH
	<ol>
		<li>Place 0.05 g of adsorbent in each of conical flasks, which contain 25 mL of a CuSO4 solution (40 mg L-1) with a selected initial pH (2, 3, 4, 5, 6, and 7).</li>
		<li>Fit lids on the conical flasks and put them in a thermostatic orbital shaker (with a stirring rate of 150 rpm) at 25 &#176;C for 24 h to reach adsorption equilibrium conditions.</li>
		<li>Repeat step 4.1.3-4.1.4.</li>
	</ol>
	</li>
	<li>Adsorption kinetics
	<ol>
		<li>Place 0.25 g of adsorbent in a beaker which contains 125 mL of a CuSO4 solution (30 mg L-1 or 100 mg L-1, pH 5) in a 25 &#176;C water bath with magnetic stirring (at 200 rpm).</li>
		<li>Use pipettes to draw 5 mL of the solution when the contact time reaches 0.5, 1, 2.5, 5, 10, 30, 60, 120, and 180 min.</li>
		<li>Repeat step 4.1.3-4.1.4.</li>
	</ol>
	</li>
</ol>

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(15), 1-12 (2018).</li><li>Vunain, E., Kenneth, D., Biswick, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+characterization+of+low-cost+activated+carbon+prepared+from+Malawian+baobab+fruit+shells+by+H3PO4+activation+for+removal+of+Cu(II)+ions:+equilibrium+and+kinetics+studies.">Synthesis and characterization of low-cost activated carbon prepared from Malawian baobab fruit shells by H3PO4 activation for removal of Cu(II) ions: equilibrium and kinetics studies.</a> Applied Water Science. 7 (8), 4301-4319 (2017).</li><li>Bohli, T., Ouederni, A., Villaescusa, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Simultaneous+adsorption+behavior+of+heavy+metals+onto+microporous+olive+stones+activated+carbon:+analysis+of+metal+interactions.">Simultaneous adsorption behavior of heavy metals onto microporous olive stones activated carbon: analysis of metal interactions.</a> Euro-Mediterranean Journal for Environmental Integration. 2 (1), 19 (2017).</li><li>Bouhamed, F., Elouear, Z., Bouzid, J., Ouddane, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multi-component+adsorption+of+copper,+nickel+and+zinc+from+aqueous+solutions+onto+activated+carbon+prepared+from+date+stones.">Multi-component adsorption of copper, nickel and zinc from aqueous solutions onto activated carbon prepared from date stones.</a> Environmental Science &amp; Pollution Research. 23 (16), 1-6 (2016).</li><li>Wu, 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=Surface+modification+of+phosphoric+acid+activated+carbon+by+using+non-thermal+plasma+for+enhancement+of+Cu(II)+adsorption+from+aqueous+solutions.">Surface modification of phosphoric acid activated carbon by using non-thermal plasma for enhancement of Cu(II) adsorption from aqueous solutions.</a> Separation &amp; Purification Technology. 197, (2018).</li></ol>

The authors have nothing to disclose.

In this protocol, one of the critical steps is the successful preparation of mesoporous carbon with better physicochemical properties by the one-step approach, where optimal experimental conditions need to be determined. So, in a previous study28, we have carried out orthogonal array microwave pyrolysis experiments, considering the effect of the impregnation ratio of bagasse and phosphoric acid, pyrolysis time, microwave oven power, and drying time. Besides, great care must be taken in tedious Cu(...

Activated carbon has unique adsorption properties, such as a developed porous structure, a high specific surface area, and various surface functional groups; therefore, it is employed as an adsorbent in water treatment or purification1,2,3,4. Besides its physical advantages, activated carbon is cost-effective and harmless to the environment, and its raw material (e.g., biomass) is abundant and easily obtained5,6. The physicochemical properties of activated carbon depend on the precursors that are used in its preparation and on the experimental conditions of the activation process7.
Two methods are typically used to prepare activated carbon: a one-step and a two-step approach8. The term one-step approach refers to precursors being carbonized and activated simultaneously while the two-step approach refers to that sequentially. In view of energy conservation and environmental protection, the one-step approach is more preferred for its lower temperature and pressure demanding.
Besides, chemical and physical activation are utilized to improve the textural properties of activated carbon. Chemical activation possesses apparent advantages over physical activation because of its lower activation temperature, shorter activation time, higher carbon yield, and more developed and controllable pore structure in a certain degree9. It has been tested that chemical activation can be performed by impregnating biomass used as feedstock with H3PO4, ZnCl2, or other specific chemicals, followed by pyrolysis to increase the porosity of the activated carbon, because lignocellulosic components of biomass can be easily removed by a subsequent heating treatment, owing to the dehydrogenation capability of these chemicals10,11. Hence, chemical activation greatly enhances the formation of activated carbon&#39;s pores or improves the adsorptive performance to contaminants12. An acidic activator is preferred to H3PO4, due to its relatively lower energy demand, higher yield, and less impact on the environment13.
Microwave pyrolysis has the superiority in time savings, uniform interior heating, energy-efficiency, and selective heating, making it an alternative heating method to synthesis-activated carbon14,15. Compared with conventional electric heating, microwave pyrolysis can enhance thermo-chemical processes and promote certain chemical reactions16. Recently, extensive studies have focused on preparing activated carbon by chemical activation from biomass using one-step microwave pyrolysis9,17,18,19. So, it is considerably informative and environment-friendly to synthesis biomass-based activated carbon by microwave-assisted H3PO4 activation.
In addition, to improve the adsorption affinities of activated carbon toward specific heavy-metal ions, modification by heteroatom [N, O, sulfur (S), etc.] doping into carbon structures has been proposed, and this has proven to be a desirable method20,21,22,23,24,25,26. Defective sites in or at the edges of a graphite layer can be replaced by heteroatoms to generate functional groups27. Hence, nitrification and reduction modification are used to modify resultant carbon samples to dope N/O functional groups which play a crucial role in efficiently coordinating with heavy metal to form complexing and ion-exchange28.
Based on the findings above, we present a protocol to synthesize N/O dual-doped mesoporous carbon from biomass by chemical activation and two different pyrolysis methods followed up by modification. This protocol also determines which heating method favors the ensuing modification for doping of the N/O functional groups and, thus, enhancing the adsorption performance.

<table><tbody><tr><td>All chemicals and reagents (phosphoric acid, etc.)</td><td>Nanjing Chemical Reagent Co., Ltd</td><td></td><td>Analytical grade</td></tr><tr><td>Electric furnace</td><td>Luoyang Bolaimaite Experiment Electric Furnace Co., Ltd</td><td></td><td></td></tr><tr><td>Microwave oven</td><td>Nanjing Yudian Automation Technology Co., Ltd</td><td></td><td>2.45 GHz frequency</td></tr><tr><td>Surface-area and porosimetry analyzer</td><td>Beijing Gold APP Instrument Co., Ltd</td><td></td><td>Vc-Sorb 2800TP</td></tr><tr><td>Fourier transform infrared (FTIR) spectrometer</td><td>Nicolet</td><td></td><td>6700</td></tr><tr><td>Flame atomic absorption spectrophotometry</td><td>Beijing Purkinje General Instrument Corporation</td><td></td><td>A3</td></tr><tr><td>Element Analyzer</td><td>Germany Heraeus Co.</td><td></td><td>CHN-O-RAPID&amp;nbsp;</td></tr></tbody></table>

preparation of biomass-based mesoporous carbon with higher nitrogen-/oxygen-chelating adsorption for cu(ii) through microwave pre-pyrolysis

An environment-friendly technique for synthesizing biomass-based mesoporous activated carbon with high nitrogen-/oxygen-chelating adsorption for Cu(II) is proposed. Bagasse impregnated with phosphoric acid is utilized as the precursor. To pyrolyze the precursor, two separate heating modes are used: microwave pyrolysis and conventional electric-heating pyrolysis. The resulting bagasse-derived carbon samples are modified with nitrification and reduction modification. Nitrogen (N)/oxygen (O) functional groups are simultaneously introduced to the surface of activated carbon, enhancing its adsorption of Cu(II) by complexing and ion-exchange. Characterization and copper adsorption experiments are performed to investigate the physicochemical properties of four prepared carbon samples and determine which heating method favors the subsequent modification for doping of N/O functional groups. In this technique, based on analyzing data of nitrogen adsorption, Fourier transform infrared spectroscopy, and batch adsorption experiments, it is proven that microwave-pyrolyzed carbon has more defect sites and, therefore, time-saving effective microwave pyrolysis contributes more N/O species to the carbon, although it leads to a lower specific surface area. This technique offers a promising route to synthesis adsorbents with higher nitrogen and oxygen content and a higher adsorption capacity of heavy-metal ions in wastewater remediation applications.

Nitrogen adsorption/desorption isotherms of four samples are presented in Figure 1. All adsorption isotherms show a rapid increase in low P/P0 region and these isotherms belong to type IV (IUPAC classification) demonstrating their pore structure that consists of micropores and dominant mesopores32.
The surface physical parameters for all samples obtained from the n...

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Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for CuII Through Microwave Pre-Pyrolysis

Here, we present a protocol to synthesize nitrogen/oxygen dual-doped mesoporous carbon from biomass by chemical activation in different pyrolysis modes followed by modification. We demonstrate that the microwave pyrolysis benefits the subsequent modification process to simultaneously introduce more nitrogen and oxygen functional groups on the carbon.

Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for Cu(II) Through Microwave Pre-Pyrolysis

An environment-friendly technique for synthesizing biomass-based mesoporous activated carbon with high nitrogen-/oxygen-chelating adsorption for Cu(II) is ...

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9.8K Views.  Nanjing Agricultural University. Here, we present a protocol to synthesize nitrogen/oxygen dual-doped mesoporous carbon from biomass by chemical activation in different pyrolysis modes followed by modification. We demonstrate that the microwave pyrolysis benefits the subsequent modification process to simultaneously introduce more nitrogen and oxygen functional groups on the carbon.

Video: Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for CuII Through Microwave Pre-Pyrolysis

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Chemistry

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are demonstrated here. The catalyst forms a substitutional solid solution structure, with a small and uniform particle size around 2 nm. This is realized by careful control over the impregnation, calcination, and reduction steps during catalyst preparation and is identified by advanced in situ synchrotron techniques. The catalyst propane dehydrogenation performance continuously improves with increasing Cu:Pt atomic ratio.

A convenient method for the synthesis of 2 nm supported bimetallic nanoparticle Pt-Cu catalysts for propane dehydrogenation is reported here. In situ synchrotron X-ray techniques allow for the determination of the catalyst structure, which is typically unobtainable using laboratory instruments.

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Reducing Willow Wood Fuel Emission by Low Temperature Microwave Assisted Hydrothermal Carbonization

Biomass is a sustainable fuel, as its CO2 emissions are reintegrated in biomass growth. However, the inorganic precursors in the biomass cause a negative environmental impact and slag formation. The selected short rotation coppice (SRC) willow wood has a high ash content (<img alt="Equation 1" src="/files/ftp_upload/58970/58970eq1.jpg" /> = 1.96%) and, therefore, a high content of emission and slag precursors. Therefore, the reduction of minerals from SRC willow wood by low temperature microwave assisted hydrothermal carbonization (MAHC) at 150 &#176;C, 170 &#176;C, and 185 &#176;C is investigated. An advantage of MAHC over conventional reactors is an even temperature conductance in the reaction medium, as microwaves penetrate the whole reactor volume. This allows a better temperature control and a faster cooldown. Therefore, a succession of depolymerization, transformation and repolymerization reactions can be analyzed effectively. In this study, the analysis of the mass loss, ash content and composition, heating values and molar O/C and H/C ratios of the treated and untreated SCR willow wood showed that the mineral content of the MAHC coal was reduced and the heating value increased. The process water showed a decreasing pH and contained furfural and 5-methylfurfural. A process temperature of 170 &#176;C showed the best combination of energy input and ash component reduction. The MAHC allows a better understanding of the hydrothermal carbonization process, while a large-scale industrial application is unlikely because of the high investment costs.

A protocol for the emission precursor depletion from low quality biomass by low temperature microwave assisted hydrothermal carbonization treatment is presented. This protocol includes the microwave parameters and the analysis of the biocoal product and process water.

Biomass is a sustainable fuel, as its CO2 emissions are reintegrated in biomass growth. However, the inorganic precursors in the biomass cause a negative ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...

Synthesis of Metal Nanoparticles Supported on Carbon Nanotube with Doped Co and N Atoms and its Catalytic Applications in Hydrogen Production

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented herein. The novel strategy is based on a facile one-pot pyrolysis treatment of cobalt (II) acetylacetonate and nitrogen-rich organic precursors under Ar atmosphere at 800 &#176;C, resulting in the formation of Co- and N- co-doped carbon nanotube with earthworm-like morphology. The obtained catalyst was found to have a high density of defect sites, as confirmed by Raman spectroscopy. Here, cobalt (II) nanoparticles were stabilized on the atomically dispersed cobalt- and nitrogen-doped carbon nanotubes. The catalyst was confirmed to be effective in the catalytic hydrolysis of ammonia borane, in which the turnover frequency was 5.87 mol H2&#183;molCo-1&#183;min-1, and the specific hydrogen generation rate was determined to be 2447 mL H2&#183;gCo-1&#183;min-1. A synergistic function between the Co nanoparticle and the doped carbon nanotubes was proposed for the first time in the catalytic hydrolysis of ammonia borane reaction under a mild condition. The resulting hydrogen production with its high energy density and minimal refueling time could be suitable for future development as energy sources for mobile and stationary applications such as road trucks and forklifts in transport and logistics.

Here, we present a protocol to synthesize Co nanoparticles supported on carbon nanotubes with Co- and N- dopants for hydrogen productions.

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented ...

Metal Oxide Heterojunction for Photocatalytic Activities

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale applications. Sol-gel-based solution combustion synthesis (SG-SCS) is a simple method to produce ordered porous materials. In this regard, Pearson&#39;s hard and soft acids and bases theory assists in selecting host-dopant reactivity to form a proper heterojunction.
The formation of a heterojunction also changes the essential properties of the materials, improving photocatalysis via charge transfer or synergistic activities. A calcination temperature of 500 &#176;C is ideal for this process based on the results of the stability assessment via a differential thermogravimetry ratio analysis (DTG).
The nanoscale dimensions of the nanoparticles (NPs) and nanocomposites (NCs) generated were validated using X-ray diffraction and high-resolution transmission electron microscopy (HRTEM). Furthermore, the scanning electron microscopy micrographs and BET analyses confirmed the porosity nature of the materials. HRTEM, X-ray photoelectron spectroscopy, and energy-dispersive X-ray investigations established the materials composition. The study found that NCs degraded the acid orange 8 (AO8) color more efficiently than bare ZnO.

The development of a heterojunction boosts the photocatalytic activities of solution combustion synthesis, which is a time-/energy-efficient process. Advanced analytical characterization techniques were used in this protocol to evaluate the materials&#39; characteristics, and nanocomposites demonstrated improved acid orange-8 dye degradation.

Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for Cu(II) Through Microwave Pre-Pyrolysis

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