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

作者表彰了中国中央大学基础研究基金 (kyz201562)、中国博士后科学基金 (编号 2014m5660429) 和江苏省重点研究开发规划 (编号:BE2018708)。

1. 制备甘蔗渣活性炭
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基于甘蔗渣的活性炭前体的制备
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<li>用去离子水冲洗甘蔗渣 (从中国江苏的一个农场获得), 并将样品放入100°c 的烘箱中10小时。</li>
		<li>用磨床将干甘蔗粉碎, 并通过50目筛子筛筛粉。</li>
		<li>将30克细甘蔗渣粉放入 15 wt% 的磷酸 (h3 po4)溶液中, 重量为 1:1, 重量为 24h. 在105°c 的烤箱中将混合物干燥 6小时, 收集所产生的产品作为甘蔗渣型活...

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在该方案中, 关键的步骤之一是采用一步法成功制备具有较好物理化学性质的介孔碳, 在这种方法中需要确定最佳实验条件。因此, 在前面的28, 我们进行了正交阵列微波热解实验, 考虑了甘蔗渣和磷酸的浸渍比, 热解时间, 微波炉功率, 和干燥时间的影响。此外, 在繁琐的铜 (ii) 吸附实验中, 特别是在调整溶液 ph 值时, 必须非常小心, 因为 ph 值对活性炭去除铜 (ii) 有很大影响 (<strong cl...

活性炭具有独特的吸附性能, 如多孔结构发达、比表面积高、表面官能团多;因此, 它被用作水处理或净化1,2,3,4的吸附剂。活性炭除了具有物理优点外, 还具有成本效益, 对环境无害, 其原料 (如生物量) 丰富, 容易获得5,6。活性炭的物理化学特性取决于其制备过程中使用的前体和活化过程的实验条件7。
通常使用两种方法制备活性炭: 一步和两步方法8。"一步到位" 一步方法指的是先质体同时被碳化和激活, 而两步方法则是按顺序提到的。从节能环保的角度来看, 一步方法更倾向于降低温度和压力要求。
此外, 还利用化学和物理活化来改善活性炭的结构性能。化学活化具有较低的活化温度、较短的活化时间、较高的碳产率、在一定程度上更发达、可控的孔隙结构 9,具有明显的优势。已测试, 化学活化可以通过浸渍生物质浸渍生物质作为原料与 h3 po 4,zncl2, 或其他特定化学品, 然后热解, 以增加活性炭的孔隙率, 因为由于这些物质的脱氢能力 10、11, 通过后续的加热处理可以很容易地去除生物质的木质纤维素成分。因此, 化学活化大大增强了活性炭毛孔的形成, 或提高了对污染物12的吸附性能。酸性激活剂比 h3 po4更受欢迎, 因为它的能源需求相对较低, 产量较高, 对环境的影响较小13.
微波热解具有节省时间、室内加热均匀、节能、选择性加热等优点, 使其成为合成活性炭14、15 的替代加热方法。与传统的电加热相比, 微波热解可以增强热化学过程, 促进某些化学反应.最近, 广泛的研究重点是利用一步微波热解9、17、18、19从生物质中化学活化制备活性炭。因此, 微波辅助 h3 po 4 活化合成生物物质活性炭具有十分丰富的信息量和环保性.
此外, 为了提高活性炭对特定重金属离子的吸附亲和力, 提出了利用异质原子 [n、o、硫 (s)等) 将掺杂到碳结构中的方法, 这已被证明是一种理想的方法20、21、22、23、24、25、26。石墨层内部或边缘的缺陷位点可以被异质原子所取代, 从而产生功能基团27。因此, 硝化和还原改性被用来修改由此产生的碳样品, 使其成为涂料 nto 功能基团, 在有效地与重金属协调形成络合和离子交换28方面发挥着至关重要的作用。
基于以上发现, 我们提出了一种利用化学活化法合成生物质中的 n o 双掺杂介孔碳的方法, 以及两种不同的热解方法, 并进行了改性。该协议还确定了哪种加热方法有利于随后对 nto 官能团的掺杂进行改性, 从而提高了吸附性能。

<table border="0" cellpadding="0" cellspacing="0" width="932">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">All chemicals and reagents (phosphoric acid, etc.)</td>
			<td style="width:377px;">Nanjing Chemical Reagent Co., Ltd</td>
			<td style="width:119px;"></td>
			<td style="width:167px;">Analytical grade</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Electric furnace</td>
			<td>Luoyang Bolaimaite Experiment Electric Furnace Co., Ltd</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Microwave oven</td>
			<td>Nanjing Yudian Automation Technology Co., Ltd</td>
			<td></td>
			<td>2.45 GHz frequency</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Surface-area and porosimetry analyzer</td>
			<td>Beijing Gold APP Instrument Co., Ltd</td>
			<td style="width:119px;"></td>
			<td>Vc-Sorb 2800TP</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Fourier transform infrared (FTIR) spectrometer</td>
			<td>Nicolet</td>
			<td style="width:119px;"></td>
			<td>6700</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Flame atomic absorption spectrophotometry</td>
			<td>Beijing Purkinje General Instrument Corporation</td>
			<td style="width:119px;"></td>
			<td>A3</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Element Analyzer</td>
			<td>Germany Heraeus Co.</td>
			<td></td>
			<td>CHN-O-RAPID&#160;</td>
		</tr>
	</tbody>
</table>

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

提出了一种对铜 (ii) 进行高氮氧螯合吸附的生物质介孔活性炭的环保技术。以磷酸浸渍的甘蔗渣为前体。为了对前体进行热解, 采用了两种独立的加热方式: 微波热解和传统的电加热热解。由此产生的甘蔗渣衍生的碳样品通过硝化和还原改性进行了改性。氮 (n)/氧 (o) 官能团同时引入活性炭表面, 通过络合和离子交换提高其对铜 (ii) 的吸附。通过表征和铜吸附实验, 研究了四个制备的碳样品的理化性质, 确定哪种加热方法有利于随后对 nto 官能团的掺杂进行改性。该技术在分析氮吸附、傅里叶变换红外光谱和批量吸附实验数据的基础上, 证明了微波热解碳具有较多的缺陷位点, 从而节省了时间的有效微波。热解对碳贡献了更多的 nno 物种, 尽管它导致了更低的比表面积。该技术为合成氮、氧含量较高的吸附剂提供了一条很有前途的途径, 并为重金属离子在废水修复应用中的吸附能力提供了更高的吸附能力。

图 1显示了四个样品的氮吸附吸附和解吸等温线。所有吸附等温线在低 pp0区呈快速增加, 这些等温线属于 iv 型 (iupac 分类), 表明它们的孔隙结构由微孔和优势中孔 32组成。
从氮吸附等温线获得的所有样品的表面物理参数见表 1。微波热解和改性都有助于较小的布鲁纳...

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

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

本文提出了一种在不同热解模式下, 通过化学活化和改性法合成生物质氮氧/双掺杂介孔碳的方案。我们证明, 微波热解有利于随后的改性过程, 同时引入更多的氮和氧官能团的碳。

微波热解法制备了更高氮素/氧螯合吸附的生物物质基介孔碳对 cu (ii) 的研究

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

该方法有助于回答生物质利用和废水补救领域关键问题，如制备改性生物质基碳，去除废水中的重金属。该技术的主要优点是微波热解有利于后续的改性过程，同时引入更多的碳氮氧功能组。首先，用去维水冲洗甘渣，将样品放入100摄氏度的干燥炉中10小时。用研磨机粉碎干袋。然后，通过 50 网筛筛对粉末进行筛分。现在，将 30 克细袋渣粉放入 15 重量百分比的磷酸溶液中，在 24 小时的重量比中保持 24 小时。在105摄氏度的烤箱中干燥混合物6小时。将所得产品收集为基于袋渣的活性炭（BAC）的前体。现在，将15克前体放入微波炉中，频率为2.45千兆赫。将微波炉的功率设置为 900 瓦，使样品热解 22 分钟。使用转子流量计确保氮流速为每分钟 20 毫升。转子流量表的入口使用软管连接到氮气瓶，而进气口则连接到微波炉的进气口。使产生的碳冷却到氮气中室温后，在烧杯中三化并收集碳样品。现在，加入300毫升的0.1摩尔盐酸。在室温下，使用磁力搅拌器搅拌混合物超过 12 小时。用真空过滤过滤纸过滤碳。然后，用去维水冲洗样品，直到洗涤水的pH值大于6。在105摄氏度的真空干燥炉中干燥基于微波-热解袋的活性炭（MBAC），24小时。在零摄氏度的烧杯中混合50毫升浓缩硫酸和50毫升浓缩硝酸。然后，在混合溶液中加入 10 克 MBAC。使用磁搅拌器在 200 rpm 转速下搅拌混合物 120 分钟。用真空过滤过滤纸过滤硝化的MBAC。用去压水清洗碳，直到洗涤水达到pH6。然后，在90摄氏度的干燥炉中将洗涤的碳干燥24小时。在三颈烧瓶中，加入5.05克所得产品、50毫升去维水、20毫升15摩尔铵溶液。在 200 rpm 转速下用磁搅拌器搅拌该混合物 15 分钟。然后，加入28克二硫化钠，使混合物在室温下搅拌20小时。20 小时后，将反流冷凝器放入烧瓶中，并使用油浴将混合物加热至 100 摄氏度。在烧瓶中加入120毫升2.9摩尔醋酸。然后，让混合物在回流下用磁搅拌器搅拌五个小时。拆下油浴，使溶液冷却至室温。过滤碳样品，用去维水清洗，直到溶液pH值大于6。干燥经过修改的 MBAC 温度为 90 摄氏度，并表示为 MBAC 氮。要通过氮吸附和脱吸等温进行结构表征，首先称重空样品管。将大约 0.15 克的碳样品添加到样品管中。在110摄氏度的真空中将样品除气5小时。然后，称量含有碳的样品管，并计算碳样品的重量。将样品管安装到表面积的测试区域，用液氮测量测量样品管，温度为零下196摄氏度。要使用 Fourier 变换红外光谱执行化学特性，首先检查温度和湿度计。温度应为 16 至 25 摄氏度，相对湿度为 20%至 50%，去除样品库中的干燥剂和防尘盖。在110摄氏度下干燥碳样品和溴化钾4小时，以避免水对光谱的影响。然后，将碳样品与溴化钾混合，并使用压机准备测试样品。将样品放在测试区域中，并设置软件的参数。然后，保存光谱，在处理光谱之前拿出样品。为了进行铜离子吸附实验，首先使用0.1-摩尔硝酸和0.1摩尔氢氧化钠溶液将硫酸铜溶液的pH值调整为pH5。然后，将 0.05 克吸附剂放在每个锥形烧瓶中，其中含有 25 毫升的 pH 调节硫酸铜溶液。将盖子放在圆锥形烧瓶上，并放入恒温轨道摇床中，搅拌速率为 150 rpm，在 5 摄氏度、25 摄氏度，然后在每个温度下 45 摄氏度，持续 240 分钟。使用 0.22 微米膜过滤器将吸附蛋白与溶液分离。最后，使用火焰原子吸收分光度法测定滤金物的铜浓度。此处显示了所有样品的结构特征和元素成分。微波热解和改性有助于减少特定表面积和总孔径体积，但氮和氧含量更大。FTIR光谱表明，改性碳材料获得了明显的氮/氧功能群，微波热解碳得到的碳含量也更多。此处显示了 pH 对铜离子吸附的影响。MBAC-氮比EBAC-氮具有更好的铜离子吸附性，尽管由于氮/氧表面组更丰富，MBAC-氮的表面积和孔径体积较低。在此模型中，提出了改性碳吸附铜离子的机理。在这个反应过程中，化学吸附主要涉及离子交换和复合。虽然试图使用西方的方法，以中孔碳为基础来准备生物量，但微波热解具有更好的物理化学特性。考虑到浸渍比、热解时间和微波炉功率的影响，确定最佳实验条件非常重要。按照这个程序，可以执行其他修改方法，可以有效地引入更多的功能组碳，以克服缺点，如减少特定的表面积和总孔隙体积。该技术开发后，为功能化纳米材料领域的研究人员探索利用生物质快速制备高吸附碳进行废水修复铺平了道路。不要忘记，使用浓缩硫酸和浓缩硝酸可能是极其危险的，在执行本程序时应始终采取防护眼镜等预防措施。

Research

JoVE Journal

Environment

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

Measuring Carbon-based Contaminant Mineralization Using Combined CO2 Flux and Radiocarbon Analyses

Measuring Carbon-based Contaminant Mineralization Using Combined CO2 Flux and Radiocarbon Analyses

测量碳为基础的污染物矿化结合使用CO<sub&gt; 2</sub&gt;助焊剂和放射性碳分析

A method is described which uses the absence of radiocarbon in industrial chemicals and fuels made from petroleum feedstocks which frequently contaminate ...

科研

环境科学

Preparation and Testing of Impedance-based Fluidic Biochips with RTgill-W1 Cells for Rapid Evaluation of Drinking Water Samples for Toxicity

准备和测试阻抗为基础与RTgill-W1细胞饮用水进行快速评估水样进行毒性射流生物芯片

This manuscript describes how to prepare fluidic biochips with Rainbow trout gill epithelial (RTgill-W1) cells for use in a field portable water toxicity ...

Assessment of Labile Organic Carbon in Soil Using Sequential Fumigation Incubation Procedures

活性有机碳评估土壤中连续熏蒸孵化程序

Management practices and environmental changes can alter soil nutrient and carbon cycling. Soil labile organic carbon, a readily decomposable C pool, is ...

Biofilm Removal Using Carbon Dioxide Aerosols without Nitrogen Purge

去除生物膜使用二氧化碳气溶胶没有氮气吹扫

Biofilms can cause serious concerns in many applications. Not only can they cause economic losses, but they can also present a public health hazard. ...

A Flow-through Exposure System for Evaluating Suspended Sediments Effects on Aquatic Life

对水生生命值评价悬浮泥沙影响的流通系统曝光

This paper describes the Fish Larvae and Egg Exposure System (FLEES). The flow-through exposure system is used to investigate the effects of suspended ...

Functionalization and Dispersion of Carbon Nanomaterials Using an Environmentally Friendly Ultrasonicated Ozonolysis Process

碳纳米材料的功能化和分散使用环境友好的超声波臭氧分解过程

Functionalization of carbon nanomaterials is often a critical step that facilitates their integration into larger material systems and devices. In the ...

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

与CO平衡的原油流变学测量<sub&gt; 2</sub&gt;在水库条件

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The ...

Experimental System of Solar Adsorption Refrigeration with Concentrated Collector

聚光集热器太阳能吸附制冷实验系统

To improve the performance of solar adsorption refrigeration, an experimental system with a solar concentration collector was set up and investigated. The ...

Optimized Procedure for Determining the Adsorption of Phosphonates onto Granular Ferric Hydroxide using a Miniaturized Phosphorus Determination Method

用小型化磷测定法测定膦酸在粒状氢氧化铁上吸附的优化方法

This paper introduces a procedure to investigate the adsorption of phosphonates onto iron-containing filter materials, particularly granular ferric ...

Characterization of Aquatic Biofilms with Flow Cytometry

流式细胞仪对水生生物膜的表征

Biofilms are dynamic consortia of microorganism that play a key role in freshwater ecosystems. By changing their community structure, biofilms respond ...