炭化与焙烧温度对植物基铁碳微电解材料去除As(Ⅲ)性能的影响

doi:10.16085/j.issn.1000-6613.2022-1588

化工进展 ›› 2023, Vol. 42 ›› Issue (7): 3652-3663.DOI: 10.16085/j.issn.1000-6613.2022-1588

炭化与焙烧温度对植物基铁碳微电解材料去除As(Ⅲ)性能的影响

李海东¹(), 杨远坤¹^,², 郭姝姝¹, 汪本金¹, 岳婷婷¹, 傅开彬¹^,², 王哲¹^,², 何守琴³, 姚俊⁴, 谌书¹^,²()

^1.西南科技大学环境与资源学院，四川绵阳 621000
^2.固体废物处理与资源化教育部重点实验室，四川绵阳 621000
^3.西南科技大学经济管理学院，四川绵阳 621000
^4.中国地质大学（北京）水资源与环境学院，北京 100083

收稿日期:2022-08-29 修回日期:2022-11-02 出版日期:2023-07-15 发布日期:2023-08-14
通讯作者: 谌书
作者简介:李海东（1997—），男，硕士研究生，研究方向为水污染治理。E-mail：3064651627@qq.com。
基金资助:
国家重点研发计划(2019YFC1803500);国家自然科学基金青年基金(42107481);川省科技计划-重点研发项目(2021YFS0289);西南科技大学科研基金(20zx7150);四川循环经济研究中心科技项目(XHJJ-1417)

Effect of carbonization and calcination temperature on As(Ⅲ) removal performance of plant-based Fe-C microelectrolytic materials

LI Haidong¹(), YANG Yuankun¹^,², GUO Shushu¹, WANG Benjin¹, YUE Tingting¹, FU Kaibin¹^,², WANG Zhe¹^,², HE Shouqin³, YAO Jun⁴, CHEN Shu¹^,²()

^1.School of Environment and Resource, Southwest University of Science and Technology, Mianyang 621010, Sichuan, China
^2.Key Laboratory of Solid Waste Treatment and Resource Recycle, Ministry of Education, Mianyang 621010, Sichuan, China
^3.School of Economics and Management, Southwest University of Science and Technology, Mianyang 621010, Sichuan, China
^4.China University of Geosciences in Beijing, Beijing 100083, China

Received:2022-08-29 Revised:2022-11-02 Online:2023-07-15 Published:2023-08-14
Contact: CHEN Shu

摘要/Abstract

摘要：

以美人蕉、还原铁粉和膨润土为原材料制备植物基铁碳微电解材料，先通过单因素实验确定Fe/C物质的量比、炭化温度和焙烧温度3个影响因素，后采用Box-Behnken响应面法对“均质化-炭化-焙烧”制备工艺进行优化，以确定最优制备条件。并结合X射线衍射（XRD）、电子顺磁共振波谱仪（EPR）、傅里叶红外光谱仪（FTIR）等表征方法，探究烧制温度对植物基铁碳微电解材料固有性质及其去除As(Ⅲ)性能的影响。结果表明，最优制备条件为Fe/C=1.05、炭化温度502.87℃、焙烧温度760.92℃。烧制温度的升高，有利于增强碳基组分得电子能力，加速As(Ⅲ)氧化为As(Ⅴ)，降低水体生物毒性的同时提高对As(Ⅲ)的去除率；当焙烧温度高于700℃时，膨润土晶体结构层瓦解，渗透性提高的同时加速Ca²⁺、Mg²⁺离子释放，并促进Fe³⁺的水解沉积物互斥作用减弱，提高对As(Ⅲ)的吸附容量；还原铁粉过量5%，在保证反应时微原电池数量的同时，表面氧化产生的Fe₃O₄、Fe₂O₃在酸性条件下易反应形成Fe²⁺、Fe³⁺，对As(Ⅲ)的吸附去除作用加强。

关键词: 铁碳微电解材料, As(Ⅲ), 响应面优化, 热解, 电化学, 造粒

Abstract:

Plant-based iron-carbon microelectrolysis materials were prepared by use of canna, reduced iron powder and bentonite as raw materials. Three main factors affected on As(Ⅲ) removal efficiency were firstly determined through single factor experiment, and the determined influencing factors were iron-carbon molar ratio, carbonization temperature and roasting temperature. In order to determine the optimal preparation conditions, box-Behnken response surface method was then used to optimize the preparation process of “homogenization, carbonization and roasting”. The effect of firing temperature on the intrinsic properties of plant-based iron-carbon microelectrolysis materials and their influence on As( $Ⅲ$ ) removal performance were finally investigated in combination with X-ray diffraction (XRD), electron paramagnetic resonance spectroscopy (EPR), Fourier transform infrared spectrometer (FTIR) and other characterization methods. The results showed that the optimum preparation conditions of Fe/C, carbonization temperature and roasting temperature were 1.05℃, 502.87℃ and 760.92℃, respectively. As increase of firing temperature, the electron separation capacity of carbon base enhanced which further accelerated the oxidation of As( $Ⅲ$ ) to As( $Ⅴ$ ) and improved the removal rate of As( $Ⅲ$ ). When the calcination temperature was higher than 700℃, the crystal structure layer of bentonite collapsed and increased their permeability, which can accelerate the release of Ca²⁺ and Mg²⁺ ions, weaken the mutual exclusion of Fe³⁺ hydrolyzed sediments, and thus improved the adsorption capacity of As( $Ⅲ$ ). When utilized amount of reduced iron powder exceeds 5%, the Fe₃O₄ and Fe₂O₃ produced by surface oxidation can easily react to form Fe²⁺ and Fe³⁺ under acidic conditions while ensuring the number of microgalvanic cells in the reaction. All of these strengthened the adsorption removal effect of As(Ⅲ).

Key words: iron micro-electrolysis material, As( $Ⅲ$ ), response surface optimization, pyrolysis, electrochemistry, granulation

中图分类号:

X522

李海东, 杨远坤, 郭姝姝, 汪本金, 岳婷婷, 傅开彬, 王哲, 何守琴, 姚俊, 谌书. 炭化与焙烧温度对植物基铁碳微电解材料去除As(Ⅲ)性能的影响[J]. 化工进展, 2023, 42(7): 3652-3663.

LI Haidong, YANG Yuankun, GUO Shushu, WANG Benjin, YUE Tingting, FU Kaibin, WANG Zhe, HE Shouqin, YAO Jun, CHEN Shu. Effect of carbonization and calcination temperature on As(Ⅲ) removal performance of plant-based Fe-C microelectrolytic materials[J]. Chemical Industry and Engineering Progress, 2023, 42(7): 3652-3663.

图/表 18

表1 美人蕉植物材料元素组成及原子比

样品

名称

灰分

图1 各因素对As(Ⅲ)去除率的影响

表2 Box-Behnken设计实验因数与水平

自变量	因数	范围和水平
自变量	因数	低（-1）	中（0）	高（+1）
Fe/C	A	0.8	1.0	1.2
炭化温度/℃	B	450	500	550
焙烧温度/℃	C	600	700	800

表3 Box-Bennken响应面实验设计及结果

实验编号	因素			As(Ⅲ)去除率（美人蕉） /％
实验编号	A	B	C	As(Ⅲ)去除率（美人蕉） /％
1	0.8	450	700	85.47
2	1.2	450	700	91.86
3	0.8	550	700	88.83
4	1.2	550	700	93.36
5	0.8	500	600	68.36
6	1.2	500	600	77.39
7	0.8	500	800	95.49
8	1.2	500	800	98.56
9	1	450	600	68.18
10	1	550	600	74.68
11	1	450	800	96.04
12	1	550	800	96.48
13	1	500	700	95.53
14	1	500	700	95.05
15	1	500	700	94.81
16	1	500	700	95.42
17	1	500	700	95.63

表4 二次回归模型检验及方差分析

模型项	平方和	自由度	均方	F值	P值
模型	1674.59	9	186.07	914.56	<0.0001
Fe/C（A）	66.24	1	66.24	325.59	<0.0001
炭化温度（B）	17.41	1	17.41	85.55	<0.0001
焙烧温度（C）	1199.52	1	1199.52	5895.98	<0.0001
AB	0.8649	1	0.8649	4.25	0.0482
AC	8.88	1	8.88	43.65	0.0003
BC	9.18	1	9.18	45.13	0.0003
A²	19.49	1	19.49	95.80	<0.0001
B²	44.65	1	44.65	219.48	<0.0001
C²	282.18	1	282.18	1387.02	<0.0001
残差	1.42	7	0.2034
失拟项	0.9460	3	0.3153	2.64	0.1859
误差值	0.4781	4	0.1195
总和	1676.01	16
R²_adj	0.9981		R²	0.9992
精密度	87.4283		R²_Pred	0.9905

图2 炭化温度-焙烧温度间交互影响As(Ⅲ)去除率的响应面3D图

图3 纤维素、半纤维素和木质素TG分析

图4 不同烧制温度下碳基材料红外光谱图

图5 不同热裂解温度下碳基材料的PFRs信号

表5 生物炭PFRs参数

样品	g值	线宽/Gs
400	2.00452±0.00006	6.27
500	2.00386±0.00002	5.29
600	2.00377±0.00003	4.75
700	2.00342±0.00001	4.38
800	2.00337±0.00002	3.65

图6 投加前后铁碳微电解填料的XRD图谱

图7 不同焙烧温度下铁碳微电解填料的XRD图谱与还原铁粉（Fe0）氧化反应的∆G-T关系

表6 铁氧化反应的标准摩尔吉布斯自由能变化表达式

编号	反应式	标准摩尔吉布斯自由能变化表达式
Y1	4Fe₃O₄+O₂ $̿$ 6Fe₂O₃	$Δ G γ 1 ⊖$ =-586770+340.20T
Y2	3/2Fe+O₂ $̿$ 1/2Fe₃O₄	$Δ G γ 2 ⊖$ =-563320+169.24T
Y3	6Fe+O₂ $̿$ 2Fe₃O₄	$Δ G γ 3 ⊖$ =-636130+255.67T
Y4	6Fe+O₂ $̿$ 2FeO	$Δ G γ 4 ⊖$ =-539080+140.56T

表6 铁氧化反应的标准摩尔吉布斯自由能变化表达式

编号	反应式	标准摩尔吉布斯自由能变化表达式
Y1	4Fe₃O₄+O₂ $̿$ 6Fe₂O₃	$Δ G γ 1 ⊖$ =-586770+340.20T
Y2	3/2Fe+O₂ $̿$ 1/2Fe₃O₄	$Δ G γ 2 ⊖$ =-563320+169.24T
Y3	6Fe+O₂ $̿$ 2Fe₃O₄	$Δ G γ 3 ⊖$ =-636130+255.67T
Y4	6Fe+O₂ $̿$ 2FeO	$Δ G γ 4 ⊖$ =-539080+140.56T

图8 不同烧制温度下膨润土结构变化

图9 不同烧制温度下膨润土Ca2+和Mg2+释放量

图10 Fe/C物质的量比-焙烧温度间交互影响As(Ⅲ)去除率的响应面3D图

图11 在750℃焙烧条件下不同Fe/C物质的量比铁碳微电解材料电化学特性和Fe 2p结合态的XPS分析

表7 美人蕉植物基铁碳微电解材料最优制备条件

碳基

材料

Fe/C

摩尔比

炭化温度

/℃

焙烧温度

/℃

相对偏差

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炭化与焙烧温度对植物基铁碳微电解材料去除As(Ⅲ)性能的影响

Effect of carbonization and calcination temperature on As(Ⅲ) removal performance of plant-based Fe-C microelectrolytic materials

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