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Article(id=1172619714602877272, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1172619710446321994, articleNumber=1009-2617(2024)03-0265-10, orderNo=null, doi=10.13355/j.cnki.sfyj.2024.03.008, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1705852800000, receivedDateStr=2024-01-22, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1757503926182, onlineDateStr=2025-09-10, pubDate=1718812800000, pubDateStr=2024-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1757503926182, onlineIssueDateStr=2025-09-10, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1757503926182, creator=13701087609, updateTime=1757503926182, updator=13701087609, issue=Issue{id=1172619710446321994, tenantId=1146029695717560320, journalId=1146120122248306696, year='2024', volume='43', issue='3', pageStart='215', pageEnd='340', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1757503925191, creator=13701087609, updateTime=1758768108393, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1177922079165923462, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1172619710446321994, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1177922079165923463, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1172619710446321994, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=265, endPage=274, ext={EN=ArticleExt(id=1172619715315908956, articleId=1172619714602877272, tenantId=1146029695717560320, journalId=1146120122248306696, language=EN, title=Preparation of Magnetic Mesoporous Carbon Loaded Hydroxyapatite and Its Adsorption Performance of U(Ⅵ), columnId=1152626641181700664, journalTitle=Hydrometallurgy of China, columnName=Experiment Research, runingTitle=null, highlight=null, articleAbstract=

Magnetic mesoporous carbon(MMC) and hydroxyapatite(HAP) composite materials with different mass ratios were prepared by co-precipitation method(MMC@HAP-x x=1, 4, and 6), and used for the removal of radioactive U(Ⅵ) in aqueous solution. The structure, functional groups and surface potential of the MMC, HAP and MMC@HAP-x were characterized by XRD, FT-IR, Zeta. The kinetics, thermodynamics, and the mechanism of MMC@HAP-x adsorption of U(Ⅳ) by the aforementioned materials were systematically studied. The results show that the optimal pH of MMC@HAP-x for U(Ⅵ) is 4.0, and the time required to reach adsorption equilibrium is less than 10 min. The theoretical saturated adsorption capacity of MMC@HAP-6 is 1 164.62 mg/g, and the adsorption process is a spontaneous chemisorption process. The fixation of U(Ⅵ) in MMC@HAP-x is due to the interaction between HAP and $\mathrm{UO}_{2}^{2+}$ to form Ca(UO2)2(PO4)2·3H2O. MMC@HAP-6 is a fast uranium adsorbent with the potential to be used for the removal of uranium from radioactive wastewater.

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王有群(1988—),男,博士,副教授,主要研究方向为环境放射化学。E-mail:。
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曾冬玲(1998—),女,硕士研究生,主要研究方向为环境放射化学。

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曾冬玲(1998—),女,硕士研究生,主要研究方向为环境放射化学。

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曾冬玲(1998—),女,硕士研究生,主要研究方向为环境放射化学。

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a—XPS全谱;b—U 4f精细谱;c—P 2p精细谱;d—O 1s精细谱。

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吸附材料 BET比表面积/(m2·g-1) 平均孔径/nm 总孔容/(cm3·g-1)
MMC 1 112.45 4.09 1.18
MMC@HAP-1 476.39 3.38 0.40
MMC@HAP-4 255.73 5.56 0.36
MMC@HAP-6 220.22 6.27 0.34
HAP 611.912 10.63 1.74
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MMC@HAP-x的孔结构参数

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吸附材料 BET比表面积/(m2·g-1) 平均孔径/nm 总孔容/(cm3·g-1)
MMC 1 112.45 4.09 1.18
MMC@HAP-1 476.39 3.38 0.40
MMC@HAP-4 255.73 5.56 0.36
MMC@HAP-6 220.22 6.27 0.34
HAP 611.912 10.63 1.74
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吸附材料、 qe,试验/
(mg·g-1)		 准一级动力学模型 准二级动力学模型
qe,理论/(mg·g-1) k1/min-1 R2 qe,理论/(mg·g-1) k2/(g·mg-1·min-1) R2
MMC 51.85 49.79 0.33 0.97 50.34 17.90×10-3 0.99
HAP 250.76 244.43 0.25 0.98 255.46 1.03×10-3 0.99
MMC@HAP-1 186.58 171.39 0.20 0.95 194.35 1.39×10-3 0.98
MMC@HAP-4 242.08 242.21 2.23 0.98 247.24 2.58×10-2 0.99
MMC@HAP-6 252.41 246.62 4.08 0.98 248.26 10.83×10-2 0.99
), ArticleFig(id=1177918517165834337, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1172619714602877272, language=CN, label=表2, caption=

MMC@HAP-x吸附U(Ⅵ)的准一级和准二级动力学拟合参数

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吸附材料、 qe,试验/
(mg·g-1)		 准一级动力学模型 准二级动力学模型
qe,理论/(mg·g-1) k1/min-1 R2 qe,理论/(mg·g-1) k2/(g·mg-1·min-1) R2
MMC 51.85 49.79 0.33 0.97 50.34 17.90×10-3 0.99
HAP 250.76 244.43 0.25 0.98 255.46 1.03×10-3 0.99
MMC@HAP-1 186.58 171.39 0.20 0.95 194.35 1.39×10-3 0.98
MMC@HAP-4 242.08 242.21 2.23 0.98 247.24 2.58×10-2 0.99
MMC@HAP-6 252.41 246.62 4.08 0.98 248.26 10.83×10-2 0.99
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吸附材料 迅速吸附阶段 缓慢吸附阶段 动态平衡阶段
kid/(mg·g-1·min-0.5) C kid/(mg·g-1·min-0.5) C kid/(mg·g-1·min-0.5) C
MMC 16.09 7.92 5.16 27.58 1.01 42.24
HAP 103.94 -54.57 18.95 159.97 1.01 243.79
MMC@HAP-1 42.38 7.88 16.74 88.35 3.77 223.07
MMC@HAP-4 9.45 213.33 1.67 241.98 — —
MMC@HAP-6 8.90 223.83 0.57 248.25 — —
), ArticleFig(id=1177918517337800803, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1172619714602877272, language=CN, label=表3, caption=

MMC@HAP-x吸附U(Ⅵ)的颗粒内扩散拟合参数

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吸附材料 迅速吸附阶段 缓慢吸附阶段 动态平衡阶段
kid/(mg·g-1·min-0.5) C kid/(mg·g-1·min-0.5) C kid/(mg·g-1·min-0.5) C
MMC 16.09 7.92 5.16 27.58 1.01 42.24
HAP 103.94 -54.57 18.95 159.97 1.01 243.79
MMC@HAP-1 42.38 7.88 16.74 88.35 3.77 223.07
MMC@HAP-4 9.45 213.33 1.67 241.98 — —
MMC@HAP-6 8.90 223.83 0.57 248.25 — —
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吸附材料 Langmuir等温吸附模型 Freundlich等温吸附模型 Sips等温吸附模型
kL/(L·mg-1) qm/(mg·g-1) R2 kF/mg1-1/n·L1/n·g-1) n R2 kS/(L·mg-1) qm/(mg·g-1) R2
MMC 0.02 113.81 0.88 8.61 0.48 0.89 0.03 165.04 0.84
HAP 2.51 613.23 0.82 325.06 6.99 0.97 0.36 850.36 0.98
MMC@HAP-1 0.09 344.09 0.97 152.64 7.21 0.86 0.03 329.67 0.97
MMC@HAP-4 2.47 590.15 0.95 371.90 9.80 0.92 1.22 657.75 0.99
MMC@HAP-6 1.78 764.16 0.48 477.44 10.00 0.83 0.45 1 164.62 0.90
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Langmuir、Freundlich和Sips等温吸附拟合参数

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吸附材料 Langmuir等温吸附模型 Freundlich等温吸附模型 Sips等温吸附模型
kL/(L·mg-1) qm/(mg·g-1) R2 kF/mg1-1/n·L1/n·g-1) n R2 kS/(L·mg-1) qm/(mg·g-1) R2
MMC 0.02 113.81 0.88 8.61 0.48 0.89 0.03 165.04 0.84
HAP 2.51 613.23 0.82 325.06 6.99 0.97 0.36 850.36 0.98
MMC@HAP-1 0.09 344.09 0.97 152.64 7.21 0.86 0.03 329.67 0.97
MMC@HAP-4 2.47 590.15 0.95 371.90 9.80 0.92 1.22 657.75 0.99
MMC@HAP-6 1.78 764.16 0.48 477.44 10.00 0.83 0.45 1 164.62 0.90
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吸附材料 ΔH/
(kJ·mol-1)		 ΔS/
(J·mol-1·K-1)		 ΔG/(kJ·mol-1)
278.15 K 288.15 K 298.15 K 308.15 K 318.15 K
MMC 4.95 19.36 -5.38 -5.57 -5.77 -5.96 -6.15
HAP 21.00 88.04 -3.49 -4.37 -5.25 -6.13 -7.01
MMC@HAP-1 5.36 32.66 -3.72 -4.05 -4.38 -4.70 -5.03
MMC@HAP-4 18.96 86.37 -5.06 -5.93 -6.79 -7.66 -8.52
MMC@HAP-6 21.20 96.00 -5.50 -6.46 -7.42 -8.38 -9.34
), ArticleFig(id=1177918517597847655, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1172619714602877272, language=CN, label=表5, caption=

MMC@HAP-x吸附U(Ⅵ)的热力学参数

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吸附材料 ΔH/
(kJ·mol-1)		 ΔS/
(J·mol-1·K-1)		 ΔG/(kJ·mol-1)
278.15 K 288.15 K 298.15 K 308.15 K 318.15 K
MMC 4.95 19.36 -5.38 -5.57 -5.77 -5.96 -6.15
HAP 21.00 88.04 -3.49 -4.37 -5.25 -6.13 -7.01
MMC@HAP-1 5.36 32.66 -3.72 -4.05 -4.38 -4.70 -5.03
MMC@HAP-4 18.96 86.37 -5.06 -5.93 -6.79 -7.66 -8.52
MMC@HAP-6 21.20 96.00 -5.50 -6.46 -7.42 -8.38 -9.34
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项目 离子 U Cu Sr Al Ce Ti
S HAP 1.00 11.27 19.08 1.90 5.30 4.97
MMC@HAP-1 1.00 6.64 3.69 1.37 2.24 2.46
MMC@HAP-4 1.00 9.52 11.53 1.91 6.93 6.48
MMC@HAP-6 1.00 15.56 16.41 2.20 13.64 7.83
Sr MMC@HAP-1 1.00 5.18 1.39 2.36 2.02 1.70
MMC@HAP-4 1.00 1.65 1.00 0.76 0.77 1.18
MMC@HAP-6 1.00 1.16 0.86 0.39 0.63 0.72
), ArticleFig(id=1177918517740453993, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1172619714602877272, language=CN, label=表6, caption=

HAP、MMC@HAP-x在多离子系统中的选择性系数和相对选择性系数

, figureFileSmall=null, figureFileBig=null, tableContent=
项目 离子 U Cu Sr Al Ce Ti
S HAP 1.00 11.27 19.08 1.90 5.30 4.97
MMC@HAP-1 1.00 6.64 3.69 1.37 2.24 2.46
MMC@HAP-4 1.00 9.52 11.53 1.91 6.93 6.48
MMC@HAP-6 1.00 15.56 16.41 2.20 13.64 7.83
Sr MMC@HAP-1 1.00 5.18 1.39 2.36 2.02 1.70
MMC@HAP-4 1.00 1.65 1.00 0.76 0.77 1.18
MMC@HAP-6 1.00 1.16 0.86 0.39 0.63 0.72
), ArticleFig(id=1177918517853700202, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1172619714602877272, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
吸附材料 O P Ca Fe U
MMC-HAP-C 70.93 10.26 16.16 2.65 0.00
MMC-HAP-C-U 69.22 11.66 14.91 2.61 1.61
), ArticleFig(id=1177918517912420459, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1172619714602877272, language=CN, label=表7, caption=

MMC@HAP-C吸附U(Ⅵ)前、后的元素组成 %

, figureFileSmall=null, figureFileBig=null, tableContent=
吸附材料 O P Ca Fe U
MMC-HAP-C 70.93 10.26 16.16 2.65 0.00
MMC-HAP-C-U 69.22 11.66 14.91 2.61 1.61
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磁性介孔碳负载羟基磷灰石的制备及对U(Ⅵ)的吸附性能
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曾冬玲 1 , 陈磊 1 , 郑智阳 2 , 张志宾 1 , 曹小红 1 , 王有群 1 , 刘云海 1
湿法冶金 | 试验研究 2024,43(3): 265-274
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湿法冶金 | 试验研究 2024, 43(3): 265-274
磁性介孔碳负载羟基磷灰石的制备及对U(Ⅵ)的吸附性能
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曾冬玲1, 陈磊1, 郑智阳2, 张志宾1, 曹小红1, 王有群1 , 刘云海1
作者信息
  • 1 东华理工大学 核资源与环境国家重点实验室, 江西 南昌 330000
  • 2 核工业二九〇研究所, 广东 韶关 512029

    • 曾冬玲(1998—),女,硕士研究生,主要研究方向为环境放射化学。

通讯作者:

王有群(1988—),男,博士,副教授,主要研究方向为环境放射化学。E-mail:。
Preparation of Magnetic Mesoporous Carbon Loaded Hydroxyapatite and Its Adsorption Performance of U(Ⅵ)
Dongling ZENG1, Lei CHEN1, Zhiyang ZHENG2, Zhibin ZHANG1, Xiaohong CAO1, Youqun WANG1 , Yunhai LIU1
Affiliations
  • 1 School of Chemistry and Materials Science, East China Institute of Technology, Nanchang 330000, China
  • 2 Institute of Nuclear Industry 290, Shaoguan 512029, China
出版时间: 2024-06-20 doi: 10.13355/j.cnki.sfyj.2024.03.008
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摘要
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采用共沉淀法研究制备了不同质量比的磁性介孔碳(MMC)与羟基磷灰石(HAP)复合材料(MMC@HAP-x,x=1、4和6)并用于去除溶液中U(Ⅵ)。采用XRD、FT-IR、Zeta等方法表征了MMC、HAP和MMC@HAP-x的结构、功能基团及表面电位等理化性质。探讨了MMC@HAP-x吸附U(Ⅵ)的动力学、热力学及吸附机制。结果表明:MMC@HAP-x对U(Ⅵ)的吸附最佳pH均为4.0,达到吸附平衡所需时间均小于10 min,MMC@HAP-6的理论饱和吸附量可达1 164.62 mg/g,且吸附过程是自发的化学吸附过程。U(Ⅵ)在MMC@HAP-x的固定是由于HAP与$\mathrm{UO}_{2}^{2+}$相互作用形成了Ca(UO2)2(PO4)2·3H2O。MMC@HAP-6是一种快速的铀吸附剂,有望用于放射性废水中铀的去除。
磁性介孔碳  /  羟基磷灰石  /  U(Ⅵ)  /  吸附

Magnetic mesoporous carbon(MMC) and hydroxyapatite(HAP) composite materials with different mass ratios were prepared by co-precipitation method(MMC@HAP-x x=1, 4, and 6), and used for the removal of radioactive U(Ⅵ) in aqueous solution. The structure, functional groups and surface potential of the MMC, HAP and MMC@HAP-x were characterized by XRD, FT-IR, Zeta. The kinetics, thermodynamics, and the mechanism of MMC@HAP-x adsorption of U(Ⅳ) by the aforementioned materials were systematically studied. The results show that the optimal pH of MMC@HAP-x for U(Ⅵ) is 4.0, and the time required to reach adsorption equilibrium is less than 10 min. The theoretical saturated adsorption capacity of MMC@HAP-6 is 1 164.62 mg/g, and the adsorption process is a spontaneous chemisorption process. The fixation of U(Ⅵ) in MMC@HAP-x is due to the interaction between HAP and $\mathrm{UO}_{2}^{2+}$ to form Ca(UO2)2(PO4)2·3H2O. MMC@HAP-6 is a fast uranium adsorbent with the potential to be used for the removal of uranium from radioactive wastewater.

magnetic mesoporous carbon  /  hydroxyapatite  /  U(Ⅵ)  /  adsorption
曾冬玲, 陈磊, 郑智阳, 张志宾, 曹小红, 王有群, 刘云海. 磁性介孔碳负载羟基磷灰石的制备及对U(Ⅵ)的吸附性能. 湿法冶金, 2024 , 43 (3) : 265 -274 . DOI: 10.13355/j.cnki.sfyj.2024.03.008
Dongling ZENG, Lei CHEN, Zhiyang ZHENG, Zhibin ZHANG, Xiaohong CAO, Youqun WANG, Yunhai LIU. Preparation of Magnetic Mesoporous Carbon Loaded Hydroxyapatite and Its Adsorption Performance of U(Ⅵ)[J]. Hydrometallurgy of China, 2024 , 43 (3) : 265 -274 . DOI: 10.13355/j.cnki.sfyj.2024.03.008
正文
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铀生产加工过程中会产生大量含铀放射性废水,因此必须采用合适的方法进行处理。目前,含铀废水的处理方法主要包括蒸发法、膜分离法、离子交换法、吸附法等[1-2],其中,吸附法因具有效率高、成本低等特点受到广泛关注。
由于羟基磷灰石(HAP)具有无毒、易得、低成本和良好的离子交换性能等优点,被广泛应用于U(Ⅵ)的吸附研究中,但HAP比表面积小、易聚集、不易回收[3-4],通过与磁性纳米粒子复合,可使HAP在外加磁场时易于回收,迅速与溶液分离[5-6]。磁性介孔碳(MMC)是一种磁性多孔材料,具有高比表面积、高孔隙率、强磁性和优异的化学稳定性等优点,可作为HAP的优异载体。
试验以MMC为载体,研究采用共沉淀法制备不同质量比的磁性介孔碳(MMC)与羟基磷灰石(HAP)复合材料MMC@HAP-x(x=1,4和6),通过XRD、FT-IR、Zeta等手段表征了MMC@HAP-x的结构和化学性质,考察了废水pH、吸附时间和温度等对MMC@HAP-x吸附U(Ⅵ)性能的影响,并利用各种吸附模型研究MMC@HAP-x对铀的吸附行为(动力学、等温线和热力学)和吸附机制。
1 试验部分
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1.1 主要仪器设备与试剂
电子分析天平(AE166,德国梅特勒-托利多公司);电热恒温鼓风干燥箱(DHG-9343BS-Ⅲ,天津泰斯特仪器有限公司);开启式管式炉(LTDE,杭州卓驰仪器有限公司);精密pH计(PHS-3f,上海精密科学仪器有限公司);紫外-可见分光光度计(Shimadzu UV-2550,日本岛津公司);X-射线衍射谱仪(D8,德国Bruke公司);傅里叶变换红外光谱仪(FTS-63A,美国Bio-RAD公司);扫描电子显微镜、能谱仪(Nova Nano 450,荷兰FEI公司);Zeta电位仪(Stabino PMX 400,美国麦奇克有限公司)。
Fe(NO3)3·9H2O(AR,成都西亚化工有限公司);C12H22O11(AR,国药化学试剂有限公司);SBA-15(700~800 m2/g,南京先丰纳米材料科技有限公司);NaOH(AR,西陇化工股份有限公司);UO2(NO3)2•6H2O(99%,上海阿拉丁生化科技股份有限公司)。
1.2 材料的制备
采用硬模板法和共浸渍法制备磁性介孔碳(MMC)。将0.404 g Fe(NO3)3·9H2O溶解于含1.25 g蔗糖和0.14 g H2SO4的水溶液中;然后加入1 g SBA-15模板,将其分别在80 ℃的烘箱中加热6 h、160 ℃的烘箱中加热6 h;之后将所得材料在700 ℃氮气流中煅烧6 h,所得产物用1 mol/L NaOH溶液(50%乙醇-50%H2O)洗涤数次后进行干燥,得所需磁性介孔碳(MMC)。
采用共沉淀法制备不同质量比的MMC@HAP-x(x=1,4和6)。将0.5 g MMC加入0.5 mL CaCl2(1 mol/L),再加入0.5 mL (NH4)2HPO4(0.6 mol/L)混合均匀,用浓氨水在搅拌条件下调节pH至10~11,在40 ℃下搅拌4 h,之后离心、洗涤、过滤、干燥、研磨,得MMC与HAP质量比为10/1的MMC@HAP-1。利用相同方法制得质量比分别为10/4和10/6的磁性介孔碳负载的羟基磷灰石(MMC@HAP-4和MMC@HAP-6)。
1.3 吸附试验
精确移取调节pH和浓度后的一定体积铀标准溶液至锥形瓶中,加入0.010 0 g MMC@HAP-x,在振荡箱中恒温振荡一定时间后,离心,取上清液,采用ICP测定其中U(Ⅵ)浓度,根据式(1)[7]计算吸附量(qe):
qe=$\frac{({\rho }_{0}-{\rho }_{e})V}{m}$。
式中:ρ0、ρe—吸附前、后溶液中U(Ⅵ)质量浓度,mg/L;V—溶液体积,L;m—吸附剂质量,g。
2 试验结果与讨论
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2.1 MMC@HAP-x的物化性能表征
2.1.1 FT-IR分析
采用FT-IR分析MMC@HAP-x的表面功能基团,结果如图1所示。可以看出:MMC@HAP-x和HAP都在559、600和1 021 cm-1出现磷酸盐(PO43-)的吸收峰[8];在961、1 021、3 400 cm-1出现的吸收峰为材料表面的O—H伸缩振动峰[9],555、602 cm-1处的振动峰为Fe—O峰[10]。上述结果表明MMC与HAP成功复合。
2.1.2 XRD分析
采用粉末X射线衍射(PXRD)测定样品的物相结构,结果如图2所示。可以看出:所制备样品HAP、MMC@HAP-4和MMC@HAP-6在25.5°、31.9°、33.9°、39.6°、46.6°、49.2°和64.0°处出现了明显的衍射峰,这与HAP的标准卡片(PDF#73-1731)相吻合[11];MMC@HAP-1的衍射峰宽且低,说明材料的结晶度偏低;MMC和MMC@HAP-1图谱中,30.0°、35.4°和62.5°处出现的衍射峰为Fe3O4(PDF#86-1347),表明材料中磁性氧化铁含量较多;随HAP在复合材料中占比增大,MMC@HAP-4和MMC@HAP-6的图谱中均出现明显的HAP和Fe3O4特征峰,表明成功制备目标材料。
2.1.3 N2吸附—脱附曲线
采用N2吸附—脱附方法测定了MMC和MMC@HAP-x材料的多孔结构,结果如图3所示,孔结构参数见表1。由图3(a)看出:5种吸附材料的N2吸附—脱附曲线均为Ⅳ型等温线[12],均出现了H4型回滞环,表明所有材料均为介孔结构。由表1看出:随HAP含量增加,MMC@HAP-x比表面积由1 112.45 m2/g降至220.22 m2/g。由图3(b)看出:MMC、MMC@HAP-1和MMC@HAP-4孔径分布较窄,平均孔径分别为4.09、3.38和5.56 nm。
2.1.4 Zeta电位
图4为MMC@HAP-x表面电位随pH的变化曲线,HAP的Zeta电位在测试范围内一直为负值,而MMC则在6.82之前一直处于正电位。HAP与MMC复合后,MMC@HAP-1、MMC@HAP-4、MMC@HAP-6的零电位点对应的pH(pHIZC)分别为4.53,4.31和4.02,MMC@HAP-x的表面电位为负值时,MMC@HAP-x将与带正电的铀酰离子($\mathrm{UO}_{2}^{2+}$)产生静电引力,有利于MMC@HAP-x对U(Ⅵ)的吸附。
2.1.5 VSM
VSM测量MMC@HAP-x的磁滞回线如图5所示。可以看出:合成的MMC和MMC@HAP-x的磁滞回线都呈S形。随MMC与HAP占比从10/1增至10/6,MMC@HAP-x的比饱和磁化强度(Ms)从1.42 (A·m2)/kg降至0.80(A·m2)/kg。由于HAP的存在,使得MMC@HAP-x的Ms低于MMC。上述结果表明,HAP和MMC成功复合,并使得MMC@HAP-x材料具有超顺磁性(图5内插图)。材料使用后可利用外磁体对其聚集分离。
2.2 吸附材料对U(Ⅵ)的吸附性能
2.2.1 溶液初始pH对U(Ⅵ)吸附性能的影响
配制铀质量浓度为50 mg/L的溶液,用0.1 mol/L HNO3和0.5 mol/L NaOH溶液调节pH,随后加入10 mg吸附剂(以下性能试验除相应变量外,均在该条件下进行),溶液初始pH对MMC、HAP、MMC@HAP-x吸附U(Ⅵ)的影响试验结果如图6所示。
由图6看出,pH在2~7范围内,MMC、HAP、MMC@HAP-1、MMC@HAP-4、MMC@HAP-6对U(Ⅵ)的吸附量均随pH升高呈先升高后降低趋势:pH=2时,MMC@HAP-x、HAP吸附材料发生酸碱中和反应,其结构被破坏,因此U(Ⅵ)吸附量较低,溶液中U(Ⅵ)质量浓度无明显变化;随pH升高,MMC@HAP-x对铀吸附性能增强,这是由羟基和磷官能团引起的[13];pH大于5时,U(Ⅵ)吸附量逐渐下降,这可能是由于在pH考察范围内溶液中铀离子存在形式发生变化所致[14];pH继续升高时,表面带负电荷的MMC@HAP-x和溶液中U(Ⅵ)阴离子(如(UO2)3$\mathrm{(OH)}_{7}^{-}$和UO2$\mathrm{(OH)}_{4}^{2-}$)之间的静电斥力增强,铀吸附量明显下降。因此,确定HAP、MMC@HAP-4、MMC@HAP-6的最佳吸附pH为4,而MMC和MMC@HAP-1的最佳吸附pH分别为6和5。
2.2.2 吸附动力学
为了研究吸附动力学,采用准一级、准二级动力学和粒内扩散模型(式(2)~(4)[15-17])对所得试验数据进行拟合。
$q_{t}=q_{\mathrm{e}}\left(1-\mathrm{e}^{-k_{1} t}\right) ;$
$q_{t}=\frac{q_{\mathrm{e}}^{2} k_{2} t}{1+q_{\mathrm{e}} k_{2} t} ;$
$q_{t}=k_{\mathrm{id}} t^{0.5}+C。$
式中:k1—准一级动力学吸附常数,min-1;k2—准二级动力学吸附速率常数,g/(mg·min);qt—吸附t时间时MMC@HAP-x对U(Ⅵ)的吸附量,mg/g;qe—吸附平衡时MMC@HAP-x对U(Ⅵ)的吸附量,mg/g;kid—颗粒内扩散速率常数,mg/(g·min0.5);C—颗粒内扩散模型中边界层厚度成正比的常数,mmol/g。
准一级、准二级动力学拟合曲线如图7所示,拟合参数见表2。可以看出:MMC@HAP-1对U(Ⅵ)的吸附量在0~8 min内快速增加,之后在8~30 min内缓慢增加,直至达到吸附平衡(186.58 mg/g);MMC@HAP-4和MMC@HAP-6对U(Ⅵ)的吸附量在0~1 min内快速增大,1~5 min内缓慢增加,直至达到吸附平衡(242.08 mg/g和252.41 mg/g);MMC、HAP和MMC@HAP-x吸附U(Ⅵ)的准一级动力学拟合线性相关度较准二级的更大,说明上述材料对U(Ⅵ)的吸附过程由化学作用支配,且对比k2可知,MMC@HAP-6对U(Ⅵ)的吸附速率最快。
颗粒内扩散模拟合曲线如图8所示,拟合参数见表3。可以看出:MMC@HAP-1对U(Ⅵ)的吸附过程可分为迅速吸附、缓慢吸附和动态平衡3个阶段;而对于MMC@HAP-4与MMC@HAP-6,根据已测得试验数据,将吸附过程分为迅速吸附阶段和缓慢吸附阶段,主要是由于材料的初始吸附效率过快,根据已有手段未能测得快速吸附阶段的数据;但最终MMC@HAP-x表面的活性位点均达到饱和状态,吸附达到动态平衡。
2.2.3 吸附等温线
试验探讨了不同铀浓度条件下,MMC、HAP、MMC@HAP-x对U(Ⅵ)的吸附行为,并绘制吸附等温线,同时采用Langmuir等温吸附模型对试验数据进行拟合,明确其对U(Ⅵ)的吸附机制。利用控制变量法,固定其他试验条件,利用相同的U(Ⅵ)母液稀释所得不同浓度U(Ⅵ)溶液,探究溶液U(Ⅵ)浓度对MMC、HAP和MMC@HAP-x吸附U(Ⅵ)的影响。MMC、HAP和MMC@HAP-x对U(Ⅵ)的吸附量均呈先快速增加后缓慢增加并逐渐趋于饱和趋势。由试验数据可知,MMC、HAP和MMC@HAP-4、MMC@HAP-4、MMC@HAP-6对U(Ⅵ)的饱和吸附量分别为76.35、607.52、342.62、620.88和852.39 mg/g,可以看出,MMC@HAP-x对U(Ⅵ)的吸附性能优于单纯的HAP与MMC材料,其中以MMC@HAP-6最优。
应用Langmuir、Freundlich和Sips等温吸附模型(式(5)~(7)[18-19])对试验数据进行拟合,拟合曲线如图9所示,拟合参数见表4。
qe=$\frac{{q}_{m}{k}_{L}{\rho }_{e}}{1+{k}_{L}{\rho }_{e}}$;
qe=kF${\rho }_{e}^{1/n}$;
qe=$\frac{{q}_{m}{k}_{S}{\rho }_{e}^{\beta }}{1+{k}_{S}{\rho }_{e}^{\beta }}$。
式中:ρe—吸附平衡时尾液中U(Ⅵ)质量浓度,mg/L;qe—吸附平衡时MMC@HAP-x对U(Ⅵ)的吸附量,mg/g;qm—MMC@HAP-x对U(Ⅵ)的最大吸附量,mg/g;kL—Langmuir平衡常数,L/mg;kF—Freundlich平衡常数,mg1-1/n·L1/n·g-1;n—吸附强度;kS—Sips平衡常数,L/mg,β—Sips吸附参数,表示吸附材料的不均匀性,越接近1表示材料表面越均匀。
由图9、表4看出:MMC、HAP和MMC@HAP-x吸附U(Ⅵ)的Sips等温吸附模型线性相关度R2(0.84、0.98、0.97、0.99、0.90)均大于Langmuir和Freundlich吸附等温模型线性相关度,说明Sips模型对U(Ⅵ)在MMC@HAP-x上的吸附过程拟合效果最好,即MMC@HAP-x材料表面的活性位点属于非均匀分布,U(Ⅵ)在MMC@HAP-x材料表面的吸附过程为非均相吸附。
2.2.4 吸附热力学
在温度288.15~313.15 K范围内,考察温度对MMC@HAP-x吸附性能的影响及吸附过程中的热力学变化,试验结果如图10所示。采用公式(8)~(10)[20]计算吸附热力学参数,结果见表5。可以看出:MMC@HAP-x吸附U(Ⅵ)的吸附量随温度升高而缓慢增加,说明升温对MMC@HAP-x吸附U(Ⅵ)有利;MMC、HAP和MMC@HAP-x的ΔH>0、ΔS>0、ΔG<0,表明其对U(Ⅵ)的吸附为自发的吸热过程。
kd=$\frac{{q}_{e}}{{\rho }_{e}}$×1 000;
ln kd=$\frac{\Delta S}{R}$-$\frac{\Delta H}{RT}$;
ΔG=ΔH-TΔS。
式中:kd—吸附分配系数,L/mg;R—理想气体常数,8.314J/(mol·K);T—热力学温度,K;ΔG—吉布斯自由能变,kJ/mol;ΔH—焓变,kJ/mol;ΔS—熵变,J/(mol·K)。
2.2.5 吸附的选择性
配制含Cu2+、Sr2+、Al3+、Ce3+、Ti4+的$\mathrm{UO}_{2}^{2+}$溶液(外加金属离子质量浓度为25 mg/L),考察杂质金属阳离子对MMC@HAP-x吸附U(Ⅵ)的影响,试验结果如图11所示。根据式(11)~(12)计算HAP、MMC@HAP-x的选择性系数S和相对选择系数Sr,结果见表6。可以看出:MMC@HAP-x对U(Ⅵ)具有较好的选择性能,且随HAP掺杂比例逐渐增大,材料对U(Ⅵ)的选择性能提升。
S$\left(\frac{U\left(Ⅵ\right)}{MMC@HAP-x}\right)$=$\frac{{K}_{d}^{U\left(Ⅵ\right)}}{{K}_{d}^{MMC@HAP-x}}$;
Sr=$\frac{S(MMC@HAP-x)}{S\left(HAP\right)}$。
式中:Kd—U(Ⅵ)的分配系数,mg/L。
2.3 吸附机制
采用SEM-EDS对负载MMC@HAP-6样品进行表征,结果如图12~13、表7所示。可以看出:MMC@HAP-6无固定的形貌结构,呈大颗粒状,且表面粗糙,说明HAP散乱分布在MMC表层上(图12(a)、(c));而MMC@HAP-6吸附U(Ⅵ)后的表面微观形貌呈无序的细小絮状与片状(图12(b)、(d)),表明MMC@HAP-6吸附U(Ⅵ)后的结构更为无序;而由所测得的EDS数据(图13、表7)可知,吸附后的MMC@HAP-6中含有U元素,结合SEM-EDS的数据结果判断,MMC@HAP-6已成功从溶液中吸附U(Ⅵ)。
采用FT-IR分析吸附U(Ⅵ)后的MMC@HAP-6的表面官能团,结果如图14所示。可以看出:MMC@HAP-6吸附U(Ⅵ)前后的FT-IR图谱没有明显变化;吸附后在920.15 cm-1处出现新峰,对应的是$\mathrm{UO}_{2}^{2+}$的伸缩振动峰[21];除此峰外没有出现其他新峰,表明吸附后未引入其他新的基团。
采用XRD表征吸附前后材料的结构,结果如图15所示。可以看出:MMC@HAP-6吸附U(Ⅵ)后结构并未发生明显改变;在16.43°、17.94°和24.57°处出现的峰分别与Ca(UO2)2(PO4)2·3H2O(PDF#39-1351)的(001),(101),(110)相对应[22],表明U(Ⅵ)通过与MMC@HAP-6相互作用形成的沉淀物已成功固定在材料上。
采用XPS探究材料的表面结构特征和元素化学状态,结果如图16所示。可以看出:负载铀的MMC@HAP-6包含与O 1s、Ca 2p和P 2p相对应的峰,这与MMC@HAP-6一致;此外,负载铀的MMC@HAP-6出现2个属于U 4f(382.37、393.16 eV)的振动峰[23](图16(b)),表明MMC@HAP-6成功地从溶液中吸附了U(Ⅵ);在P 2p的精细谱中(图16(c)),132.87、133.94 eV处出现的峰分别归属于MMC@HAP-6中磷酸基团P 2p3/2和P 2p1/2的轨道自旋分裂峰,由于$\mathrm{PO}_{4}^{3-}$和U(Ⅵ)离子之间的强烈反应,使得负载铀的MMC@HAP-6中P 2p3/2和P 2p1/2的峰位分别偏移至133.38、135.37 eV;在O 1s的精细谱中(图16(d)),位于533.35、532.16 eV的分裂峰分别属于—OH基团和$\mathrm{PO}_{4}^{3-}$基团,在530.87 eV的峰归属于Fe—O键[24]。在O 1s光谱图中,它们的结合能和峰值强度在吸附铀前后发生了较明显变化,在530.61 eV处出现了1个新峰,属于$\mathrm{UO}_{2}^{2+}$离子。基于上述结果推断,MMC@HAP-6对U(Ⅵ)的吸附主要归因于羟基(—OH)配合,以及U(Ⅵ)与$\mathrm{PO}_{4}^{3-}$和Ca2+在MMC@HAP-6中的强相互作用。
3 结论
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采用共沉淀法成功制备了不同质量比的磁性介孔碳(MMC)与羟基磷灰石(HAP)复合材料MMC@HAP-x(x=1、4和6)。MMC@HAP-x对U(Ⅵ)的最佳吸附pH均为4.0,达到吸附平衡所需时间分别为8、5和5 min,其理论饱和吸附量分别为329.67、657.75和1 164.62 mg/g。MMC@HAP-6对U(Ⅵ)的吸附是由于其携带的羟基等功能基团与铀酰离子相互作用形成了Ca(UO2)2(PO4)2·3H2O,且吸附过程是自发的化学吸附,属于非均匀吸附过程。MMC@HAP-6初步解决了HAP比表面积小、难以回收的问题,避免了繁琐的过滤和离心过程,提高了吸附效率,是一种从放射性溶液中去除U(Ⅵ)的潜在高效吸附剂。
基金
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  • 国家自然科学基金资助项目(22076022)
文献
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doi: 10.13355/j.cnki.sfyj.2024.03.008
  • 接收时间：2024-01-22
  • 首发时间：2025-09-10
  • 出版时间：2024-06-20
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  • 收稿日期：2024-01-22
基金
国家自然科学基金资助项目(22076022)
作者信息
    1 东华理工大学 核资源与环境国家重点实验室, 江西 南昌 330000
    2 核工业二九〇研究所, 广东 韶关 512029

通讯作者:

王有群(1988—),男,博士,副教授,主要研究方向为环境放射化学。E-mail:。
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https://castjournals.cast.org.cn/joweb/sfyj/CN/10.13355/j.cnki.sfyj.2024.03.008
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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