膨润土改性制备多孔结构钛锂离子筛前驱体

黄成华; 李燕; 张菁菁; 税亿; 吴娜; 张理元

doi:10.7513/j.issn.1004-7638.2022.03.001

膨润土改性制备多孔结构钛锂离子筛前驱体

doi: 10.7513/j.issn.1004-7638.2022.03.001

黄成华^1,,
李燕¹,
张菁菁¹,
税亿¹,
吴娜¹,
张理元^{1, 2, ,}

1.
内江师范学院化学化工学院, 四川内江 641112
2.
果蔬类废弃物资源化四川省高校重点实验室, 四川内江 641112

基金项目: 四川省科技计划项目 (项目号2019YJ0383)。

详细信息

作者简介:
黄成华 (1963—)，女，四川资中人，本科，副教授，主要从事离子交换吸附材料研究，E-mail：758361920@qq.com

通讯作者:
张理元，博士，副教授，E-mail：zhangliyuansir@126.com

中图分类号: TF823,TQ424
计量
- 文章访问数: 313
- HTML全文浏览量: 93
- PDF下载量: 50
- 被引次数: 0
出版历程
- 收稿日期: 2022-05-05
- 刊出日期: 2022-06-30

Synthesis of porous bentonite modified titanium-lithium ion sieve precursor

1.
College of Chemistry and Chemical Engineering, Neijiang Normal University, Neijiang 641112, Sichuan, China
2.
Key Laboratory of Fruit Waste Treatment and Resource Recycling of the Sichuan Provincial College, Neijiang 641112, Sichuan, China

摘要

摘要: 以Ti(SO₄)₂为钛源，CH₃COOLi·2H₂O为锂源，NH₃·H₂O为沉淀剂，H₂O₂为络合剂，采用沉淀胶溶法制备了钛酸锂前驱体溶胶，添加膨润土，经搅拌、陈化、干燥、煅烧后得到膨润土改性Li₂TiO₃粉体。研究了络合剂H₂O₂与Ti的摩尔比(R)、煅烧温度、膨润土与溶胶的固液比对Li₂TiO₃的表面形貌及晶体结构的影响。采用扫描电镜、X射线衍射、热重-差示扫描量热、红外光谱对样品进行表征。结果表明，当R=6时，未改性的Li₂TiO₃在750 ℃煅烧下，晶体结构最完整。按1.67 g/L的固液比添加膨润土对样品进行改性后，煅烧温度为750 ℃时各晶面结晶最完整，得到表面呈均匀多孔结构的Li₂TiO₃。
- Li₂TiO₃ /
- 无机沉淀胶溶法 /
- 膨润土 /
- 络合剂
Abstract: The lithium titanate precursor sol was prepared by inorganic precipitation-peptization method with titanium sulfate as titanium source, lithium acetate as lithium source, followed by adding bentonite as modifier. Bentonite modified Li₂TiO₃ powder was obtained after stirring, aging, drying and calcination. The effects of molar ratio (R) of complexing agent H₂O₂ to Ti, calcination temperature, solid-liquid ratio of bentonite to sol on the surface morphology and crystal structure of precursor Li₂TiO₃ were studied. The samples were characterized by scanning electron microscopy, X-ray diffraction, thermogravimetry-differential scanning calorimetry and infrared spectroscopy. The results show that the crystal structure of unmodified Li₂TiO₃ is the most complete when calcined at 750 ℃ with R = 6. After the sample was modified by bentonite with a solid-liquid ratio of 1.67 g/L, the crystallinity of each crystal surface was the most complete when the calcination temperature was 750 ℃, and Li₂TiO₃ with uniform porous structure on the surface was obtained.
- Li₂TiO₃ /
- precipitation-peptization method /
- bentonite /
- complexing agent

HTML全文

图 1 H₂O₂与Ti的摩尔比(R)不同时的Li₂TiO₃的SEM形貌

Figure 1. SEM images of Li₂TiO₃ with different molar ratios of H₂O₂ to Ti

(a) R=3；(b) R=4；(c) R=5；(d) R=6；(e) R=7；(f) R=9

下载: 全尺寸图片幻灯片

图 2 H₂O₂与Ti的摩尔比不同时的Li₂TiO₃的XRD谱

Figure 2. XRD patterns of Li₂TiO₃ with different molar ratios of H₂O₂ to Ti

(a) R=3；(b) R=4；(c) R=5；(d) R=6；(e) R=7；(f) R=9

下载: 全尺寸图片幻灯片

图 3 膨润土-Li₂TiO₃在不同煅烧温度下的XRD谱（固液比为1.667 g/L，R=6）

Figure 3. XRD patterns of bentonite-Li₂TiO₃ calcined at different temperatures with a solid-to-liquid ratio of 1.667 g/L and R value of 6

(a) 600 ℃；(b) 650 ℃；(c) 700 ℃； (d) 750 ℃；(e) 800 ℃；(f) 900 ℃

下载: 全尺寸图片幻灯片

图 4 膨润土-Li₂TiO₃热重-差示扫描量热曲线

Figure 4. TG-DSC curve of bentonite-Li₂TiO₃

下载: 全尺寸图片幻灯片

图 5 按不同固液比添加膨润土改性处理的Li₂TiO₃的XRD谱（R=6）

Figure 5. XRD patterns of Li₂TiO₃modified by adding bentonite at different solid-to-liquid ratios with R value of 6 value of 6

(a) 0.333 g/L；(b) 1 g/L；(c) 1.667 g/L；(d) 2.5 g/L；(e) 3.333 g/L

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图 6 按不同固液比添加膨润土改性处理的Li₂TiO₃的SEM形貌（R=6）

(a) 煅烧后膨润土；(b) 0.333 g/L；(c) 1 g/L；(d) 1.667 g/L；(e) 2.5 g/L；(f) 3.333 g/L

Figure 6. SEM images of Li₂TiO₃ modified by adding bentonite at different solid-liquid ratios with R value of 6

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图 7 Li₂TiO₃和膨润土-Li₂TiO₃(1.667 g/ L)的FTIR谱

(a) Li₂TiO₃ ； (b) 膨润土-Li₂TiO₃

Figure 7. FTIR spectra of Li₂TiO₃ and bentonite-Li₂TiO₃

下载: 全尺寸图片幻灯片

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