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利用导向剂法制备磁性LSX型分子筛及改性

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王洪亮, 张震, 张勇平. 利用导向剂法制备磁性LSX型分子筛及改性[J]. 矿产综合利用, 2024, 45(5): 148-152. doi: 10.3969/j.issn.1000-6532.2024.05.021
引用本文: 王洪亮, 张震, 张勇平. 利用导向剂法制备磁性LSX型分子筛及改性[J]. 矿产综合利用, 2024, 45(5): 148-152. doi: 10.3969/j.issn.1000-6532.2024.05.021
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WANG Hongliang, ZHANG Zhen, ZHANG Yongping. Preparation and Modification of Magnetic LSX Type Molecular Sieve by Directing Agent Method[J]. Multipurpose Utilization of Mineral Resources, 2024, 45(5): 148-152. doi: 10.3969/j.issn.1000-6532.2024.05.021
Citation: WANG Hongliang, ZHANG Zhen, ZHANG Yongping. Preparation and Modification of Magnetic LSX Type Molecular Sieve by Directing Agent Method[J]. Multipurpose Utilization of Mineral Resources, 2024, 45(5): 148-152. doi: 10.3969/j.issn.1000-6532.2024.05.021
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利用导向剂法制备磁性LSX型分子筛及改性

  • 1.

    中国地质科学院郑州矿产综合利用研究所，国家非金属矿资源综合利用工程技术研究中心，自然资源部多金属矿综合利用评价重点实验室，河南省黄金资源综合利用重点实验室，河南　郑州　450006

  • 2.

    中国航天员科研训练中心 人因工程全国重点实验室，北京 100094

  • 基金项目: 人因工程国家重点实验室基金资助(HFNKL2023WW03)
详细信息
    作者简介: 王洪亮（1987- ），男，硕士，副研究员，从事沸石分子筛、碳分子筛与矿物材料研制

  • 中图分类号: TQ028.15

Preparation and Modification of Magnetic LSX Type Molecular Sieve by Directing Agent Method

  • 1.

    Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, China National Engineering Research Center for Utilization of Industrial Minerals, Key Laboratory for Polymetallic Ores' Evaluation and Utilization, MNR, Key Laboratory of Comprehensive Utilization of Gold Resource in Henan Province, Zhengzhou 450006, Henan, China

  • 2.

    National Key Laboratory of Human Factors Engineering，China Astronaut Research and Training Center, Beijing 100094, China

    摘要

  • 这是一篇材料学领域的论文。采用胶体导向剂与Fe3O4制备了磁性LSX分子筛原粉，经银离子交换与水合肼还原后生成了含银原子的磁性LSX分子筛，利用扫描电镜、振动样品磁强计、X衍射分析仪、光电子能谱仪、比表面吸附仪对样品的表面形貌、磁性、物相结构、元素组成与比表面积进行了分析表征，结果表明磁性LSX分子筛为LSX分子筛与Fe3O4的复合材料，微孔比表面积为679.38 m2/g，合成时胶体导向剂较佳加入量0.5%，磁性随Fe3O4加入量增加而增大，经银交换后与水合肼还原后的磁性LSX分子筛，比表面积减少。

    This is an article in the field of materials science. Magnetic LSX molecular sieves were prepared by colloidal directing agent and Fe3O4. After silver ion exchange and hydrazine hydrate reduction, magnetic LSX molecular sieves containing silver atoms were prepared, the surface morphology, magnetic properties, phase structure, elemental composition and specific surface area of the samples were characterized by scanning electron microscopy, vibrating sample magnetometer, X-ray diffraction analyzer, photoelectron spectroscopy and specific surface adsorption instrument. The results showed that magnetic LSX molecular sieve is the composite material of LSX molecular sieve and Fe3O4. The micropore specific surface area was 679.38 m2/g. The optimum dosage of colloidal guide agent was 0.5%. The magnetic properties increased with the increase of Fe3O4 content. The specific surface area of magnetic LSX molecular sieve reduced after silver exchange with hydrazine hydrate.

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  • 图 1  磁性LSX的SEM（放大2 000倍）

    Figure 1. 

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    图 2  磁性LSX的SEM（放大20 000倍）

    Figure 2. 

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    图 3  纯Fe3O4与磁性LSX型分子筛的磁性曲线

    Figure 3. 

    下载: 全尺寸图片 幻灯片

    图 4  含银离子与银原子的磁性LSX型分子筛XRD

    Figure 4. 

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    图 5  含银原子的磁性LSX型分子筛XPS

    Figure 5. 

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    图 6  含银原子磁性LSX型分子筛Ag3d XPS

    Figure 6. 

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    图 7  磁性LSX型分子筛相对压力与吸附量关系(77 K液氮)

    Figure 7. 

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    表 1  磁性LSX原粉静态水吸附量

    Table 1.  Static water adsorption capacity of magnetic LSX raw powders

    编号1234567
    胶体导向剂加入量/%00.511.50.50.50.5
    Fe3O4加入量/%0000135
    25 ℃/75%Rh吸水量/%3030.626.912.325.320.117.7
    注：1号样品为商业化LSX粉体，无磁性，用于性能对照。
    下载: 导出CSV

    表 2  三种材料的饱和磁场强度与饱和磁感应强度

    Table 2.  Saturation magnetic field intensity and saturation magnetic induction intensity of three materials

    名称 饱和磁场
    强度/（kA/m)    		 饱和磁感应
    强度/(emu/g)
    纯Fe3O4 1 184.0 73.50
    磁性LSX，Fe3O4加入量1% 1 189.6 3.41
    磁性LSX，Fe3O4加入量3% 1 188.8 17.71
    下载: 导出CSV

    表 3  磁性LSX型分子筛的拟合参数与比表面积

    Table 3.  Fitting parameters and specific surface area of magnetic LSX molecular sieve

    名称 拟合
    截距/
    mL    		 拟合
    斜率/
    mL    		 拟合
    系数    		 微孔比
    表面积
    S/(m2/g)
    磁性LSX原粉 -2.35×10-6 0.006 42 0.999 77 679.38
    含银离子的磁性LSX -2.41×10-6 0.007 39 0.999 83 590.18
    含银原子的磁性LSX 2.06×10-6 0.011 35 0.999 97 384.07
    下载: 导出CSV
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收稿日期:  2022-11-21
刊出日期:  2024-10-25

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