羟基自由基辅助沸石分子筛合成的研究进展

doi:10.6023/A22100420

化学学报 ›› 2023, Vol. 81 ›› Issue (1): 100-110.DOI: 10.6023/A22100420 上一篇

综述

羟基自由基辅助沸石分子筛合成的研究进展

张红丹, 兰欣雨, 程鹏^*()

沈阳师范大学化学化工学院能源与环境催化研究所沈阳 110034

投稿日期:2022-10-10 发布日期:2022-11-02

作者简介:

张红丹, 博士, 沈阳师范大学化学化工学院讲师, 硕士研究生导师, 主持国家自然科学基金青年项目1项, 省部级项目2项. 主要从事微纳米材料的设计合成及光催化性能研究和多级孔沸石分子筛的制备及C4烃裂解性能的研究.

兰欣雨, 沈阳师范大学化学化工学院2020级本科生. 主要从事超大孔沸石分子筛的探索合成.

程鹏, 博士, 沈阳师范大学化学化工学院副教授, 硕士研究生导师, 主持在研及完成国家自然科学基金2项, 省自然基金1项, 省教育厅重点项目1项. 入选辽宁省“兴辽英才计划”青年拔尖人才, 辽宁省高等学校创新人才支持计划, 沈阳市科技创新人才支持计划. 主要从事沸石分子筛的绿色合成及低碳烷烃裂解性能的研究.

基金资助:
项目受国家自然科学基金(22172102); 项目受国家自然科学基金(21701117); 项目受国家自然科学基金(22202137); “兴辽英才计划”(XLYC2007190); 沈阳市中青年科技创新人才支持计划(RC210044)

Advances in Hydroxyl Free Radical Assisted Synthesis of Zeolite

Hongdan Zhang, Xinyu Lan, Peng Cheng()

Institute of Catalysis for Energy and Environment, College of Chemistry and Chemical Engineering, Shenyang Normal University, Shenyang 110034, China

Received:2022-10-10 Published:2022-11-02
Contact: ^*E-mail: chengp1987@126.com
Supported by:
National Natural Science Foundation of China(22172102); National Natural Science Foundation of China(21701117); National Natural Science Foundation of China(22202137); LiaoNing Revitalization Talents Program(XLYC2007190); Shenyang Young and Middle-aged Scientific and Technological Innovation Talents Support Plan(RC210044)

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摘要/Abstract

作为化学工业中最重要的固体催化剂之一, 沸石分子筛在不同的领域发挥着广泛的应用. 随着消耗量的逐年增加, 如何绿色高效地制备沸石分子筛材料已经成为了研究热点. 羟基自由基是具有高活性的物种, 能够促进分子筛初始凝胶中硅铝酸盐的解聚和再聚合, 进而加速了分子筛的晶化过程. 众多研究表明, 除了能够加速沸石的结晶, 羟基自由基在其合成过程中还有其他的作用. 本综述从不同的产生方式入手, 系统地介绍了羟基自由基在沸石合成中的作用, 提出了该策略存在的问题, 并对其发展前景进行了展望.

关键词: 沸石, 羟基自由基, 结构导向剂, 合成, 加速

As one of the most important solid catalysts in chemical industry, zeolites are widely used in different fields. How to prepare zeolites greenly and efficiently has become a research hot issue with the increase of consumption year by year. Hydroxyl free radical is a highly active species, which can promote the depolymerization and repolymerization of aluminosilicates in the zeolite initial gel, and then accelerating the zeolite crystallization process. Besides accelerating the crystallization of zeolite, many studies have shown hydroxyl free radicals have other functions in zeolite synthesis. In this review, the role of hydroxyl free radicals in the synthesis of zeolites is systematically introduced via different generation methods. The challenges of the hydroxyl free radical assisted strategy are put forward, and its development directions are prospected.

Key words: zeolite, hydroxyl free radical, structure directing agent, synthesis, acceleration

引用此文

张红丹, 兰欣雨, 程鹏. 羟基自由基辅助沸石分子筛合成的研究进展[J]. 化学学报, 2023, 81(1): 100-110.

Hongdan Zhang, Xinyu Lan, Peng Cheng. Advances in Hydroxyl Free Radical Assisted Synthesis of Zeolite[J]. Acta Chimica Sinica, 2023, 81(1): 100-110.

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图/表 11

图1. 298 K, 紫外辐射和暗箱条件下的晶化过程. (A~D) NaX和NaZ-21在紫外辐射(A和B, 4.0 mW/cm2)和暗箱(C和D)条件下晶化24 h XRD谱图(绘制了相应的模拟XRD谱图进行比较(A图和B图, 红色)). (E)暗箱和紫外辐射(2.0, 4.0和8.0 mW/cm2)条件下钠硅物质的量比为4.4的NaA沸石的晶化曲线[19]

Figure 1. Crystallization processes under UV irradiation and dark conditions at 298 K. (A~D) The experimental XRD patterns of NaX and NaZ-21 synthesized under the UV conditions (A and B, black, 4.0 mW/cm2) and dark conditions (C and D, black) for 24 h, respectively. The corresponding simulated XRD patterns are plotted for comparison (A and B, red). (E) Crystallization curves of zeolite NaA under dark conditions and under UV conditions with irradiance of 2.0, 4.0 and 8.0 mW/cm2, with a Na2O/SiO2 molar ratio of 4.4[19]

图2. 紫外辐射辅助介孔材料合成的示意图[22]

Figure 2. Schematic illustration of UV assisted synthesis of mesoporous materials[22]

图3. 钛低聚物在?OH辅助下的解聚路线[25]

Figure 3. The deoligomerization pathway of titanium oligomers with the assistance of hydroxyl free radicals[25]

图4. (A)不同晶化时间不同过硫酸钠(SPS)浓度产物的产率; (B)不同加入量有机结构导向剂(TPAOH)和过硫酸钠浓度(0.02 mol/L)条件下不同晶化时间产物的产率[32]

Figure 4. (A) Yield of products with different crystallization times and different concentrations of sodium persulfate (SPS); (B) yield of products at different crystallization times under the conditions of different dosage of organic structure directing agent (TPAOH) and sodium persulfate concentration (0.02 mol/L)[32]

图5. 在Fenton试剂存在下, ?OH路线辅助Y型沸石的合成的示意图[42]

Figure 5. Schematic illustration of ?OH radical-assisted route for the synthesis of zeolite Y in the presence of Fenton’s reagent[42]

图6. 自由基化晶种辅助ECR-1合成的示意图[50]

Figure 6. Schematic illustration of radicalized seed assisted synthesis of zeolite ECR-1[50]

图7. 超声波辐射辅助ZSM-5合成的示意图[55]

Figure 7. Schematic illustration of ultrasonic radiation assisted synthesis of ZSM-5[55]

图8. γ射线辐射辅助A型沸石的快速合成[58]

Figure 8. Accelerated synthesis of zeolite A under Gamma rays (γ-rays) irradiation[58]

图9. 过氧化氢辅助高硅Y型沸石合成的示意图[59]

Figure 9. Schematic illustration of H2O2 assisted synthesis of high-silica zeolite Y[59]

图10. 半导体光催化剂光催化反应机理加速沸石合成的示意图[62]

Figure 10. Schematic diagram of the photocatalytic reaction mechanism of the semiconductor photocatalyst accelerating zeolite synthesis[62]

产生方法	优势	局限性
紫外辐射 γ射线辐射高能电子束辐射可见光辐射	强度易于控制	制备装置要求高; 对人体有不可逆转的伤害
等离子体超声波辐射	操作简便, 强度可控	•OH产生量不可控
Fenton试剂过硫酸盐 (NH₄)₂Ce(NO₃)₆	通过控制化学试剂的加入量进而控制•OH的量(半定量)	引入杂原子, 对分子筛的制备有一定影响
H₂O₂分解	方法简单, 无杂原子干扰	分解过程受外界条件影响较大
自由基化的晶种	无外来条件的干扰, 制备过程更纯净	因分子筛结构及组成众多, 自由基化的特定条件(球磨、煅烧等)不具有普适性

表1. 分子筛制备过程中不同方法产生羟基自由基的优势与局限性

Table 1. Advantages and disadvantages of different methods to produce hydroxyl free radicals in the zeolite synthesis process

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羟基自由基辅助沸石分子筛合成的研究进展

Advances in Hydroxyl Free Radical Assisted Synthesis of Zeolite

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