SiO2/COPs的合成及其在光催化反应中的协同效应

doi:10.1016/S1872-2067(21)63812-3

催化学报 ›› 2021, Vol. 42 ›› Issue (10): 1821-1830.DOI: 10.1016/S1872-2067(21)63812-3

• 论文 • 上一篇

SiO₂/COPs的合成及其在光催化反应中的协同效应

李成斌^a, 李贺^a, 李纯志^a^,^b, 任小敏^a^,^b, 杨启华^a()

^a中国科学院大连化学物理研究所, 催化基础国家重点实验室, 辽宁大连116023
^b中国科学院大学, 北京100049

收稿日期:2021-02-08 接受日期:2021-03-13 出版日期:2021-10-18 发布日期:2021-06-20
通讯作者: 杨启华
作者简介:*电话: (0411)84379552; 传真: (0411)84694447; 电子信箱:yangqh@dicp.ac.cn
第一联系人：
^†共同第一作者.
基金资助:
国家重点研发计划(2017YFB0702800);国家自然科学基金(21733009);国家自然科学基金(22002162);中国科学院战略性科技先导专项(XDB17020200)

One-pot synthesis of mesosilica/nano covalent organic polymer composites and their synergistic effect in photocatalysis

Chengbin Li^a, He Li^a, Chunzhi Li^a^,^b, Xiaomin Ren^a^,^b, Qihua Yang^a()

^aState Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China

Received:2021-02-08 Accepted:2021-03-13 Online:2021-10-18 Published:2021-06-20
Contact: Qihua Yang
About author:First author contact:
^†These authors contributed equally to this work.
Supported by:
National Key R&D Program of China(2017YFB0702800);National Natural Science Foundation of China(21733009);National Natural Science Foundation of China(22002162);Strategic Priority Research Program of the Chinese Academy of Sciences(XDB17020200)

摘要/Abstract

摘要：

共价有机聚合物(COPs)是一类由轻质元素(C, H, O, N和B等)通过共价键的方式连接而成的有机多孔材料. COPs的共轭结构赋予其优异的可见光吸收特性, 已经在光催化水分解制氢、二氧化碳还原、有机合成和污染物降解等领域显示出巨大的应用潜力. 虽然COPs具有能带结构易调控和高孔隙率等优点, 但其光催化活性仍有待提升. 使用助催化剂是提升COPs的光催化活性, 促进表面反应普遍采用的策略. 此外, 底物活化官能团的引入和光催化剂表面性质的调控也是提高光催化剂反应活性的有效方法. 虽然可以通过改变COPs单体种类、化学键的类型和拓扑结构来调控COPs的组成, 但要同时兼顾COPs的结构和亲疏水性的调控以及底物活化官能团的引入仍十分困难. 与纯COPs相比, 与其他材料进行杂化为扩大COPs的化学组成和功能性提供了更多可能. 迄今为止, 在COPs纳米孔中封装分子、纳米颗粒或将COPs涂覆在其他固体材料上是制备基于COPs复合材料的常用策略. 但是, 考虑到COPs和无机材料合成条件的不相容性, 在纳米尺度精确控制复合材料的组分、结构和形貌仍然是一项艰巨的任务.
本文制备了稳定在十六烷基三甲基溴化铵(CTAB)疏水核中的COPs胶体, 其粒度分布在16 nm左右. 通过溶胶-凝胶法在CTAB周围水解聚合四乙氧基硅烷, 得到SiO₂/COPs复合材料. 表征结果表明, COPs均匀分布在氧化硅的骨架中. 该复合材料具有分别来自于SiO₂和COPs的介孔和微孔结构. 与纯COPs相比, 复合材料的表面疏水性降低. SiO₂/COPs具有可见光响应特性, 其吸收带边随COPs含量的增加而红移, 表明在复合材料中COPs在高含量时发生团聚. SiO₂/COPs作为光催化剂, 可高效催化α-溴代苯乙酮的还原脱卤反应(汉斯酯为还原剂), 其催化活性和SiO₂/COPs比例相关, 在COPs含量为22.6 wt%时达到最优. SiO₂/COPs的催化活性较COPs有大幅度提高. 在优化的SiO₂/COPs比例下, SiO₂/COPs的TOF是COPs的近12倍. 控制实验表明, SiO₂中的羟基对汉斯酯为还原剂有活化作用. 此外, 本文研究发现, 复合材料的活性与SiO₂/COPs的比值呈火山型曲线, 表明在光催化反应中SiO₂和COPs之间存在协同效应. 由此可见, 将光催化剂和反应物活化材料耦合是提高光催化反应活性的有效策略.

关键词: 共价有机聚合物, 介孔氧化硅, 杂化材料, 协同效应, 光催化, 还原脱卤反应

Abstract:

Organic-inorganic hybrid materials provide a desirable platform for the development of novel functional materials. Here, we report the one-pot synthesis of mesoporous hybrid nanospheres by the in-situ sol-gel condensation of tetraethoxysilane around surfactant micelle-confined nano covalent organic polymer (nanoCOP) colloids. The hybrid nanospheres containing nanoCOPs uniformly distributed in the mesosilica network, inherited the visible light responsive properties of the nanoCOPs. The turnover frequency of the hybrid nanospheres is almost 12 times that of its corresponding bulk COP counterpart for the photocatalytic reductive dehalogenation of α-bromoacetophenone, which is attributed to activation of the Hantzsch ester reductant by the hydroxyl group. The existence of a volcano relationship between the activity and nanoCOP/mesosilica ratio confirmed the synergistic effect between nanoCOP and mesosilica. Our preliminary results suggest that hybridization of semiconductors and reactant-activating materials is an efficient strategy for enhancing the activity of a catalyst for photocatalysis.

Key words: Covalent organic polymers, Mesoporous silica, Hybrid materials, Synergy effect, Photocatalysis, Reductive dehylogenation reaction

李成斌, 李贺, 李纯志, 任小敏, 杨启华. SiO₂/COPs的合成及其在光催化反应中的协同效应[J]. 催化学报, 2021, 42(10): 1821-1830.

Chengbin Li, He Li, Chunzhi Li, Xiaomin Ren, Qihua Yang. One-pot synthesis of mesosilica/nano covalent organic polymer composites and their synergistic effect in photocatalysis[J]. Chinese Journal of Catalysis, 2021, 42(10): 1821-1830.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63812-3

https://www.cjcatal.com/CN/Y2021/V42/I10/1821

图/表 12

Fig. 1. (a) Schematic illustration of the mesoporous silica-nanoCOP hybrid material preparation procedure; (b) A photograph of the Tyndall effect with laser penetration through the TP-TAPB nanoCOP solution; (c) The size distribution of the TP-TAPB nanoCOP solution obtained from DLS; (d) A photograph of the representative C/S-0.65 catalyst.

Fig. 2. (a) FTIR spectra of the C/S-x samples; (b) Solid state 13C CP-MAS NMR spectrum of C/S-0.65.

Table 1 The physicochemical parameters of C/S-x, mesoSiO2, and TP-TAPB COF/COP.

Sample	BET SSA (m²/g)	V total (cm³/g)	Pore size (nm)	COF/COPContent^a(wt%)	N content^b(mmol/g)	Water contact angle (°)
TP-TAPB COF	628	0.5	1-2	100	6.09	43.5
TP-TAPB COP	664	1.2	1-2	100	6.22	33.0
C/S-0.3	641	0.6	1-2, 3.4	34.2	2.33	26.8
C/S-0.65	660	2.1	1.6, 3.2	22.6	1.82	27.2
C/S-1.3	656	2.0	1.6, 3.2	18.1	1.64	25.3
C/S-2.6	662	0.9	1-2, 3.4	14.4	1.48	21.6
MesoSiO₂	608	0.9	1.6, 3.4	0	0	23.8

Fig. 3. (a-d) High-resolution scanning electron microscopy (HRSEM) images of the C/S-x samples; HRSEM image (e), and the corresponding high-angle annular dark ?eld scanning transmission electron microscopy (HAADF-STEM) image (f) of C/S-1.3 after in-situ photodeposition of 3 wt% Pt (inset is the particle size distribution of the Pt NPs).

Fig. 4. (a-d) HRTEM images of C/S-x; (e) STEM image and EDS elemental mapping images of C/S-0.65.

Fig. 5. (a) N2 sorption isotherms (the N2 sorption isotherms were vertically shifted) and (b) non-local density functional theory (NLDFT) pore size distribution curves of the C/S-x samples and mesoSiO2.

Fig. 6. (a) UV-vis diffuse reflectance spectra (UV-vis DRS) of the C/S-x samples; (b) Band gap energy of C/S-0.65; (c) Schematic energy band structure of the C/S-x samples; EPR spectra of DMPO ?O2￣ (d) and TEMPO h+ (e) for the C/S-x and TP-TAPB COF materials under blue LED light irradiation and (f) transient absorption spectra of TP-TAPB COF and C/S-0.65 (inset).

Fig. 7. (a) Reaction profiles for C/S-x, TP-TAPB COF, and TP-TAPB COP; (b) The relationship between activity and the nanoTP-TAPB/SiO2 ratio.

Table 2 Photoreductive dehalogenation of α-bromoacetophenone with different catalysts under blue LED light irradiation.a.

Photocatalyst	Yield^b(%)	TOF^c(h^-1)	Photocatalyst	Yield^b(%)
TP-TAPB COF	88	15	mesoSiO₂	7
NanoTP-TAPB COP	83	6	C/S-0.65^d	1
C/S-0.3	65	22	C/S-0.65^e	15
C/S-0.65	87	68	C/S-0.65^f	81
C/S-1.3	88	58	C/S-0.65^g	1
C/S-2.6	86	54	C/S-0.65^h	33
C/SMe-0.65	37	18	C/S-0.65ⁱ	36

Scheme 1. Proposed mechanism for the photocatalytic dehalogenation reaction over the C/S-x catalysts.

Fig. 8. Reaction profiles of C/S-0.65 (a) and TP-TAPB COF (b) in the photoreductive dehalogenation of α-bromoacetophenone using different amounts of HE.

Table 3 Photoreductive dehalogenation of phenacyl bromide derivatives using C/S-0.65 as photocatalyst.a

Substrate	Product	Substrate	Product
1a	2a 85%	1e	2e 37%
1b	2b 35%	1f	2f 91%
1c	2c 78%	1g	2g 67%
1d	2d 39%	1h	2h 71%

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SiO₂/COPs的合成及其在光催化反应中的协同效应

One-pot synthesis of mesosilica/nano covalent organic polymer composites and their synergistic effect in photocatalysis

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