多孔TiO2/g-C3N4异质结的制备及其光催化辅酶再生性能研究

doi:10.11949/0438-1157.20250443

摘要/Abstract

摘要：

光催化辅酶再生对生物氧化还原反应具有重要意义。采用溶胶-凝胶法制备了多孔TiO₂-60，经300℃煅烧获得TiO₂-300，再与三聚氰胺混合煅烧得到多孔TiO₂/g-C₃N₄异质结。考察了TiO₂煅烧、三聚氰胺用量对催化剂结构和性能的影响，并优化了催化剂用量。结果表明：TiO₂的煅烧使晶相从金红石相转变为锐钛矿晶型，制备的TiO₂/g-C₃N₄具有高比表面积、宽吸收边、窄带隙及更好的电荷分离效率；随着三聚氰胺用量的增加，比表面积和孔体积先增加后减小，光吸收和电荷分离性能先上升后下降；优化后，催化活性和收率分别为4.8 mmol/(L·g·min)和72%，分别是g-C₃N₄的7.4倍和5.3倍，且在5次循环中性能稳定。

关键词: 多孔TiO₂, g-C₃N₄, 异质结, 光催化, 辅酶再生

Abstract:

Photocatalytic coenzyme regeneration holds great significance for bio-redox reactions. Porous TiO₂-60 was prepared via sol-gel method. After calcined at 300℃, TiO₂-300 was obtained and then mixed with melamine and calcined again to get a porous TiO₂/g-C₃N₄ heterojunction. The effects of TiO₂ calcination and melamine dosage on the structure and performance of catalyst were studied, and the catalyst dosage was optimized. The results showed that TiO₂ calcination engendered the crystal phase to transform from rutile to anatase. The as-prepared TiO₂/g-C₃N₄ featured high specific surface area, broad absorption edge, narrow band gap, and better charge separation efficiency. With increasing melamine dosage, the specific surface area and pore volume first increase and then decreased, while the light absorption and charge separation properties first increase and then decreased. After optimization, the catalytic activity and yield reached 4.8 mmol/(L·g·min) and 72% respectively, about 7.4 and 5.3 times those of g-C₃N₄. Moreover, the catalyst showed stable performance over five cycles.

Key words: porous TiO₂, g-C₃N₄, heterojunction, photocatalysis, NADH regeneration

中图分类号:

TQ 028.8

孙菲雪, 刘宁, 刘文芳, 孟子晖. 多孔TiO₂/g-C₃N₄异质结的制备及其光催化辅酶再生性能研究[J]. 化工学报, 2025, 76(12): 6351-6365.

Feixue SUN, Ning LIU, Wenfang LIU, Zihui MENG. Fabrication of porous TiO₂/g-C₃N₄heterojunction and investigation on its photocatalytic performance of coenzyme regeneration[J]. CIESC Journal, 2025, 76(12): 6351-6365.

图/表 17

图1 多孔TiO2(a)和TiO2/g-C3N4(b)的制备流程图

Fig.1 Preparation routes of porous TiO2 (a) and TiO2/g-C3N4 (b)

图2 TiO2-60(a)，TiO2-300(b)，TiO2-60/g-C3N4(c)和TiO2-300/g-C3N4(d)的SEM照片

Fig.2 SEM images of TiO2-60 (a), TiO2-300 (b), TiO2-60/g-C3N4 (c) and TiO2-300/g-C3N4 (d)

图3 TiO2-60/g-C3N4和TiO2-300/g-C3N4的XRD谱图(a)、FTIR谱图(b)、N2等温吸附-脱附曲线(c)和孔径分布曲线(d)

Fig.3 XRD patterns(a), FTIR spectra (b), N2 isothermal adsorption-desorption curves (c) and pore size distribution curves (d) of TiO2-60/g-C3N4 and TiO2-300/g-C3N4

表1 TiO2-60/g-C3N4和TiO2-300/g-C3N4的孔结构参数和光学性质

Table 1 Pore structure parameters and optical properties of TiO2-60/g-C3N4 and TiO2-300/g-C3N4

样品	S_BET/(m²/g)	V/(cm³/g)	D_ave/nm	E_g/eV	λ_g/nm
TiO₂-300/g-C₃N₄	276	0.31	18.8	2.59	455
TiO₂-60/g-C₃N₄	108	0.18	16.7	2.63	440
TiO₂-300	226	0.28	23.6	2.85	410
TiO₂-60	128	0.21	21.4	2.90	400
g-C₃N₄	13	—	—	2.65	450

图4 TiO2-300/g-C3N4的TEM(a)和HRTEM(b)图像

Fig.4 TEM (a) and HRTEM (b) image of TiO2-300/g-C3N4

图5 TiO2-300/g-C3N4的原位XPS

Fig.5 In-situ XPS of TiO2-300/g-C3N4

图6 g-C3N4、TiO2-300和TiO2-300/g-C3N4的XPS价带谱C 1s (a)和能带结构图(b)

Fig.6 VB XPS of g-C3N4, TiO2-300 and TiO2-300/g-C3N4(a) and band structure diagram (b)

图7 TiO2-60/g-C3N4和TiO2-300/g-C3N4的UV-vis DRS(a)、PL光谱(b)、电化学阻抗(c)和光电流测试结果(d)

Fig.7 UV-vis DRS (a), PL spectra (b), electrochemical impedance (c) and photocurrent test results (d) of TiO2-60/g-C3N4 and TiO2-300/g-C3N4

图8 TiO2-60/g-C3N4和TiO2-300/g-C3N4的反应动力学曲线(a)，催化活性和NADH收率(b)；TiO2-300/g-C3N4体系在不同光照时间下的紫外-可见吸收光谱(c)

Fig.8 Reaction kinetic curves (a) and catalytic activity and NADH yield (b) of TiO2-60/g-C3N4 and TiO2-300/g-C3N4; (c) UV-vis spectra of TiO2-300/g-C3N4 system under different illumination times

图9 TiO2/g-C3N4-m的SEM照片

Fig.9 SEM images of TiO2/g-C3N4-m

图10 TiO2/g-C3N4-m的XRD谱图(a)； FTIR谱图(b)； N2等温吸附-脱附曲线(c)；孔径分布曲线(d)

Fig.10 XRD patterns (a)； FTIR spectra (b)； N2 isothermal adsorption-desorption curves (c) and pore size distribution curves (d) of TiO2/g-C3N4-m

表2 TiO2/g-C3N4-m的孔结构参数和光学性质

Table 2 Pore structure parameters and optical properties of TiO2/g-C3N4-m

样品	S_BET/(m²/g)	V/(cm³/g)	D_ave/nm	E_g/eV	λ_g/nm
TiO₂/g-C₃N₄-1.5	243	0.29	17.5	2.71	430
TiO₂/g-C₃N₄-1.8	276	0.31	18.8	2.59	455
TiO₂/g-C₃N₄-2.1	176	0.28	13.2	2.64	450

图11 TiO2/g-C3N4-m的UV-vis DRS(a)和PL光谱(b)

Fig.11 UV-vis DRS (a) and PL spectra (b) of TiO2/g-C3N4-m

图12 TiO2/g-C3N4-m的反应动力学曲线(a)与催化活性和NADH收率(b)

Fig.12 Reaction kinetic curves (a) and catalytic activity and NADH yield (b) of TiO2/g-C3N4-m

图13 不同TiO2/g-C3N4用量的反应动力学曲线(a)与催化活性和NADH收率(b)

Fig.13 Reaction kinetic curves (a) and catalytic activity and NADH yield (b) with different dosage of TiO2/g-C3N4

图14 TiO2/g-C3N4的重复利用性：反应动力学曲线(a); XRD谱图(b); SEM图(c),(d)

Fig.14 Reusability of TiO2/g-C3N4: reaction kinetic curves(a); XRD patterns(b); SEM photos(c),(d)

图15 再生NADH的生物活性

Fig.15 Biological activity of regenerated NADH

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多孔TiO₂/g-C₃N₄异质结的制备及其光催化辅酶再生性能研究

Fabrication of porous TiO₂/g-C₃N₄heterojunction and investigation on its photocatalytic performance of coenzyme regeneration

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