Ni2+取代对ZnTi-LDH选择性光氧化去除NO的性能增强

doi:10.11949/0438-1157.20220912

摘要/Abstract

摘要：

以NiCl₂·6H₂O为镍源，采用水热法首次合成了不同Ni²⁺取代量的锌钛层状双金属氢氧化物(NiZnTi-LDH)，通过X射线衍射、透射电镜、低温氮吸附、X射线光电子能谱与紫外-可见漫反射等测试研究了Ni²⁺取代对ZnTi-LDH晶相结构、微观形貌、孔结构、表面氧空位与光吸收性能的影响。以NiZnTi-LDH为催化剂，分别考察了模拟太阳光与可见光照射下的NO光氧化消除性能。结果表明：Ni²⁺部分取代Zn²⁺可在ZnTi-LDH的能带结构中形成一新的中间能级，产生可见光响应，同时Ni取代可于ZnTi-LDH表面形成氧空位(O_V)。可见光照射下，ZnTi-LDH无NO氧化活性，最优催化剂27% NiZnTi-LDH的NO去除率为52.1%，NO _x 脱除选择性高达97.4%。模拟太阳光照射下，27% NiZnTi-LDH的NO光氧化去除率为64.8%，是ZnTi-LDH的2.76倍，NO _x 脱除选择性可达96.9%，且NO $3 -$ 生成量占总硝酸盐的95.6%。Ni²⁺取代及由此形成的O_V不仅促进光生电荷分离，同时利于超氧自由基(·O $2 -$ )的生成，在增强NO消除性能的同时，抑制有毒NO₂的产生，实现NO至NO $3 -$ 的深度光氧化。

关键词: 锌钛LDH, 镍取代, 深度光氧化, 一氧化氮, 氧空位, 性能增强

Abstract:

Ni-substituted Zn-Ti layered double hydroxide (NiZnTi-LDH) with different Ni²⁺ substitution ratios were firstly synthesized by using NiCl₂·6H₂O as nickel source via hydrothermal method. The effects of Ni²⁺ substitution on the crystal phase, morphology, pore structure, surface oxygen vacancy and light absorption properties of ZnTi-LDH were investigated by X-ray diffraction, transmission electron microscopy, low temperature nitrogen adsorption, X-ray photoelectron spectroscopy and UV-visible diffuse reflectance. Using NiZnTi-LDH as catalyst, the photo-oxidation and elimination performance of NO under simulated sunlight and visible light irradiation were investigated respectively. The results showed that partial Ni²⁺ substitution for Zn²⁺ formed a new intermediate energy level in the band structure of ZnTi-LDH that consequently produced visible light response, meanwhile Ni²⁺ substitution generated oxygen vacancies (O_V) on ZnTi-LDH surface. Under visible light irradiation, ZnTi-LDH had no NO oxidation activity, and the optimal 27% NiZnTi-LDH catalyst showed a NO removal rate of 52.1% with a De-NO _x selectivity up to 97.4%. Under simulated solar light irradiation, 27% NiZnTi-LDH exhibited a NO photo-oxidation removal rate of 64.8% that was 2.76 times of ZnTi-LDH and De-NO _x selectivity was 96.9%, meanwhile the produced NO $3 -$ accounted for 95.6% of total nitrate. Ni²⁺ substitution and the resulting O_V not only promoted the separation of photogenerated carriers, but also facilitated the generation of superoxide radical (·O $2 -$ ). As a result, the photo-oxidative activity of NO removal was enhanced and the production of toxic NO₂ was effectively inhibited, consequently achieving deep photo-oxidation of NO to NO $3 -$ .

Key words: ZnTi-LDH, Ni²⁺-substitution, deep photo-oxidation, NO, oxygen vacancy, performance enhancement

中图分类号:

O 643.36

杜智华, 杨娟, 戴俊, 冷冲冲, 张鸽. Ni²⁺取代对ZnTi-LDH选择性光氧化去除NO的性能增强[J]. 化工学报, 2022, 73(11): 4998-5010.

Zhihua DU, Juan YANG, Jun DAI, Chongchong LENG, Ge ZHANG. Performance enhancement of selective photo-oxidation for NO removal on ZnTi-LDH by Ni²⁺ substitution[J]. CIESC Journal, 2022, 73(11): 4998-5010.

图/表 14

图1 NiZnTi-LDH样品的XRD和FT-IR谱图

Fig.1 XRD patterns and FT-IR spectra of NiZnTi-LDH samples

图2 ZnTi-LDH和27% NiZnTi-LDH样品的SEM、TEM与HRTEM照片

Fig.2 SEM, TEM and HRTEM images of ZnTi-LDH and 27% NiZnTi-LDH samples

图3 NiZnTi-LDH样品的N2吸附-脱附等温线和相应的BJH孔径分布

Fig.3 N2 adsorption-desorption isotherms and the corresponding BJH pore size distribution of NiZnTi-LDH samples

图4 ZnTi-LDH和27% NiZnTi-LDH的XPS谱图

Fig.4 XPS spectra of ZnTi-LDH and 27% NiZnTi-LDH

图5 NiZnTi-LDH样品的室温EPR谱

Fig.5 Room temperature EPR spectra of NiZnTi-LDH samples

图6 NiZnTi-LDH样品的UV-Vis DRS光谱，ZnTi-LDH与27% NiZnTi-LDH样品的(αhν)2对hν曲线及其XPS价带谱

Fig.6 UV-Vis DRS spectra of NiZnTi-LDH samples, (αhν)2vshν curves and valence band XPS spectra of ZnTi-LDH and 27% NiZnTi-LDH sample

图7 ZnTi-LDH与27% NiZnTi-LDH的态密度(DOS)

Fig.7 Density of states (DOS) for ZnTi-LDH and 27% NiZnTi-LDH

表1 Ni2+与二价金属（Ni2++Zn2+）的实测摩尔比，NiZnTi-LDH样品的BET比表面积、孔体积，及比表面积归一化的NO去除率（NOrem/SBET）

Table 1 Actual molar ratios of Ni2+ to divalent metal （Ni2++Zn2+）， BET surface area， pore volume of NiZnTi-LDH samples and NO removal normalized by specific surface area （NOrem/SBET）

Sample	Ni/(Ni + Zn)^①	比表面积/(m²/g)	孔体积/(cm³/g)	NO_rem/S_BET^②
ZnTi-LDH	0	103	0.311	0.228
9% NiZnTi-LDH	8.90%	116	0.283	0.338
18% NiZnTi -LDH	17.86%	131	0.302	0.404
27% NiZnTi -LDH	26.81%	146	0.330	0.445
40% NiZnTi -LDH	39.73%	156	0.368	0.371

图8 模拟太阳光与可见光照射下不同光催化剂的NO去除率和有毒NO2的生成

Fig.8 NO removal percentage and toxic NO2 generation on different photocatalysts under simulated solar light and visible light irradiation respectively

图9 27% NiZnTi-LDH与ZnTi-LDH光氧化去除NO的NO3-与NO2-产生量(插图为催化剂淋洗液的离子色谱图)

Fig. 9 Production amount of NO2- and NO3- during photo-oxidation NO removal over 27% NiZnTi-LDH and ZnTi-LDH respectively (inset is ion chromatography spectra of catalyst eluent)

图10 27% NiZnTi-LDH光氧化消除NO的循环稳定性和6次循环实验后催化剂的XRD谱图与红外光谱

Fig.10 Cycling stability of 27% NiZnTi-LDH for photo-oxidative removal of NO, XRD and IR spectra of the catalyst after 6 cycles

图11 光催化去除NO的自由基捕获实验；ZnTi-LDH、27% NiZnTi-LDH和40% NiZnTi-LDH悬浮液DMPO/∙O2-的EPR谱、瞬态光电流响应谱和DMPO/∙OH的EPR谱

Fig.11 Radical trapping experiments of photocatalytic removal of NO; EPR spectra of DMPO/∙O2-, transient photocurrent response and EPR spectra of DMPO/∙OH of ZnTi-LDH, 27% NiZnTi-LDH and 40% NiZnTi-LDH

表2 光催化去除NO各种催化剂的性能比较

Table 2 Comparison of photocatalytic NO removal performance over various catalysts

Sample	Catalyst amount/g	Light source	NO removal rate/%	NO _x removal selectivity/%	Ref.
SrTiO₃/SrCO₃	0.05	300W Xe lamp (290—780 nm)	47	86.17	[43]
TiO₂/HAp	0.1	300W Xe lamp (290—780 nm)	44.6	92.0	[44]
ZnAlFe-LDHs	0.05	Xe lamp (≥510 nm)	13	92	[7]
Bi₂O₃/CuBi₂O₄	0.1	300W Xe lamp (≥420 nm)	30	93.3	[8]
Ni/Mg₂Al-LDH	0.4	8W UV lamp	42	87	[11]
Ag/ZnTi-LDH	0.1	Xe lamp (290—780 nm)	43	92	[10]
Pt-TiO₂	0.05	500W tungsten lamp (≥420 nm)	25.9	66	[9]
amorphous carbon nitride	0.1	150W tungsten lamp (≥420 nm)	57.1	86.3	[45]
Bi₂O₂CO₃/Bi₄O₅Br₂	0.1	300W Xe lamp (290—780 nm)	53.2	89.3	[46]
27% NiZnTi-LDH	0.1	Xe lamp (420—780 nm)	52.1	97.4	this work
27% NiZnTi-LDH		Xe lamp (290—780 nm)	64.8	96.9

图12 NiZnTi-LDH光氧化去除NO性能增强机理示意图

Fig. 12 Performance enhancing mechanism diagram of photo-oxidative NO removal over NiZnTi-LDH

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Ni²⁺取代对ZnTi-LDH选择性光氧化去除NO的性能增强

Performance enhancement of selective photo-oxidation for NO removal on ZnTi-LDH by Ni²⁺ substitution

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