中空孔结构对W掺杂MFI分子筛丙酮吸附行为的研究

doi:10.11949/0438-1157.20211439

摘要/Abstract

摘要：

吸附容量高、吸附速率快以及憎水性强是分子筛用于挥发性有机物(VOCs)高效吸附的主要性能指标。分别以纯硅(S-1)和W掺杂(WS-1)MFI分子筛为母体，通过一步水热脱硅/补钨后处理制备了具有全空腔(HWS-1_S)和多孔芯(HWS-1_W)的两种中空结构分子筛，并以典型的VOCs气体分子丙酮为探针，系统研究了中空结构形态对于分子筛吸附性能的影响。结果表明：HWS-1_S表面部分开孔，内部全空腔且与外部连通，相比于母体S-1，相对结晶度较低，微孔孔容减少；HWS-1_W表面开孔细微，内部出现不规则的大/中孔结构，相比母体WS-1，相对结晶度提高，微孔孔容增大。干气条件下，HWS-1_S与HWS-1_W相比母体S-1和WS-1对丙酮具有更快的吸附速率；HWS-1_S微孔孔容损失严重，导致吸附容量有限(27.4 mg·g^-1)；HWS-1_W由于重结晶修复了部分结构缺陷，提高了丙酮吸附容量(51.2 mg·g^-1）。通过吸附动力学拟合，HWS-1_S和HWS-1_W符合典型的孔扩散机理，对丙酮主要以物理吸附为主。湿气条件下，W掺杂可有效中和中空分子筛表面硅醇基团，在一定程度上提高了W掺杂中空分子筛抗水汽竞争吸附能力。

关键词: VOCs, 丙酮, 吸附, W掺杂分子筛, 中空结构, 吸附动力学

Abstract:

Zeolite adsorbents for the adsorption and removal of volatile organic compounds (VOCs) have attracted considerable attention in recent years. However, the low adsorption capacity, slow adsorption rate, and hydrophilic nature strongly restrict the development of zeolite-type VOCs adsorbents. In this paper, tungsten-substituted MFI zeolites (HWS-1_S and HWS-1_W) with two kinds of hollow structures (fully and multichambered) are prepared by post-treating the siliceous MFI (S-1) and tungsten-substituted MFI (WS-1) through desilication and tungstation, respectively. And the effect of the hollow morphology on VOCs adsorption performance is investigated by using acetone as an adsorbate. The results show that HWS-1_S and HWS-1_W exhibit faster adsorption rates for acetone compared to the parent S-1 and WS-1 benefitted from their highly interconnected hollow structures. HWS-1_S shows a limited adsorption capacity (27.4 mg·g^-1) of acetone than S-1 due to its reduced micropore volume, while HWS-1_W presents an increased adsorption capacity (51.2 mg·g^-1) of acetone compared with WS-1, which could be ascribed to the defect removal by tungstation. Acetone dominatly performs as physical absorption on both HWS-1_S and HWS-1_W based on the fitting results of adsorption kinetics. Moreover, substitution of W atoms within zeolite frameworks can neutralize silanol groups and further enhance the hydrophobicity of zeolite adsorbents, leading an effective resistance of competitive adsorption of water.

Key words: VOCs, acetone, adsorption, tungsten-substituted zeolite, hollow structure, adsorption kinetics

中图分类号:

TQ 424.25

王旭, 张乐瑶, 张昊轩, 演嘉辉, 吴玉帅, 吴冬, 陈汇勇, 马晓迅. 中空孔结构对W掺杂MFI分子筛丙酮吸附行为的研究[J]. 化工学报, 2022, 73(3): 1194-1206.

Xu WANG, Leyao ZHANG, Haoxuan ZHANG, Jiahui YAN, Yushuai WU, Dong WU, Huiyong CHEN, Xiaoxun MA. Effect of hollow structure on the acetone adsorption property of tungsten-substituted MFI zeolite[J]. CIESC Journal, 2022, 73(3): 1194-1206.

图/表 12

图1 S-1、WS-1、HWS-1_S和HWS-1_W的XRD谱图

Fig.1 XRD patterns of S-1, WS-1, HWS-1_S, and HWS-1_W zeolites

表1 微孔和中空分子筛的金属含量、合成收率、相对结晶度及织构参数

Table 1 Metal （W） contents， synthesis yields， crystallinities and textual properties of various zeolite samples

样品	金属含量/ %(质量)	产率/%	相对结晶度/%	比表面积/(m²·g^-1)	外表面积/(m²·g^-1)	S_外表面积/S_比表面积	微孔孔容/(cm³·g^-1)	总孔容/(cm³·g^-1)	V_微孔孔容/V_总孔容
S-1	—	100	100	427	63	0.15	0.17	0.24	0.71
WS-1	0.01	100	100	352	68	0.19	0.10	0.23	0.43
HWS-1_S	0.09	70	78	253	51	0.20	0.08	0.29	0.28
HWS-1_W	0.13	75	106	385	91	0.24	0.12	0.34	0.35

图2 S-1、WS-1、HWS-1_S和HWS-1_W的SEM图片[(a)~(d)]和TEM图片[(e)~(f)]

Fig.2 SEM [(a)—(d)] and TEM [(e)—(f)] images of S-1, WS-1, HWS-1_S, and HWS-1_W zeolites

图3 S-1、WS-1、HWS-1_S和HWS-1_W的N2吸-脱附等温线（a）； BJH孔径分布（b）

Fig.3 N2 physisorption isotherms (a), and BJH pore size distribution (b) of S-1, WS-1, HWS-1_S and HWS-1_W zeolites

图4 S-1、WS-1、HWS-1_S和HWS-1_W的紫外-可见漫反射光谱谱图

Fig.4 UV-visible spectra of S-1, WS-1, HWS-1_S and HWS-1_W zeolites

图5 S-1、WS-1、HWS-1_S和HWS-1_W的紫外-拉曼谱图

Fig.5 UV-Raman spectra of S-1, WS-1, HWS-1_S and HWS-1_W zeolites

图6 母体及中空分子筛吸附干气丙酮的穿透曲线（a）；穿透吸附与饱和吸附的接近程度（b）

Fig.6 Breakthrough curves of acetone adsorption on parent and corresponding hollow zeolites (a), and differences between saturation capacities and breakthrough capacities on parent and corresponding hollow zeolite adsorbents (b)

表2 Yoon-Nelson模型拟合吸附穿透曲线

Table 2 Fitting of breakthrough curves by using Yoon-Nelson model

样品	Yoon-Nelson模型拟合值			实验值
样品	$τ$ /min^①	$k'$ ^②/min^-1	R²	$τ$ /min
S-1	218	0.024	0.995	216
HWS-1_S	106	0.076	0.996	102
WS-1	140	0.036	0.998	141
HWS-1_W*^③	163	0.092	0.999	162
HWS-1_W	196	0.085	0.998	197

表2 Yoon-Nelson模型拟合吸附穿透曲线

Table 2 Fitting of breakthrough curves by using Yoon-Nelson model

样品	Yoon-Nelson模型拟合值			实验值
样品	$τ$ /min^①	$k'$ ^②/min^-1	R²	$τ$ /min
S-1	218	0.024	0.995	216
HWS-1_S	106	0.076	0.996	102
WS-1	140	0.036	0.998	141
HWS-1_W*^③	163	0.092	0.999	162
HWS-1_W	196	0.085	0.998	197

表3 微孔和中空分子筛的动力学模型拟合参数

Table 3 Fitting parameters of acetone adsorption kinetics of parent and corresponding hollow zeolite adsorbents

理论模型	参数	S-1	WS-1	HWS-1_S	HWS-1_W
准一级模型	k₁/min^-1	0.006	0.008	0.01	0.003
	q_e/(mg·g^-1)	64.73	45.64	34.91	110.99
	R²	0.983	0.991	0.988	0.992
准二级模型	k₂/min^-1	5.79×10^-5	7.91×10^-5	1.28×10^-4	7.75×10^-6
	q_e/(mg·g^-1)	87.22	68.93	53.63	198.83
	R²	0.968	0.987	0.985	0.992
班厄姆模型	k₃/min^-^z	9.80×10^-4	1.95×10^-3	2.20×10^-3	1.14×10^-3
	q_e/(mg·g^-1)	59.77	38.33	28.26	62.25
	z	1.388	1.371	1.445	1.346
	R²	0.999	0.999	0.998	0.997
表观扩散系数	(D/r₀²) $×$ 10^-4/s^-1	5.10	8.63	12.9	7.56
表观扩散系数	R²	0.993	0.995	0.996	0.988

表3 微孔和中空分子筛的动力学模型拟合参数

Table 3 Fitting parameters of acetone adsorption kinetics of parent and corresponding hollow zeolite adsorbents

理论模型	参数	S-1	WS-1	HWS-1_S	HWS-1_W
准一级模型	k₁/min^-1	0.006	0.008	0.01	0.003
	q_e/(mg·g^-1)	64.73	45.64	34.91	110.99
	R²	0.983	0.991	0.988	0.992
准二级模型	k₂/min^-1	5.79×10^-5	7.91×10^-5	1.28×10^-4	7.75×10^-6
	q_e/(mg·g^-1)	87.22	68.93	53.63	198.83
	R²	0.968	0.987	0.985	0.992
班厄姆模型	k₃/min^-^z	9.80×10^-4	1.95×10^-3	2.20×10^-3	1.14×10^-3
	q_e/(mg·g^-1)	59.77	38.33	28.26	62.25
	z	1.388	1.371	1.445	1.346
	R²	0.999	0.999	0.998	0.997
表观扩散系数	(D/r₀²) $×$ 10^-4/s^-1	5.10	8.63	12.9	7.56
表观扩散系数	R²	0.993	0.995	0.996	0.988

图7 S-1（a）、WS-1（b）、HWS-1_S（c）和HWS-1_W（d）上丙酮吸附动力学拟合

Fig.7 Fitting of acetone adsorption kinetics on S-1 (a), WS-1 (b), HWS-1_S (c), and HWS-1_W (d) zeolite adsorbents

图8 微孔和中空分子筛吸附丙酮过程的Weber-Morris模型拟合（a）和表观扩散系数线性拟合（b）

Fig.8 W-M model curves (a) and fitting of apparent diffusion coefficients (b) of parent and hollow zeolites adsorbents

表4 干气和10%湿度条件下W掺杂中空分子筛丙酮吸附性能

Table 4 Acetone adsorption breakthrough times and saturation adsorption capacities of parent and corresponding hollow zeolite adsorbents at RH = 0 and RH = 10%

样品	穿透时间 $t$ /min^①		饱和吸附量 $Q e$ /(mg·g^-1)		(Q_wet/Q_dry)/%
样品	RH=0	RH=10%	RH=0	RH=10%	(Q_wet/Q_dry)/%
S-1	120	96	59.2	49.7	83.9
HWS-1_S	48	36	27.4	21.5	78.5
WS-1	80	60	36.8	32.1	87.2
HWS-1_W*^②	135	100	42.3	36.4	86.0
HWS-1_W	160	120	51.2	40.4	78.9
HWS-1_W_R^③	156	110	50.1	38.8	77.4

表4 干气和10%湿度条件下W掺杂中空分子筛丙酮吸附性能

Table 4 Acetone adsorption breakthrough times and saturation adsorption capacities of parent and corresponding hollow zeolite adsorbents at RH = 0 and RH = 10%

样品	穿透时间 $t$ /min^①		饱和吸附量 $Q e$ /(mg·g^-1)		(Q_wet/Q_dry)/%
样品	RH=0	RH=10%	RH=0	RH=10%	(Q_wet/Q_dry)/%
S-1	120	96	59.2	49.7	83.9
HWS-1_S	48	36	27.4	21.5	78.5
WS-1	80	60	36.8	32.1	87.2
HWS-1_W*^②	135	100	42.3	36.4	86.0
HWS-1_W	160	120	51.2	40.4	78.9
HWS-1_W_R^③	156	110	50.1	38.8	77.4

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