有机-无机氧化硅空心球的合成及VOCs吸附应用

doi:10.15541/jim20210638

无机材料学报 ›› 2022, Vol. 37 ›› Issue (9): 991-1000.DOI: 10.15541/jim20210638 CSTR: 32189.14.10.15541/jim20210638

有机-无机氧化硅空心球的合成及VOCs吸附应用

王红宁¹(), 黄丽¹, 清江³, 马腾洲³(), 黄维秋², 陈若愚¹()

1.常州大学精细石油化工江苏省重点实验室, 常州 213164
2.常州大学江苏省油气储运技术重点实验室, 常州 213016
3.上海海关工业品与原材料检测技术中心, 上海 200135

收稿日期:2021-10-18 修回日期:2022-02-18 出版日期:2022-09-20 网络出版日期:2022-03-15
通讯作者: 陈若愚, 教授. E-mail: chry@cczu.edu.cn;
马腾洲, 研究员. E-mail: 13564737997@163.com
作者简介:王红宁(1980-), 女, 博士研究生. E-mail: 444873772@qq.com
基金资助:
国家自然科学基金面上项目(52174058);海关总署课题(2020HK251)

Mesoporous Organic-inorganic Hybrid Siliceous Hollow Spheres: Synthesis and VOCs Adsorption

WANG Hongning¹(), HUANG Li¹, QING Jiang³, MA Tengzhou³(), HUANG Weiqiu², CHEN Ruoyu¹()

1. Jiangsu Province Key Laboratory of Fine Petrochemical Engineering, Changzhou University, Changzhou 213164, China
2. Jiangsu Key Laboratory of Oil and Gas Storage and Transport Technology, Changzhou University, Changzhou 213016, China
3. Technical Center for Industrial Product and Raw Material Inspection and Testing, Shanghai Customs, Shanghai 200135, China

Received:2021-10-18 Revised:2022-02-18 Published:2022-09-20 Online:2022-03-15
Contact: CHEN Ruoyu, professor. E-mail: chry@cczu.edu.cn;
MA Tengzhou, professor. E-mail: 13564737997@163.com
About author:WANG Hongning (1980-), female, PhD candidate. E-mail: 444873772@qq.com
Supported by:
National Natural Science Foundations of China(52174058);Programme of General Administration of Customs China.(2020HK251)

摘要/Abstract

摘要：

介孔有机-无机复合氧化硅空心球(MOSs)在碱性条件下以反向胶束为模板经过正硅酸乙酯(TEOS)和1,2-双(三乙氧基甲硅烷基)乙烷(BTSE)共缩合被成功合成, 并通过不同手段对样品的结构和性能进行表征。MOSs用于去除挥发性有机物(VOCs), 研究其对水蒸气、正己烷、甲苯和92#汽油的静态吸附性能, 并以商业硅胶(SG)和活性炭(AC)为参考。实验结果发现, 初始BTSE/(BTSE+TEOS) 摩尔比为10%时, (MOS-10%)的样品具有均匀的中空介观结构和最大的VOCs吸附容量(1.28 g·g^-1正己烷, 1.25 g·g^-1甲苯和1.14 g·g^-192#汽油), 静态水蒸气吸附量最小(0.630 g·g^-1)。通过穿透曲线评估单一组分VOC(正己烷或甲苯)在MOS-10%上的动态吸附行为, 动态正己烷和甲苯吸附结果以及高湿度条件下的正己烷吸附性能表明, 与商业吸附剂相比, MOS-10%具有最佳的穿透时间、吸附能力和疏水性。对于二元组分同时吸附(正己烷和甲苯), MOS-10%的正己烷吸附性能优于甲苯。介孔有机-无机复合氧化硅空心球的动态VOCs吸附容量较大归因于有机基团、表面积和孔体积的共同作用。MOSs的VOCs去除能力强和可回收性优良, 显示出巨大的VOCs捕获潜力。

关键词: 介孔有机-无机氧化硅空心球, VOCs吸附, 稳定性, 解吸

Abstract:

Mesoporous organic-inorganic hybrid siliceous hollow spheres (MOSs) were successfully synthesized by co-condensation of tetraethylorthosilicate (TEOS) and 1, 2-bis(triethoxysilyl)ethane (BTSE) with reverse micelle as template under basic condition. Structure and property of the prepared samples were characterized by different methods. The MOSs was used for VOCs removal with commercial silica gel (SG) and activated carbon (AC) as references. It is found that the sample with initial BTSE/(BTSE+TEOS) molar ratio of 10% (MOS-10%) displays uniform hollow mesostructure with the highest static VOCs adsorption capacities (1.28 g·g^-1 n-hexane, 1.25 g·g^-1 toluene and 1.14 g·g^-1 92# gasoline), and the lowest water vapor adsorption capacity of 0.630 g·g^-1. Dynamic single component (n-hexane, toluene adsorption under dry condition or n-hexane adsorption under high humidity condition, 95% RH) adsorption results show that MOS-10% has the best breakthrough times, adsorption capacities, and hydrophobicity. For binary component (n-hexane and toluene) adsorption, MOS-10% preferred to adsorb n-hexane rather than adsorb toluene. The higher dynamic VOCs capacity of MOS is attributed to the cooperation of the introduced organic groups, surface area and pore volume. The MOSs with high VOCs removal capacity and excellent recyclability show great potential for VOCs adsorption.

Key words: mesoporous organic-inorganic hybrid siliceous hollow sphere, VOCs adsorption, stability, desorption

中图分类号:

O613

王红宁, 黄丽, 清江, 马腾洲, 黄维秋, 陈若愚. 有机-无机氧化硅空心球的合成及VOCs吸附应用[J]. 无机材料学报, 2022, 37(9): 991-1000.

WANG Hongning, HUANG Li, QING Jiang, MA Tengzhou, HUANG Weiqiu, CHEN Ruoyu. Mesoporous Organic-inorganic Hybrid Siliceous Hollow Spheres: Synthesis and VOCs Adsorption[J]. Journal of Inorganic Materials, 2022, 37(9): 991-1000.

图/表 25

图1 不同有机硅源量MOSs的TEM照片

Fig. 1 TEM images of MOSs with different initial BTSE/ (BTSE+TEOS) molar ratios (a) MOS-0; (b) MOS-5%; (c) MOS-7.5%; (d) MOS-10%; (e) MOS-12.5%; (f) MOS-15%

图2 不同样品的N2吸附脱附等温线(a)和孔径分布图(b)

Fig. 2 N2 sorption isotherms (a) and pore size distributions (b) of MOSs with different initial BTSE/(BTSE+TEOS) molar ratios (A) MOS-0; (B) MOS-5%; (C) MOS-7.5%; (D) MOS-10%; (E)MOS-12.5%; (F) MOS-15%. In (a), the Y-axis values of (B-F) are 300, 600, 800, 1000, and 1300 m2·g-1, respectively. In (b), the Y-axis values of (B-F) are 0.1, 0.4, 0.8, 1.0, 1.2, and 1.4 cm3·g-1, respectively

表1 不同有机硅源量MOSs样品的结构参数

Table 1 Structural parameters of MOSs with different initial BTSE/(BTSE+TEOS) molar ratios

Sample	S_BET/ (m²·g^-1)	V_t/ (cm³·g^-1)	Pore size/ nm
MOS-0	591	0.721	2.5
MOS-5%	612	0.722	2.7
MOS-7.5%	612	0.776	2.8
MOS-10%	696	0.887	2.6
MOS-12.5%	655	0.873	2.7
MOS-15%	648	0.857	2.7

图3 不同有机硅源量MOSs的红外光谱图

Fig. 3 FT-IR spectra of MOSs with different initial BTSE/ (BTSE+TEOS) molar ratios (A) MOS-0; (B) MOS-5%; (C) MOS-7.5%; (D) MOS-10%; (E) MOS- 12.5%; (F) MOS-15%; (G) CTAB

图4 不同有机硅源量MOSs的XRD图谱

Fig. 4 XRD patterns of MOSs with different initial BTSE/ (BTSE+TEOS) molar ratios (A) MOS-0; (B) MOS-5%; (C) MOS-7.5%; (D) MOS-10%; (E) MOS- 12.5%; (F) MOS-15%

图5 不同有机硅源量MOSs的热重曲线

Fig. 5 TGA curves of MOSs with different initial BTSE/ (BTSE+TEOS) molar ratios (A) MOS-0; (B) MOS-5%; (C) MOS-7.5%; (D) MOS-10%; (E) MOS- 12.5%; (F) MOS-15%;

图6 不同样品对正己烷、甲苯和汽油的静态吸附容量(a, c, e)和解吸效率(b, d, f)

Fig. 6 Histograms of static VOCs (n-hexane, toluene and 92# gasoline) adsorption capacities (a, c, e) and desorption efficiencies (b, d, f) of different samples (A) MOS-0; (B) MOS-5%; (C) MOS-7.5%; (D) MOS-10%; (E) MOS-12.5%; (F) MOS-15%; (G) SG; (H) AC

图6 不同样品对正己烷、甲苯和汽油的静态吸附容量(a, c, e)和解吸效率(b, d, f)

图8 SG(■), AC(●)和MOS-10%(▲)的正己烷穿透曲线(第一次(a), 第五次(b)), 五次的平衡吸附容量的比较(c)和五次解吸效率的比较(d)

Fig. 8 Breakthrough curves for n-hexane of SG (■), AC (●) and MOS-10% (▲) under dry condition for the (a) first time and (b) fifth time and comparison of the qe (c) and desorption efficiency (d) of 5 times

图9 干燥条件下MOS-10%的甲苯动态吸附穿透曲线

Fig. 9 Toluene breakthrough curves on MOS-10% under dry condition

图10 MOS-10%五次干燥条件下正己烷(a)和甲苯(b)动态吸附的Yoon and Nelson模拟

Fig. 10 Yoon and Nelson model fitting for 5 times adsorption of n-hexane (a) and toluene (b) on MOS-10% under dry condition Colorful figures are available on website

图11 在RH 95%的条件下MOS-10%正己烷动态吸附的穿透曲线

Fig. 11 n-hexane breakthrough curves on MOS-10% under 95% RH

图12 干燥条件下MOS-10%上正己烷与甲苯五次动态同时吸附的穿透曲线正己烷(a)和甲苯(b), 以及五次平衡吸附容量的比较(c)和五次解吸效率的比较(d)

Fig. 12 Simultaneous breakthrough adsorption n-hexane (a) and toluene (b) on MOS-10% under dry condition, comparison of the equilibrium adsorption capacities (c) and desorption efficiency (d) for 5 times, respectively

表S1 商业化AC、SG的结构参数

Table S1 Structural parameters of AC and SG

Sample	S_BET/(m²·g^-1)	S_m/(m²·g^-1)	V_t/(cm³·g^-1)	V_m/(cm³·g^-1)	Pore size/nm
AC	1451	973	1.03	0.48	5.6
SG	430	15	0.710	0.010	6.9

表S2 不同有机硅源量MOSs在30~900 ℃, 氮气气氛(10 ℃/min)下获得的热重结果

Table S2 TGA results of different MOSs under nitrogen atmosphere in the range of 30-900 ℃ (10 ℃/min)

Sample	First event		Second event		Residual mass /%
Sample	(Tons-T_f )/℃	Δm/%	（Tons-T_f )/℃	Δm/%
MOS-0	30-200	1.7	200-900	8.1	90.2
MOS-5%	30-200	1.7	200-900	7.6	90.7
MOS-7.5%	30-200	1.9	200-900	12.6	85.5
MOS-10%	30-200	5.3	200-900	20.1	74.6
MOS-12.5%	30-200	1.5	200-900	7.9	90.6
MOS-15%	30-200	1.4	200-900	9.0	89.6

表S3 不同样品的水蒸气吸附容量、解吸百分率和表面羟基含量

Table S3 Water vapor adsorption capacities, desorption efficiencies and the densities of surface hydroxyl groups of different samples

Sample	Adsorption		Desorption		-OH/(×10²⁰, g^-1)
Sample	Average/(g·g^-1)	STDE^a/%	Average/%	STDE^a/%	-OH/(×10²⁰, g^-1)
MOS-0%	0.903	0.0168	99.4	0.205	3.11
MOS-5%	0.667	0.0177	99.3	0.329	2.35
MOS-7.5%	0.656	0.0165	99.4	0.283	2.31
MOS-10%	0.630	0.0137	99.4	0.134	2.23
MOS-12.5%	0.697	0.0156	99.4	0.230	2.44
MOS-15%	0.697	0.0136	99.4	0.365	2.45
SG	0.433	0.0984	97.7	0.867	1.72
AC	0.482	0.0305	93.5	11.1	1.77

表S4 干燥条件下, 不同样品对正己烷吸附的五次动态吸附参数比较

Table S4 Comparison of dynamic n-hexane adsorption parameters on different samples for 5 times under dry condition

Sample	t_b/min	t_e/min	q_e/(g·g^-1)	Desorption efficiency/%
MOS-10%-1st	50	104	1.23	99.8
MOS-10%-2nd	48	102	1.20	99.5
MOS-10%-3rd	46	100	1.19	99.4
MOS-10%-4th	48	102	1.22	99.6
MOS-10%-5th	48	102	1.21	99.2
SG-1st	16	72	0.361	98.9
SG-2nd	14	70	0.321	97.5
SG-3rd	14	70	0.334	98.7
SG-4th	12	72	0.321	98.6
SG-5th	10	72	0.343	97.6
AC-1st	38	50	0.574	73.7
AC-2nd	28	44	0.465	83.6
AC-3rd	28	42	0.461	90.9
AC-4th	26	44	0.452	98.6
AC-5th	24	42	0.458	97.2

表S5 干燥条件下, MOS-10%的五次甲苯动态吸附参数比较

Table S5 Comparison of dynamic toluene adsorption parameters on MOS-10% for 5 times under dry condition

	t_b/min	t_e/min	q_e/(g·g^-1)	Desorption efficiency/%
1st	48	100	1.21	99.7
2nd	46	98	1.18	99.5
3rd	44	96	1.17	99.3
4th	46	98	1.18	99.4
5th	46	98	1.18	99.1

表S6 在干燥条件下MOS-10%和AC吸附前和五次动态吸附正己烷后的孔结构参数

Table S6 Structural parameters of MOS-10% and AC before and after 5 times dynamic n-hexane adsorption under dry condition

Sample	S_BET/(m²·g^-1)	S_m/(m²·g^-1)	V_t/(cm³·g^-1)	V_m/(cm³·g^-1)	Pore size/nm
MOS-10%	696	0	0.887	0	2.64
MOS-10%-5th	638	0	0.830	0	2.64
AC	1654	652	1.06	0.48	5.58
AC-5th	1310	395	0.880	0.38	5.51

表S7 MOS-10%s在干燥条件下, 五次单组份正己烷和甲苯动态吸附的拟合参数

Table S7 Simulation parameters of 5 times dynamic n-hexane and toluene adsorption on MOS-10% under dry condition

	n-hexane			Toluene
	τ₀/min	K׳/min^-1	R²	τ₀/min	K׳/min^-1	R²
1st	63.1	0.150	0.984	58.4	0.0948	0.979
2nd	61.3	0.172	0.990	52.8	0.105	0.977
3rd	56.7	0.174	0.979	51.5	0.114	0.987
4th	57.1	0.169	0.986	54.1	0.111	0.978
5th	58.9	0.165	0.984	54.2	0.110	0.982

表S8 在RH 95%的条件下MOS-10%五次正己烷动态吸附参数

Table S8 Dynamic n-hexane adsorption parameters on MOS-10% for 5 times under 95% RH

	t_b/min	t_e/min	q_e,hexane /g·g^-1	q_e,t /g·g^{-1 adsorbent}	q_e,_water/g·g^{-1 adsorbent}	q_e,hexane/ q_e,_water	Desorption efficiency /%
1st	46	100	1.23	1.23	0.006	205	99.6
2nd	44	98	1.20	1.20	0.003	400	99.7
3rd	42	96	1.19	1.19	0.006	199	99.6
4th	42	96	1.21	1.21	0.003	404	99.4
5th	44	98	1.17	1.20	0.008	147	99.2

表S9 干燥条件下MOS-10%样品正己烷-甲苯五次动态同时吸附参数

Table S9 Comparison of simultaneous adsorption n-hexane and toluene parameters on MOS-10% for 5 times under dry condition

	Dynamic adsorption capacity, q_e /(g·g^-1)
	Single component		Bi-component
	n-hexane	Toluene	n-hexane	Toluene	Total VOCs
1st	1.23	1.21	0.642	0.569	1.21
2nd	1.20	1.18	0.631	0.547	1.18
3rd	1.19	1.17	0.613	0.532	1.15
4th	1.22	1.18	0.607	0.550	1.16
5th	1.21	1.18	0.628	0.547	1.18

图S1 AC和SG的N2吸附脱附等温线(a)和孔径分布图(b)

Fig. S1 N2 adsorption-desorption isotherms (a) and pore size distributions (b) of AC and SG

图S2 不同样品的正己烷、甲苯、汽油静态吸附容量与其结构参数的关系图

Fig. S2 Relationship between VOCs adsorption capacities and structure parameters of different samples (A) MOS-0; (B) MOS-5%; (C) MOS-7.5%; (D) MOS-10%; (E) MOS- 12.5%; (F) MOS-15%; (G) SG; (H) AC

图S3 MOS-10%和AC以及五次动态吸附正己烷后MOS-10%和AC的N2吸附-解吸等温线(a)和孔径分布图(b)

Fig. S3 N2 adsorption-desorption isotherms (a) and pore size distributions (b) of MOS-10% and AC, respectively

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有机-无机氧化硅空心球的合成及VOCs吸附应用

Mesoporous Organic-inorganic Hybrid Siliceous Hollow Spheres: Synthesis and VOCs Adsorption

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