Synthesis of silica powder with high pore volume by skeleton reinforcement

doi:10.1016/j.cjche.2021.07.026

中国化学工程学报 ›› 2022, Vol. 42 ›› Issue (2): 219-226.DOI: 10.1016/j.cjche.2021.07.026

Synthesis of silica powder with high pore volume by skeleton reinforcement

Hongwei Shan¹, Xiaodong Zhou³, Hao Jiang², Yanjie Hu², Haibo Jiang², Chunzhong Li¹

1. Shanghai Engineering Research Center of Hierarchical Nanomaterials, Key Laboratory for Ultrafine Materials of Ministry of Education, School of Chemical Engineering, East China University of Science & Technology, Shanghai 200237, China;
2. School of Materials Science and Engineering, East China University of Science & Technology, Shanghai 200237, China;
3. State Key Laboratory of Chemical Engineering, School of Chemical Engineering, East China University of Science & Technology, Shanghai 200237, China

收稿日期:2020-05-13 修回日期:2021-06-07 出版日期:2022-02-28 发布日期:2022-03-30
通讯作者: Haibo Jiang,E-mail:jianghaibo@ecust.edu.cn;Chunzhong Li,E-mail:czli@ecust.edu.cn
基金资助:
This work was financially supported by the National Natural Science Foundation of China (21838003, 91834301, 21878092), the Shanghai Scientific and Technological Innovation Project (18JC₁410600), the Social Development Program of Shanghai (17DZ1200900, 18DZ2252400), and the Innovation Program of Shanghai Municipal Education Commission, and the Fundamental Research Funds for the Central Universities (222201718002).

Synthesis of silica powder with high pore volume by skeleton reinforcement

Hongwei Shan¹, Xiaodong Zhou³, Hao Jiang², Yanjie Hu², Haibo Jiang², Chunzhong Li¹

1. Shanghai Engineering Research Center of Hierarchical Nanomaterials, Key Laboratory for Ultrafine Materials of Ministry of Education, School of Chemical Engineering, East China University of Science & Technology, Shanghai 200237, China;
2. School of Materials Science and Engineering, East China University of Science & Technology, Shanghai 200237, China;
3. State Key Laboratory of Chemical Engineering, School of Chemical Engineering, East China University of Science & Technology, Shanghai 200237, China

Received:2020-05-13 Revised:2021-06-07 Online:2022-02-28 Published:2022-03-30
Contact: Haibo Jiang,E-mail:jianghaibo@ecust.edu.cn;Chunzhong Li,E-mail:czli@ecust.edu.cn
Supported by:
This work was financially supported by the National Natural Science Foundation of China (21838003, 91834301, 21878092), the Shanghai Scientific and Technological Innovation Project (18JC₁410600), the Social Development Program of Shanghai (17DZ1200900, 18DZ2252400), and the Innovation Program of Shanghai Municipal Education Commission, and the Fundamental Research Funds for the Central Universities (222201718002).

摘要/Abstract

摘要： In this paper, a method composed of gelation of basic skeleton (first step) and skeleton reinforcement process (second step) was introduced to synthesize silica powder with high pore volume through the reaction between water glass and sulfuric acid. No organic solvents were involved in the entire preparation process and the final product was collected by spray drying. The effect of concentration of base solution, gelation point pH value and skeleton reinforcement time on the BET specific surface area and pore volume of the prepared silica powder were investigated intensively. The results show that, a basic skeleton with good dispersibility and high porosity was obtained when the concentration of base solution was 0.1 mol·L^-1 and the gelation pH value reached 6.5. Then the basic skeleton grew into a more uniform porous structure after 30 min skeleton reinforcement. Under these optimum conditions, silica powder prepared by skeleton reinforcement method had a BET specific surface area of 358.0 m²·g^-1, and its pore volume reached 2.18 cm³·g^-1, which was much higher than that of prepared by skeleton-free method (1.62 cm³·g^-1) and by direct gelation method (0.31 cm³·g^-1).

关键词: Water glass, Silica powder, High pore volume, Skeleton reinforcement, Spray drying

Abstract: In this paper, a method composed of gelation of basic skeleton (first step) and skeleton reinforcement process (second step) was introduced to synthesize silica powder with high pore volume through the reaction between water glass and sulfuric acid. No organic solvents were involved in the entire preparation process and the final product was collected by spray drying. The effect of concentration of base solution, gelation point pH value and skeleton reinforcement time on the BET specific surface area and pore volume of the prepared silica powder were investigated intensively. The results show that, a basic skeleton with good dispersibility and high porosity was obtained when the concentration of base solution was 0.1 mol·L^-1 and the gelation pH value reached 6.5. Then the basic skeleton grew into a more uniform porous structure after 30 min skeleton reinforcement. Under these optimum conditions, silica powder prepared by skeleton reinforcement method had a BET specific surface area of 358.0 m²·g^-1, and its pore volume reached 2.18 cm³·g^-1, which was much higher than that of prepared by skeleton-free method (1.62 cm³·g^-1) and by direct gelation method (0.31 cm³·g^-1).

Key words: Water glass, Silica powder, High pore volume, Skeleton reinforcement, Spray drying

Hongwei Shan, Xiaodong Zhou, Hao Jiang, Yanjie Hu, Haibo Jiang, Chunzhong Li. Synthesis of silica powder with high pore volume by skeleton reinforcement[J]. 中国化学工程学报, 2022, 42(2): 219-226.

Hongwei Shan, Xiaodong Zhou, Hao Jiang, Yanjie Hu, Haibo Jiang, Chunzhong Li. Synthesis of silica powder with high pore volume by skeleton reinforcement[J]. Chinese Journal of Chemical Engineering, 2022, 42(2): 219-226.

参考文献

[1] J. Fricke, Aerogels-highly tenuous solids with fascinating properties, J. Non-Cryst. Solids 100(1-3) (1988) 169-173.
[2] S.K. Kang, S.Y. Choi, Synthesis of low-density silica gel at ambient pressure:Effect of heat treatment, J. Mater. Sci. 35(19) (2000) 4971-4976.
[3] B. Zhu, W. Wei, G. Ma, Y. Zhuang, J. Liu, L. Song, X. Hu, H. Wang, J. Li, A pressurized carbonation Sol-gel process for preparing large pore volume silica and its performance as a flatting agent and an adsorbent, J. Supercrit. Fluids 97(2015) 1-5.
[4] A.M. Rabea, M. Mohseni, S.M. Mirabedini, M.H. Tabatabaei, Surface analysis and anti-graffiti behavior of a weathered polyurethane-based coating embedded with hydrophobic nano silica, Appl. Surf. Sci. 258(10) (2012) 4391-4396.
[5] D.L. Manuale, E. Greco, A. Clementz, G.C. Torres, C.R. Vera, J.C. Yori, Biodiesel purification in one single stage using silica as adsorbent, Chem. Eng. J. 256(2014) 372-379.
[6] G. Hayase, K. Kugimiya, M. Ogawa, Y. Kodera, K. Kanamori, K. Nakanishi, The thermal conductivity of polymethylsilsesquioxane aerogels and xerogels with varied pore sizes for practical application as thermal superinsulators, J. Mater. Chem. A 2(18) (2014) 6525-6531.
[7] A. Sayari, Catalysis by crystalline mesoporous molecular sieves, Chem. Mater. 8(8) (1996) 1840-1852.
[8] I. Smirnova, S. Suttiruengwong, W. Arlt, Feasibility study of hydrophilic and hydrophobic silica aerogels as drug delivery systems, J. Non-Cryst. Solids 350(2004) 54-60.
[9] W. Stöber, A. Fink, E. Bohn, Controlled growth of monodisperse silica spheres in the micron size range, J. Colloid Interface Sci. 26(1) (1968) 62-69.
[10] A. Venkateswara Rao, S.D. Bhagat, Synthesis and physical properties of TEOSbased silica aerogels prepared by two step (acid-base) sol-gel process, Solid State Sci. 6(9) (2004) 945-952.
[11] D.B. Mahadik, A.V. Rao, R. Kumar, S.V. Ingale, P.B. Wagh, S.C. Gupta, Reduction of processing time by mechanical shaking of the ambient pressure dried TEOS based silica aerogel granules, J. Porous Mater. 19(1) (2012) 87-94.
[12] K. Yang, A.N. Maozhong, C. Yang, L. Zhang, W. Shao, Preparation and characterization of large-particle pure silica sol, J. Chin. Chem. Soc. 40(2012) 108-115.
[13] S.K. Estok, T.A. Hughes, M.K. Carroll, A.M. Anderson, Fabrication and characterization of TEOS-based silica aerogels prepared using rapid supercritical extraction, J. Sol-Gel Sci. Technol. 70(3) (2014) 371-377.
[14] Z. Li, X. Cheng, S. He, D. Huang, H. Bi, H. Yang, Preparation of ambient pressure dried MTMS/TEOS co-precursor silica aerogel by adjusting NH₄OH concentration, Mater. Lett. 129(2014) 12-15.
[15] A. Berggren, A.E.C. Palmqvist, K. Holmberg, Surfactant-templated mesostructured materials from inorganic silica, Soft Matter 1(3) (2005) 219- 226.
[16] H. Gao, J.L. Yang, Nanoscale silicon dioxide prepared by Sol-gel process, Mod. Appl. Sci. 4(9) (2010) 152.
[17] S. He, Y. Huang, G. Chen, M. Feng, H. Dai, B. Yuan, X. Chen, Effect of heat treatment on hydrophobic silica aerogel, J. Hazard. Mater. 362(2019) 294-302.
[18]
[18] R. Filipović, Z. Obrenović, I. Stijepović, L.M. Nikolić, V.V. Srdić, Synthesis of mesoporous silica particles with controlled pore structure, Ceram. Int. 35(8) (2009) 3347-3353.
[19] Y.J. Huang, S. He, M.M. Feng, H.M. Dai, Y.L. Pan, X.D. Cheng, Organic solventsaving preparation of water glass based aerogel granules under ambient pressure drying, J. Non-Cryst. Solids 521(2019) 119507.
[20] T. Zhang, Y. Wang, G. Luo, S. Bai, Effects of precipitation and drying processes on the synthesis of silica materials with a large-pore-volume and narrowpore-diameter distribution, Ind. Eng. Chem. Res. 55(12) (2016) 3579-3587.
[21] T. Błaszczyński, A. Ślosarczyk, M. Morawski, Synthesis of silica aerogel by supercritical drying method, Procedia Eng. 57(2013) 200-206.
[22] A. Venkateswara Rao, E. Nilsen, M.-A. Einarsrud, Effect of precursors, methylation agents and solvents on the physicochemical properties of silica aerogels prepared by atmospheric pressure drying method, J. Non-Cryst. Solids 296(3) (2001) 165-171.
[23] G.W. Liu, B. Zhou, A. Du, J. Shen, G.M. Wu, Greatly strengthened silica aerogels via co-gelation of binary sols with different concentrations:A method to control the microstructure of the colloids, Colloids Surf. A:Physicochem. Eng. Aspects 436(2013) 763-774.
[24] B.A. Fleming, Kinetics of reaction between silicic acid and amorphous silica surfaces in NaCl solutions, J. Colloid Interface Sci. 110(1) (1986) 40-64.
[25] R.K. Iler, The Chemistry of Silica-Solubility, Polymerization, Colloid and Surface Properties, and Biochemistry, John Wiley & Sons, Hoboken, 1979.
[26] J.J. Zhao, J. Shen, L.P. Zou, W.Q. Wang, G.Q. Zu, Z.H. Zhang, A low-cost preparation of SiO₂ aerogel monoliths from silica sol, J. Inorg. Mater. 30(2015) 1081-1084.
[27] M.S. Tsai, C.H. Yang, P.Y. Huang, Effects of seeds concentration on the formation of colloidal silica, Mater. Sci. Eng.:B 123(3) (2005) 238-241.
[28] A.E. Ahmed, F. Adam, Indium incorporated silica from rice husk and its catalytic activity, Microporous & Mesoporous Mater. 103(2007) 284-295.
[29] M. Thommes, B. Smarsly, M. Groenewolt, P.I. Ravikovitch, A.V. Neimark, Adsorption hysteresis of nitrogen and argon in pore networks and characterization of novel micro- and mesoporous silicas, Langmuir 22(2) (2006) 756-764.

Synthesis of silica powder with high pore volume by skeleton reinforcement

Synthesis of silica powder with high pore volume by skeleton reinforcement

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 1

编辑推荐

Metrics

本文评价