A new process of acidic hydrolysis of residual chlorosilane liquid for the preparation of silica and hydrochloric acid

Jixiang Cai; Bing Huang; Qikun Ma; Wenwen Zhang

Korean Journal of Chemical Engineering, Vol.34, No.6, 1793-1800, June, 2017

DOI10.1007/s11814-017-0093-2 Export Citation

A new process of acidic hydrolysis of residual chlorosilane liquid for the preparation of silica and hydrochloric acid

Jixiang Cai, Bing Huang^†, Qikun Ma¹, and Wenwen Zhang

The Faculty of Environmental Science and Engineering, Kunming University of Science and Technology, Kunming, Yunnan, China
¹**Kunming Metallurgical Institute New Materials Co., Ltd., Kunming, Yunnan, China

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We propose a novel process for the preparation of silica and concentrated hydrochloric acid using chlorosilane residual liquid originating from the polysilicon production process. The process was designed and optimized after conducting pilot plant tests. The effects of circulating acid concentration, flow rate, chlorosilane residual liquid treatment load and other factors on silica products were studied. The results showed that the circulating acid flowrate can effectively control the formation of gel, and the amount of chlorosilane residual liquid has significant influence on the hydrolysis efficiency and operation of the hydrolysis tower. The prepared silica was characterized using XRD, XRF, FTIR, SEM, DLS, TG-MS and N2 adsorption/desorption experiments. The results indicated that silica consisted of amorphous particles, which were spherical, had surface hydroxyl, and showed heterogeneous distribution. The average particle size was 50-80 μm and had high specific surface area (565.049m2g-1), large pore volume (0.449 cm3g-1), and a narrow pore size distribution (3.419 nm). The new technology provides a simple, efficient and environmentally friendly way for treating chlorosilane residual liquid, as well as a cost-effective method for the preparation of silica.

Keywords:Chlorosilane Residual Liquid;Silica;Hydrochloric Acid;Acidic Hydrolysis Process;Polysilicon

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[2] Yu WW, Falkner JC, Shih BS, Colvin VL, Chem. Mater., 16, 3318 (2004)

[3] Su M, Korean J. Chem. Eng., 34(2), 484 (2017)

[4] Pihan E, Slaoui A, Cabarrocas PRI, Focsa A, Thin Solid Films, 451, 328 (2004)

[5] Ding Y, Yamada R, Gresback R, Zhou S, Pi XD, Nozaki T, J. Phys. D-Appl. Phys., 47, 9 (2014)

[6] Yasar-Inceoglu O, Lopez T, Farshihagro E, Mangolini L, Nanotechnology, 23, 10 (2012)

[7] Zhang J, Chen S, Zhang H, Zhang S, Yao X, Shi Z, RSC Adv., 6, 12061 (2016)

[8] Carbonaro CM, Corpino R, Ricci PC, Salis M, Anedda A, J. Mater. Sci., 48(12), 4452 (2013)

[9] Chen C, You KS, Ahn JW, Ahn WS, Korean J. Chem. Eng., 27(3), 1010 (2010)

[10] Gribov BG, Zinov'ev KV, Inorg. Mater., 39, 653 (2003)

[11] Chen XZ, Shi DP, Gao X, Luo ZH, Powder Technol., 205(1-3), 276 (2011)

[12] Robert E, Zijlema T, US Patent, 7,943,109 (2011).

[13] Braga AFB, Moreira SP, Zampieri PR, Bacchin JMG, Mei PR, Sol. Energy Mater. Sol. Cells, 92(4), 418 (2008)

[14] Lynch D, Jom, 61, 41 (2009)

[15] Kirii S, Narukawa M, Takesue H, US Patent, 6,846,473 (2005).

[16] Masuda N, Tachino N, US Patent, 8,197,783 (2012).

[17] Breneman WC, EP Patent, 1622831 A1 (2006).

[18] Fabry L, Paetzold U, Stepp M, US Patent, 8,557,210 (2013).

[19] Hesse K, Schreieder F, US Patent, 7708970 B2 (2010).

[20] Naumann K, Zon G, Mislow K, J. Am. Chem. Soc., 91, 7012 (2002)

[21] Nelson WM, Naidoo P, Ramjugernath D, J. Chem. Thermodyn., 91, 420 (2015)

[22] Szabo G, Szieberth D, Nyulaszi L, Struct. Chem., 26, 231 (2015)

[23] Ruff K, US Patent, 5,080,804 (1992).

[24] Burgie RA, Heng OA, US Patent, 5,118,486 (1992).

[25] Ferron S, Kelly J, Vermeulen R, US Patent, 7569193 B2 (2009).

[26] Michael LS, US Patent, 7,736,614 (2010).

[27] Breneman WC, Reeser DM, US Patent, 4,690,810 (1987).

[28] Herman JE, US Patent, 6,090,360 (2000).

[29] Coleman LM, Tambo W, US Patent, 4519999 A (1985).

[30] Zhang XL, Fan YL, J. Non-Cryst. Solids, 358, 337 (2012)

[31] Pinto PR, Mendes LC, Dias ML, Azuma C, Colloid Polym. Sci., 284, 529 (2006)

[32] Fidalgo A, Ciriminna R, Ilharco LM. Pagliaro M, Chem. Mater., 17, 6686 (2005)

[33] Pijarn N, Jaroenworaluck A, Sunsaneeyametha W, Stevens R, Powder Technol., 203(3), 462 (2010)

[34] Uchino T, Aboshi A, Kohara S, Ohishi Y, Sakashita M, Aoki K, Phys. Rev. B, 69 (2004)

[35] Lee S, Ha KR, Korean J. Chem. Eng., 33(8), 2469 (2016)

[36] Yan F, Jiang JG, Tian SC, Liu ZW, Shi J, Li KM, Chen XJ, Xu YW, Acs Sustain. Chem. Eng., 4, 4654 (2016)

[37] Cerveny S, Schwartz GA, Otegui J, Colmenero J, Loichen J, Westermann S, J. Phys. Chem. C, 116, 24340 (2012)

[38] Su M, Su H, Du B, Li X, Ren G, Wang S, Korean J. Chem. Eng., 32(5), 852 (2015)

[39] Adam F, Kandasamy K, Balakrishnan S, J. Colloid Interface Sci., 304(1), 137 (2006)

[40] Kim JM, Chang SM, Kong SM, Kim KS, Kim J, Kim WS, Ceram. Int., 35, 1015 (2009)

[41] Ek S, Root A, Peussa M, Niinisto L, Thermochim. Acta, 379(1-2), 201 (2001)

[42] Chen XJ, Jiang JG, Yan F, Tian SC, Li KM, RSC Adv., 4, 8703 (2014)

[43] Jal PK, Sudarshan M, Saha A, Patel S, Mishra BK, Colloids Surf. A: Physicochem. Eng. Asp., 240, 173 (2004)