Effects of Solvent Treatment and High-Pressure Homogenization Process on Dispersion Properties of Palygorskite
Total Page:16
File Type:pdf, Size:1020Kb
Powder Technology 235 (2013) 652–660 Contents lists available at SciVerse ScienceDirect Powder Technology journal homepage: www.elsevier.com/locate/powtec Effects of solvent treatment and high-pressure homogenization process on dispersion properties of palygorskite Jixiang Xu a,b, Wenbo Wang a,c, Aiqin Wang a,c,⁎ a Center of Eco-material and Green Chemistry, Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou 730000, China b Graduate University of the Chinese Academy of Science, Beijing 100049, China c R&D Center of Xuyi Palygorskite Applied Technology, Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Xuyi 211700, China article info abstract Article history: Dispersion of natural palygorskite in distilled water, methanol, ethanol, isopropanol, dimethyl formamide, Received 12 September 2012 and dimethyl sulfoxide was carried out using high-pressure homogenization. The effects of solvent parame- Received in revised form 20 September 2012 ters on the microstructure, morphology and colloidal properties of palygorskite were investigated in detail. Accepted 19 November 2012 Elemental analysis, infrared spectroscopy (IR) and thermogravimetric analysis (TGA) confirmed that some Available online 27 November 2012 solvent molecules were encapsulated within the tunnels of palygorskite. The efficiency of the homogeniza- tion process to disperse palygorskite aggregates was closely correlated to the solvent parameters, particularly Keywords: Palygorskite solvent vapor pressure and viscosity. A well disaggregated palygorskite was obtained after dispersing in di- Dispersion methyl sulfoxide. It was also confirmed that colloidal stability and suspension viscosity were affected by Solvents the solvent nature. A more stable suspension with higher viscosity of 2364 mPa s was obtained by dispersing Homogenization palygorskite in isopropanol. © 2012 Elsevier B.V. All rights reserved. 1. Introduction wrapping of palygorskite rods are considered to be the mechanism of dispersion. Physical methods including high shear mixing and Palygorskite is a crystalline hydrated magnesium aluminum sili- ultrasonication in aqueous media were frequently employed as sim- cate with rod-like morphology. Because of its natural abundance, ple approaches to disperse palygorskite aggregates [11,12]. These the nanometric dimension of the single rod-like crystal, the excellent methods disaggregate palygorskite by strong shear action and the thermal/mechanical stability, and the silanol-based chemistry of the shear strength decides on the efficiency of disaggregation and the de- surface, palygorskite is a good candidate for an inorganic constituent gree of disruption of rod-like crystal. in many nanotechnological applications such as photocatalysis [1], Recently, we proposed an interesting method that use high-pressure dye adsorption [2,3], metallic nanoparticle support [4], polymer homogenization process to disperse the aggregates of palygorskite [13]. nanocomposites [5,6]. Most of these applications would profit of the The main mechanism by which the homogenization process accom- availability of highly dispersed or individualized palygorskite rods. plished this dispersion came from the turbulent flow and cavitation of However, due to the interparticle van der Waals and hydrogen bond- the liquid, which produced intense shear forces on the particles ing interactions, the naturally presented palygorskite is in the form of presented in the liquid, thus breaking the aggregates into smaller micrometric aggregates which is not readily dispersible in either units [14]. Whereas, homogenization process is dependent on many water or common organic solvents like swelling bentonites [7]. It be- factors including: (1) the nature of the liquid media, namely the vapor comes a significant obstacle in the application of palygorskite, and the pressure, viscosity, and surface tension. These parameters can govern disaggregation of the crystal bundles of palygorskite becomes a key to the threshold of the cavitation and the energy resulting from bubble expand the application of palygorskite. collapse, which will then influence the dispersion of palygorskite. Until now, improved dispersion of palygorskite has been achieved Most of the available results in the literature, however, were mainly fo- by introduction of a second component to the palygorskite surface cused on aqueous suspensions [15,16], and relatively little attention such as noncovalent or covalent adsorption of quaternary ammonium was paid on organic suspensions; (2) Homogenizing pressure. The salts in water, organosilanes or polymer chains with special reactive level of homogenizing pressure influences the strength of particle colli- group in organic solvent [8–10]. Surfactant coating and polymer sion, the size of cavitation and the probability of cavitation events per unit volume; (3) The nature of gas solubilized in the suspension, which can influence the number of cavitation events and gas content; ⁎ Corresponding author at: Center of Eco-material and Green Chemistry, Lanzhou Institute (4) Ambient suspension temperature and pressure. Because many of of Chemical Physics, Chinese Academy of Science, Lanzhou 730000, China. Fax: +86 931 8277088. the solvent parameters are temperature dependent, a change of tem- E-mail address: [email protected] (A. Wang). perature will affect the suspension properties and the gas solubility. 0032-5910/$ – see front matter © 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.powtec.2012.11.035 J. Xu et al. / Powder Technology 235 (2013) 652–660 653 For these reasons, it is necessary to examine how these factors influence dispersed in 50 mL of distilled water and stirred with a high-speed the dispersion of aggregates during homogenizing process. In a previ- mixer as in colloidal stability measurements, and then the viscosity ous work, we have studied the effects of homogenizing pressure on was measured under the constant shear rate of 30 rpm using spindle the morphology of palygorskite and found that the crystal bundles 3 at ambient temperature. were perfectly disaggregated without disrupting the rod-like crystals after homogenization the suspension at 30 MPa [13]. 2.4. Characterization In this study, the influences of dispersed media on the homogeni- zation process were considered. The dispersion of palygorskite aggre- The elemental analyses were performed using an Elementar Vario EL gates in a series of common solvents including distilled water, Elemental Analyzer. The IR spectra of the obtained samples were mea- methanol, ethanol, isopropanol, dimethyl formamide, and dimethyl sured using a Thermo Nicolet NEXUS TM spectrophotometer. The KBr sulfoxide were carried out with the aid of high-pressure homogeniza- pressed-disk technique was used. The XRD was performed on an X′ tion technology. The effects of solvent parameters on microstructure, Pert PRO diffractometer equipped with a Cu Kα radiation source morphology of resultant palygorskite were investigated systematical- (40 kV, 40 mA), and the diffraction data were collected from 3 to 50° ly via elemental analysis, infrared spectroscopy (IR), X-ray diffraction (2θ)inafixed time mode. The morphology of the samples was observed (XRD), thermogravimetric analysis (TGA), field emission scanning using FESEM (JSM-6701F, JEOL, Ltd.). Before the FESEM observation, all electron microscopy (FESEM) techniques. Sedimentation volume samples were fixed on copper stubs and coated with gold. N2 and viscosity measurements were also performed to study the colloi- adsorption-desorption isotherm was recorded using a Micromeritics dal properties of suspensions. ASAP 2010 apparatus at 77 K (Micromeritics, Norcross, GA, USA). Before measurements, all the samples were preheated at 90 °C under N2 for 2. Experimental 10 h to remove moisture. The TGA were performed on a Diamond TG-DTA 6300 thermoanalyzer under a nitrogen atmosphere from ambi- 2.1. Materials ent temperature to 800 °C at a heating rate of 10 °C min–1. Before anal- ysis, the samples were dried at 105 °C for 8 h. Palygorskite mineral, obtained from Jiuchuan technology Co., Jiangsu, China, is composed of 1.29% CaO, 10.47% Al2O3, 1.52% Na2O, 3. Results and discussion 20.41% MgO, 64.31% SiO2, 0.13% K2O and 0.87% Fe2O3 as determined by X-ray fluorescence spectrometer (PANalytical Co., MiniPal 4). Dis- 3.1. Elemental analysis tilled water was used as received. Methanol, ethanol, isopropanol, di- methyl formamide, and dimethyl sulfoxide are all of analytical grade, In order to determine if there were organic solvents presented in the and obtained from Shanghai Guoyao Chemical Reagent Corporation. obtained palygorskite samples (Table 1), the elemental analysis was performed and the percentages of carbon in the results of elemental 2.2. Dispersion of palygorskite analysis were chosen for this determination. Because no additive was added into the suspension, the increased content of carbon in obtained 50.0 g of palygorskite was dispersed in 500 mL of various dis- samples was only from the used dispersed medium. As listed in persed media (distilled water, methanol, ethanol, isopropanol, di- Table 1, the percentages of carbon of the unhomogenized and homoge- methyl formamide, and dimethyl sulfoxide, respectively) and stirred nized palygorskite dispersed by water are 0.91% and 1.28%, respectively, at 800 rpm for 120 min by mechanical stirring to obtain a homoge- which increased to 3.97%, 1.59%, 3.97%, 3.41%, and 4.14% for palygorskite neous suspension. The obtained suspension