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Elimination of Ferric Ion Effect on Separation Between Kyanite and Quartz Using Citric Acid As Regulator

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Elimination of Ferric Ion Effect on Separation Between Kyanite and Quartz Using Citric Acid As Regulator minerals Article Elimination of Ferric Ion Effect on Separation between Kyanite and Quartz Using Citric Acid as Regulator Yanping Niu 1, Ya Li 1, Haoran Sun 2,*, Chuanyao Sun 3, Wanzhong Yin 2 and Hongfeng Xu 4 1 Heilongjiang Province Geology Ore Test and Application Institute, Harbin 150000, China; [email protected] (Y.N.); [email protected] (Y.L.) 2 College of Resources and Civil Engineering, Northeastern University, Shenyang 110816, China; [email protected] 3 State Key Laboratory of Mineral Processing, BGRIMM Technology Group, Beijing 100160, China; [email protected] 4 Heilongjiang Mining Group Co., Ltd., Harbin 150000, China; [email protected] * Correspondence: [email protected]; Tel.: +86-188-4250-4743 Abstract: Ferric ions produced during grinding influence the flotation separation between kyanite and quartz adversely. In this study, citric acid was used as a regulator to eliminate the effect of ferric ions on the separation of kyanite from quartz with sodium oleate (NaOL) as a collector. The microflotation test results indicated that the quartz was selectively activated by FeCl3 and maintained significant quartz recovery. However, the citric acid could selectively eliminate the effect of ferric ions on the quartz and minimally influenced the kyanite. Contact angle tests demonstrated that FeCl significantly increased the interaction between NaOL and quartz, resulting in the high 3 hydrophobicity of quartz, and the addition of citric acid made the quartz surface hydrophilic again but slightly influenced the kyanite. Fourier-transform infrared spectroscopy showed that FeCl Citation: Niu, Y.; Li, Y.; Sun, H.; Sun, 3 C.; Yin, W.; Xu, H. Elimination of facilitated NaOL adsorption onto the quartz surface, and the addition of citric acid eliminated the Ferric Ion Effect on Separation activation of FeCl3 on the quartz, resulting in the nonadsorption of NaOL onto the quartz surface. between Kyanite and Quartz Using However, the FeCl3 and citric acid exhibited a negligible effect on NaOL adsorption onto the kyanite Citric Acid as Regulator. Minerals surface. X-ray photoelectron spectroscopy analysis indicated that the citric acid eliminated FeCl3 2021, 11, 599. https://doi.org/ activation on the quartz. 10.3390/min11060599 Keywords: kyanite; quartz; citric acid; ferric ion; selective elimination Academic Editors: Zhiyong Gao, Wenjihao Hu, Peipei Wang, Kirsten Claire Corin and Ljudmilla Bokányi 1. Introduction Received: 6 May 2021 Kyanite is an essential metamorphic nesosilicate with the chemical formula Al SiO , Accepted: 31 May 2021 2 5 Published: 3 June 2021 and it is widely used in metallurgy, building materials, ceramics, and other industrial sectors [1,2]. It can also be used for preparing silicon–aluminum alloys and metal fibers [3]. Publisher’s Note: MDPI stays neutral However, with the extensive exploitation of kyanite resources, low-grade kyanite, rich in with regard to jurisdictional claims in quartz and muscovite impurities, has become relatively more abundant [4]. Thus, reducing published maps and institutional affil- the impurity contents (for example, quartz) is required to improve the quality of kyanite iations. concentration powder. Kyanite is produced in commercial grades using several mineral processing methods, such as hand sorting, gravity separation, magnetic separation, flotation, and roasting [5–8]. Because kyanite properties are becoming increasingly complex, flotation is widely applied for kyanite beneficiation. Many studies on the separation of kyanite and quartz were Copyright: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. focused on the development of collectors, such as anionic sodium hexadecanesulfonate [9], This article is an open access article dodecylamine hydrochloride [10], sodium dodecyl sulfate [11], and potassium oleate [12]. distributed under the terms and Nonetheless, despite the several novel collectors used in these experimental studies, sodium conditions of the Creative Commons oleate (NaOL) remains the most widely used collector for the direct flotation separation Attribution (CC BY) license (https:// between kyanite and quartz [13,14]. creativecommons.org/licenses/by/ The minerals are crushed and ground before the flotation process is started, and ferric 4.0/). ions released from the steel-grinding medium may activate gangue minerals [15]. Therefore, Minerals 2021, 11, 599. https://doi.org/10.3390/min11060599 https://www.mdpi.com/journal/minerals Minerals 2021, 11, x FOR PEER REVIEW 2 of 10 Minerals 2021, 11, 599 2 of 10 The minerals are crushed and ground before the flotation process is started, and ferric ions released from the steel-grinding medium may activate gangue minerals [15]. There- fore,the flotation the flotation separation separation of kyanite of kyanite from from quartz quartz in the in presencethe presence of NaOL of NaOL as a as collector a collector can cancause cause a large a large amount amount of quartz of quartz to float to togetherfloat together with kyanite, with kyanite, reducing reducing the grade the of grade kyanite of kyanitein the concentrate in the concentrate [16–18]. Thus,[16–18]. the Thus, activation the activation of quartz of by quartz ferric ion by shouldferric ion be eliminatedshould be eliminatedto enhance to flotation enhance separation flotation separation between kyanite between and kyanite quartz and efficiently. quartz efficiently. CitricCitric acid acid is is an environmentally friendly friendly organic organic chelating agent, agent, which has been widelywidely used in recent years.years. Many researchresearch studiesstudies havehaveshown shown that that citric citric acid acid can can form form a astable stable complex complex with with iron, iron, prevent prevent iron iron precipitation, precipitation, increase increase the the concentration concentration of of soluble solu- bleiron iron in water,in water, and and promote promote the the production production of of more more activeactive oxygenoxygen free radicals [19 [19––21]21].. Therefore,Therefore, inin this study,study, aa citric citric acid acid regulator regulator was was employed employed to to achieve achieve efficient efficient separation separa- tionthrough through flotation flotation and and increase incre thease differencethe difference in the in flotationthe flotation performance performance of kyanite of kyanite and andquartz quartz using using NaOL NaOL as a as collector a collector in the in presencethe presence of ferric of ferric ions. ions. The effectsThe effects of the of citric the citric acid acidand ferricand ferric ions onions the on flotation the flotation behavior behavior of these of two these minerals two minerals were investigated were investigated through throughexperimental experim microflotationental microflotation tests. Furthermore, tests. Furthermore, the effects the ofeffects the differentof the different adsorption ad- sorptionbehaviors behaviors and selective and reactionselective mechanisms reaction mechanisms of the citric of acid theand citric ferric acid ion and on ferric the flotation ion on theseparation flotation between separation the between two minerals the two were minerals determined were determined through contact through angle contact measure- angle measurments,ements, Fourier-transform Fourier-transform infrared infrared (FTIR) analysis, (FTIR) analysis, and X-ray and photoelectron X-ray photoelectron spectroscopy spec- troscopy(XPS) measurements. (XPS) measurements. 2.2. Materials Materials and and Methods Methods 2.1.2.1. Materials Materials and and Reagents Reagents SeparateSeparate kyanite andand quartzquartz minerals minerals were were obtained obtained from from Henan Henan and and Hebei Hebei Provinces Prov- in China, respectively [22]. The X-ray powder diffraction patterns of the samples are shown inces in China, respectively [22]. The X-ray powder diffraction patterns of the samples are in Figure1, and the chemical analysis results are listed in Table1. The kyanite and quartz shown in Figure 1, and the chemical analysis results are listed in Table 1. The kyanite and purities were 98.60% and 99.31%, respectively. quartz purities were 98.60% and 99.31%, respectively. 150000 ☆ ☆ Quartz 120000 90000 60000 Intensity (Counts) ☆ 30000 ☆ ☆ ☆ ☆☆ ☆ ☆ ☆ ☆ ☆ ☆☆ 0 10 20 30 40 50 60 70 80 90 o 2θ ( ) (a) (b) FigureFigure 1. 1. XX-ray-ray powder powder diffraction diffraction patterns patterns of ( a)) kyanite and ( (b)) quartz quartz.. TableTable 1. Chemical composition analysis of mineral samples (wt%). Minerals SiO2 Al2O3 TFe MgO CaO TiO2 Mn Loss onLoss Ignition on Minerals SiO Al O TFe MgO CaO TiO Mn Kyanite 36.522 60.402 3 0.81 0.18 — 0.0602 — Ignition0.51 Quartz 99.31 — 0.08 — — — — — Kyanite 36.52 60.40 0.81 0.18 — 0.060 — 0.51 Quartz 99.31 — 0.08 — — — — — The −0.074 + 0.045 mm fraction was used for the experimental flotation tests and con- tact angle analyses. Analytical grades of citric acid, NaOL, and FeCl3 were obtained from − AladdinThe Industrial0.074 + Corporation, 0.045 mm fraction Shanghai, was China used for, NaOH the experimental and HCl solutions flotation were tests used and to adjustcontact the angle pH, analyses.and deionized Analytical water gradeswas used of citricfor all acid, experimental NaOL, and tests FeCl. 3 were obtained from Aladdin Industrial Corporation, Shanghai, China, NaOH and HCl solutions were used to adjust the pH, and deionized water was used for all experimental tests. Minerals 2021, 11, x FOR PEER REVIEW 3 of 10 Minerals 2021, 11, 599 3 of 10 2.2. Microflotation Tests Microflotation
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