Effect of Acid Etching on the Floatability of Dolomite and Its Mechanism of Action

doi:10.12068/j.issn.1005-3026.2024.01.012

Abstract

Abstract:

The effect of acid etching on the floatability of dolomite and its mechanism of action were investigated by flotation tests， flotation kinetic fitting， surface roughness characterization， specific surface area analysis， XPS analysis， adsorption performance analysis and wettability analysis under sodium oleate system. The research results showed that acid etching increased the surface roughness and specific surface area of dolomite， exposing more active sites， strengthened the adsorption sodium oleate， enhanced the hydrophobic of dolomite， and thus improved the performance of dolomite. Moreover， regarding flotation kinetic fitting， the classical first-order model， first-order model with rectangular distribution of floatability， and the second-order kinetic model all displayed the R² values higher than 95%. Compare with other models， the classical first-order model exhibited the best fit. At a sodium oleate mass concentration of 60 mg/L， the k value of classical first-order for dolomite reached a maximum value of 1.88 min^-1. However， in this case， before acid etching， the k value of classical first-order model for dolomite was only 1.15 min^-1. These results further confirmed that acid etching could improve the flotation rate of dolomite. In summary， this study can provide a new research perspective for dolomite flotation， with a certain theoretical and practical significance.

Key words: dolomite, roughness, acid etching, floatability, flotation kinetics

CLC Number:

TU 45

Jun GUO, Wan-zhong YIN, Bin YANG, Zhang-lei ZHU. Effect of Acid Etching on the Floatability of Dolomite and Its Mechanism of Action[J]. Journal of Northeastern University(Natural Science), 2024, 45(1): 93-100.

Figures/Tables 16

Fig. 1 XRD pattern of dolomite

Fig. 2 Schematic diagram of flotation tests

Fig. 3 Sodium oleate adsorption isotherm

Fig. 4 Effect of sodium oleate concentration on the flotation recovery of dolomite before and after acid etching

Fig. 5 Effect of pulp pH on the flotation recovery of dolomite before and after acid etching

Table 1 Flotation kinetic models

序号	浮选动力学模型	公式
模型1	经典一级模型^［15］	$R = R ∞ 1 - e x p - k 1 t$
模型2	一级矩阵分布模型^［16］	$R = R ∞ 1 - 1 k 2 t 1 - e x p - k 2 t$
模型3	二级动力学模型^［17］	$R = R ∞ 2 k 3 t / 1 + R ∞ k 3 t$
模型4	二级矩阵分布模型^［18］	$R = R ∞ 1 - 1 k 4 t l n 1 + k 4 t$

Table 1 Flotation kinetic models

序号	浮选动力学模型	公式
模型1	经典一级模型^［15］	$R = R ∞ 1 - e x p - k 1 t$
模型2	一级矩阵分布模型^［16］	$R = R ∞ 1 - 1 k 2 t 1 - e x p - k 2 t$
模型3	二级动力学模型^［17］	$R = R ∞ 2 k 3 t / 1 + R ∞ k 3 t$
模型4	二级矩阵分布模型^［18］	$R = R ∞ 1 - 1 k 4 t l n 1 + k 4 t$

Fig. 6 Non‐linear fitting of flotation kinetics before and after acid etching

Fig. 7 Effect of sodium oleate concentrations on the flotation rate constant of dolomite before and after acid etching

Fig. 8 AFM images of dolomite before and after acid etching

Table 2 Surface roughness and specific surface area of dolomite before and after acid etching

试样	R_a/nm	R_q/nm	粗糙度	比表面积
试样	R_a/nm	R_q/nm	nm	m²·g^-1
酸蚀前	0.163	0.268	0.2～1.3	0.324
酸蚀后	0.216	0.370	0.5～2.2	0.386

Table 3 XPS analysis results of dolomite

试样	Ca2p	Mg1s	C1s	O1s
酸蚀前	6.71	1.97	36.61	54.71
酸蚀后	9.60	4.22	38.24	47.94

Fig. 9 XPS energy spectrum of dolomite before and after acid etching

Fig. 10 Residual sodium oleate concentration in supernatant after sodium oleate adsorbed on dolomite

Fig. 11 Adsorption density of sodium oleate on dolomite before and after acid etching

Table 4 Contact angle of dolomite before and after acid etching

酸蚀前	酸蚀后	酸蚀前+油酸钠	酸蚀后+油酸钠
32.18	25.71	72.67	88.35

Fig. 12 Possible mechanistic model of roughness in wettability and flotation kinetics

References 23

1	Yekeler M， Ulusoy U.Characterisation of surface roughness and wettability of salt‐type minerals：calcite and barite［J］.Mineral Processing and Extractive Metallurgy，2004，113（3）：145-152.
2	Ulusoy U， Yekeler M.Correlation of the surface roughness of some industrial minerals with their wettability parameters［J］.Chemical Engineering and Processing：Process Intensification，2005，44（5）：555-563.
3	Yekeler M， Ulusoy U， Hiçyılmaz C.Effect of particle shape and roughness of talc mineral ground by different mills on the wettability and floatability［J］.Powder Technology，2004，140（1/2）：68-78.
4	Xia W C， Ni C， Xie G Y.The influence of surface roughness on wettability of natural/gold‐coated ultra‐low ash coal particles［J］.Powder Technology，2016，288：286-290.
5	Xing Y W， Zhang Y F， Ding S H，et al.Effect of surface roughness on the detachment between bubble and glass beads with different contact angles［J］.Powder Technology，2020，361：812-816.
6	Hassas V B， Caliskan H， Guven O，et al.Effect of roughness and shape factor on flotation characteristics of glass beads［J］.Colloids and Surfaces A：Physicochemical and Engineering Aspects，2016，492：88-99.
7	Tong Z Y， Liu L， Yuan Z T，et al.The effect of comminution on surface roughness and wettability of graphite particles and their relation with flotation［J］.Minerals Engineering，2021，169：106959.
8	Wu H Q， Fang S， Shu K Q，et al.Selective flotation and adsorption of ilmenite from titanaugite by a novel method：ultrasonic treatment［J］.Powder Technology，2020，363：38-47.
9	Zhang N N， Ejtemaei M， Nguyen A V，et al.XPS analysis of the surface chemistry of sulfuric acid‐treated kaolinite and diaspore minerals with flotation reagents［J］.Minerals Engineering，2019，136：1-7.
10	Li H X， Chai W C， Cao Y J，et al.Flotation enhancement of low‐grade bauxite using oxalic acid as surface pretreatment agent［J］.Applied Surface Science，2022，577：151964.
11	Zhu G L， Zhao Y H， Zheng X Y，et al.Surface features and flotation behaviors of spodumene as influenced by acid and alkali treatments［J］.Applied Surface Science，2020，507：145058.
12	Cao S H， Yin W Z， Yang B，et al.Insights into the influence of temperature on the adsorption behavior of sodium oleate and its response to flotation of quartz［J］.International Journal of Mining Science and Technology，2022，32（2）：399-409.
13	付亚峰，杨晓峰，印万忠，等.木质素磺酸钙对水镁石浮选中蛇纹石的抑制机理［J］.中南大学学报（自然科学版），2022，53（2）：371-378.
	Fu Ya‑feng， Yang Xiao‑feng， Yin Wan‑zhong，et al.Inhibitory role of calcium lignosulfonate on serpentine during brucite flotation［J］.Journal of Central South University （Science and Technology），2022，53（2）：371-378.
14	姚金，印万忠，王余莲，等.油酸钠浮选体系中菱镁矿与白云石和石英的交互影响［J］.东北大学学报（自然科学版），2013，34（9）：1330-1334.
	Yao Jin， Yin Wan‑zhong， Wang Yu‑lian，et al.Interactive effect of dolomite and quartz on the floatability of magnesite in sodium oleate flotation system［J］.Journal of Northeastern University （Natural Science），2013，34（9）：1330-1334.
15	Hassanzadeh A， Huu H D， Brockmann M.Assessment of flotation kinetics modeling using information criteria； case studies of elevated‐pyritic copper sulfide and high‐grade carbonaceous sedimentary apatite ores［J］.Journal of Dispersion Science and Technology，2020，41（7）：1083-1094.
16	Zhang H J， Liu J T， Cao Y J，et al.Effects of particle size on lignite reverse flotation kinetics in the presence of sodium chloride［J］.Powder Technology，2013，246：658-663.
17	Stanojlović R D， Sokolović J M.A study of the optimal model of the flotation kinetics of copper slag from copper mine BOR［J］.Archives of Mining Sciences，2014，59（3）：821-834.
18	Ruiz‑Cabello F M， Trefalt G， Csendes Z，et al.Predicting aggregation rates of colloidal particles from direct force measurements［J］.The Journal of Physical Chemistry B，2013，117（39）：11853-11862.
19	Xu M Q.Modified flotation rate constant and selectivity index［J］.Minerals Engineering，1998，11（3）：271-278.
20	Polat M， Chander S.First‐order flotation kinetics models and methods for estimation of the true distribution of flotation rate constants［J］.International Journal of Mineral Processing，2000，58（1/2/3/4）：145-166.
21	Azizi A.A study on the modified flotation parameters and selectivity index in copper flotation［J］.Particulate Science and Technology，2017，35（1）：38-44.
22	Zhu Z L， Wang D H， Yang B，et al.Water droplets and air bubbles at magnesite nano‐rough surfaces：analysis of induction time，adhesion and detachment using a dynamic microbalance［J］.Minerals Engineering，2020，155：106449.
23	Zhu Z L， Yin W Z， Wang D H，et al.The role of surface roughness in the wettability and floatability of quartz particles［J］.Applied Surface Science，2020，527：146799.

[1]	ZHAO Xu， YIN Wan-zhong， YAO Jin， ZHU Zhang-lei. Effect of Roughness on Floatability of Dolomite in Sodium Oleate System and Its Mechanism [J]. Journal of Northeastern University(Natural Science), 2023, 44(8): 1188-1194.
[2]	ZHANG Jia-hao， ZOU Ping， WEI Shi-yu， LIANG Fu-qiang. Experimental Study on Single-Excitation 3-D Ultrasonic Turning Technology [J]. Journal of Northeastern University(Natural Science), 2023, 44(8): 1152-1159.
[3]	YANG Jin-jin， WANG Zhe-chao， QIAO Li-ping， LI Wei. Analysis of Evolution Characteristics and Influencing Factors of Vortex Structure in Rough-Walled Fracture [J]. Journal of Northeastern University(Natural Science), 2023, 44(5): 697-704.
[4]	FANG Rui， ZOU Ping， DUAN Jing-wei， WEI Shi-yu. Experimental Research on Friction Reduction Characteristics and Surface Quality of 3D Ultrasonic Vibration Assisted Turning [J]. Journal of Northeastern University(Natural Science), 2023, 44(2): 233-241.
[5]	SUN Yao， TANG Ben-jia， GONG Ya-dong， LI Si-hui. Preparation Method and Experimental Study of Array Microholes on the Surface of Nickel-Based Single Crystal Superalloy [J]. Journal of Northeastern University(Natural Science), 2023, 44(12): 1719-1725.
[6]	ZHOU Xiao-hong， GAO Shu-ling， MENG Ling-guo， ZHAO Qiang. Influence of Wall Roughness on Slurry Flow and Particles Separation Behaviors in Spirals [J]. Journal of Northeastern University(Natural Science), 2023, 44(12): 1769-1777.
[7]	JIANG Shi-jie， HU Ke， CHEN Pi-feng， ZHAN Ming. Theoretical and Experimental Investigation on the Three-Dimensional Surface Roughness of Fused Filament Fabrication Products [J]. Journal of Northeastern University(Natural Science), 2022, 43(9): 1290-1297.
[8]	WEN Xue-long， HAN Feng-bing， GONG Ya-dong， HUANG Xiong-jun. Effect of Deposition Time on the Surface Properties of Vacuum Ion Plating TiC Coated Micro-grinding Tools [J]. Journal of Northeastern University(Natural Science), 2022, 43(6): 857-863.
[9]	WEN Xue-long， WANG Cheng-bao， GONG Ya-dong， SUN Fu-qiang. Preparation of Coated Micro-grinding Tools and Experimental Research on Grinding Surface Quality [J]. Journal of Northeastern University(Natural Science), 2022, 43(5): 681-688.
[10]	WEN Xue-long， LI Jia-yu， LI Xin-yan. Influencing Factors of Grinding Surface Quality of TiC-Coated Micro-grinding Tools [J]. Journal of Northeastern University(Natural Science), 2022, 43(4): 534-540.
[11]	ZHOU Yun-guang， TIAN Chuan-chuan， MA Lian-jie， BI Chang-bo. Experimental Study on Surface Quality in Micro-scale Grinding of Zirconia Ceramics [J]. Journal of Northeastern University(Natural Science), 2022, 43(1): 83-88.
[12]	ZHAO Chun-yu， CHENG Da-zhong， GENG Hao-bo. Research on 2-D Surface Topography Detection Method of Turning Workpieces [J]. Journal of Northeastern University(Natural Science), 2021, 42(9): 1299-1306.
[13]	JIANG Shi-jie， HU Ke， CHEN Pi-feng， SIYAJEU Yannick. Theoretical Model and Experimental Verification of Surface Roughness of Fused Filament Fabrication Plates [J]. Journal of Northeastern University(Natural Science), 2021, 42(7): 980-986.
[14]	SUN Wen-han， LIU Wen-gang， YANG Ting， DAI Shu-juan. Effect of TX-100 on Flotation of Magnesite and Dolomite Using NaOL as Collector [J]. Journal of Northeastern University(Natural Science), 2021, 42(2): 226-231.
[15]	JIAO An-yuan， ZHANG Guo-fu， DING Hao-dong， LIU Wei-jun. Experiment of Magnetic Abrasive Finishing on TC4 Titanium Alloy Hole [J]. Journal of Northeastern University Natural Science, 2020, 41(9): 1304-1310.