Inorganic Chemicals Industry >

2022 , Vol. 54 >Issue 10: 109 - 115

DOI: https://doi.org/10.19964/j.issn.1006-4990.2021-0761

Research & Development

Preparation and characterization of anhydrous calcium sulfate whisker

  • Yuanhao QI ,
  • Jinxiu WU ,
  • Zhaogang LIU ,
  • Yanhong HU ,
  • Fushan FENG ,
  • Jianfei LI ,
  • Xin WANG ,
  • Conglin LIU
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  • 1. School of Materials and Metallurgy, Inner Mongolia University of Science and Technology, Baotou 014010, China
    2. Green Extraction and Efficient Utilization of Light Rare Earth Resources Key Laboratory of Ministry of Education
    3. Inner Mongolia Autonomous Region Rare Earth Hydrometallurgy and Light Rare Earth Application Key Laboratory

Received date: 2021-12-20

  Online published: 2022-11-03

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Abstract

Calcium sulfate whiskers with high aspect ratio were prepared by hydrothermal method using ammonium sulfate wastewater produced in the production process of a rare earth plant as raw material and calcium chloride as calcium source. Firstly,the effects of reaction time,reaction temperature and aging time on the aspect ratio of calcium sulfate whisker were studied by orthogonal experiment to determine the optimal process conditions.Based on the optimal process conditions of orthogonal experiment,the effect of pH value on the morphology of calcium sulfate whiskers was studied.The surface morphology and phase of calcium sulfate whiskers were characterized and analyzed by scanning electron microscopy（SEM）,X-ray diffraction（XRD）, infrared analyzer（FT-IR） and thermogravimetric-differential thermal analyzer（TG-DSC）.The results showed that the optimum preparation conditions of calcium sulfate whisker were reaction time of 5 h,reaction temperature of 140 °C,aging time of 4.5 h.When the pH value of the solution system was 1,pure anhydrous calcium sulfate whiskers were prepared,which had the best morphology and high aspect ratio.The average length was 117.44 μm and the average aspect ratio was 40.2.

Key words： ammonium sulfate wastewater; calcium sulfate whisker; hydrothermal method; aspect ratio

Cite this article

Yuanhao QI , Jinxiu WU , Zhaogang LIU , Yanhong HU , Fushan FENG , Jianfei LI , Xin WANG , Conglin LIU . Preparation and characterization of anhydrous calcium sulfate whisker[J]. Inorganic Chemicals Industry, 2022 , 54(10) : 109 -115 . DOI: 10.19964/j.issn.1006-4990.2021-0761

References

[1] 谢晴, 蒋美雪, 彭同江, 等. 磷石膏常压酸化法制备无水硫酸钙晶须的实验研究[J].人工晶体学报, 2019, 48(6): 1060-1066, 1071.
[1] XIE Qing, JIANG Meixue, PENG Tongjiang, et al.Experimental study on preparation of anhydrous calcium sulfate whisker by phosphogypsum at atmospheric acidification method[J].Journal of Synthetic Crystals, 2019, 48(6): 1060-1066, 1071.
[2] 付艳娥.利用化工废物合成硫酸钙晶须的研究[J].辽宁化工, 2014, 43(2): 182-183.
[2] FU Yane.Research on producing calcium sulfate whisker from che- mical waste[J].Liaoning Chemical Industry, 2014, 43(2): 182-183.
[3] 徐伟, 李梅, 张栋梁, 等. 稀土石膏常压酸化法制备硫酸钙晶须的研究[J].无机盐工业, 2020, 52(8): 66-71.
[3] XU Wei, LI Mei, ZHANG Dongliang, et al.Study on preparation of calcium sulfate whisker by atmospheric pressure acidification using rare earth gypsum[J].Inorganic Chemicals Industry, 2020, 52(8): 66-71.
[4] 马天玲.利用脱硫石膏制备硫酸钙晶须的研究[D].沈阳:东北大学, 2008: 2-7.
[4] MA Tianling.Study on calcium sulfate whiskers preparation from desulphurization gypsum[D].Shenyang:Northeastern University, 2008: 2-7.
[5] 马继红.硫酸钙晶须的制备及在道路改性沥青中的应用研究[D].青岛:山东科技大学, 2005: 4-13.
[5] MA Jihong.Preparation of calcium sulphate whisker and its application study in the paving asphalt[D].Qingdao:Shandong University of Science and Technology, 2005: 4-13.
[6] 秦军, 谢占金, 于杰, 等. 磷石膏制备硫酸钙晶须的初步研究[J].无机盐工业, 2010, 42(10): 50-53.
[6] QIN Jun, XIE Zhanjin, YU Jie, et al.Preliminary research on preparation of calcium sulphate whiskers from phosphogypsum[J].Inorganic Chemicals Industry, 2010, 42(10): 50-53.
[7] 甄德帅, 梁爽, 张兴文, 等. 硫酸钙晶须制备及应用综述[J].广东化工, 2017, 44(11): 140-141.
[7] ZHEN Deshuai, LIANG Shuang, ZHANG Xingwen, et al.Review of the preparation and application of calcium sulfate whisker[J].Guangdong Chemical Industry, 2017, 44(11): 140-141.
[8] LU Yunhua, ZHANG Weipeng, LI Xingwei, et al.Synthesis of new polyether titanate coupling agents with different polyethyleneglycol segment lengths and their compatibilization in calcium sulfate whisker/poly（vinyl chloride） composites[J].RSC Advances, 2017,7(50): 31628-31640.
[9] 耿世伟, 曹钰, 罗康碧, 等. 硫酸钙晶须的表面改性研究现状[J].化工新型材料, 2019, 47(10): 224-227.
[9] GENG Shiwei, CAO Yu, LUO Kangbi, et al.Research status on surface modification of calcium sulfate whisker[J].New Chemical Materials, 2019, 47(10): 224-227.
[10] 郑良川, 陆田玉, 杨本宏, 等. 废弃磷石膏水热法制备硫酸钙晶须[J].安徽化工, 2015, 41(5): 53-55, 57.
[10] ZHENG Liangchuan, LU Tianyu, YANG Benhong, et al.Preparation of calcium sulfate whiskers from waste phosphogypsum by hydrothermal method[J].Anhui Chemical Industry, 2015, 41(5): 53-55, 57.
[11] 厉伟光, 徐玲玲, 戴俊.柠檬酸废渣制备硫酸钙晶须的研究[J].人工晶体学报, 2005, 34(2): 323-327.
[11] LI Weiguang, XU Lingling, DAI Jun.Preparation of calcium sulfate whisker from the residue of citric acid[J].Journal of Synthetic Crystals, 2005, 34(2): 323-327.
[12] 崔益顺, 刘勇, 詹磊, 等. 盐泥制备硫酸钙晶须工艺研究[J].四川理工学院学报:自然科学版, 2012, 25(5): 19-21.
[12] CUI Yishun, LIU Yong, ZHAN Lei, et al.Study on preparation for calcium sulfate whisker from salt deposit[J].Journal of Sichuan University of Science ＆ Engineering:Natural Science Edition, 2012, 25(5): 19-21.
[13] WAN Lianjian, PAN Ruizhi, XU Jun.Mechanical properties and microstructure of CaSO4 whisker reinforced cement mortar[J].Journal of Wuhan University of Technology-Mater.Sci.Ed., 2019, 34(5): 1170-1176.
[14] 宋景尧, 史培阳, 姜茂发.工艺制度对脱硫灰制备硫酸钙晶须的影响作用[J].冶金工程, 2017, 4(2): 85-90.
[14] SONG Jingyao, SHI Peiyang, JIANG Maofa.Effect of process system on the preparation of calcium sulfate whiskers from desulphurization gypsum[J].Metallurgical Engineering, 2017, 4(2): 85-90.
[15] LIU J Y, HU X Y, HU M D, et al.Polycaprolactone/calcium sulfate whisker/barium titanate piezoelectric ternary composites for tissue reconstruction[J].Advanced Composites Letters, 2020, 29: 1-5.
[16] GAO Jing, LI Qiang, LIU Fuli.Calcium sulfate whisker prepared by flue gas desulfurization gypsum:A physical-chemical coupling production process[J].Chinese Journal of Chemical Engineering, 2020, 28(8): 2221-2226.
[17] 黄旭, 黄健, 牛韵雅, 等. 磷石膏制备的耐热半水硫酸钙晶须表面疏水改性研究[J].硅酸盐通报, 2019, 38(7): 2021-2027.
[17] HUANG Xu, HUANG Jian, NIU Yunya, et al.Research on surface hydrophobic modification of heat-resistant calcium sulfate hemihydrate whisker prepared from phosphogypsum[J].Bulletin of the Chinese Ceramic Society, 2019, 38(7): 2021-2027.
[18] 易伟, 徐晓晴, 刘晓刚, 等. 磷石膏水热合成法制备石膏晶须的研究[J].铜业工程, 2013(6): 8-14.
[18] YI Wei, XU Xiaoqing, LIU Xiaogang, et al.Preparation of calcium sulfate whisker using phosphogysum by hydrothermal meth-od[J].Copper Engineering, 2013(6): 8-14.
[19] 吴锦绣, 贾恒俊, 贾慧灵, 等. 纳米荧光粉YPO4:2%Sm3+水热工艺条件的优化及荧光性能[J].过程工程学报, 2020, 20(5): 583-590.
[19] WU Jinxiu, JIA Hengjun, JIA Huiling, et al.Optimization of hydrothermal process conditions of nanometer fluorescent powder YPO4:2%Sm3+ and fluorescence property[J].The Chinese Journal of Process Engineering, 2020, 20(5): 583-590.
[20] 曹冬梅, 张家凯, 高春娟, 等. 海水卤水制备硫酸钙晶须新工艺[J].化学工业与工程, 2010, 27(3): 195-198.
[20] CAO Dongmei, ZHANG Jiakai, GAO Chunjuan, et al.Preparation of calcium sulphate whisker using seawater or brine[J].Chemical Industry and Engineering, 2010, 27(3): 195-198.
[21] 唐娜, 黑云皓, 吴腾飞, 等. 以浓厚卤水为原料制备半水硫酸钙晶须的研究[J].无机盐工业, 2020, 52(4): 88-92.
[21] TANG Na, Yunhao HEI, WU Tengfei, et al.Study on preparation of hemihydrate calcium sulfate whisker from dense brine[J].Inorganic Chemicals Industry, 2020, 52(4): 88-92.
[22] CHEN Xiaojuan, YANG Liuchun, ZHANG Junfeng, et al.Exploration of as（Ⅲ）/as（Ⅴ） uptake from aqueous solution by synthesized calcium sulfate whisker[J].Chinese Journal of Chemical Engineering, 2014, 22(11/12): 1340-1346.
[23] LIU Chengjun, ZHAO Qing, WANG Yeguang, et al.Hydrothermal synthesis of calcium sulfate whisker from flue gas desulfurization gypsum[J].Chinese Journal of Chemical Engineering, 2016, 24(11): 1552-1560.
[24] ZHOU Di, WEI Rufei, ZHU Yulong, et al.Calcium sulfate whisker one-step preparation using semi-dry flue gas desulfurization ash and directional growth control[J].Journal of Cleaner Production, 2021,290.Doi:10.1016/j.jclepro.2020.125754 .
[25] 李武.无机晶须[M].北京:化学工业出版社, 2005.
[26] 李文博, 李海滨, 赵桂娟, 等. 硫酸钙晶须水泥砂浆力学性能及增强机理[J].西安科技大学学报, 2020, 40(3): 417-423.
[26] LI Wenbo, LI Haibin, ZHAO Guijuan, et al.Mechanical properties and strengthening mechanism of cement mortar with calcium sulfate whiskers[J].Journal of Xi'an University of Science and Technology, 2020, 40(3): 417-423.
[27] 郑绍聪, 朱丽苹, 谢刚, 等. 高纯天然石膏水热法制备硫酸钙晶须研究[J].无机盐工业, 2019, 51(7): 39-42.
[27] ZHENG Shaocong, ZHU Liping, XIE Gang, et al.Experimental study on preparation of calcium sulfate whiskers from high purity natural gypsum with hydrothermal method[J].Inorganic Chemicals Industry, 2019, 51(7): 39-42.
[28] MARTINS A F, DE OLIVEIRA D M, PEREIRA A G B, et al.Chitosan/TPP microparticles obtained by microemulsion method applied in controlled release of heparin[J].International Journal of Biological Macromolecules, 2012, 51(5): 1127-1133.
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