Ca(H2PO4)2-H3PO4-K2SO4体系中石膏晶型及形貌调控

人工晶体学报 ›› 2021, Vol. 50 ›› Issue (6): 1104-1111.

Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄体系中石膏晶型及形貌调控

吴钦^1,2, 杨林^1,3, 易芸^1,2, 耿平兰⁴, 曹建新^1,2

1.贵州大学化学与化工学院,贵阳 550025;
2.贵州大学,贵州省绿色化工与清洁能源技术重点实验室,贵阳 550025;
3.贵州大学,贵州省工业废弃物高效利用工程研究中心,贵阳 550025;
4.贵州省产品质量检验检测院,贵阳 550016

收稿日期:2021-03-09 出版日期:2021-06-15 发布日期:2021-07-08
通讯作者: 杨林,教授。E-mail:ce.lyang@gzu.edu.cn;曹建新,教授。E-mail:jxcao@gzu.edu.cn
作者简介:吴钦(1995—),男,贵州省人,硕士研究生。E-mail:wqinbit@163.com
基金资助:
国家重点研发计划(2018YFC1900202);贵州省科技计划(黔科合服企[2018]4011)

Regulation of Gypsum Crystalline and Morphology in Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄ System

WU Qin^1,2, YANG Lin^1,3, YI Yun^1,2, GENG Pinglan⁴, CAO Jianxin^1,2

1. School of Chemistry and Chemical Engineering, Guizhou University, Guiyang 550025, China;
2. Key Laboratory of Guizhou Province for Green Chemical Industry and Clean Energy Technology, Guizhou University, Guiyang 550025, China;
3. Engineering Research Center of Efficient Utilization for Industrial Waste, Guizhou University, Guiyang 550025, China;
4. Guizhou Institute of Products Quality Inspection & Testing, Guiyang 550016, China

Received:2021-03-09 Online:2021-06-15 Published:2021-07-08

摘要/Abstract

摘要： 为将Ca(H₂PO₄)₂制备KH₂PO₄过程中的石膏资源化利用,以H₃PO₄与CaCO₃反应制备Ca(H₂PO₄)₂溶液,并与K₂SO₄溶液反应,进行Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄体系中石膏晶型和形貌调控研究。结果表明:通过改变反应时间、反应温度、SO^2-₄过量系数和CaO含量等参数可对Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄体系中石膏晶型和形貌进行调控,制得短柱状α-CaSO₄·0.5H₂O。体系在温度高于95 ℃和CaO含量为3.0%~5.0%(质量分数,下同)时形成α-CaSO₄·0.5H₂O,在CaO含量为5.5%主要形成CaSO₄·2H₂O;反应时间长于20 min和SO^2-₄过量系数大于1.4将形成K₂SO₄(CaSO₄)₅·H₂O,导致石膏晶体表面缺陷增加。本实验条件下,适宜反应条件为:反应时间10 min、反应温度95 ℃、SO^2-₄过量系数1.2和CaO含量5.0%,此条件下可制得长度42~70 μm、直径13~24 μm的短柱状α-CaSO₄·0.5H₂O,其抗折和抗压强度分别可达5.61 MPa和33.74 MPa,滤液中钾收率和脱钙率分别可达94.23%和83.80%。

关键词: α-CaSO₄·0.5H₂O, Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄体系, 石膏, 晶型, 形貌, 调控

Abstract: In order to make the resource utilization of gypsum in the process of preparing KH₂PO₄ from Ca(H₂PO₄)₂, the Ca(H₂PO₄)₂ solution prepared by the reaction of H₃PO₄ and CaCO₃ was mixed with K₂SO₄ solution. Then the regulation of gypsum crystalline and morphology in Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄ system was studied. The results show that the short columnar α-CaSO₄·0.5H₂O can be obtained from Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄ system by changing the reaction condition,including reaction time, reaction temperature, SO^2-₄ excess coefficient (ξ) and CaO content. The α-CaSO₄·0.5H₂O is formed at temperatures above 95 ℃ and CaO content of 3.0% to 5.0%(mass fraction, the same below), while CaSO₄·2H₂O is formed at low temperatures and CaO content of 5.5%. Meanwhile, with the increase of CaO content in the range of 3.0% to 5.0%, the aspect ratio of α-CaSO₄·0.5H₂O decreases. As the reaction time is longer than 20 min and the SO^2-₄ excess coefficient is greater than 1.4, K₂SO₄(CaSO₄)₅·H₂O is easily formed, resulting in the increase of surface defects of gypsum crystals. Under the conditions of reaction time of 5 min, reaction temperature of 95 ℃, SO^2-₄ excess coefficient of 1.2 and CaO content of 5.0%, a short columnar α-CaSO₄·0.5H₂O crystals with length of 42 μm to 70 μm and diameter of 13 μm to 24 μm are prepared, the flexural strength and compressive strength of which are 5.61 MPa and 33.74 MPa, respectively. The yield of potassium and decalcification rate of the filtrate are 94.23% and 83.80%, respectively.

Key words: α-CaSO₄·0.5H₂O, Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄ system, gypsum, crystalline, morphology, regulation

中图分类号:

O782

吴钦, 杨林, 易芸, 耿平兰, 曹建新. Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄体系中石膏晶型及形貌调控[J]. 人工晶体学报, 2021, 50(6): 1104-1111.

WU Qin, YANG Lin, YI Yun, GENG Pinglan, CAO Jianxin. Regulation of Gypsum Crystalline and Morphology in Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄ System[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2021, 50(6): 1104-1111.

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Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄体系中石膏晶型及形貌调控

Regulation of Gypsum Crystalline and Morphology in Ca(H₂PO₄)₂-H₃PO₄-K₂SO₄ System

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