常压Mg-Na复合盐溶液体系制备α-半水石膏

doi:10.19964/j.issn.1006-4990.2023-0116

Abstract

Abstract:

The species and concentration of salt solution are the key factors of the preparation process of α-hemihydrate gypsum in the atmospheric salt solution method.With Mg（NO₃）₂ as main composition，three kinds of mixed salt solution，including Mg（NO₃）₂-NaCl、Mg（NO₃）₂-Na₂SO₄ and Mg（NO₃）₂-NaNO₃，were employed to investigate the crystal transformation from dihydrate gypsum to α-hemihydrate gypsum，and the effects of the concentration of mixed salts，crystal modifier type and dosage on the transformation rate of dihydrate gypsum and crystal morphology were studied in the Mg（NO₃）₂-NaCl solution.The results showed that in the mixed salt solution of Mg（NO₃）₂-1%NaCl，the minimum Mg（NO₃）₂ mass fraction for the complete conversion of gypsum dihydrate to gypsum hemihydrate within 4 h was 27%.As the mass fraction of Mg（NO₃）₂ increasing from 27% to 36%，the supersaturation of the solution and transformation rate of dihydrate gypsum were increased，and the induction period was decreased from 90 min to 20 min.Using DL-malic acid，maleic acid and 3-nitrophthalic acid as crystal modifiers，the transformation rate of dihydrate gypsum was decreased and the aspect ratio was reduced.When the mass fraction of DL-malic acid was 1%，the absolute dry compressive strength of the α-hemihydrate gypsum was 21.74 MPa.

Key words: α-hemihydrate gypsum, atmospheric salt solution method, crystal modifier, crystal morphology, mechanical property

CLC Number:

TQ177.3

LI Yunfei, LIU Shuqing, TANG Shengwei, ZHANG Tao. Preparation of α-hemihydrate gypsum in Mg-Na mixed salt solution system under atmospheric pressure[J]. Inorganic Chemicals Industry, 2023, 55(11): 100-106.

Figures/Tables 15

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References 19

1	逄鲁峰，孙立刚，付鹏，等.一种新型石膏自流平材料的研究与工程应用［J］.新型建筑材料，2021，48（10）：6-10.
	PANG Lufeng， SUN Ligang， FU Peng，et al.Research and engineering application of a new type of gypsum based self-leveling material［J］.New Building Materials，2021，48（10）：6-10.
2	ZAMANIAN A， HESARAKI S， KHORAMI M.Physical and in-vitro biological evaluation of a novel calcium sulfate-apatite nanocomposite［J］.Journal of the Australian Ceramic Society，2010，46（2）：43-47.
3	LIU Chuanbei， GAO Jianming， TANG Yongbo，et al.Preparation and characterization of gypsum-based materials used for 3D robocasting［J］.Journal of Materials Science，2018，53（24）：16415-16422.
4	WU Xiaoqin， WU Zhongbiao.Modification of FGD gypsum in hydrothermal mixed salt solution［J］.Journal of Environmental Sciences（China），2006，18（1）：170-175.
5	胡成，向玮衡，陈平，等.丁二酸对水热合成α-半水脱硫石膏微晶形貌及力学强度的影响［J］.无机盐工业，2021，53（4）：76-80.
	HU Cheng， XIANG Weiheng， CHEN Ping，et al.Effects of succinic acid on crystallite morphology and mechanical strength of α-hemihydrate desulfurized gypsum synthesized by hydrothermal method［J］.Inorganic Chemicals Industry，2021，53（4）：76-80.
6	江瀚宁，李玉平，王志云，等.硫酸铝、草酸钾及其共混物对α-半水石膏制备及性能的影响［J］.无机盐工业，2022，54（10）：121-126.
	JIANG Hanning， LI Yuping， WANG Zhiyun，et al.Effect of potassium oxalate and aluminum sulfate and their compounds on preparation and properties of α-hemihydrate gypsum［J］.Inorganic Che-micals Industry，2022，54（10）：121-126.
7	REIGL S， VAN DRIESSCHE A E S， MEHRINGER J，et al.Revisiting the roles of salinity，temperature and water activity in phase selection during calcium sulfate precipitation［J］.CrystEngComm，2022，24（8）：1529-1536.
8	LIU Tianjie， FAN Hao， XU Yanxia，et al.Effects of metal ions on the morphology of calcium sulfate hemihydrate whiskers by hydrothermal method［J］.Frontiers of Chemical Science and Engineering，2017，11（4）：545-553.
9	YANG Baojun， DONG Yinzhe， WANG Bainian，et al.A mild alcohol-salt route to synthesize α-hemihydrate gypsum microrods from flue gas desulfurization gypsum in large scale［J］.Materials Research Express，2019，6（4）：045507.
10	SUKIMOTO S， HARA N， MUKAIYAMA H.Effects of salts on the formation of α-calcium sulfate hemihydrates in aqueous salts solution under the atmospheric pressure［J］.Gypsum & Lime，1985，1985（199）：363-370.
11	CHEN Xuemei， GAO Jianming， WU Ye，et al.Preparation of CSHW with flue gas desulfurization gypsum［J］.Materials，2022，15（7）：2691.
12	杨后文，刘丰，江郡，等.常压水热法制备半水脱硫石膏的工艺因素研究［J］.矿产综合利用，2021（1）：140-143，198.
	YANG Houwen， LIU Feng， JIANG Jun，et al.Research on process condition on the preparation of hemihydrate desulfurization gypsum with hydrothermal method under atmospheric pressure［J］.Multipurpose Utilization of Mineral Resources，2021（1）：140-143，198.
13	JIANG Guangming， WANG Hao， CHEN Qiaoshan，et al.Preparation of alpha-calcium sulfate hemihydrate from FGD gypsum in chloride-free Ca（NO₃）₂ solution under mild conditions［J］.Fuel，2016，174：235-241.
14	杨润，陈德玉，米阳，等.常压无氯复合盐溶液磷石膏制备α-半水石膏［J］.非金属矿，2019，42（4）：1-5.
	YANG Run， CHEN Deyu， MI Yang，et al.Preparation of α-semi hydrated gypsum from phosphogypsum in atmospheric pressure chlorine-free complex salt solution［J］.Non-Metallic Mines，2019，42（4）：1-5.
15	李军，胡俊要，王涛，等.一种常压盐溶液法制取α-超高强石膏的方法：中国，107382111B［P］.2020-06-19.
16	LI Zirui， LIU Yong， XING Dongxian，et al.Effect of maleic acid and pH on the preparation of α-calcium sulfate hemihydrate from phosphogypsum in Mg（NO₃）₂ solution［J］.Journal of Material Cycles and Waste Management，2022，24（1）：143-154.
17	李显波.高强α半水磷石膏晶形调控及水化硬化性能研究［D］.贵阳：贵州大学，2019.
	LI Xianbo.Crystal morphology control and hydration hardening properties of high strength α-hemihydrate phosphogypsum［D］.Guiyang：Guizhou University，2019.
18	GAO Dejun， ZHANG Dian， PENG Yanzhou，et al.Effects of different carboxyl additives on the growth habits of hemihydrate gypsum crystals［J］.Construction and Building Materials，2022，316：126037.
19	LI Xianbo， ZHANG Qin.Effect of molecular structure of organic acids on the crystal habit of α-CaSO₄·0.5H₂O from phosphogypsum［J］.Crystals，2020，10（1）：24.

项目	w（O）/%	w（Ca）/%	w（S）/%
EDS检测值	51.3	26.7	22.0
理论值	49.6	27.6	22.1

[1]	WANG Peixiong, GONG Xiaomei, DING Jiaqi, CAO Hong. Effect of crystal modifier on preparation of α-hemihydrates gypsum from industrial gypsum [J]. Inorganic Chemicals Industry, 2024, 56(4): 112-117.
[2]	YANG Fengling, QIAO Guoxin, YANG Pu, REN Lei, WANG Qiong, WU Haibin, CHENG Fangqin. Research progress and application of α-hemihydrate gypsum preparation from desulfurization gypsum [J]. Inorganic Chemicals Industry, 2024, 56(2): 11-20.
[3]	LI Peng, WANG Likun, MENG Qiuyan. Study on effect of α-hemihydrate gypsum on performance of cement mortar and its hydration mechanism [J]. Inorganic Chemicals Industry, 2023, 55(3): 98-103.
[4]	LIU Chao, FAN Chuigang, LIU Runguo, YU Dongxue, LI Songgeng. Preparation of α-hemihydrate gypsum from phosphogypsum by flotation and atmospheric trans-crystallization in solution [J]. Inorganic Chemicals Industry, 2023, 55(11): 107-114.
[5]	LI Sen, WANG Jin, WANG Yingying, CAI Mingfang. Synthesis and modification of NaA zeolite and its application in polyurethane system [J]. Inorganic Chemicals Industry, 2023, 55(10): 78-85.
[6]	LI Mingchuan,WEI Jiazhan,CHEN Ping,DUAN Pengxuan. Effect of crystal modifier and autoclave parameters on preparation of α-hemihydrate gypsum from phosphogypsum [J]. Inorganic Chemicals Industry, 2022, 54(8): 132-137.
[7]	XU Cheng,SHENG Jiefa,HAO Yuning,WU Binghui,MA Xiaoming,LIU Jianwu,YAN Shenghu,ZHANG Yue. Study on process of preparing α-hemihydrate gypsum by azeotropic reflux method [J]. Inorganic Chemicals Industry, 2022, 54(7): 117-123.
[8]	XU Qingying,YANG Dingyi,LÜ Wei,LI Xiang,QIAN Yunfeng,DU Baocong. Effect of grinding time on properties of phosphogypsum based cementitious materials [J]. Inorganic Chemicals Industry, 2022, 54(5): 101-108.
[9]	JIANG Hanning,LI Yuping,WANG Zhiyun,WEN Huimin,YE Baoquan. Effect of potassium oxalate and aluminum sulfate and their compounds on preparation and properties of α-hemihydrate gypsum [J]. Inorganic Chemicals Industry, 2022, 54(10): 121-126.
[10]	Zheng Nan,Tian Peng,Zhu Xingkun,Sun Xue,Pang Hongchang,Ning Guiling. Preparation and flame retardant properties of basic magnesium carbonate composite flame retardant [J]. Inorganic Chemicals Industry, 2021, 53(2): 47-50.
[11]	Jia Pengli. Study on solidification mechanism of MPC for enrichment heavy metals Cu and Ni [J]. Inorganic Chemicals Industry, 2020, 52(3): 94-97.
[12]	Guo Shenghui,Hu Longtao,Yang Li,Gao Jiyun,Hou Ming. Effect of pre-alloying raw material on property of diamond tools by microwave pressureless sintering [J]. Inorganic Chemicals Industry, 2020, 52(12): 23-28.
[13]	Chen Ping,Tian Yu,Hu Cheng. Effect of type and concentration of salt solution on synthesis of α-semi-water desulfurization gypsum [J]. Inorganic Chemicals Industry, 2020, 52(10): 130-134.
[14]	WU Shi-Qin, LI Jun, JIN Yang, MA Yu-Jing, CHEN Xi. Effect of Fe3+， Mg2+， and Al3+ on phase transformation process of CaSO4·2H2O to CaSO4·0.5H2O in CaCl2-HCl-H2O electrolyte solution [J]. INORGANICCHEMICALSINDUSTRY, 2015, 47(4): 30-.
[15]	WANG Lu-Ming. Study on modification of fire[WT5.25BZ][JX-6][KG-2/3]-[KG-3][JX6][WT5HZ]retardant Mg(OH)₂ and composite effect with PS [J]. INORGANICCHEMICALSINDUSTRY, 2011, 43(12): 29-.

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Inorganic Acid-Base-Salt Committee of CIESC

Preparation of α-hemihydrate gypsum in Mg-Na mixed salt solution system under atmospheric pressure

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