无水硫酸钙晶须的制备及表征

doi:10.19964/j.issn.1006-4990.2021-0761

Abstract

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

CLC Number:

TQ132.32

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

Figures/Tables 11

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名称	质量浓度/（g·L^-1）	名称	质量浓度/（g·L^-1）
SO₄^2-	43.2	K₂O	0.043
MgO	8.15	CaO	0.77
Al₂O₃	＜0.001	Na₂O	0.13
REO	＜0.01	Cl^-	1.23
Fe₂O₃	0.001 4

实验序号	A 反应时间/h	B 反应温度/℃	C 陈化时间/h	长径比
1	4	120	3.0	27.30
2	4	130	3.5	9.30
3	4	140	4.0	18.20
4	4	150	4.5	4.97
5	5	120	3.5	9.44
6	5	130	3.0	16.62
7	5	140	4.5	30.55
8	5	150	4.0	4.03
9	6	120	4.0	6.85
10	6	130	4.5	19.34
11	6	140	3.0	15.65
12	6	150	3.5	8.87
13	7	120	4.5	8.70
14	7	130	4.0	12.43
15	7	140	3.5	12.33
16	7	150	3.0	9.12

因素	A 反应时间/h	B 反应温度/℃	C 陈化时间/h
K1	59.77	52.29	68.69
K2	60.64	57.69	39.94
K3	50.71	76.73	41.51
K4	42.58	26.99	63.56
k1	14.94	13.07	17.17
k2	15.16	14.42	9.98
k3	12.68	19.18	10.38
k4	10.65	6.75	15.89
极差范围	4.52	12.44	7.19
主次因素		B>C>A
最优水平	A₂	B₃	C₁
最优条件		A₂B₃C₁

序号	偏差平方和	自由度	方差
A	705.03	3	235.01
B	1 371.90	3	457.30
C	1 144.00	3	381.30

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Preparation and characterization of anhydrous calcium sulfate whisker

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