磷石膏转晶制备α型高强石膏工艺条件的优化研究

doi:10.19964/j.issn.1006-4990.2022-0010

Abstract

Abstract:

Based on industrial solid waste phosphogypsum as raw material，α high-strength gypsum was prepared by semi-liquid autoclave method.By taking autoclave temperature，autoclave time，1# crystal conversion agent，2# crystal conversion agent and slurry moisture content as factors，an orthogonal test of 5 factors and 4 levels was carried out.By taking the mechanical properties as an index，the process conditions for the preparation of α high-strength gypsum by crystal conversion were optimized. The results showed that when the reaction temperature was 137 ℃，the slurry moisture content was 20%（mass fraction），the dosage of 1# crystallizing agent was 0.3%（mass fraction），the dosage of 2# crystallizing agent was 1.27%（mass fraction），and the constant temperature of reaction was 20 min，α high-strength gypsum with 2 h flexural，2 h compressive and dry compressive strengths of 7.0，21.7 and 44.7 MPa could be prepared，respectively.

Key words: phosphogypsum, α high-strength gypsum, crystal conversion

CLC Number:

X781.5

ZENG Ying,YAN Bo,RUAN Yunchun,ZHANG Tao,TIAN Rendao,HU Hong,NIE Dengpan. Study on optimization of technological conditions for preparing α high-strength gypsum from phosphogypsum by crystal conversion[J]. Inorganic Chemicals Industry, 2022, 54(11): 112-117.

Figures/Tables 11

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References 20

1	MA Baoguo, LU Wenda, SU Ying, et al.Synthesis of α-hemihydrate gypsum from cleaner phosphogypsum[J].Journal of Cleaner Production,2018,195: 396-405.
2	陈家伟.工业副产石膏制备α型高强石膏的产业化[J].广州化工,2019,47(10):133-136.
	CHEN Jiawei.Industrialization of production of α high-strength plaster by industrial by-product gypsum[J].Guangzhou Chemical Industry,2019,47(10):133-136.
3	杨敏,钱觉时,王智,等.杂质对磷石膏应用性能的影响[J].材料导报,2007,21(6):104-106.
	YANG Min, QIAN Jueshi, WANG Zhi, et al.Effect of impurities on the working performance of phosphogypsum[J].Materials Review,2007,21(6):104-106.
4	冯金煌.磷石膏及其综合利用的探讨[J].无机盐工业,2001,33(4):34-36.
	FENG Jinhuang.Phosphogypsum and its comprehensive utilizati-on[J].Inorganic Chemicals Industry,2001,33(4):34-36.
5	CAMPOS M P, COSTA L J P, NISTI M B, et al.Phosphogypsum recycling in the building materials industry：Assessment of the radon exhalation rate[J].Journal of Environmental Radioactivity,2017,172: 232-236.
6	段庆奎,董文亮,王惠琴,等. α型超高强石膏（K型石膏）研究与开发[J].非金属矿,2001,24(3):26，7.
	DUAN Qingkui, DONG Wenliang, WANG Huiqin, et al.Research and development of α-type ultra-high-strength gypsum（K-type gypsum）[J].Non-Metallic Mines,2001,24(3):26，7.
7	桂苗苗,丛钢.脱硫石膏蒸压法制α-半水石膏的研究[J].重庆建筑大学学报,2001,23(1):62-65，81.
	GUI Miaomiao, CONG Gang.Study on the α-hemihydrate gypsum made by desulphogypsum through autoclave process[J].Journal of Chongqing Jianzhu University,2001,23(1):62-65，81.
8	杨兆娟,王海晏,向兰.利用水热法对磷石膏进行除杂脱水的工艺探讨[J].青海大学学报：自然科学版,2007,25(2):44-47.
	YANG Zhaojuan, WANG Haiyan, XIANG Lan.Technical study on impurities removal and dehydration of phosphogypsum by hydrothermal method[J].Journal of Qinghai University：Nature Science,2007,25(2):44-47.
9	DUAN Zhengyang, LI Jianxi, LI Tianguo, et al.Influence of crystal modifier on the preparation of α-hemihydrate gypsum from phosphogypsum[J].Construction and Building Materials,2017,133: 323-329.
10	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.
	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.
11	CHEN Jianmin, GAO Jun, YIN Hengbo, et al.Size-controlled preparation of α-calcium sulphate hemihydrate starting from calcium sulphate dihydrate in the presence of modifiers and the dissolution rate in simulated body fluid[J].Materials Science and Engineering：C,2013,33(6):3256-3262.
12	栾扬,赵志曼,李黎山,等.复合转晶剂对磷建筑石膏晶体转晶影响的叠加效应研究[J].硅酸盐通报,2018,37(10):3086-3090.
	LUAN Yang, ZHAO Zhiman, LI Lishan, et al.Superposition effect of composition medium crystal agent on the crystal transformation of phosphogypsum[J].Bulletin of the Chinese Ceramic Society,2018,37(10):3086-3090.
13	MI Yang, CHEN Deyu, HE Yulong, et al.Morphology-controlled preparation of α-calcium sulfate hemihydrate from phosphogypsum by semi-liquid method[J].Crystal Research and Technology,2018,53(1). Doi:10.1002/crat.201700162. doi: 10.1002/crat.201700162
14	LIU Jinfeng, DONG Faqin, TAN Hongbin, et al.Facile preparation of high-strength α-CaSO 4·0.5H2O regulated by maleic acid from phosphogypsum：Experimental and molecular dynamics simulation studies[J].SN Applied Sciences,2020,2(10):1-11.
15	MI Yang, CHEN Deyu, WANG Shuzhou.Utilization of phosphogypsum for the preparation of α-calcium sulfate hemihydrate in chloride-free solution under atmospheric pressure[J].Journal of Chemical Technology & Biotechnology,2018,93(8):2371-2379.
16	陈燕.石膏建筑材料[M].北京：中国建材工业出版社，2003.
17	FU Hailu, GUAN Baohong, JIANG Guangming, et al.Effect of supersaturation on competitive nucleation of CaSO₄ phases in a concentrated CaCl₂ solution[J].Crystal Growth & Design,2012,12(3):1388-1394.
18	董一苇,徐祖顺,杨婷婷,等.化学石膏制备α-半水石膏的研究进展[J].材料导报,2021,35(S2):241-247.
	DONG Yiwei, XU Zushun, YANG Tingting, et al.Research progress on the preparation of α-calcium sulfate hemihydrate from chemical gypsum[J].Materials Reports,2021,35(S2):241-247.
19	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.
20	刘冬梅,张典,彭艳周,等.柠檬酸钠对半水石膏不同晶面结晶习性及力学性能的影响[J].材料导报,2021,35(18):18052-18058.
	LIU Dongmei, ZHANG Dian, PENG Yanzhou, et al.Effect of sodium citrate on crystal habit and mechanical properties of different crystal surfaces of hemihydrate gypsum[J].Materials Reports,2021,35(18):18052-18058.

水平	因素
水平	A 反应温度/ ℃	B 料浆含水率/ %	C 1#转晶剂/ %	D 2#转晶剂/ %	E 恒温时间/ min
1	130	18	0.3	1.07	20
2	137	20	0.4	1.17	30
3	144	22	0.5	1.27	40
4	150	24	0.6	1.37	50

编号	A	B	C	D	E	2 h抗折强度/MPa	2 h抗压强度/MPa	绝干抗折强度/MPa	绝干抗压强度/MPa
L1	1	1	1	1	1	4.9	15.4	10.8	36.1
L2	1	2	2	2	2	1.4	3.5	3.0	6.8
L3	1	3	3	3	3	2.7	8.7	7.0	19.5
L4	1	4	4	4	4	1.0	2.5	4.2	8.5
L5	2	1	2	3	4	5.0	15.8	10.3	34.1
L6	2	2	1	4	3	7.0	21.7	12.3	44.7
L7	2	3	4	1	2	1.4	4.6	5.8	16.3
L8	2	4	3	2	1	2.4	8.4	7.0	26.8
L9	3	1	3	4	2	3.0	9.8	7.9	24.4
L10	3	2	4	3	1	4.8	20.3	10.4	32.4
L11	3	3	1	2	4	1.1	3.7	5.0	17.4
L12	3	4	2	1	3	3.0	10.3	8.4	31.1
L13	4	1	4	2	3	1.5	4.8	5.2	17.9
L14	4	2	3	4	1	2.0	7.3	7.7	22.8
L15	4	3	2	4	1	4.5	17.0	9.1	37.1
L16	4	4	1	3	2	6.3	19.5	10.9	41.3

水平	2 h抗折强度/MPa					2 h抗压强度/MPa
水平	A	B	C	D	E	A	B	C	D	E
K₁	2.500	3.600	4.825	2.825	4.150	7.525	11.450	15.075	9.400	15.275
K₂	3.950	3.800	3.475	1.600	3.025	12.625	13.200	11.650	5.100	9.350
K₃	2.975	2.425	2.525	4.700	3.550	11.025	8.500	8.550	16.075	11.375
K₄	3.575	3.175	2.175	3.875	2.275	12.150	10.175	8.050	12.750	7.325
R	1.450	1.375	2.650	3.100	1.875	5.100	4.700	7.025	10.975	7.950

w（2#转晶剂）/%	实验编号	2 h抗折强度/MPa	2 h抗压强度/MPa	绝干抗折强度/MPa	绝干抗压强度/MPa
1.07	L1	4.9	15.4	10.8	36.1
	L7	1.4	4.6	5.8	16.3
	L12	3.0	10.3	8.4	31.1
	L14	2.0	7.3	7.7	22.8
1.17	L2	1.4	3.5	3.0	6.8
	L8	2.4	8.4	7.0	26.8
	L11 L13	1.1 1.5	3.7 4.8	5.0 5.2	17.4 17.9
1.27	L3	2.7	8.7	7.0	19.5
	L5	5.0	15.8	10.3	34.1
	L10	4.8	20.3	10.4	32.4
	L16	6.3	19.5	10.9	41.3
1.37	L4	1.0	2.5	4.2	8.5
	L6	7.0	21.7	12.3	44.7
	L9	3.0	9.8	7.9	24.4
	L15	4.5	17.0	9.1	37.1

w（1#转晶剂）/%	实验编号	2 h抗折强度/MPa	2 h抗压强度/MPa	绝干抗折强度/MPa	绝干抗压强度/MPa
0.3	L1	4.9	15.4	10.8	36.1
	L6	7.0	21.7	12.3	44.7
	L10	4.8	20.3	10.4	32.4
	L16	6.3	19.5	10.9	41.3
0.4	L5	5.0	15.8	10.3	34.1
	L12	3.0	10.3	8.4	31.1
	L15	4.5	17.0	9.1	37.1
0.5	L3	2.7	8.7	7.0	19.5
	L8	2.4	8.4	7.0	26.8
	L9	3.0	9.8	7.9	24.4
	L14	2.0	7.3	7.7	22.8
0.6	L4	1.0	2.5	4.2	8.5
	L7	1.5	4.6	5.8	16.3
	L11	1.1	3.7	5.0	17.4
	L13	1.5	4.8	5.2	17.9

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Inorganic Acid-Base-Salt Committee of CIESC

Study on optimization of technological conditions for preparing α high-strength gypsum from phosphogypsum by crystal conversion

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