钛石膏综合利用及硫钙分离新工艺研究

doi:10.19964/j.issn.1006-4990.2021-0639

Abstract

Abstract:

In order to solve the problem of comprehensive utilization of titanium gypsum，a mild wet chemical conversion method was put forward.Using low-price ammonium bicarbonate as raw material，titanium gypsum solid waste was converted into high-quality calcium carbonate products，and ammonium sulfate and iron-rich slag were obtained at the same time.The test results showed that under the conditions of mass ratio of titanigypsum to ammonium bicarbonate of 1∶1，reaction temperature of 65 ℃ and reaction time of 1.25 h，the conversion rate of titanigypsum could reach more than 95%.The converted solid calcium carbonate and iron slag were heated and boiled with NH₄Cl to recover ammonium carbonate，and the solid-liquid separation after the reaction was completed.Further reaction of the recovered ammonium carbonate with the separation liquid could obtain calcium carbonate with purity of more than 98% and iron slag with iron content of more than 61%.

Key words: titanium gypsum, titanium dioxide, ammonium bicarbonate, calcium sulfate, calcium carbonate, iron slag

CLC Number:

TQ132.32

MA Lei,SHENG Yu,ZHOU Junhong,YANG Yujun,LUO Hui,PAN Chunying,WANG Guo. Study on new process of comprehensive utilization and separation of sulfur and calcium of titanium gypsum[J]. Inorganic Chemicals Industry, 2022, 54(7): 124-128.

Figures/Tables 14

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References 9

1	石鑫，杨绍利，马兰.“三石膏”综合利用现状及其新工艺［J］.现代化工，2020，40（9）：8-13，19.
	SHI Xin， YANG Shaoli， MA Lan.Present situation of comprehensive utilization of“three-gypsum”and new technologies［J］.Modern Chemical Industry，2020，40（9）：8-13，19.
2	朱静平，张婷婷，刘洪，等.钛石膏制备片状钙白粉的生产工艺研究［J］.非金属矿，2019，42（4）：51-52，76.
	ZHU Jingping， ZHANG Tingting， LIU Hong，et al.Technical study on the preparation of flaky calcium white powder from titanium gypsum［J］.Non-Metallic Mines，2019，42（4）：51-52，76.
3	谭纪林.钛石膏作缓凝剂在水泥生产中的应用［J］.水泥，2017（2）：20-23.
	TAN Jilin.Application of titanium gypsum as retarder in cement production［J］.Cement，2017（2）：20-23.
4	张璐，吕广忠.金属矿山充填采矿法中充填材料的应用及展望［J］.现代矿业，2010，26（1）：20-22.
	ZHANG Lu， LV Guangzhong.The application and prospect of filling material in metal mine filling mining methods［J］.Modern Mining，2010，26（1）：20-22.
5	危流永，郑伯坤.红石膏胶结充填技术［J］.矿业研究与开发，2014，34（5）：16-18.
	WEI Liuyong， ZHENG Bokun.Cemented filling technology of gypsum rubrum［J］.Mining Research and Development，2014，34（5）：16-18.
6	孙家瑛，郑京彪，周震雷.钛石膏-粉煤灰复合制备路基回填材料试验研究［J］.公路，2001，46（6）：107-110.
	SUN Jiaying， ZHENG Jingbiao， ZHOU Zhenlei.Study on composite for backfill material made by waste gypsum from TiO₂ production and fly ash［J］.Highway，2001，46（6）：107-110.
7	王晓琪，姚媛媛，陈宝成，等.硫酸法钛石膏作为土壤调理剂在油菜上的施用效果研究［J］.水土保持学报，2018，32（4）：333-338，345.
	WANG Xiaoqi， YAO Yuanyuan， CHEN Baocheng，et al.Effects of titanium gypsum produced by sulfuric acid method as soil conditioner on rape seedlings［J］.Journal of Soil and Water Conservation，2018，32（4）：333-338，345.
8	高强，鲍树涛.大型钛石膏制硫酸联产水泥的应用实践［J］.硫酸工业，2019（2）：11-16，19.
	GAO Qiang， BAO Shutao.Application practice of co-production of sulphuric acid and cement with large titanium gypsum［J］.Sulphuric Acid Industry，2019（2）：11-16，19.
9	刘凤铃，彭佥赟，刘洪.钛石膏制备CaSO₄晶须［J］.化工设计通讯，2018，44（1）：70-72.
	LIU Fengling， PENG Qianyun， LIU Hong.Preparation of CaSO₄ whiskers by titanium［J］.Chemical Engineering Design Communications，2018，44（1）：70-72.

w（Al₂O₃）	w（SiO₂）	w（K₂O）	w（Fe₂O₃）	w（TiO₂）
1.1	3.27	0.21	11.44	3.36
w（MnO）	w（P₂O₅）	w（CaO）	w（SO₃）	w（CO₂）
0.29	0.03	34.49	38.16	6.54

序号	反应时间/h	产物质量/g	产物w（SO₃）/%	转化率/%
1	0.50	13.48	2.11	92.02
2	1.00	13.48	1.14	95.69
3	1.25	13.74	1.28	95.16
4	2.00	13.47	1.43	94.59
5	2.50	13.56	1.71	93.53

序号	碳酸氢铵实际用量/g	碳酸氢铵过剩率/%	产物质量/g	产物 w（SO₃）/%	转化率/ %
1	27.50	103.70	13.74	1.18	95.16
2	20.60	52.59	13.55	1.55	93.74
3	13.75	1.85	13.32	1.66	93.31
4	6.88	-49.00	14.28	13.71	47.07
5	0.00	-100.00	15.06	25.99	0.00

序号	反应温度/ ℃	产物质量/ g	产物硫组分含量w（SO₃）/%	转化率/ %
1	27	12.92	2.27	94.05
2	45	12.74	1.46	96.18
3	65	13.16	1.85	95.16
4	85	13.34	7.34	80.74
5	95	15.13	27.16	28.83

序号	转化时间/h	反应后滤渣量/g	产物量/g	转化率/%
1	1.0	10.13	3.54	35.86
2	2.5	7.63	5.76	58.33
3	3.0	6.09	7.21	73.01
4	3.5	5.47	7.69	77.88
5	4.0	3.90	9.03	91.45
6	5.0	4.01	9.41	95.36

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Study on new process of comprehensive utilization and separation of sulfur and calcium of titanium gypsum

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序号	转化温度/℃	是否鼓入空气	产物量/g	转化率/%
1	55	鼓入	1.09	13.23
2	65	鼓入	1.35	16.39
3	75	鼓入	2.48	30.12
4	85	鼓入	3.83	46.51
5	85	否	0.56	6.80

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