硫酸法钛白废酸浓缩工艺研究

王海波; 孙科

doi:10.7513/j.issn.1004-7638.2023.05.018

硫酸法钛白废酸浓缩工艺研究

doi: 10.7513/j.issn.1004-7638.2023.05.018

王海波,
孙科

钒钛资源综合利用国家重点实验室, 四川攀枝花 617000

详细信息

中图分类号: TQ111,X758
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出版历程
- 收稿日期: 2023-06-29
- 网络出版日期: 2023-11-04
- 刊出日期: 2023-10-31

Study on concentration process of titanium white waste acid by sulfuric acid method

Wang Haibo,
Sun Ke

State Key Laboratory of Vanadium and Titanium Resources Comprehensive Utilization, Panzhihua 617000, Sichuan, China

摘要

摘要: 为了提升废酸浓缩效率，以现场废酸为原料，在实验室采用真空旋转蒸发仪模拟现场废酸真空蒸发浓缩，开展废酸浓缩工艺单因素试验及正交试验，然后以实验室研究结果为依据，在现场开展了废酸浓缩工艺优化工业试验。结果表明，在相同的硫酸浓度条件下，废酸相对纯硫酸密度大，且随着硫酸浓度的增加，两者密度差逐渐减少；随着废酸浓缩时间、浓缩温度及浓缩真空度的增加，废酸浓缩浓度均逐渐增加，影响废酸浓缩浓度的关键影响因素为浓缩时间、浓缩真空度、浓缩时间×浓缩真空度、浓缩温度，重要度排序为浓缩时间＞浓缩真空度＞浓缩真空度×浓缩时间＞浓缩温度。工业试验结果表明，当废酸浓缩时间、浓缩温度及浓缩真空度分别由2.06 h、108 ℃及30 kPa提升至2.68 h、112 ℃及45 kPa时，一级浓缩酸浓度均值由29.5%提升至38.5%。研究结果为硫酸法钛白生产企业提升废酸浓缩效率提供了重要的数据及理论支撑。
- 硫酸法钛白 /
- 废酸 /
- 蒸发浓缩 /
- 硫酸浓度
Abstract: In order to improve the efficiency of waste acid concentration, the single factor test and orthogonal test of waste acid concentration process were carried out in the laboratory by using vacuum rotary evaporator to simulate the vacuum evaporation concentration of waste acid. Then, based on the results of laboratory research, the industrial test of waste acid concentration process optimization was carried out in the field. The results show that the density of waste acid is larger than that of pure sulfuric acid under the same sulfuric acid concentration, and the density difference between them decreases with the increase of sulfuric acid concentration. With the increase of concentration time, temperature and vacuum degree of waste acid, the concentration of waste acid increases gradually. The key influencing factors affecting the concentration of waste acid are concentration time, concentration vacuum degree, concentration time ×concentration vacuum degree and concentration temperature. The order of importance is concentration time > concentration vacuum degree > concentration vacuum degree × concentration time > concentration temperature. The industrial test results show that when the concentration time, concentration temperature and concentration vacuum degree of waste acid increase from 2.06 h, 108 °C and 30 kPa to 2.68 h, 112 °C and 45 kPa, respectively, the average concentration of primary concentrated acid increases from 29.5% to 38.5%. The research results provide important data and theoretical support for improving the concentration efficiency of waste acid in titanium dioxide production enterprises by sulfuric acid method.
- sulfate process titanium dioxide /
- waste acid /
- evaporator concentration process /
- sulfuric acid concentration

HTML全文

图 1 废酸及硫酸的浓度与密度对应关系

Figure 1. Relationship between density, concentration of waste acid and sulfuric acid

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图 2 废酸浓度、沸点及真空度之间关系

Figure 2. Relationship between the concentration of waste acid, boiling point and the vacuum degree

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图 3 废酸浓缩时间对废酸浓缩效率的影响

Figure 3. Effect of concentration time on concentration effect of waste acid

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图 4 废酸浓缩真空度对废酸浓缩效率的影响

Figure 4. Effect of vacuum degree on concentration effect of waste acid

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图 5 废酸浓缩温度对废酸浓缩效率的影响

Figure 5. Effect of concentration temperature of waste acid on concentration effect of waste acid

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图 6 废酸浓缩正交试验帕累托图

Figure 6. Pareto diagram of orthogonal test of waste acid concentration

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表 1 废酸主要化学成分

Table 1. Main chemical components of waste acid g/L

H₂SO₄	CaSO₄	FeSO₄	TiOSO₄	MgSO₄	MnSO₄	Al₂(SO₄)₃	H₂SiO₃
245.00	1.26	126.29	10.76	6.36	0.64	9.99	1.64

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表 2 废酸浓缩工艺正交试验设计及结果

Table 2. Orthogonal experimental design and results of waste acid concentration process

标准序	运行序	中心点	区组	温度/ ℃	负压/kPa	时间/min	酸浓度/%
9	1	0	1	108	52.5	20	30.79
1	2	1	1	103	40	10	24.25
8	3	1	1	113	65	30	53.32
5	4	1	1	103	40	30	26.63
6	5	1	1	113	40	30	32.78
2	6	1	1	113	40	10	25.42
7	7	1	1	103	65	30	40.58
4	8	1	1	113	65	10	29.33
10	9	0	1	108	52.5	20	31.09
3	10	1	1	103	65	10	26.7

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表 3 工业试验结果

Table 3. Industrial test results

	No.	t/h	T/℃	P/kPa	一级酸浓度/%
	No.	t/h	T/℃	P/kPa	测试值	平均
优化前	1-1	2.06	108	30	29.0	29.5
	1-2				30.2
	1-3				29.4
优化后	2-1	2.68	112	45	37.8	38.5
	2-2				39.2
	2-3				38.6

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参考文献(13)

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