造纸污泥焙烧改性-浸出回收二氧化钛的研究

doi:10.16552/j.cnki.issn1001-1625.2025.0442

摘要/Abstract

摘要： 本文以含钛造纸污泥为原料,采用碳酸钠混合焙烧-两段酸浸-氟化氢铵(NH₄HF₂)浸出的联合工艺回收二氧化钛(TiO₂)。系统考察了焙烧温度、Na₂CO₃与造纸污泥的质量比、H₂SO₄浓度、NH₄HF₂浓度等关键参数对TiO₂回收率及纯度的影响。结果表明,在焙烧温度为850 ℃、Na₂CO₃与造纸污泥质量比为0.7∶1.0、焙烧时间为120 min的条件下,经过初次酸浸(酸浸温度为70 ℃、H₂SO₄浓度为3.0 mol/L、液固比为5∶1、酸浸时间为60 min)、二次酸浸(酸浸温度为50 ℃、H₂SO₄浓度为1.5 mol/L、液固比为5∶1、酸浸时间为60 min)及NH₄HF₂浸出(NH₄HF₂浓度为90 g/L、液固比为5∶1、浸出时间为60 min、浸出温度为60 ℃)后,TiO₂回收效果最好,回收率达81.20%、纯度为94.85%。该工艺通过碳酸钠高温焙烧破坏钛氧复合化合物及硅酸盐物相结构,结合酸浸与氟化氢铵浸出,实现了钛的高效分离,为含钛造纸污泥的资源化利用提供理论参考。

关键词: 含钛造纸污泥, TiO₂, 回收率, 纯度, 焙烧, 浸出

Abstract: In this paper, titanium-containing paper sludge was utilized as the raw material for the recovery of titanium dioxide (TiO₂) through a combined process of sodium carbonate mixed roasting-two stage acid leaching-ammonium hydrogen fluoride (NH₄HF₂) leaching. The effects of key parameters such as roasting temperature, mass ratio of Na₂CO₃ to paper sludge, H₂SO₄ concentration and NH₄HF₂ concentration on the recovery rate and purity of TiO₂ were systematically investigated. The results show that under the roasting temperature of 850 ℃, mass ratio of Na₂CO₃ to paper sludge of 0.7∶1.0 and roasting time of 120 min, the optimal recovery effect of TiO₂ is achieved through a first acid leaching (acid leaching temperature is 70 ℃, H₂SO₄ concentration is 3.0 mol/L, liquid-to-solid ratio is 5∶1, acid leaching time is 60 min), second acid leaching (acid leaching temperature is 50 ℃, H₂SO₄ concentration is 1.5 mol/L, liquid-to-solid ratio is 5∶1, acid leaching time is 60 min), and NH₄HF₂ leaching (NH₄HF₂ concentration is 90 g/L, liquid-to-solid ratio is 5∶1, leaching time is 60 min, leaching temperature is 60 ℃). Under these conditions, the TiO₂ recovery rate is 81.20%, and the purity is 94.85%. The process destroys the phase structure of titanium-oxygen compounds and silicates by high-temperature roasting of sodium carbonate. Combined with acid leaching and NH₄HF₂ leaching, the efficient separation of titanium is realized, which provides a theoretical reference for the resource utilization of titanium-containing paper sludge.

Key words: titanium-containing paper sludge, TiO₂, recovery rate, purity, roasting, leaching

中图分类号:

TQ134.1⁺1

李娜, 丁希楼, 贾勇, 孟冠华. 造纸污泥焙烧改性-浸出回收二氧化钛的研究[J]. 硅酸盐通报, 2025, 44(12): 4436-4447.

LI Na, DING Xilou, JIA Yong, MENG Guanhua. Roasting Modification-Leaching Recovery of TiO₂ from Paper Sludge[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2025, 44(12): 4436-4447.

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