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过程工程学报 ›› 2022, Vol. 22 ›› Issue (4): 478-486.DOI: 10.12034/j.issn.1009-606X.221133CSTR: 32067.14.jproeng.221133

• 研究论文 • 上一篇    下一篇

磷化渣废液除锌制备高纯度磷酸三钠

曾璐婵1,2， 李雲1,2*， 郭宏飞1,2*， 张金凤3， 曹吉林1,2   

  1. 1. 河北工业大学化工学院，天津 300130 2. 河北省绿色化工与高效节能重点实验室，天津 300130 3. 天津市生态环境科学研究院，天津 300384
  • 收稿日期:2021-04-21 修回日期:2021-05-22 出版日期:2022-04-28 发布日期:2022-04-24
  • 通讯作者: 李雲 liyun@hebut.edu.cn
  • 作者简介:曾璐婵(1996-)，女，河北省河间市人，硕士研究生，化学工程专业，E-mail: 2539981781@qq.com；通讯联系人，李雲，E-mail: liyun@hebut.edu.cn；郭宏飞，E-mail: guohongfei@hebut.edu.cn.
  • 基金资助:
    孔道疏水的Al-beta沸石固体酸催化剂制备及其高效催化乳酸合成丙交酯

Preparation of high-purity trisodium phosphate from the phosphating slag waste liquid after the removal of zinc

Luchan ZENG1,2,  Yun LI1,2*,  Hongfei GUO1,2*,  Jinfeng ZHANG3,  Jilin CAO1,2   

  1. 1. College of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China 2. Hebei Provincial Key Laboratory of Green Chemical Technology and High Efficient Energy Saving, Tianjin 300130, China 3. Tianjin Academy of Eco-Environmental Sciences, Tianjin 300384, China
  • Received:2021-04-21 Revised:2021-05-22 Online:2022-04-28 Published:2022-04-24

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摘要： 为了实现磷化渣碱溶后所得废液的综合利用，采用中和沉淀法和硫化钠沉淀法去除磷化渣废液中的杂质锌，对中和沉淀法和硫化钠沉淀法的工艺条件进行优化，并由此设计磷化渣废液除锌制备高纯度磷酸三钠的生产工艺。对于中和沉淀法，在反应体系pH=8.85，反应时间为10 min时，Zn2+去除率可达97.96%；对于硫化钠沉淀法，在反应体系pH=6.85，硫化钠投加量与Zn2+的摩尔比为1:1，反应时间为10 min时，Zn2+去除率可达99.80%。相比于中和沉淀法除锌制备磷酸三钠工艺，硫化钠沉淀法除锌制备磷酸三钠工艺具有更高的磷酸三钠纯度，为98.85%，固相产品中Zn2+含量更低，仅为0.0004%，符合化工行业分析纯标准。该工艺大幅度地回收了磷化渣废液中的PO43-离子和Na+离子，为实现磷化渣综合利用的工业化提供新思路。

关键词: 磷化渣废液, 资源化利用, 除锌, 中和沉淀法, 硫化钠沉淀法, 磷酸三钠

Abstract: Phosphating slag is the hazardous waste produced during the phosphating process, which has an adverse effect on the quality of phosphating coating and phosphating cost. It is an effective method to utilize phosphating slag by extracting iron and zinc ions from phosphating slag via alkali dissolution; however, the treatment of liquid waste of residual phosphating slag is a challenge topic. In this work, the neutralization and sodium sulfide precipitation methods were used to remove the zinc from the phosphating slag waste liquid. The corresponding process conditions were optimized. And the production processes of highly purified trisodium phosphate from phosphating slag waste liquid after zinc removal were designed respectively. The removal rate of Zn2+ could reach 97.96% via neutralization precipitation method under the pH of the reaction system of 8.85, and the reaction time of 10 min, while the removal rate of Zn2+ could reach 99.80% via the sodium sulfide precipitation method under the pH of the reaction system of 6.85, the molar ratio of sodium sulfide to Zn2+ of 1:1, and the reaction time of 10 min. After adjusting the pH of the treated waste liquid to 12.30±0.03 by using 10 mol/L of NaOH solution, the phosphate anions and sodium ions were recovered by cooling and crystallization at 5℃ to produce the trisodium phosphate. The trisodium phosphate produced from waste liquid after zinc removal by neutralization precipitation method possessed the purity of 97.72% and Zn2+ content of 0.0014%, which is in line with the chemical industry standard of chemical purity. Compared with the production process of trisodium phosphate after zinc removal by using neutralization precipitation method, that using sodium sulfide precipitation method exhibited higher purity of trisodium phosphate with the value of 98.85%, and lower Zn2+ content in trisodium phosphate with the value of 0.0004%, which met the analytical purity standard of the chemical industry. The process is capable of efficiently recovering the PO43- and Na+ ions from the phosphating slag waste liquid, thereby paving a new avenue for the comprehensive utilization of phosphating slag in industry.

Key words: Phosphating slag waste liquid, Resource utilization, Removal of zinc, Neutralization precipitation method, Sodium sulfide precipitation method, Trisodium phosphate