无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ
研究与开发

聚磷酸镁铵的制备工艺研究

  • 许淼 ,
  • 许德华 ,
  • 首志欣 ,
  • 杨文贡 ,
  • 王辛龙
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  • 四川大学化学工程学院教育部磷资源综合利用与清洁加工工程研究中心,四川 成都 610065
许淼(1999— ),男,硕士,研究方向为磷化工;E-mail:scuxumiao@gmail.com
许德华(1987— ),男,副研究员,研究方向为磷化工;E-mail:dhxu@scu.edu.cn

收稿日期: 2024-01-30

  网络出版日期: 2024-03-26

基金资助

国家重点研发计划课题项目(2022YFC2904704);四川省重点研发项目(2023YFS0353)

Study on preparation process of magnesium ammonium polyphosphate

  • XU Miao ,
  • XU Dehua ,
  • SHOU Zhixin ,
  • YANG Wengong ,
  • WANG Xinlong
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  • Ministry of Education Research Center for Comprehensive Utilization and Clean Processing Engineering of Phosphorus Resources,School of Chemical Engineering,Sichuan University,Chengdu 610065,China

Received date: 2024-01-30

  Online published: 2024-03-26

摘要

针对磷酸铁锂前驱体磷酸铁生产过程中副产物磷酸镁铵难以利用的问题,提出了一种通过焙烧制备含钙镁等中微量元素磷肥(聚磷酸镁铵)的新思路,在焙烧温度为250~550 ℃、焙烧时间为0.5~3.0 h的条件下,开展了磷酸镁铵制备聚磷酸镁铵的工艺及机理研究,并通过热重-傅里叶红外(TG-IR)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)、氮气物理吸附仪、激光粒度仪对样品的晶型、焙烧过程中的样品质量变化及气相产物、形貌、比表面积和孔隙率及颗粒粒径分布进行了表征,揭示了反应过程机理。实验结果表明,在一定范围内,提高焙烧温度和延长焙烧时间都能促进磷酸盐的聚合及提高脱氮率,基于产物中磷形态分布和脱氮率等指标得出焙烧的优选焙烧温度为350 ℃、焙烧时间为2 h时,在此条件下所得聚磷酸镁铵中磷的聚合度分布为1~3,聚合率达到45.28%,脱氮率达到79.90%。得到的聚磷酸镁铵相比原样磷酸镁铵,有效钙、有效镁及水溶磷和有效磷等养分指标均有30%以上的提升,可作为一种新型的含钙镁等中微量元素的磷肥。

本文引用格式

许淼 , 许德华 , 首志欣 , 杨文贡 , 王辛龙 . 聚磷酸镁铵的制备工艺研究[J]. 无机盐工业, 2024 , 56(12) : 88 -93 . DOI: 10.19964/j.issn.1006-4990.2024-0065

Abstract

A new approach was proposed to prepare phosphate fertilizers(magnesium ammonium polyphosphate) containing trace elements such as calcium and magnesium through calcination,in response to the problem of difficult utilization of by-product magnesium ammonium phosphate in the production process of lithium iron phosphate(precursor of iron phosphate).The process and mechanism of preparing magnesium ammonium polyphosphate from magnesium ammonium phosphate were studied under the conditions of calcination temperature of 250~550 ℃ and calcination time of 0.5~3.0 h.The crystal structure,sample quality change during calcination,gas phase products,morphology,specific surface area,porosity,and particle size of the samples were analyzed by thermogravimetric Fourier transform infrared(TG-IR),X-ray diffraction(XRD),scanning electron microscopy(SEM),nitrogen physical adsorption analyzer,and laser particle size analyzer.The diameter distribution was characterized,revealing the mechanism of the reaction process.The experimental results showed that within a certain range,increasing the calcination temperature and prolonging the calcination time could promote the polymerization of phosphate and improve the denitrification rate.Based on the distribution of phosphorus forms and denitrification rate in the product,the optimal calcination temperature was 350 ℃ and the calcination time was 2 h.Under these conditions,the polymerization degree distribution of phosphorus in magnesium ammonium polyphosphate obtained was 1~3,the polymerization rate reached 45.28%,and the denitrification rate reached 79.90%.The obtained magnesium ammonium polyphosphate showed an improvement of over 30% in nutrient indicators such as available calcium,available magnesium,water-soluble phosphorus,and available phosphorus compared to the original magnesium ammonium phosphate.It could be used as a new type of phosphorus fertilizer containing trace elements such as calcium and magnesium.

参考文献

[1] 况新亮,刘垂祥,熊朋.锂离子电池产业分析及市场展望[J].无机盐工业202254(8):12-19,32.
  KUANG Xinliang, LIU Chuixiang, XIONG Peng.Industry analysis and market prospect of lithium ion battery[J].Inorganic Chemicals Industry202254(8):12-19,32.
[2] 王紫涵,李军,陈明,等.硝酸铁和磷酸共沉淀法制备电池级磷酸铁工艺研究[J].无机盐工业202355(7):51-57.
  WANG Zihan, LI Jun, CHEN Ming,et al.Study on preparation of battery grade ferric phosphate by co-precipitation of ferric nitrate and phosphoric acid[J].Inorganic Chemicals Industry202355(7):51-57.
[3] 王君婷,马航,查坐统,等.磷酸铁工业废水处理工艺研究进展[J].无机盐工业202456(6):26-33.
  WANG Junting, MA Hang, ZHA Zuotong,et al.Research progress of iron phosphate industrial wastewater treatment process[J].Inorganic Chemicals Industry202456(6):26-33.
[4] 王维,李伟,李立敏,等.磷酸铁生产废水回用及零排放的预处理研究[J].无机盐工业202456(8):99-103.
  WANG Wei, LI Wei, LI Limin,et al.Study on pretreatment of iron phosphate production wastewater reuse and zero discharge[J].Inorganic Chemicals Industry202456(8):99-103.
[5] 吴航,张丽芳,白威,等.聚合温度对聚磷酸钙聚合度及结构的影响[J].无机材料学报201227(2):174-178.
  WU Hang, ZHANG Lifang, BAI Wei,et al.Effect of polymerization temperature on polymerization degree and structure of calcium polyphosphate[J].Journal of Inorganic Materials201227(2):174-178.
[6] 赵蕾蕾,舒艺周,漆增连,等.不同APP添加量对复合肥料造粒性能的影响[J].无机盐工业202456(8):74-82.
  ZHAO Leilei, SHU Yizhou, QI Zenglian,et al.Effect of different APP addition on granulation performance of compound fertilizer[J].Inorganic Chemicals Industry202456(8):74-82.
[7] 袁太艳,严正娟,黄成东,等.聚磷酸铵在紫色土壤中的吸附-解吸特征[J].浙江农业学报202335(2):403-416.
  YUAN Taiyan, YAN Zhengjuan, HUANG Chengdong,et al.Adsorption-desorption characteristics of ammonium polyphosphate in purple soils[J].Acta Agriculturae Zhejiangensis202335(2):403-416.
[8] 苗林平,许淼,王辛龙,等.聚磷酸钙镁的制备研究[J].无机盐工业202254(9):63-68.
  MIAO Linping, XU Miao, WANG Xinlong,et al.Study on preparation of calcium magnesium polyphosphate[J].Inorganic Chemicals Industry202254(9):63-68.
[9] 刘续,汤建伟,刘咏,等.水溶性农用聚磷酸铵的研究与应用进展[J].无机盐工业202052(12):7-11.
  LIU Xu, TANG Jianwei, LIU Yong,et al.Research and application progress of water-soluble agricultural ammonium polyphosphate[J].Inorganic Chemicals Industry202052(12):7-11.
[10] YANG Jingxu, XIE Wenji, KONG Xingjian,et al.Reactive extrusion of ammonium polyphosphate in a twin-screw extruder:Polydispersity improvement[J].Chemical Engineering and Processing-Process Intensification2018133:58-65.
[11] XIE Wenji, WANG Xinlong, LI Yongsheng,et al.Simultaneous determination of various phosphates in water-soluble ammonium polyphosphate[J].Chromatographia201982(11):1687-1695.
[12] 王娇,杜昌文,申亚珍,等.中红外光声光谱法测定土壤顶空氨气浓度[J].土壤201446(6):1017-1023.
  WANG Jiao, DU Changwen, SHEN Yazhen,et al.Measurement of ammonia in soil headspace by mid-infrared photoacoustic spectroscopy[J].Soils201446(6):1017-1023.
[13] 曾庆玲,王露,沈春花,等.鸟粪石循环利用处理高氨氮废水的热解行为[J].环境工程学报20137(7):2541-2546.
  ZENG Qingling, WANG Lu, SHEN Chunhua,et al.Thermal decomposition behavior of struvite in recycling treatment of high ammonia-nitrogen wastewater[J].Chinese Journal of Environmental Engineering20137(7):2541-2546.
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