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

无机盐工业 ›› 2023, Vol. 55 ›› Issue (12): 74-81.doi: 10.19964/j.issn.1006-4990.2023-0047

• 研究与开发 • 上一篇    下一篇

氢氧化镁与七水硫酸镁水热法合成碱式硫酸镁晶须

蒋德敏1(), 李顺梅1, 李青青1, 陈雨欣1, 刘代俊2   

  1. 1.重庆三峡学院三峡库区水环境演变与污染防治重庆高校市级重点实验室, 重庆 404100
    2.四川大学化学工程学院, 四川成都 6100653
  • 收稿日期:2023-02-01 出版日期:2023-12-10 发布日期:2023-12-14
  • 作者简介:蒋德敏(1987— ),男,硕士,实验师,主要从事无机材料的制备及其在环境中的应用研究;E-mail:jdmhuagong@163.com
  • 基金资助:
    重庆市教委科技项目(KJQN201901208);重庆三峡学院青年项目(19QN04);重点实验室开放项目(WEPKL2019YB07)

Hydrothermal synthesis of basic magnesium sulfate whiskers from magnesium hydroxide and magnesium sulfate heptahydrate

JIANG Demin1(), LI Shunmei1, Li Qingqing1, Chen Yuxin1, LIU Daijun2   

  1. 1. Key Laboratory of Water Environment Evolution and Pollution Control in Three Gorges Reservoir,Chongqing Three Gorges University,Chongqing 404100,China
    2. School of Chemical Engineering,Sichuan University,Chengdu 6100653,China
  • Received:2023-02-01 Published:2023-12-10 Online:2023-12-14

摘要:

为了获得高品质的碱式硫酸镁晶须,采用氢氧化镁和七水硫酸镁为原料,通过水热法合成碱式硫酸镁晶须。考察了七水硫酸镁与氢氧化镁的物质的量比、水热时间、搅拌转速、七水硫酸镁的添加量及水热温度等条件因素对晶须生长的影响,利用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、选区电子衍射(SAED)及傅里叶红外光谱(FT-IR)等对晶须产品进行了分析。结果表明:优化的工艺参数为七水硫酸镁与氢氧化镁物质的量比为3∶1、水热时间为2 h、搅拌转速为400 r/min、七水硫酸镁添加量为4.93 g、水热温度为180 ℃、80 mL水作为反应介质;在优化条件下合成的产品主要为纤维状晶须,晶须的直径为300~500 nm、长度为80~100 µm,其长径比大于160。工艺参数的优化可有效提高碱式硫酸镁晶须的分散性和长径比。

关键词: 碱式硫酸镁晶须, 水热法, 形貌, 氢氧化镁, 七水硫酸镁

Abstract:

To obtain the high-quality basic magnesium sulfate whiskers,magnesium hydroxide and magnesium sulfate heptahydrate were used to prepare basic magnesium sulfate whiskers with the hydrothermal method.The influences of hydrothermal parameters on whisker morphology were investigated,which included the molar ratio of magnesium sulfate heptahydrate to magnesium hydroxide,hydrothermal time,stirring speed,addition amount of magnesium sulfate heptahydrate,and hydrothermal temperature.The whisker products were characterized by the various instruments of X-ray diffractometry(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),selected area electron diffraction(SAED),and Fourier-transform infrared spectrum(FT-IR).The results showed that the optimized process parameters were as following:the molar ratio of magnesium sulfate heptahydrate to magnesium hydroxide was 3∶1,hydrothermal time was 2 h,stirring speed was 400 r/min,addition amount of magnesium sulfate heptahydrate was 4.93 g,hydrothermal temperature was 180 ℃ and the reaction medium of water was 80 mL.The products synthesized at the optimized conditions were mainly fibrous whiskers.The aspect ratio of fibrous whisker was more than 160 with the diameter of 300~500 nm and the length of 80~100 µm.Therefore,the optimization of the process parameters could effectively improve the dispersion and aspect ratio of basic magnesium sulfate whiskers.

Key words: basic magnesium sulfate whisker, hydrothermal method, morphology, magnesium hydroxide, magnesium sulfate heptahydrate

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