直接沉淀法制备氢氧化镁晶须的研究
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摘要
我国拥有丰富的镁盐矿物,以及盐湖镁资源和海水镁资源,并且镁资源种类齐全、分布广泛。本文利用我国丰富的镁资源,提取氯化镁溶液,通过添加沉淀剂和助剂采用直接沉淀法制备出氢氧化镁晶须。我国长期使用溴化阻燃剂以及其他一些有机阻燃剂,其发烟量与毒性都较大,对环境造成二次污染,已被限制使用。氢氧化镁晶须用作阻燃剂具有无毒无烟无污染的特性,氢氧化镁晶须用作材料填充剂具有较好的分散性和相容性,提高复合材料的刚度、强度等。因此,氢氧化镁晶须的制备在镁资源利用、环境保护以及功能材料开发方面具有重大意义。
以氯化镁和碱液为原料采用直接沉淀法制备氢氧化镁晶须,其制备过程主要分为四个阶段,即沉淀反应、晶化反应、洗涤过程和干燥过程。对氢氧化镁在制备过程中不同工艺条件进行研究,包括沉淀剂的选择、溶剂的选择、洗涤剂的选择以及干燥温度和干燥时间的选择,原料配比的选择；对制备氢氧化镁晶须的助剂进行优选,包括单助剂、复配助剂和外离子助剂。研究结果显示,采用直接沉淀法制备氢氧化镁晶须,以氢氧化钠为沉淀剂,乙醇／水(1：1)为溶剂,MgCl2与NaOH反应配比为1：2,选择硬脂酸锌或氯化铁为助剂,使用水+乙醇进行洗涤,在真空度为0.08Mpa、温度为100℃下干燥3h。制备出了粒度均一、晶型完整的氢氧化镁晶须。
以硬脂酸锌或氯化铁为助剂制备氢氧化镁晶须,对其液相反应阶段的工艺条件进行研究,研究结果表明,以硬脂酸锌为助剂制备氢氧化镁晶须的工艺条件为：沉淀温度40℃、晶化温度90℃、晶化时间2h；以氯化铁为外离子制备氢氧化镁晶须的工艺条件为：沉淀时间40min、沉淀温度50℃、外加离子量0.4mol%。产品的SEM图中颗粒边界分明,无团聚现象,晶须的长径比约为10.7。XRD图中(101)面衍射强度增加,说明添加上述助剂后,氢氧化镁晶须在生长过程中具有择优取向性。
对氢氧化镁晶须的生长机理进行探讨,从晶体成核以及晶体的生长速率对氢氧化镁晶须的生长动力学进行分析,证明晶须的生长符合经典的晶体生长理论；外离子的加入使晶体在生长过程中能够择优生长,对氢氧化镁晶须的形成起到导晶的作用；氢氧化镁晶须的生长是以Mg(OH)6~4负离子配位八面体为生长基元进行生长的,利用负离子配位多面体生长基元理论可以合理解释氢氧化镁晶须的生长和生成。
China has rich minerals of magnesium, as well as the salt lake magnesium resources and seawater magnesium resources, the magnesium is full of variety and wide of distribution. We extract magnesium chloride from China's affluet magnesium,and magnesium hydroxide whisker was prepared to add a precipitator and auxiliaries by direct precipitation method. Magnesium hydroxide whisker used as a flame retardant have characteristics of non-toxic smoke-free non-polluting.our country are long-term use of brominated flame retardants and other organic flame retardants, They has been limited due to amount of smoke and toxic to the environment by second pollution. Magnesium hydroxide whisker used as a material filler have better dispersity and compatibility to enhance stiffness and strength of composite material. It is great significance in magnesium resource utilization, environmental protection, as well as functional materials.
Magnesium hydroxide whisker is prepared with magnesium chloride and alkali liquor as raw materials by direct precipitation method,.Its preparation process is mainly divided into four stages, namely precipitation reaction, crystallization reaction, washing process and drying process. We study the different processing conditions of magnesium hydroxide whisker in the preparation process, including the choice of precipitation agent, the choice of solvent, the choice of raw material ratio, the choice of detergent,the choice of drying temperature and drying time; choosing the additives of magnesium hydroxide whisker in its preparation process, including single additives, compounding additives and foreign ion additives. The results show that the magnesium hydroxide whisker can be prepared by direct precipitation method with NaOH as the precipitation agent, and ethanol/water (1:1) as solvent, MgCl2and NaOH reaction ratio is1:2, the zinc stearate or ferric chloride as additives, washing in G4sand core funnel with water+ethanol,,drying in vacuum drying oven with the vacuum degree of0.08Mpa and the drying temperature of100℃for the3h. The magnesium hydroxide whisker by prepared is uniformity particle size and integrity crystal.
Magnesium hydroxide whisker is prepared to add zinc stearate or ferric chloride, the process conditions of its liquid reaction stage is optimized.The results are as follows:the process conditions for magnesium hydroxide whisker be prepared to add zinc stearate:the precipitation temperature is40℃, the crystallization temperature is90℃, the crystallization time is2h; the process conditions for magnesium hydroxide whisker be prepared to add ferric chloride:the precipitation time is40min, the precipitation temperature is50℃, the quanlity of foreign ion is0.4mol%. The SEM chart of is clear,no reunion phenomenon,and whisker aspect ratio is about10.7. In the XRD chart, the diffraction intensity of the (101) plane is increased.lt's show that the growth of magnesium hydroxide whisker has preferred sexual orientation to add the additives.
In the text,the growth of mechanism Magnesium hydroxide whisker are discussed. The growth kinetics of magnesium hydroxide whisker were analyzed from the point of crystal nucleation process and crystal growth rat, it's proofed that whisker growth accord with the classical crystal growth theory. The foreign ions led to the preferential growth in the crystal growth process, it's a guide crystal role in the form of magnesium hydroxide whisker; Mg (OH)6~4+anionic coordination octahedron is the growth units of magnesium hydroxide whisker. Anion coordination polyhedron growth units theory can reasonably explain growth and generation of magnesium hydroxide whisker.
以氯化镁和碱液为原料采用直接沉淀法制备氢氧化镁晶须,其制备过程主要分为四个阶段,即沉淀反应、晶化反应、洗涤过程和干燥过程。对氢氧化镁在制备过程中不同工艺条件进行研究,包括沉淀剂的选择、溶剂的选择、洗涤剂的选择以及干燥温度和干燥时间的选择,原料配比的选择；对制备氢氧化镁晶须的助剂进行优选,包括单助剂、复配助剂和外离子助剂。研究结果显示,采用直接沉淀法制备氢氧化镁晶须,以氢氧化钠为沉淀剂,乙醇／水(1：1)为溶剂,MgCl2与NaOH反应配比为1：2,选择硬脂酸锌或氯化铁为助剂,使用水+乙醇进行洗涤,在真空度为0.08Mpa、温度为100℃下干燥3h。制备出了粒度均一、晶型完整的氢氧化镁晶须。
以硬脂酸锌或氯化铁为助剂制备氢氧化镁晶须,对其液相反应阶段的工艺条件进行研究,研究结果表明,以硬脂酸锌为助剂制备氢氧化镁晶须的工艺条件为：沉淀温度40℃、晶化温度90℃、晶化时间2h；以氯化铁为外离子制备氢氧化镁晶须的工艺条件为：沉淀时间40min、沉淀温度50℃、外加离子量0.4mol%。产品的SEM图中颗粒边界分明,无团聚现象,晶须的长径比约为10.7。XRD图中(101)面衍射强度增加,说明添加上述助剂后,氢氧化镁晶须在生长过程中具有择优取向性。
对氢氧化镁晶须的生长机理进行探讨,从晶体成核以及晶体的生长速率对氢氧化镁晶须的生长动力学进行分析,证明晶须的生长符合经典的晶体生长理论；外离子的加入使晶体在生长过程中能够择优生长,对氢氧化镁晶须的形成起到导晶的作用；氢氧化镁晶须的生长是以Mg(OH)6~4负离子配位八面体为生长基元进行生长的,利用负离子配位多面体生长基元理论可以合理解释氢氧化镁晶须的生长和生成。
China has rich minerals of magnesium, as well as the salt lake magnesium resources and seawater magnesium resources, the magnesium is full of variety and wide of distribution. We extract magnesium chloride from China's affluet magnesium,and magnesium hydroxide whisker was prepared to add a precipitator and auxiliaries by direct precipitation method. Magnesium hydroxide whisker used as a flame retardant have characteristics of non-toxic smoke-free non-polluting.our country are long-term use of brominated flame retardants and other organic flame retardants, They has been limited due to amount of smoke and toxic to the environment by second pollution. Magnesium hydroxide whisker used as a material filler have better dispersity and compatibility to enhance stiffness and strength of composite material. It is great significance in magnesium resource utilization, environmental protection, as well as functional materials.
Magnesium hydroxide whisker is prepared with magnesium chloride and alkali liquor as raw materials by direct precipitation method,.Its preparation process is mainly divided into four stages, namely precipitation reaction, crystallization reaction, washing process and drying process. We study the different processing conditions of magnesium hydroxide whisker in the preparation process, including the choice of precipitation agent, the choice of solvent, the choice of raw material ratio, the choice of detergent,the choice of drying temperature and drying time; choosing the additives of magnesium hydroxide whisker in its preparation process, including single additives, compounding additives and foreign ion additives. The results show that the magnesium hydroxide whisker can be prepared by direct precipitation method with NaOH as the precipitation agent, and ethanol/water (1:1) as solvent, MgCl2and NaOH reaction ratio is1:2, the zinc stearate or ferric chloride as additives, washing in G4sand core funnel with water+ethanol,,drying in vacuum drying oven with the vacuum degree of0.08Mpa and the drying temperature of100℃for the3h. The magnesium hydroxide whisker by prepared is uniformity particle size and integrity crystal.
Magnesium hydroxide whisker is prepared to add zinc stearate or ferric chloride, the process conditions of its liquid reaction stage is optimized.The results are as follows:the process conditions for magnesium hydroxide whisker be prepared to add zinc stearate:the precipitation temperature is40℃, the crystallization temperature is90℃, the crystallization time is2h; the process conditions for magnesium hydroxide whisker be prepared to add ferric chloride:the precipitation time is40min, the precipitation temperature is50℃, the quanlity of foreign ion is0.4mol%. The SEM chart of is clear,no reunion phenomenon,and whisker aspect ratio is about10.7. In the XRD chart, the diffraction intensity of the (101) plane is increased.lt's show that the growth of magnesium hydroxide whisker has preferred sexual orientation to add the additives.
In the text,the growth of mechanism Magnesium hydroxide whisker are discussed. The growth kinetics of magnesium hydroxide whisker were analyzed from the point of crystal nucleation process and crystal growth rat, it's proofed that whisker growth accord with the classical crystal growth theory. The foreign ions led to the preferential growth in the crystal growth process, it's a guide crystal role in the form of magnesium hydroxide whisker; Mg (OH)6~4+anionic coordination octahedron is the growth units of magnesium hydroxide whisker. Anion coordination polyhedron growth units theory can reasonably explain growth and generation of magnesium hydroxide whisker.
引文
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