多晶相水合碳酸镁结晶生长过程调控研究
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摘要
水合碳酸镁是一种重要的化工原料或产品,其结晶生长是制备过程中最基本、最重要的环节。本文旨在通过对水合碳酸镁结晶生长过程的系统研究,完善水合碳酸镁反应结晶过程控制手段和机制,为工业化提供理论指导和技术支持。主要内容归纳如下：
实验研究了水合碳酸镁热力学性质。无定形亚稳态是由40～100nm的纳米级颗粒聚集而成,是包含细小晶粒和非晶态的具有网络组织结构的复杂物相,其组成可表示为xMgCO3·Mg(OH)2-yH2O。无定形碳酸镁具有“动态溶解”性质,反应物将不断转化为无定形物继而形成稳定晶体。采用简化方程、经验模型和BP神经网络拟合和预测溶解度,三者各有优缺点。实验表明,水合碳酸镁溶解度均随温度升高而降低,在NaCl溶液中溶解度显著提高。
系统研究了结晶工艺参数对无定形亚稳态晶型转化的影响。研究表明,无定形亚稳态碳酸镁既可以向三水碳酸镁转变也可以向碱式碳酸镁转变,工艺参数的改变可以使结晶过程发生热力学和动力学控制结晶路径的转换。转化过程遵循颗粒介导机理,无定形纳米粒子充当了生长单元的角色。建立无定形亚稳态碳酸镁结晶动力学模型,利用XRD测定转化率。实验得到无定形物结晶活化能为31.70kJ·mol-1。采用BP神经网络模拟结晶工艺条件与产品粒度的关系,有效补充了结晶模型在对产品尺寸描述上的不足。
从成核、生长、二次过程和外场强化四个层次研究了三水碳酸镁结晶生长调控。1)诱导期和无定形物转变时间受温度、浓度和晶种影响。在此基础上,提出搅拌一陈化合成工艺,通过对搅拌时间的控制,达到将成核与生长阶段分离的目的,合成出尺寸可控、形态良好的三水碳酸镁微棒。2)在SDS存在下,合成出平均长度为87～180μm、长径比为18～45的三水碳酸镁晶须。SDS在晶体或无定形纳米颗粒表面的物理吸附,促使三水碳酸镁发生定向生长,形成晶须。3)实验采用FBRM和形貌分析考察了三水碳酸镁的二次过程。结果表明,MgCl2对其聚结过程具有促进作用,聚结使颗粒形成束状形貌。4)采用超声场强化三水碳酸镁结晶。反应结晶的不同阶段引入超声所产生的效果不同；集中的超声作用更有利于晶体成核,增大颗粒尺寸,而持续作用促进二次成核,减小颗粒尺寸。
实验考察了三水碳酸镁相转移合成碱式碳酸镁过程及动力学。三水碳酸镁分解后可能再度形成无定形物,并经由颗粒介导途径转化为碱式碳酸镁。相转移过程为：三水碳酸镁溶解→无定形纳米颗粒形成→碱式碳酸镁结晶。温度升高、前驱物尺寸减小和电解质溶液都可以加快相转移速率。较小尺寸前驱物热解得到花状颗粒,较大尺寸前驱物热解则得到中空管状颗粒。静态环境热解产物为多孔玫瑰花状微球,局部过饱和导致了微球的形成。通过分析固相中MgO含量估测热解过程转化率,对无定形亚稳态结晶模型参数重新定义,可以很好描述相转移动力学过程,测得相转移活化能为66.24kJ.mo1-1。
本文还研究了碱式碳酸镁生长过程调控。首次在SDS辅助作用下,低温(<55℃)合成得到碱式碳酸镁微球。SDS的加入可以有效抑制无定形纳米颗粒向三水碳酸镁生长,使其直接向碱式碳酸镁转变。在较高温度下(>60℃)采用搅拌—陈化法,通过控制搅拌时间,得到了尺寸可控、形态良好的碱式碳酸镁微球;微球的微观形貌取决于晶种数量和无定形生长物质之间的分配比例。本文还利用微波场强化碱式碳酸镁合成,实验结果表明微波场可以强化反应进程,促进初始纳米颗粒的组装,但微波没有改变产物晶习。
Hydrated magnesium carbonate is an important kind of chemical raw material or product. The crystallization and growth process is the most basic and the most important link of its preparation. This paper aims to study the crystallization and growth process of hydrated magnesium carbonate systematically, improving the control means and mechanisms of the reactive crystallization process. Based on these, theoretical guidance and technical support can be provided for the industrialization. The main contents are summarized as follows:
The thermodynamic properties of hydrated magnesium carbonate were studied experimentally. The study reveals that the metastable phase is gathered by nanoparticles with the size of40-100nm. It forms a framework structure, which is a complex substance containing fine crystalline and amorphous phase. The composition can be expressed as xMgCO3·Mg(OH)2-yH2O. A nature of dynamic solubility is appeared. The reactant will convert to amorphous substance continuously and then form stable crystal. Simplified equation, the empirical model and the BP neural network were used to fit and predict solubility. They have their own pros and cons. Experiments show that hydrated magnesium carbonate solubility decreases with increasing temperature and increases significantly in NaCl solution.
The effects of crystallization process parameters on the crystalline transformation of metastable phase were studied systematically. The study shows that the metastable magnesium carbonate transfers to either nesquehonite or hydromagnesite. Changes in process parameters can make the conversion process shift from thermodynamic control to kinetically control. The transformation process is a particle-mediated process, in which amorphous nano-particles play the role of the growth units. A crystallization kinetics model of metastable magnesium carbonate was established combining the system characteristics. XRD was used to determine the conversion rate. Based on these, activation energy of the metastable phase crystallization was measured for31.70kJ-mol-1. To supplement the lack of metastable phase crystallization model for the description on product size, BP neural network was adapted to simulate the relationship between crystallization process conditions and product size.
The regulation of nesquehonite crystallization and growth was studied from the four levels of nucleation, growth, secondary processes and outfield strengthen.1) The induction period and amorphous transition time were affected by temperature, concentration as well as seed. According to the nucleation characteristics, stirring-aging method was proposed to synthesize nesquehonite microrods. By controlling stirring time, the nucleation stage and growth stage of nesquehonite can be separated. Nesquehonite microrods with controllable size, uniform size distribution and good shape were got.2) High length and high aspect ratio MgCO3·3H2O whiskers were synthesized in the presence of SDS. The obtained whiskers have an average length of87～180μm with an aspect ratio of18～45. Physical adsorption of SDS on nano-crystalline or amorphous nano-particles surface promoted oriented growth of nesquehonite. As a result, whiskers were formed.3) What's more, FBRM and morphology analysis were used to study the secondary processes of nesquehonite. The results show that MgCl2promotes aggregation, forming the bundle morphology.4) Ultrasonic was used to enhance MgCO3·3H2O crystallization. The effects of ultrasound introduced at different crystallization stages were different. Concentrated ultrasound was more conducive on nucleation and increased the particle size. By contrast, continuous ultrasound destroyed the forming nuclei, promoted secondary nucleation and reduced the particle size.
In this paper, MgCO3·3H2O was severed as a precursor to prepare porous hydromagnesite crystals through pyrogenation under different conditions. The phase transformation process was system studied. The results show that amorphous material could be re-formed after nesquehonite decomposition. Hydromagnesite will be crystallized via particles-mediated pathway. The phase transformation process can be described as: nesquehonite dissolution→amorphous nanoparticles formation→hydromagnesite crystallization. The higher the pyrogenation temperature and the smaller the size of the precursor, the faster phase transfer rate will be. Electrolyte solution can also promote the phase transformation rate. Flower-like hydromagnesite particles were got by the smaller size precursor while hollow tubular particles were formed by the bigger size precursor. The pyrogenation product under static environment was porous rosette-like microspheres. The local supersaturation is the main reason to cause the formation of microspheres. The nesquehonite conversion rate during the transformation process was estimated by analyzing MgO content. The metastable phase crystallization model can be a useful description of the phase transformation kinetics after redefining the parameters. The activation energy of nesquehonite phase transformation process was calculated for66.24kJ·mol-1.
The growth process of the metastable phase directly converts into hydromagnesite was also studied. Hydromagnesite microspheres were synthesized at lower temperatures (<55℃) with the aassistance of SDS for the first time. SDS can effectively inhibit the conversion of amorphous nano-particles to MgCO3·3H2O but grow into4MgCO3·Mg(OH)2·4H2O directly. Hydromagnesite microspheres with different size, uniform distribution and good shape were got via stirring-aging method at higher temperatures (>60℃). The morphology of the microspheres depends on the allocation proportion between the number of seed and amorphous growth substances. Microwave was additionally used for hydromagnesite synthesis. Experimental results show that the microwave field can enhance the reaction kinetics and promote the assembly of nano-particles. Thereby, the particle size was increased; however, the microwave crystal habit was not changed.
实验研究了水合碳酸镁热力学性质。无定形亚稳态是由40～100nm的纳米级颗粒聚集而成,是包含细小晶粒和非晶态的具有网络组织结构的复杂物相,其组成可表示为xMgCO3·Mg(OH)2-yH2O。无定形碳酸镁具有“动态溶解”性质,反应物将不断转化为无定形物继而形成稳定晶体。采用简化方程、经验模型和BP神经网络拟合和预测溶解度,三者各有优缺点。实验表明,水合碳酸镁溶解度均随温度升高而降低,在NaCl溶液中溶解度显著提高。
系统研究了结晶工艺参数对无定形亚稳态晶型转化的影响。研究表明,无定形亚稳态碳酸镁既可以向三水碳酸镁转变也可以向碱式碳酸镁转变,工艺参数的改变可以使结晶过程发生热力学和动力学控制结晶路径的转换。转化过程遵循颗粒介导机理,无定形纳米粒子充当了生长单元的角色。建立无定形亚稳态碳酸镁结晶动力学模型,利用XRD测定转化率。实验得到无定形物结晶活化能为31.70kJ·mol-1。采用BP神经网络模拟结晶工艺条件与产品粒度的关系,有效补充了结晶模型在对产品尺寸描述上的不足。
从成核、生长、二次过程和外场强化四个层次研究了三水碳酸镁结晶生长调控。1)诱导期和无定形物转变时间受温度、浓度和晶种影响。在此基础上,提出搅拌一陈化合成工艺,通过对搅拌时间的控制,达到将成核与生长阶段分离的目的,合成出尺寸可控、形态良好的三水碳酸镁微棒。2)在SDS存在下,合成出平均长度为87～180μm、长径比为18～45的三水碳酸镁晶须。SDS在晶体或无定形纳米颗粒表面的物理吸附,促使三水碳酸镁发生定向生长,形成晶须。3)实验采用FBRM和形貌分析考察了三水碳酸镁的二次过程。结果表明,MgCl2对其聚结过程具有促进作用,聚结使颗粒形成束状形貌。4)采用超声场强化三水碳酸镁结晶。反应结晶的不同阶段引入超声所产生的效果不同；集中的超声作用更有利于晶体成核,增大颗粒尺寸,而持续作用促进二次成核,减小颗粒尺寸。
实验考察了三水碳酸镁相转移合成碱式碳酸镁过程及动力学。三水碳酸镁分解后可能再度形成无定形物,并经由颗粒介导途径转化为碱式碳酸镁。相转移过程为：三水碳酸镁溶解→无定形纳米颗粒形成→碱式碳酸镁结晶。温度升高、前驱物尺寸减小和电解质溶液都可以加快相转移速率。较小尺寸前驱物热解得到花状颗粒,较大尺寸前驱物热解则得到中空管状颗粒。静态环境热解产物为多孔玫瑰花状微球,局部过饱和导致了微球的形成。通过分析固相中MgO含量估测热解过程转化率,对无定形亚稳态结晶模型参数重新定义,可以很好描述相转移动力学过程,测得相转移活化能为66.24kJ.mo1-1。
本文还研究了碱式碳酸镁生长过程调控。首次在SDS辅助作用下,低温(<55℃)合成得到碱式碳酸镁微球。SDS的加入可以有效抑制无定形纳米颗粒向三水碳酸镁生长,使其直接向碱式碳酸镁转变。在较高温度下(>60℃)采用搅拌—陈化法,通过控制搅拌时间,得到了尺寸可控、形态良好的碱式碳酸镁微球;微球的微观形貌取决于晶种数量和无定形生长物质之间的分配比例。本文还利用微波场强化碱式碳酸镁合成,实验结果表明微波场可以强化反应进程,促进初始纳米颗粒的组装,但微波没有改变产物晶习。
Hydrated magnesium carbonate is an important kind of chemical raw material or product. The crystallization and growth process is the most basic and the most important link of its preparation. This paper aims to study the crystallization and growth process of hydrated magnesium carbonate systematically, improving the control means and mechanisms of the reactive crystallization process. Based on these, theoretical guidance and technical support can be provided for the industrialization. The main contents are summarized as follows:
The thermodynamic properties of hydrated magnesium carbonate were studied experimentally. The study reveals that the metastable phase is gathered by nanoparticles with the size of40-100nm. It forms a framework structure, which is a complex substance containing fine crystalline and amorphous phase. The composition can be expressed as xMgCO3·Mg(OH)2-yH2O. A nature of dynamic solubility is appeared. The reactant will convert to amorphous substance continuously and then form stable crystal. Simplified equation, the empirical model and the BP neural network were used to fit and predict solubility. They have their own pros and cons. Experiments show that hydrated magnesium carbonate solubility decreases with increasing temperature and increases significantly in NaCl solution.
The effects of crystallization process parameters on the crystalline transformation of metastable phase were studied systematically. The study shows that the metastable magnesium carbonate transfers to either nesquehonite or hydromagnesite. Changes in process parameters can make the conversion process shift from thermodynamic control to kinetically control. The transformation process is a particle-mediated process, in which amorphous nano-particles play the role of the growth units. A crystallization kinetics model of metastable magnesium carbonate was established combining the system characteristics. XRD was used to determine the conversion rate. Based on these, activation energy of the metastable phase crystallization was measured for31.70kJ-mol-1. To supplement the lack of metastable phase crystallization model for the description on product size, BP neural network was adapted to simulate the relationship between crystallization process conditions and product size.
The regulation of nesquehonite crystallization and growth was studied from the four levels of nucleation, growth, secondary processes and outfield strengthen.1) The induction period and amorphous transition time were affected by temperature, concentration as well as seed. According to the nucleation characteristics, stirring-aging method was proposed to synthesize nesquehonite microrods. By controlling stirring time, the nucleation stage and growth stage of nesquehonite can be separated. Nesquehonite microrods with controllable size, uniform size distribution and good shape were got.2) High length and high aspect ratio MgCO3·3H2O whiskers were synthesized in the presence of SDS. The obtained whiskers have an average length of87～180μm with an aspect ratio of18～45. Physical adsorption of SDS on nano-crystalline or amorphous nano-particles surface promoted oriented growth of nesquehonite. As a result, whiskers were formed.3) What's more, FBRM and morphology analysis were used to study the secondary processes of nesquehonite. The results show that MgCl2promotes aggregation, forming the bundle morphology.4) Ultrasonic was used to enhance MgCO3·3H2O crystallization. The effects of ultrasound introduced at different crystallization stages were different. Concentrated ultrasound was more conducive on nucleation and increased the particle size. By contrast, continuous ultrasound destroyed the forming nuclei, promoted secondary nucleation and reduced the particle size.
In this paper, MgCO3·3H2O was severed as a precursor to prepare porous hydromagnesite crystals through pyrogenation under different conditions. The phase transformation process was system studied. The results show that amorphous material could be re-formed after nesquehonite decomposition. Hydromagnesite will be crystallized via particles-mediated pathway. The phase transformation process can be described as: nesquehonite dissolution→amorphous nanoparticles formation→hydromagnesite crystallization. The higher the pyrogenation temperature and the smaller the size of the precursor, the faster phase transfer rate will be. Electrolyte solution can also promote the phase transformation rate. Flower-like hydromagnesite particles were got by the smaller size precursor while hollow tubular particles were formed by the bigger size precursor. The pyrogenation product under static environment was porous rosette-like microspheres. The local supersaturation is the main reason to cause the formation of microspheres. The nesquehonite conversion rate during the transformation process was estimated by analyzing MgO content. The metastable phase crystallization model can be a useful description of the phase transformation kinetics after redefining the parameters. The activation energy of nesquehonite phase transformation process was calculated for66.24kJ·mol-1.
The growth process of the metastable phase directly converts into hydromagnesite was also studied. Hydromagnesite microspheres were synthesized at lower temperatures (<55℃) with the aassistance of SDS for the first time. SDS can effectively inhibit the conversion of amorphous nano-particles to MgCO3·3H2O but grow into4MgCO3·Mg(OH)2·4H2O directly. Hydromagnesite microspheres with different size, uniform distribution and good shape were got via stirring-aging method at higher temperatures (>60℃). The morphology of the microspheres depends on the allocation proportion between the number of seed and amorphous growth substances. Microwave was additionally used for hydromagnesite synthesis. Experimental results show that the microwave field can enhance the reaction kinetics and promote the assembly of nano-particles. Thereby, the particle size was increased; however, the microwave crystal habit was not changed.
引文
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