风化壳淋积型稀土矿浸取动力学与传质研究
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摘要
在导师悉心指导下,围绕本人主持的在研国家自然科学基金项目——“风化壳淋积型稀土矿贫矿浸取动力学与传质研究”(№50664004),确定了博士论文题目为“风化壳淋积型稀土矿浸取动力学与传质研究”,在风化壳淋积型稀土矿浸取应用基础研究方面开展了一些研究工作：
1.风化壳淋积型稀土矿浸取稀土动力学研究
针对代表性的江西龙南足洞稀土风化壳淋积型稀土矿,从浸取动力学角度出发,考察了浸取反应温度、浸出剂初始浓度、搅拌强度及矿石粒度对稀土浸出速率的影响。
研究结果表明,风化壳淋积型稀土矿浸取是一个典型的液-固非均相反应,浸取过程较好地符合收缩未反应芯模型,尝试法求出动力学控速步骤为属固膜扩散控制,导出了浸出动力学方程为：
求得风化壳淋积型稀土矿浸取反应级数为2级,浸取反应活化能为9.24 kJ/mol。
2.风化壳淋积型稀土矿浸取铝动力学研究
以代表性的江西龙南足洞稀土原矿,针对风化壳淋积型稀土矿离子相形态铝,开展浸取铝动力学研究,考察了浸取反应温度对铝浸出速率的影响。研究表明,风化壳淋积型稀土矿铝的浸取也是一个典型的液-固非均相反应,其浸取过程也可用“收缩未反应芯模型”描述。用尝试法求出铝浸取动力学控速步骤,结果发现1-(1-η)1/3对浸取时间t作图得到一系列直线,且通过原点。通过铝浸取Arrhenius图,求得风化壳淋积型稀土矿浸取铝反应动力学方程为：
计算得出铝浸取反应活化能为41.57 kJ/mol介于40 kJ/mol到160 kJ/mol之间,表明风化壳淋积型稀土矿铝浸取过程受化学反应动力学控制。而且铝浸取的表观活化能远高于稀土浸取表观活化能,显示铝浸取平衡时间长于稀土浸取平衡时间,铝浸取速率远低于稀土浸取速率。
3.风化壳淋积型稀土矿浸取传质研究
用色层塔板理论研究和实验方法,研究了风化壳淋积型稀土矿浸取传质过程,探索淋浸速度、浸出剂初始浓度、矿石粒度及原矿品位对浸出效果的影响,用浸理论塔板高度评价浸取传质效果,对浸取传质过程进行了优化。
实验表明,风化壳淋积型稀土矿浸取理论塔板高度与浸取流速关系可用Van Deemter方程描述,稀土矿浸取理论塔板高度存在最小值,在此流速条件下,浸取浸取过程传质效果最好,该浸取流速为最佳值(Uopt),低于或高于此流速(Uopt),浸取过程塔板高度均增大。
通过研究浸取剂初始浓度对稀土浸取传质过程影响,结果显示,由于风化壳淋积型稀土矿浸取动力学受固膜内扩散控制,当浸取剂浓度足够高时,再提高浸取剂初始浓度,对稀土浸取理论塔板高度的影响不大,此时对传质的影响不明显。因而浸取剂初始浓度以选择2%～3%为宜。
通过研究不同矿石粒度下风化壳淋积型稀土矿的浸取过程,结果表明,随着矿石粒度的增大,浸取理论塔板高度增大,浸取过程传质效果较差,柱效降低。而随着矿石粒度的减小,浸取渗透性能下降,当浸取流速低于是佳流速Uopt时,理论塔板高度将增大,浸取过程传质效果变差。
研究稀土矿品位风化壳淋积型稀土矿浸取的影响表明,原矿稀土品位越高,浸取理论塔板高度越小,随着矿石品位的降低,浸取过程理论塔板高度增大。
4.风化壳淋积型稀土矿稀土浸取动力学分离铝研究
基于风化壳淋积型稀土矿其浸取稀土为内膜扩散控制动力学模型,而铝为离子交换反应化学控制动力学模型这一显著差异,进一步探索不同浸取条件下稀土浸取行为与铝浸取行为。结果表明,风化壳淋积型稀土矿稀土浸取曲线与铝浸取曲线变化并不同步,稀土浸取曲线随着浸取进程的增长,浸取稀土浓度出现峰值,而铝浸取曲线随着浸取进程的增长,铝浓度不变显著。
在不同浸取流速条件下,风化壳淋积型稀土矿浸取液稀土浓度峰值浓度随浸取流速变化明显,而浸取液中铝的浓度随浸取流速变化不显著,浸取过程中稀土与铝在浸取动力学分离存在差异,在一定的浸取流速条件下,浸取过程中稀土与铝存在分离作用。
通过研究风化壳淋积型稀土矿浸出液中铝与稀土相对含量随浸取流速变化,结果表明,在低流速时,浸出液中铝与稀土相对含量随浸取流速增大而减小,到一定流速时,再加快流速,浸出液中铝与稀土相对含量随浸取流速增大而增大,浸取过程中有一最佳流速,经优化得到优化流速为U=0.23mL/min,此时,稀土浸出液中含铝最低,AI/RE=0.012,因而在浸取过程中产生了浸取动力学分离铝效果。
5.风化壳淋积型稀土矿贫矿浸取传质过程优化研究
针对这些风化壳淋积型稀土矿贫矿的复杂性,以江西有代表性的龙南风化壳淋积型稀土矿贫矿为对象,用色层理论和实验方法探索其浸取传质特性,实验不同流速条件下稀土贫矿浸取行为,用理论塔板高度评价浸取传质效果,对浸取传质过程进行优化。
研究结果表明,风化壳淋积型稀土矿贫矿浸取曲线峰形窄,峰高较低。浸取传质过程可用理论塔板高度变化来进行优化,风化壳淋积型稀土矿贫矿浸取时,随着浸取流速的增大,起初浸取理论塔板高HETP减小,但超过0.9mL/min速度后,浸取理论塔板高HETP增大,因而浸取有一个最佳流速,风化壳淋积型稀土矿贫矿浸取优化流速为0.9mL/min。
对于风化壳淋积稀土矿贫矿,不同装矿高度条件下其浸取稀土曲线显示,浸出液稀土峰值浓度随浸矿柱径比增加而降低,表明浸取柱径比越大,浸取过程扩散距离越长,扩散作用越强。风化壳淋积型稀土矿贫矿浸取稀土时装矿高度越低,理论塔板高度越低,表明浸取传质效果越好。
对稀土贫矿浸取时浸矿剂浓度优化结果表明,贫矿浸出液稀土峰值浓度高随浸取剂浓度的提高而升高,但当浸矿剂浓度达到2%后,浸矿剂浓度再升高,对贫矿浸取稀土峰值浓度影响不大,因而浸取剂初始浓度以选择～2%为宜
For the weathered crust elution-deposited rare earth ores, with the application and development of the green chemistry of extraction process, especially popularization of the in-situ leaching process, the high selectivity leaching, high performance and low consumption extraction technology becomes more and more important and stringent in industrial design. In order to improve extraction process with high performance and low consumption, the basie theoretic and applied experiments of leaching process have investigated in this dissertation.
1 Kinetics on Leaching Rare Earth from the Weathered Crust Elution-deposited Rare Earth Ores
In order to know the mechanism of the rare earth leaching and choose the more suitable technology of extraction rare earth from this ore, the kinetic of leaching rare earth from the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was investigated. The effects of the main leaching parameters such as temperature and ore particle size on leaching process were examined and discussed in order to elucidate the kinetics and mechanism of leaching rare earth. It was found that the higher the leaching temperature or the smaller the ore particle size, the faster the leaching progress. The leaching mechanism was analyzed with different kinetics models. The results show that the leaching process can be described by the shrinking-core model, the leaching rate was controlled by the inner diffusion of reactants and leaching products through mineral porous layer, the leaching process follows the kinetic model 1—2/3α—(1—α)2/3=kt, the apparent activation energy was 9.24 kJ/mol obtained from calculating the experimental data and the order of the ore particle size found to be approximately 2.An empirical equation relating the rare earth leached rate constant with ore particle size and leaching temperature was established as:
2 Kinetics on Leaching aluminum from the Weathered Crust Elution-deposited Rare Earth Ores
For the weathered crust elution-deposited rare earth ores, the aluminum is existing as exchangeable phase state with contents of 4.56×10-2%, and is the main impurities in the rare earth leach liquor. In order to know the mechanism of the aluminum leaching and inhibit aluminium during leaching rare earth, the kinetic of leaching aluminum from the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was investigated. The effects of the temperature on leaching process were examined and discussed, the leaching mechanism was analyzed with different kinetics models. The results show that the leaching process can be described with the shrinking-core model too. The leaching rate was controlled by the the ion-exchange chemical reaction controls. The leaching process follows the kinetic model 1-(1-α)1/3=kt, the apparent activation energy was 41.57 kJ/mol obtained from calculating the experimental data. An Empirical equations were established as: 1-(1-η)1/3=1.9x104·e41570/RT·t
3 Mass transfer in Leaching of the weathering crust elution-deposited rare earth ores
The mass transfer in leaching of rare earth from the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was investigated. The effects of the flowrate, the concentration of leach reagents and rare earth ore grade on leaching performance were examined with column leahing, these experiment datum were analyzed with the chromatographic nonequilibrium plate theory in order to elucidate the mass transfer phenomena. It was found that the relationship between the height equivalent to a theoretical plate(HETP) and leaching flowrate can be described by van Deemter equation, there is a optimum flowrate in the leaching process. The results show that the dependence of leaching efficiency on flowrate of reagents. It provides a scientific approach to leaching the weathered crust elution-deposited rare earth ores with high efficiency and low material consumption, and is applied to optimize the rare earth extraction conditions and to improve the rare earth received rate.
4 Kinetics Separation Aluminum in Leaching the Weathered Crust Elution-deposited Rare Earth Ores
Comparing with the kinetics on leaching rare earth from the weathered crust elution-deposited rare earth ores, the kinetics on leaching aluminum has a great difference. The leaching rare erath rate was controlled by the inner diffusion of reactants and leaching products through mineral porous layer, but the leaching aluminum rate was controlled by the the ion-exchange chemical reaction controls. The apparent activation energy of leach aluminum is 41.57 kJ/mol, higher than rare earth as 9.24 kJ/mol. The leach reaction speed of leach aluminum is slower than rare earth. The results show that there are kinetic separation of aluminum from rare earth in leaching process. The kinetic separation of aluminum from rare earth in leaching the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was carried out. The effects of the flowrate on kinetic separation aluminum in leaching the weathered crust elution-deposited rare earth ores were examined with column leahing. It was found that there is a optimum flowrate for kinetic separation aluminum in the leaching process. The optimum condition was established:the flowrate is U=0.23mL/min, the Al/RE in leach liquor is 0.012.
5 Optimisation of mass transfer in column elution of rare earths from low grade weathered crust elution-deposited rare earth ore
Along with exploitation of high-grade weathered crust elution-deposited rare earth ores during the recent decades, the quality of rare earth ores is becoming lower and lowe. It has been a serious worldwide problem that how to exploit low-grade rare earth ores availably. In order to improve extraction process from the low-grade rare earth ores, an investigation was carried out to optimize the leaching and mass transfer of rare earth metals with ammonium sulfate solution during the column elution of a low grade weathered crust elution-deposited rare earth ore. The effects of flow rate, concentration of leach reagent and ore grade on the leaching performance were examined. The experimental data was analysed using chromatographic non-equilibrium plate theory in order to elucidate the mass transfer phenomena. It was found that the relationship between the height equivalent to a theoretical plate (HETP) and the leaching flow rate can be described by the Van Deemter equation and there is an optimum flow rate in the leaching process. Compared with similar higher grade weathered crust elution-deposited rare earth ores which have a sharp peak followed by a short tail, the leach curve of low grade ores has a long tail following a broader peak.
1.风化壳淋积型稀土矿浸取稀土动力学研究
针对代表性的江西龙南足洞稀土风化壳淋积型稀土矿,从浸取动力学角度出发,考察了浸取反应温度、浸出剂初始浓度、搅拌强度及矿石粒度对稀土浸出速率的影响。
研究结果表明,风化壳淋积型稀土矿浸取是一个典型的液-固非均相反应,浸取过程较好地符合收缩未反应芯模型,尝试法求出动力学控速步骤为属固膜扩散控制,导出了浸出动力学方程为：
求得风化壳淋积型稀土矿浸取反应级数为2级,浸取反应活化能为9.24 kJ/mol。
2.风化壳淋积型稀土矿浸取铝动力学研究
以代表性的江西龙南足洞稀土原矿,针对风化壳淋积型稀土矿离子相形态铝,开展浸取铝动力学研究,考察了浸取反应温度对铝浸出速率的影响。研究表明,风化壳淋积型稀土矿铝的浸取也是一个典型的液-固非均相反应,其浸取过程也可用“收缩未反应芯模型”描述。用尝试法求出铝浸取动力学控速步骤,结果发现1-(1-η)1/3对浸取时间t作图得到一系列直线,且通过原点。通过铝浸取Arrhenius图,求得风化壳淋积型稀土矿浸取铝反应动力学方程为：
计算得出铝浸取反应活化能为41.57 kJ/mol介于40 kJ/mol到160 kJ/mol之间,表明风化壳淋积型稀土矿铝浸取过程受化学反应动力学控制。而且铝浸取的表观活化能远高于稀土浸取表观活化能,显示铝浸取平衡时间长于稀土浸取平衡时间,铝浸取速率远低于稀土浸取速率。
3.风化壳淋积型稀土矿浸取传质研究
用色层塔板理论研究和实验方法,研究了风化壳淋积型稀土矿浸取传质过程,探索淋浸速度、浸出剂初始浓度、矿石粒度及原矿品位对浸出效果的影响,用浸理论塔板高度评价浸取传质效果,对浸取传质过程进行了优化。
实验表明,风化壳淋积型稀土矿浸取理论塔板高度与浸取流速关系可用Van Deemter方程描述,稀土矿浸取理论塔板高度存在最小值,在此流速条件下,浸取浸取过程传质效果最好,该浸取流速为最佳值(Uopt),低于或高于此流速(Uopt),浸取过程塔板高度均增大。
通过研究浸取剂初始浓度对稀土浸取传质过程影响,结果显示,由于风化壳淋积型稀土矿浸取动力学受固膜内扩散控制,当浸取剂浓度足够高时,再提高浸取剂初始浓度,对稀土浸取理论塔板高度的影响不大,此时对传质的影响不明显。因而浸取剂初始浓度以选择2%～3%为宜。
通过研究不同矿石粒度下风化壳淋积型稀土矿的浸取过程,结果表明,随着矿石粒度的增大,浸取理论塔板高度增大,浸取过程传质效果较差,柱效降低。而随着矿石粒度的减小,浸取渗透性能下降,当浸取流速低于是佳流速Uopt时,理论塔板高度将增大,浸取过程传质效果变差。
研究稀土矿品位风化壳淋积型稀土矿浸取的影响表明,原矿稀土品位越高,浸取理论塔板高度越小,随着矿石品位的降低,浸取过程理论塔板高度增大。
4.风化壳淋积型稀土矿稀土浸取动力学分离铝研究
基于风化壳淋积型稀土矿其浸取稀土为内膜扩散控制动力学模型,而铝为离子交换反应化学控制动力学模型这一显著差异,进一步探索不同浸取条件下稀土浸取行为与铝浸取行为。结果表明,风化壳淋积型稀土矿稀土浸取曲线与铝浸取曲线变化并不同步,稀土浸取曲线随着浸取进程的增长,浸取稀土浓度出现峰值,而铝浸取曲线随着浸取进程的增长,铝浓度不变显著。
在不同浸取流速条件下,风化壳淋积型稀土矿浸取液稀土浓度峰值浓度随浸取流速变化明显,而浸取液中铝的浓度随浸取流速变化不显著,浸取过程中稀土与铝在浸取动力学分离存在差异,在一定的浸取流速条件下,浸取过程中稀土与铝存在分离作用。
通过研究风化壳淋积型稀土矿浸出液中铝与稀土相对含量随浸取流速变化,结果表明,在低流速时,浸出液中铝与稀土相对含量随浸取流速增大而减小,到一定流速时,再加快流速,浸出液中铝与稀土相对含量随浸取流速增大而增大,浸取过程中有一最佳流速,经优化得到优化流速为U=0.23mL/min,此时,稀土浸出液中含铝最低,AI/RE=0.012,因而在浸取过程中产生了浸取动力学分离铝效果。
5.风化壳淋积型稀土矿贫矿浸取传质过程优化研究
针对这些风化壳淋积型稀土矿贫矿的复杂性,以江西有代表性的龙南风化壳淋积型稀土矿贫矿为对象,用色层理论和实验方法探索其浸取传质特性,实验不同流速条件下稀土贫矿浸取行为,用理论塔板高度评价浸取传质效果,对浸取传质过程进行优化。
研究结果表明,风化壳淋积型稀土矿贫矿浸取曲线峰形窄,峰高较低。浸取传质过程可用理论塔板高度变化来进行优化,风化壳淋积型稀土矿贫矿浸取时,随着浸取流速的增大,起初浸取理论塔板高HETP减小,但超过0.9mL/min速度后,浸取理论塔板高HETP增大,因而浸取有一个最佳流速,风化壳淋积型稀土矿贫矿浸取优化流速为0.9mL/min。
对于风化壳淋积稀土矿贫矿,不同装矿高度条件下其浸取稀土曲线显示,浸出液稀土峰值浓度随浸矿柱径比增加而降低,表明浸取柱径比越大,浸取过程扩散距离越长,扩散作用越强。风化壳淋积型稀土矿贫矿浸取稀土时装矿高度越低,理论塔板高度越低,表明浸取传质效果越好。
对稀土贫矿浸取时浸矿剂浓度优化结果表明,贫矿浸出液稀土峰值浓度高随浸取剂浓度的提高而升高,但当浸矿剂浓度达到2%后,浸矿剂浓度再升高,对贫矿浸取稀土峰值浓度影响不大,因而浸取剂初始浓度以选择～2%为宜
For the weathered crust elution-deposited rare earth ores, with the application and development of the green chemistry of extraction process, especially popularization of the in-situ leaching process, the high selectivity leaching, high performance and low consumption extraction technology becomes more and more important and stringent in industrial design. In order to improve extraction process with high performance and low consumption, the basie theoretic and applied experiments of leaching process have investigated in this dissertation.
1 Kinetics on Leaching Rare Earth from the Weathered Crust Elution-deposited Rare Earth Ores
In order to know the mechanism of the rare earth leaching and choose the more suitable technology of extraction rare earth from this ore, the kinetic of leaching rare earth from the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was investigated. The effects of the main leaching parameters such as temperature and ore particle size on leaching process were examined and discussed in order to elucidate the kinetics and mechanism of leaching rare earth. It was found that the higher the leaching temperature or the smaller the ore particle size, the faster the leaching progress. The leaching mechanism was analyzed with different kinetics models. The results show that the leaching process can be described by the shrinking-core model, the leaching rate was controlled by the inner diffusion of reactants and leaching products through mineral porous layer, the leaching process follows the kinetic model 1—2/3α—(1—α)2/3=kt, the apparent activation energy was 9.24 kJ/mol obtained from calculating the experimental data and the order of the ore particle size found to be approximately 2.An empirical equation relating the rare earth leached rate constant with ore particle size and leaching temperature was established as:
2 Kinetics on Leaching aluminum from the Weathered Crust Elution-deposited Rare Earth Ores
For the weathered crust elution-deposited rare earth ores, the aluminum is existing as exchangeable phase state with contents of 4.56×10-2%, and is the main impurities in the rare earth leach liquor. In order to know the mechanism of the aluminum leaching and inhibit aluminium during leaching rare earth, the kinetic of leaching aluminum from the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was investigated. The effects of the temperature on leaching process were examined and discussed, the leaching mechanism was analyzed with different kinetics models. The results show that the leaching process can be described with the shrinking-core model too. The leaching rate was controlled by the the ion-exchange chemical reaction controls. The leaching process follows the kinetic model 1-(1-α)1/3=kt, the apparent activation energy was 41.57 kJ/mol obtained from calculating the experimental data. An Empirical equations were established as: 1-(1-η)1/3=1.9x104·e41570/RT·t
3 Mass transfer in Leaching of the weathering crust elution-deposited rare earth ores
The mass transfer in leaching of rare earth from the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was investigated. The effects of the flowrate, the concentration of leach reagents and rare earth ore grade on leaching performance were examined with column leahing, these experiment datum were analyzed with the chromatographic nonequilibrium plate theory in order to elucidate the mass transfer phenomena. It was found that the relationship between the height equivalent to a theoretical plate(HETP) and leaching flowrate can be described by van Deemter equation, there is a optimum flowrate in the leaching process. The results show that the dependence of leaching efficiency on flowrate of reagents. It provides a scientific approach to leaching the weathered crust elution-deposited rare earth ores with high efficiency and low material consumption, and is applied to optimize the rare earth extraction conditions and to improve the rare earth received rate.
4 Kinetics Separation Aluminum in Leaching the Weathered Crust Elution-deposited Rare Earth Ores
Comparing with the kinetics on leaching rare earth from the weathered crust elution-deposited rare earth ores, the kinetics on leaching aluminum has a great difference. The leaching rare erath rate was controlled by the inner diffusion of reactants and leaching products through mineral porous layer, but the leaching aluminum rate was controlled by the the ion-exchange chemical reaction controls. The apparent activation energy of leach aluminum is 41.57 kJ/mol, higher than rare earth as 9.24 kJ/mol. The leach reaction speed of leach aluminum is slower than rare earth. The results show that there are kinetic separation of aluminum from rare earth in leaching process. The kinetic separation of aluminum from rare earth in leaching the weathered crust elution-deposited rare earth ores with ammonium sulfate solution was carried out. The effects of the flowrate on kinetic separation aluminum in leaching the weathered crust elution-deposited rare earth ores were examined with column leahing. It was found that there is a optimum flowrate for kinetic separation aluminum in the leaching process. The optimum condition was established:the flowrate is U=0.23mL/min, the Al/RE in leach liquor is 0.012.
5 Optimisation of mass transfer in column elution of rare earths from low grade weathered crust elution-deposited rare earth ore
Along with exploitation of high-grade weathered crust elution-deposited rare earth ores during the recent decades, the quality of rare earth ores is becoming lower and lowe. It has been a serious worldwide problem that how to exploit low-grade rare earth ores availably. In order to improve extraction process from the low-grade rare earth ores, an investigation was carried out to optimize the leaching and mass transfer of rare earth metals with ammonium sulfate solution during the column elution of a low grade weathered crust elution-deposited rare earth ore. The effects of flow rate, concentration of leach reagent and ore grade on the leaching performance were examined. The experimental data was analysed using chromatographic non-equilibrium plate theory in order to elucidate the mass transfer phenomena. It was found that the relationship between the height equivalent to a theoretical plate (HETP) and the leaching flow rate can be described by the Van Deemter equation and there is an optimum flow rate in the leaching process. Compared with similar higher grade weathered crust elution-deposited rare earth ores which have a sharp peak followed by a short tail, the leach curve of low grade ores has a long tail following a broader peak.
引文
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