扎布耶盐湖卤水含钾六元体系的五元、四元子体系273K介稳相平衡研究
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摘要
西藏扎布耶盐湖富含锂、钾、硼、铷、铯等资源。为了更好地开发和利用该盐湖卤水资源，本文针对其卤水组成，采用等温蒸发法研究了文献中未见报道的含钾六元体系Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-), B_4O_7~(2-) H_2O部分五元及四元子体系273K介稳相平衡，包括4个五元子体系：L i~+//Cl~-, CO2~-3, SO_4~(2-) B_4O_7~(2-) H_2O，K//Cl~-, CO_3~(2-), SO_4~(2-), B_4O_7~(2-) H_2O，Li~+, K~+//Cl~-,CO_3~(2-), SO_4~(2-) H_2O和Li~+, K~+//Cl~-, SO_4~(2-) B4O2~-7~-H_2O；4个四元体系：K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O，L i~+, K~+//Cl~-, SO_4~(2-) H_2O， Li~+, K~+//Cl~-, B_4O_7~(2-) H_2O和K, Na~+//Cl~-, SO_4~(2-) H_2O。
测定了上述各体系273K平衡液相中各组分的溶解度﹑密度及pH值，绘制了四元体系的相图、水图、密度-组成图和pH-组成图；绘制了五元体系介稳相平衡立体图、分别以Li_2CO_3、Li_2B_4O_7盐饱和的平面投影相图、水图、密度~-组成图、pH-组成图及锂盐图。
五元体系Li~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O273K属于简单共饱和型，无复盐或固溶体生成。介稳相图由1个零变量点，4条单变量线和4个相区组成。4个相区为：LiCl H_2O、Li_2CO_3、Li_2SO_4H_2O、LiBO_28H_2O结晶区。由于LiCl与H_2O存在极大的相似性，使其有极强的盐析能力和使其他水合物脱水的作用，在该体系中LiCl对Li_2SO_4有强的盐析作用。
五元体系K~+//Cl~-,CO_3~(2-), SO_4~(2-),B_4O_7~(2-) H_2O及四元体系K~+//Cl, SO_4~(2-), B_4O_7~(2-) H_2O属于简单共饱和型，无复盐或固溶体生成。介稳相图由1个零变量点，4条单变量线和4个相区组成。4个相区为：KCl、K_2B_4O_74H_2O、K_2CO_33/2H_2O、 K_2SO_4结晶区。体系中，硼酸钾表现出明显的介稳性。碳酸钾对其他盐具有强烈的盐析作用，对介稳平衡液相的物化性质影响很大，使平衡液相呈碱性。
五元体系Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-) H_2O及四元子体系Li~+, K~+//Cl~-, SO_4~(2-) H_2O273K介稳相平衡中有锂钾硫酸盐复盐KLiSO_4生成。其五元介稳相平衡立体图由4个共饱点，13条单变量曲线和7个结晶相区组成。7个结晶相区分别对应于LiCl H_2O、Li_2SO_4H_2O、K_2SO_4、KCl、Li_2CO_3、K_2CO_33/2H_2O和锂钾硫酸复盐KLiSO_4的结晶区。该五元体系Li_2CO_3饱和投影图由4个共饱点，9条单变量曲线和6个结晶区组成。研究表明，低温有利于K2SO_4的析出，高温有利于Li_2CO_3的析出。
五元体系Li~+, K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O273K介稳相图由4个共饱点，13条单变量曲线和7个相区组成。7个结晶相区分别对应于LiCl H_2O、Li_2SO_4H_2O、 K2SO_4、KCl、K_2B_4O_7·4H_2O、LiBO_2·8H_2O及锂钾硫酸复盐KLiSO_4结晶区。该五元体系Li2B4O7饱和投影图由4个共饱点，9条单变量曲线和6个结晶区组成。体系4个共饱点均在Li_2B_4O_7饱和投影范围内，共饱点E1为相称共饱点，E2、E3、 E4为不相称共饱点。LiCl H_2O结晶区面积最小，K_2SO_4结晶区面积最大。
273K时硼酸钾、硼酸锂的固相结晶析出形式分别为K_2B_4O_74H_2O和LiBO28H_2O，对应的完整分子式分别为K_2[B_4O_5(OH)_4]2H_2O和Li[B(OH)_4]6H_2O。硼酸盐在水溶液中溶解行为复杂，含硼水盐体系存在明显介稳现象，平衡液相中硼酸根过饱和富集，介稳相图结晶相区明显小于稳定相图结晶相区。各体系中， LiBO28H_2O和K2B4O74H_2O对应的共饱和溶解度曲线上各物化性质随液相化学组成的变化无明显规律性。
在含钾六元体系Li~+, K~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O子体系273K介稳相图中，碳酸锂和硫酸钾结晶相区较大，蒸发时极易析出；溶液中氯化锂含量的高低与硫酸锂析出相区的大小呈正相关性；硼酸盐均以单盐形式存在，可由蒸发制备；氯化锂和碳酸钾结晶相区较小，不能通过蒸发的方式获取。以上析盐规律对于从盐湖卤水中提取锂盐、钾盐和硼酸盐具有重要意义。
Zhabuye Salt Lake, located in Tibet, famous for its abundance resources, such as lithium, potassium, borate, rubidium, and cesium. In order to comprehensive utilize the resource in the Zhabuye Salt Lake, the metastable equilibria of subsystems of the hexahydric system Li~+, K~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O were studied at273K using an isothermal evaporation method, respectively, which have not been reported in the literature. They are four quinary systems Li~+//Cl~-, CO_3~(2-), SO_4~(2-), B_4O_7~(2-) H_2O, K+//Cl-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O,Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-) H_2O and Li~+, K~+//Cl-, SO_4~(2-), B_4O_7~(2-) H_2O, four quaternary systems K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O, Li~+, K~+//Cl~-,SO_4~(2-) H_2O, Li~+, K~+//Cl~-, B_4O_7~(2-) H_2O,and K~+, Na~+//Cl~-, SO_4~(2-) H_2O.
The solubilities, densities and pH values of the equilibrated solutions were determined. The metastable equilibrium phase diagrams, the water-content diagrams, the density vs composition diagrams and the pH values vs composition diagrams of the quaternary systems were plotted the stereo-diagram and projected phase diagrams (saturated with Li_2CO_3or Li2B4O7), corresponding water content diagrams, density vs composition diagrams, the pH value vs composition diagrams and lithium content diagrams of the quinary systems were constructed.
There is no double salt or solid solution formed in the simple quinary system Li~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O. The metastable phase diagram of the system consists of one invariant point, four univariant curves and four crystallization fields. Because of the structure similarity between LiCl and H_2O, salt LiCl has strong salting-out effect and the role of making other hydrate dehydration, with strong salting-out effect onsalt Li2SO_4in this system.
The quinary system K~+//Cl~-, CO_3~(2-), SO_4~(2-),B_4O_7~(2-) H_2O and the quaternary system K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O are of simple type. No double salt or solid solution formed. The metastable phase diagram of the quinary system consists of one invariant point, four univariant curves and four crystallization fields. Salt K2CO3has strong salting-out effect on the other salts. Due to the large solubility, salt K2CO3has strong effect on the physicochemical properties in the solution of this equilibrium system, which presents alkalescency. Potassium borate is metastabled obviously.
Results show that the double salt KLiSO+4is formed in the quinary system Li~+, K~+//Cl~-, CO_3~(2-),SO_4~(2-) H_2O and the subsystem Li~+, K~+//Cl~-, SO_4~(2-) H_2O. The stereo-diagram of the quinary system consists of four invariant point, thirteen univariant curves and seven crystallization fields. The projected diagram of this system (saturated with Li_2CO_3) consists of sixcrystallization fields, nine univariant curves and all the four invariant points. The crystallization fields of Li2SO_4H_2O and K2SO_4are larger, while the salt LiCl H_2O and K2CO33/2H_2O have smaller crystallization fields. A lower temperature is necessary for separating pure potassium sulfate and higher temperature is helpful to obtain lithium carbonate.
The quinary system Li~+, K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O is of complex type with the double salt KLiSO_4formed. The stereo~-diagram of the quinary system consists of four invariant point, thirteen univariant curves and seven crystallization fields. The projected diagram of this system (saturated with Li2B4O7) consists of six crystallization fields, nine univariant curves and all the four invariant points. Invariant point E1is the commensurate invariant point, while points E2, E3, E4are the incommensurate invariant points. The crystallization field of K_2SO_4is the largest, but the salt LiCl H_2O has smallest crystallization fields.
The crystallizated forms of lithium borate and potassium borate are K_2[B_4O_5(OH)_4]_2H_2O and Li[B(OH)_4]_6H_2O, respectively. Borate salt shows obviously metastablity and has complicated dissolution behaviour in aqueous solution. The borate crystallization fields in metastable equilibrium diagram are smaller than that in stability diagram. For the systems mentioned above, it is found that physicochenmical properties of the equilibrium solutions saturated with the LiBO_2·8H_2O and K_2B_4O_7·4H_2O show irregular changes with the solution composition.
In the metastable equilibria of subsystems of the hexahydric system Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-),B_4O_7~(2-) H_2O at273K, salts Li_2CO_3and K_2SO_4precipitate easily due to the larger crystallization fields. The crystallization area of Li_2SO_4H_2O has the positive correlation with the concentration of LiCl in the equilibrated solution. Borate only formed single salts in equilibrated solution, which can be separated by isothermal evaporation method. Salts LiCl H_2O and K2CO33/2H_2O have the smaller crystallization zone, thus it is difficult to obtain them only by evaporation method. This feature is very important to extract lithium, potassium and borate from the salt lake brine.
测定了上述各体系273K平衡液相中各组分的溶解度﹑密度及pH值，绘制了四元体系的相图、水图、密度-组成图和pH-组成图；绘制了五元体系介稳相平衡立体图、分别以Li_2CO_3、Li_2B_4O_7盐饱和的平面投影相图、水图、密度~-组成图、pH-组成图及锂盐图。
五元体系Li~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O273K属于简单共饱和型，无复盐或固溶体生成。介稳相图由1个零变量点，4条单变量线和4个相区组成。4个相区为：LiCl H_2O、Li_2CO_3、Li_2SO_4H_2O、LiBO_28H_2O结晶区。由于LiCl与H_2O存在极大的相似性，使其有极强的盐析能力和使其他水合物脱水的作用，在该体系中LiCl对Li_2SO_4有强的盐析作用。
五元体系K~+//Cl~-,CO_3~(2-), SO_4~(2-),B_4O_7~(2-) H_2O及四元体系K~+//Cl, SO_4~(2-), B_4O_7~(2-) H_2O属于简单共饱和型，无复盐或固溶体生成。介稳相图由1个零变量点，4条单变量线和4个相区组成。4个相区为：KCl、K_2B_4O_74H_2O、K_2CO_33/2H_2O、 K_2SO_4结晶区。体系中，硼酸钾表现出明显的介稳性。碳酸钾对其他盐具有强烈的盐析作用，对介稳平衡液相的物化性质影响很大，使平衡液相呈碱性。
五元体系Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-) H_2O及四元子体系Li~+, K~+//Cl~-, SO_4~(2-) H_2O273K介稳相平衡中有锂钾硫酸盐复盐KLiSO_4生成。其五元介稳相平衡立体图由4个共饱点，13条单变量曲线和7个结晶相区组成。7个结晶相区分别对应于LiCl H_2O、Li_2SO_4H_2O、K_2SO_4、KCl、Li_2CO_3、K_2CO_33/2H_2O和锂钾硫酸复盐KLiSO_4的结晶区。该五元体系Li_2CO_3饱和投影图由4个共饱点，9条单变量曲线和6个结晶区组成。研究表明，低温有利于K2SO_4的析出，高温有利于Li_2CO_3的析出。
五元体系Li~+, K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O273K介稳相图由4个共饱点，13条单变量曲线和7个相区组成。7个结晶相区分别对应于LiCl H_2O、Li_2SO_4H_2O、 K2SO_4、KCl、K_2B_4O_7·4H_2O、LiBO_2·8H_2O及锂钾硫酸复盐KLiSO_4结晶区。该五元体系Li2B4O7饱和投影图由4个共饱点，9条单变量曲线和6个结晶区组成。体系4个共饱点均在Li_2B_4O_7饱和投影范围内，共饱点E1为相称共饱点，E2、E3、 E4为不相称共饱点。LiCl H_2O结晶区面积最小，K_2SO_4结晶区面积最大。
273K时硼酸钾、硼酸锂的固相结晶析出形式分别为K_2B_4O_74H_2O和LiBO28H_2O，对应的完整分子式分别为K_2[B_4O_5(OH)_4]2H_2O和Li[B(OH)_4]6H_2O。硼酸盐在水溶液中溶解行为复杂，含硼水盐体系存在明显介稳现象，平衡液相中硼酸根过饱和富集，介稳相图结晶相区明显小于稳定相图结晶相区。各体系中， LiBO28H_2O和K2B4O74H_2O对应的共饱和溶解度曲线上各物化性质随液相化学组成的变化无明显规律性。
在含钾六元体系Li~+, K~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O子体系273K介稳相图中，碳酸锂和硫酸钾结晶相区较大，蒸发时极易析出；溶液中氯化锂含量的高低与硫酸锂析出相区的大小呈正相关性；硼酸盐均以单盐形式存在，可由蒸发制备；氯化锂和碳酸钾结晶相区较小，不能通过蒸发的方式获取。以上析盐规律对于从盐湖卤水中提取锂盐、钾盐和硼酸盐具有重要意义。
Zhabuye Salt Lake, located in Tibet, famous for its abundance resources, such as lithium, potassium, borate, rubidium, and cesium. In order to comprehensive utilize the resource in the Zhabuye Salt Lake, the metastable equilibria of subsystems of the hexahydric system Li~+, K~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O were studied at273K using an isothermal evaporation method, respectively, which have not been reported in the literature. They are four quinary systems Li~+//Cl~-, CO_3~(2-), SO_4~(2-), B_4O_7~(2-) H_2O, K+//Cl-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O,Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-) H_2O and Li~+, K~+//Cl-, SO_4~(2-), B_4O_7~(2-) H_2O, four quaternary systems K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O, Li~+, K~+//Cl~-,SO_4~(2-) H_2O, Li~+, K~+//Cl~-, B_4O_7~(2-) H_2O,and K~+, Na~+//Cl~-, SO_4~(2-) H_2O.
The solubilities, densities and pH values of the equilibrated solutions were determined. The metastable equilibrium phase diagrams, the water-content diagrams, the density vs composition diagrams and the pH values vs composition diagrams of the quaternary systems were plotted the stereo-diagram and projected phase diagrams (saturated with Li_2CO_3or Li2B4O7), corresponding water content diagrams, density vs composition diagrams, the pH value vs composition diagrams and lithium content diagrams of the quinary systems were constructed.
There is no double salt or solid solution formed in the simple quinary system Li~+//Cl~-, CO_3~(2-),SO_4~(2-), B_4O_7~(2-) H_2O. The metastable phase diagram of the system consists of one invariant point, four univariant curves and four crystallization fields. Because of the structure similarity between LiCl and H_2O, salt LiCl has strong salting-out effect and the role of making other hydrate dehydration, with strong salting-out effect onsalt Li2SO_4in this system.
The quinary system K~+//Cl~-, CO_3~(2-), SO_4~(2-),B_4O_7~(2-) H_2O and the quaternary system K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O are of simple type. No double salt or solid solution formed. The metastable phase diagram of the quinary system consists of one invariant point, four univariant curves and four crystallization fields. Salt K2CO3has strong salting-out effect on the other salts. Due to the large solubility, salt K2CO3has strong effect on the physicochemical properties in the solution of this equilibrium system, which presents alkalescency. Potassium borate is metastabled obviously.
Results show that the double salt KLiSO+4is formed in the quinary system Li~+, K~+//Cl~-, CO_3~(2-),SO_4~(2-) H_2O and the subsystem Li~+, K~+//Cl~-, SO_4~(2-) H_2O. The stereo-diagram of the quinary system consists of four invariant point, thirteen univariant curves and seven crystallization fields. The projected diagram of this system (saturated with Li_2CO_3) consists of sixcrystallization fields, nine univariant curves and all the four invariant points. The crystallization fields of Li2SO_4H_2O and K2SO_4are larger, while the salt LiCl H_2O and K2CO33/2H_2O have smaller crystallization fields. A lower temperature is necessary for separating pure potassium sulfate and higher temperature is helpful to obtain lithium carbonate.
The quinary system Li~+, K~+//Cl~-, SO_4~(2-), B_4O_7~(2-) H_2O is of complex type with the double salt KLiSO_4formed. The stereo~-diagram of the quinary system consists of four invariant point, thirteen univariant curves and seven crystallization fields. The projected diagram of this system (saturated with Li2B4O7) consists of six crystallization fields, nine univariant curves and all the four invariant points. Invariant point E1is the commensurate invariant point, while points E2, E3, E4are the incommensurate invariant points. The crystallization field of K_2SO_4is the largest, but the salt LiCl H_2O has smallest crystallization fields.
The crystallizated forms of lithium borate and potassium borate are K_2[B_4O_5(OH)_4]_2H_2O and Li[B(OH)_4]_6H_2O, respectively. Borate salt shows obviously metastablity and has complicated dissolution behaviour in aqueous solution. The borate crystallization fields in metastable equilibrium diagram are smaller than that in stability diagram. For the systems mentioned above, it is found that physicochenmical properties of the equilibrium solutions saturated with the LiBO_2·8H_2O and K_2B_4O_7·4H_2O show irregular changes with the solution composition.
In the metastable equilibria of subsystems of the hexahydric system Li~+, K~+//Cl~-, CO_3~(2-), SO_4~(2-),B_4O_7~(2-) H_2O at273K, salts Li_2CO_3and K_2SO_4precipitate easily due to the larger crystallization fields. The crystallization area of Li_2SO_4H_2O has the positive correlation with the concentration of LiCl in the equilibrated solution. Borate only formed single salts in equilibrated solution, which can be separated by isothermal evaporation method. Salts LiCl H_2O and K2CO33/2H_2O have the smaller crystallization zone, thus it is difficult to obtain them only by evaporation method. This feature is very important to extract lithium, potassium and borate from the salt lake brine.
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