CN108636341A - 一种提锂吸附剂的成型方法 - Google Patents
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 32
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 32
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Abstract
本发明涉及一种提锂吸附剂的成型方法。其特征在于使用钛型锂离子筛或者锰型锂离子筛作为吸附剂原粉,将聚合物溶于有机溶剂制成粘结剂,采用转动成型法对吸附剂原粉进行成球。本方法制备工艺简单,可大大减少成型吸附剂中聚合物的含量,节约成本、吸附速率快、吸附性能稳定。
Description
技术领域
本发明涉及一种提锂吸附剂的成型方法。
背景技术
锂及其化合物被广泛地运用到玻璃、陶瓷、医药、航空和电池等领域。电动汽车的发展使得可充电的锂电池备受关注。锂主要来源于锂辉石、海水和卤水,其中,卤水中锂储量约占锂资源总量的66%,因此对液态锂资源的开发是现在锂资源开采的趋势。
吸附法可选择性从卤水中吸附提锂,不受到其Mg/Li限制,工艺过程无污染,受到广泛关注。吸附提锂的技术关键在于吸附剂的吸附选择性和稳定性。常见的提锂吸附剂主要有锂离子交换树脂、铝盐吸附剂、锰基锂离子筛和钛基锂离子筛等。相对于离子交换树脂和铝盐吸附剂,锰型锂离子筛和钛型锂离子筛对锂离子吸附快、且吸附容量较高。
粉状的锰型锂离子筛和钛型锂离子筛吸附剂由于流动性差、回收困难,制约着其在工业上的实际运用。对于锰型锂离子筛和钛型锂离子筛,常见的成型方法主要是采用反溶剂法对提锂吸附剂进行造粒或制膜成型,但是成型过程中由于粘合剂的添加量较高,制得的成型吸附剂的吸附量会出现明显的下降。
发明内容
本发明的目的是为了改进现有技术的不足而提供一种提锂吸附剂的成型方法,本方法工艺简单,可减少粘合剂的添加量,制得的成型吸附剂具有吸附量高、吸附速率快、吸附选择性高、吸附稳定性好的特点。
本发明的技术方案为:一种提锂吸附剂的成型方法,其特征在于,使用钛型锂离子筛或者锰型锂离子筛作为吸附剂原粉,在60℃~80℃下,将聚合物溶于有机溶剂制成粘结剂,冷却(一般常温在30℃下),以甘油或者石墨粉作为润滑剂,将粘结剂和润滑剂分别添加到离子筛原粉中并混合均匀,采用转动成型法对混合物进行成球;将成球后的提锂吸附剂干燥去除有机溶剂,得到提锂吸附剂。
优选所述的钛型锂离子筛为H2TiO3,所采用的锰型锂离子筛为H1.33Mn1.67O4或H1.66Mn1.66O4。
优选所述的聚合物为聚氯乙烯、聚丙烯腈或聚偏氟乙烯。优选所述的有机溶剂为N,N-二甲基甲酰胺、二甲基乙酰胺或二甲基亚砜。优选粘结剂中聚合物的质量分数为1%~13%。
将粘结剂和润滑剂分别添加到离子筛原粉中,控制有机溶剂与离子筛原粉的质量比优选为0.07~1.32,润滑剂与离子筛原粉的质量比优选为0.01~0.12。
优选所述的干燥温度为40℃~80℃,干燥时间为1h~10h。
优选本发明所制得的提锂吸附剂的粒径为1mm~4mm。将干燥后的成球吸附剂用于吸附模拟卤水中锂离子,其锂吸附量可达到20mg/g~40mg/g,且吸附选择性和稳定性良好。
成球的吸附剂吸附锂离子后采用无机酸酸洗脱附,脱附后的吸附剂可重复使用。
本方法还提供了一种上述成球吸附剂在含锂溶液中吸附提锂的运用。其中,所述的含锂溶液可为卤水或海水,也可为模拟配制的含锂溶液。所述的液态锂资源中,锂离子含量为40mg/L~800mg/L。所述的成球吸附剂与液态锂溶液的固液比为1g/L~4g/L。所述的成球吸附剂在液态锂溶液中的吸附温度为20℃~50℃。所述的成球吸附剂在液态锂溶液中的吸附时间为8h~24h,将成球吸附剂用于吸附不同锂含量的溶液,其锂吸附量可达到20mg/g~42mg/g,且稳定性良好,对其他金属离子基本不存在吸附现象。
本发明所用试剂和原料均市售可得。
有益效果:
1、本发明工艺简单,可有效地减少成球吸附剂中聚合物的添加量、节约成本。
2、本发明制得的成球吸附剂对锂离子的吸附量高、吸附剂速率快、吸附选择性好。
附图说明
图1为实施例1制得的成球吸附剂的XRD图。
图2为实施例1制得的成球吸附剂的FTIR图。
图3为实施例1制得的成球吸附剂的热重分析图。
图4为实施例2制得的成球吸附剂的SEM图。
图5为实施例2制得的成球吸附剂的5次循环吸附量变化。
具体实施方式
下面通过实施例对本发明做进一步说明,其目的仅在于更好的理解本发明的内容,但并不因此将本发明限制在所述的实施例范围之中。
SEM仪器型号:S-4800,Hitachi,Japan;ICP仪器型号:Optima DV7000,PerkinElme,USA;傅里叶变换红外光谱仪型号:AVATAR360,Nicolet Instrument,USA;热分析仪型号:JC503-WCT-1D/2D,Baiwan electronic,China;XRD仪器型号:Smartlab,Rigaku,Japan,扫描范围:10-70°,步长0.02,扫描速度:20°/min,扫描电压40kV,电流40mA。
实施例1
1、采用钛型锂离子筛H2TiO3作为吸附剂原粉,在80℃下,将1g的聚氯乙烯溶于14g的N,N-二甲基甲酰胺中配成粘结剂,加入11.375g的H2TiO3和0.125g的甘油。采用滚动成型法对混合物进行成球,对获得的成球吸附剂在60℃下干燥5h,最终获得的成球吸附剂粒径为3mm。成球吸附剂的XRD图谱、FTIR图谱、热重分析图分别见图1-3。由图1可以发现所制备出的成球吸附剂的衍射峰未出现聚氯乙烯的非结晶相,说明聚氯乙烯的添加量很少。图2表明了所制备出的成球吸附剂中不含N,N-二甲基甲酰胺的溶剂峰,说明溶剂已被有效地去除。图3表明了成球吸附剂的失重率为24.39wt%,失重率较少,这说明了成球吸附剂中聚合物的含量较少。
2、称取1g的成球吸附剂,放入4L的锂离子浓度为800mg/L模拟卤水中,在50℃下恒温磁力搅拌吸附24h,钛型锂离子筛的吸附量为41.25mg/g。
实施例2
1、采用钛型锂离子筛H2TiO3作为吸附剂原粉,在60℃下,将0.5g的聚氯乙烯溶于7.14g的N,N-二甲基甲酰胺中配成粘结剂,加入7.747g的H2TiO3和0.083g的甘油。采用滚动成型法对混合物进行成球,对获得的成球吸附剂在80℃下干燥2h,最终获得的成球吸附剂粒径为2mm。成球吸附剂的SEM图像见图4。图4表明了H2TiO3的粒径约为70nm,H2TiO3在成球吸附剂表面分别均匀。
2、称取1g的成球吸附剂用于1L的锂离子浓度为40mg/L的模拟卤水吸附在30℃下恒温磁力搅拌吸附24h,其吸附量为29.49mg/g。
3、将吸附锂后的样品,在60℃下,用浓度0.1mol/L的盐酸进行酸洗脱附,脱附时间为10h。然后在80℃干燥1h得到再生后的成球吸附剂。循环过程按照2和3重复进行。成球吸附剂的循环量如图5所示,吸附剂的吸附量能稳定在28mg/g,说明了成球吸附剂具有很好的吸附循环稳定性。
4、称取1g的成球吸附剂,用于1L的钠离子、镁离子、钾离子、钙离子、锂离子各离子浓度分别约为10mmol/L的模拟卤水吸附,在20℃下恒温磁力搅拌吸附8h,计算成型吸附剂对各金属离子的吸附量。见表1。
表1成球吸附剂在模拟卤水中的吸附性能
其中,C0和Ce分别为溶液中初始和吸附平衡时的溶液中的各金属离子浓度(mg/L);Qe为成型吸附剂对各金属离子的平衡吸附量(mg/g);Kd为成型吸附剂对各金属离子的分配系数;表示锂离子对其他金属离子的分离因子;CF表示各金属的浓度因子(L/g)。由表1可知,成型吸附剂对锂离子吸附量为18.28mg/g,对其他金属离子基本不存在吸附,选择性好。
实施例3
采用锰型锂离子筛H1.33Mn1.67O4作为吸附剂原粉,在80℃下,将0.99g的聚偏氟乙烯溶于6.67g的二甲基亚砜中配成粘结剂,加入89g的H1.33Mn1.67O4和10g的甘油。采用滚动成型法对混合物进行成球,对获得的成球吸附剂在40℃下干燥10h,最终获得的成球吸附剂粒径为4mm。
成球吸附剂的吸附和实施例1相同,其吸附量为20.05mg/g。
实施例4
采用锰型锂离子筛H1.66Mn1.66O4作为吸附剂原粉,在80℃下,将0.11g的聚丙烯腈溶于10g的二甲基乙酰胺中配成粘结剂(聚丙烯腈在粘结液中的固含量为1%),加入9.6g的H1.66Mn1.66O4和0.3g的石墨。采用滚动成型法对混合物进行成球,对获得的成球吸附剂在50℃下干燥8h,最终获得的成球吸附剂粒径为2mm。
成球吸附剂的吸附和实施例1相同,其吸附量为25.22mg/g。
Claims (8)
1.一种提锂吸附剂的成型方法,其特征在于,使用钛型锂离子筛或者锰型锂离子筛作为吸附剂原粉,在60℃~80℃下,将聚合物溶于有机溶剂制成粘结剂,冷却,以甘油或者石墨粉作为润滑剂,将粘结剂和润滑剂分别添加到离子筛原粉中并混合均匀,采用转动成型法对混合物进行成球;将成球后的提锂吸附剂干燥去除有机溶剂,得到提锂吸附剂。
2.根据权利要求1所述的成型方法,其特征在于所述的钛型锂离子筛为H2TiO3,所采用的锰型锂离子筛为H1.33Mn1.67O4或H1.66Mn1.66O4。
3.根据权利要求1所述的成型方法,其特征在于所述的聚合物为聚氯乙烯、聚丙烯腈或聚偏氟乙烯。
4.根据权利要求1所述的成型方法,其特征在于所述的有机溶剂为N,N-二甲基甲酰胺、二甲基乙酰胺或二甲基亚砜。
5.根据权利要求1所述的成型方法,其特征在于粘结剂中聚合物的质量分数为1%~13%。
6.根据权利要求1所述的成型方法,其特征在于将粘结剂和润滑剂分别添加到离子筛原粉中,控制有机溶剂与离子筛原粉的质量比为0.07~1.32,润滑剂与离子筛原粉的质量比0.01~0.12。
7.根据权利要求1所述的成型方法,其特征在于所述的干燥温度为40℃~80℃,干燥时间为1h~10h。
8.根据权利要求1所述的成型方法,其特征在于制得的提锂吸附剂的粒径为1mm~4mm。
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