CN113877531A - 一种耐酸性负载纳米氧化铝生物炭的制备方法与应用 - Google Patents
一种耐酸性负载纳米氧化铝生物炭的制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种耐酸性负载纳米γ‑Al2O3生物炭的制备方法与应用。制备过程包括以下步骤:(1)制粒:将洗净、干燥的笋壳粉碎,过筛备用;(2)烘焙:取适量经(1)步骤处理后的笋壳在惰性气氛中进行烘焙,制得烘焙炭;(3)载铝:取适量烘焙炭置于水热釜内胆中,依次加入铝试剂、钾试剂以及乙醇溶液,通过溶剂热法载铝。(4)炭化:取适量的载铝烘焙炭,炭化,使用酸性溶液和去离子水对其进行反复清洗直至中性,制得耐酸性负载纳米γ‑Al2O3生物炭。本发明制备的耐酸性负载纳米γ‑Al2O3生物炭具有优良的耐酸性能,并且通过氢键作用对Re(VII)具有良好的吸附性能。
Description
技术领域
本发明属于炭材料领域,具体涉及一种耐酸性负载纳米γ-Al2O3生物炭的制备方法及其应用,具体涉及一种对Re(VII)酸性废水具有优良性能和重复利用性的耐酸性负载纳米γ-Al2O3生物炭的制备方法及其应用。
背景技术
铼是一种高熔点的稀有金属,其优良的物化性质使其广泛应用于催化剂和超级合金中。我国对铼的需求量逐年增加,但我国铼的储量较低,且目前没有可供开采的天然铼矿。由于铼具有较高的应用价值和稀缺性,故铼的价格相当昂贵。因此,开展从废渣和二次原料中高效回收铼具有重要意义。铼的二次资源回收主要以湿法工艺为主,一般用无机强酸,例如盐酸溶解含铼固废,形成含Re(VII)的酸性浸出液。
目前,工业中从强酸性溶液中回收铼需要先使用大量碱性试剂将浸出液调节至pH中性,然后使用离子交换法、溶剂萃取法等进行铼的分离,但调节过程会产生大量难以处理的含铼无机盐沉淀及高盐废水,造成含铼资源损失和二次污染,且试剂消耗量大、成本高、选择性差。因此寻找一种经济简便、选择性高、能从强酸性溶液中直接回收铼的方法是十分必要的。
生物炭是一种富含炭的生物质热解产物,其原料来源广泛,作为吸附剂已被应用于重金属的吸附分离。农林工业产生的生物质常被作为废物丢弃、焚烧,这不仅对环境造成了污染而且浪费了大量资源,利用生物质作为可持续的原料用以制备生物炭,但原状生物炭对废液中的Re(VII)选择性差。对生物炭进行负载金属氧化物改性以增加对溶液中Re(VII)的吸附选择性是可行方法之一,但一般无法在酸性溶液中使用,在强酸性溶液中易失去吸附性能。因此开发一种用于选择性分离强酸溶液中铼的生物炭材料是十分必要的。
发明内容
本发明旨在针对现有技术的不足,提供一种耐酸性负载纳米γ-Al2O3生物炭的制备方法,及其用于选择性吸附分离酸性溶液中铼的应用。
为实现上述发明目的,本发明采用如下技术方案:
一种耐酸性负载纳米γ-Al2O3生物炭的制备方法,包括如下步骤:
1)制粒:将洗净,干燥后的笋壳粉碎,过筛,制得笋壳颗粒,备用;
2)烘焙:取适量经步骤1)处理后的笋壳在管式炉中进行烘焙,并通入惰性气体,一段时间后得到烘焙炭;
3)载铝:取适量经步骤2)处理后的烘焙炭进行研磨,并与一定量的铝盐和钾盐均匀分散于一定体积、浓度的乙醇溶液,将上述混合物置于密闭压力容器中保温一段时间;
4)炭化:将步骤3)中保温后的密闭压力容器冷却至室温,将得到的载铝烘焙炭干燥后,在惰性气体保护下进行炭化;
5)干燥:将步骤4)得到的产物洗涤至中性,干燥后得到耐酸性负载纳米γ-Al2O3生物炭。
所述步骤1)中笋壳粉碎后过20-100目筛,干燥温度为60-100℃。
所述步骤2)中惰性气体为氮气、氩气和二氧化碳中的一种,流速为50-150 mL/min,烘焙温度为100-350℃,烘焙时间为0.5-3 h。
所述步骤3)中,铝试剂为硫酸铝、氯化铝、硝酸铝、偏铝酸钠中的一种或几种,钾试剂为氢氧化钾或乙酸钾,铝盐和钾盐的质量比为1:1-1:8,乙醇溶液的体积分数为20%-80%,保温温度为120-240℃,时间为3-24 h。
所述步骤4)中,炭化温度为500-800℃,炭化时间为1-3 h,惰性气体为氮气、氩气和二氧化碳中的一种,流速为50-150 mL/min。
晶粒尺寸在0.341~1.52 nm,γ-Al2O3负载量为10~35wt%。
本发明的有益效果和突出优势在于:
1.本发明以大宗农林废弃物笋壳为吸附剂原料,其来源广泛,成本低廉,用以吸附分离溶液中的Re(VII),达到以废治废的目的。
2.本发明中溶剂热载铝的过程中,钾试剂的添加是为了调节溶液pH为中性,在中性条件下将Al3+以γ-AlOOH负载在烘焙炭上,并使γ-AlOOH更好地负载在烘焙炭表面。
3.本发明所制得的一种耐酸性负载纳米γ-Al2O3生物炭,负载的氧化铝纳米晶体颗粒为γ-Al2O3,晶粒尺寸在0.34~1.52 nm。
4.本发明所制得的耐酸性负载纳米γ-Al2O3生物炭分离去除酸性废水中的Re(VII),具有优秀的耐酸性、选择性和重复利用性能。
附图说明
图1为原状生物炭及实施例1制备的耐酸性负载纳米γ-Al2O3生物炭的XRD图。
图2为实施例7实验结果,验证所制备的耐酸性负载纳米γ-Al2O3生物炭吸附分离铼的作用机理为氢键机理。
图3为实施例3所制备的耐酸性负载纳米γ-Al2O3生物炭和普通Al2O3在强酸溶液中稳定性的对比图。
具体实施方式
实施例1
一种耐酸性负载纳米γ-Al2O3生物炭制备方法及其应用,包括以下步骤:
(1) 制粒:将洗净,60°C干燥后的笋壳粉碎,过60目筛,制得笋壳颗粒,备用;
(2) 烘焙:取1 g经步骤1)处理后的笋壳,在150°C下在管式炉中进行烘焙,并通入N2,1 h后得到烘焙炭,N2流速为60 mL/min;
(3) 载铝:取0.8 g经步骤2)处理后的烘焙炭,研磨10 min,并与1.93 g的AlCl3·6H2O和2.36 g CH3COOK均匀分散于40 mL体积分数为20%的乙醇溶液,将上述混合物置于密闭压力容器中保温24 h;
(4) 炭化:将步骤3)中保温后的密闭压力容器冷却至室温,将得到的载铝烘焙炭干燥后在N2保护下、600 °C炭化2 h,N2流速为100 mL/min;
(5) 干燥:将步骤4)得到的产物洗涤至中性,干燥后得到耐酸性负载纳米γ-Al2O3生物炭,晶粒尺寸在0.74 nm。
实施例2
一种耐酸性负载纳米γ-Al2O3生物炭制备方法及其应用,包括以下步骤:
(1) 制粒:将洗净,80°C干燥后的笋壳粉碎,过80目筛,制得笋壳颗粒,备用;
(2) 烘焙:取2 g经1)步骤处理后的笋壳,在300°C下在管式炉中进行烘焙,并通入N2,1.5 h后得到烘焙炭,N2流速为60 mL/min;
(3) 载铝:取1.5 g经2)步骤处理后的烘焙炭,研磨3 min,并与2.90 g的Al 2(SO4)3和3.14 g KOH均匀分散于80 mL体积分数为40%的乙醇溶液,将上述混合物置于密闭压力容器中保温12 h;
(4) 炭化:将步骤3)中保温后的密闭压力容器冷却至室温,将得到的载铝烘焙炭干燥后在N2保护下、600 °C炭化2 h, N2流速为100 mL/min;
(5) 干燥:将步骤4)得到的产物洗涤至中性,干燥后得到耐酸性负载纳米γ-Al2O3生物炭,晶粒尺寸在1.47 nm。
实施例3
一种耐酸性负载纳米γ-Al2O3生物炭的铼吸附性能
将实施例1制备的耐酸性负载纳米γ-Al2O3生物炭对含铼溶液进行吸附实验,吸附剂与含铼溶液(20 mg/L)的固液比为0.8 g/L,HCl浓度为2 mol/L,在25℃下进行吸附实验,回收率为92.96%。
实施例4
一种耐酸性负载纳米γ-Al2O3生物炭的铼吸附性能
将实施例2制备的一种耐酸性负载纳米γ-Al2O3生物炭对含铼溶液进行吸附实验,吸附剂与含铼溶液(40 mg/L)的固液比为1 g/L,HCl浓度为4 mol/L,在30℃下进行吸附实验,回收率为90.33%。
实施例5
一种耐酸性负载纳米γ-Al2O3生物炭的铼吸附选择性
将实施例1制备的耐酸性负载纳米γ-Al2O3生物炭加入到Re(VII):SO4 2-摩尔浓度比为1:100的混合溶液,固液比为0.8 g/L,Re(VII)初始浓度为20 mg/L,盐酸浓度为2 M。将上述体系在25℃下进行吸附实验,Re(VII)回收率为91.89%。
实施例6
一种耐酸性负载纳米γ-Al2O3生物炭的铼吸附选择性
将实施例2制备的耐酸性负载纳米γ-Al2O3生物炭加入到Re(VII): NO3 -摩尔浓度比为1:100的混合溶液,固液比为1 g/L,Re(VII)初始浓度为40 mg/L,盐酸浓度为4 M。将上述体系在30℃下进行吸附实验,Re(VII)回收率为88.02%。
实施例7
一种耐酸性负载纳米γ-Al2O3生物炭对溶液中Re(VII)的吸附机理研究
取实施例2中的所制备的耐酸性负载纳米γ-Al2O3生物炭,对含铼溶液进行吸附机理探索实验,乙醇体积浓度为0~60%,吸附剂与含铼溶液(40 mg/L)的固液比为1 g/L,HCl浓度为3 mol/L,在30℃下进行实验。乙醇的添加会影响氢键的生成,当乙醇浓度逐渐增加时,耐酸性负载纳米γ-Al2O3生物炭对溶液中Re(VII)的吸附率逐渐降低,说明负载纳米γ-Al2O3生物炭对酸性溶液中的Re(VII)的吸附机理主要为负载纳米γ-Al2O3表面与铼之间发生氢键相互作用。
实施例8
一种耐酸性负载纳米γ-Al2O3生物炭的铼吸附选重复利用性能
取实施例3中的所分离出的耐酸性负载纳米γ-Al2O3生物炭,在0.2 mol/L的KOH溶液中进行解吸,解吸时间为12 h。分离耐酸性负载纳米γ-Al2O3生物炭和解吸液,耐酸性负载纳米γ-Al2O3生物炭在80℃下烘干,得到再生后的耐酸性负载纳米γ-Al2O3生物炭。取再生后的耐酸性负载纳米γ-Al2O3生物炭,加入到Re (VI)初始浓度20 mg/L的Re(VII)溶液中,固液比为0.8 g/L,HCl浓度为2 mol/L,在25℃下进行吸附实验,回收率为90.06%。由此可知:本发明制得的耐酸性负载纳米γ-Al2O3生物炭能够重复使用,按照此步骤重复利用该材料5次后,铼的回收率仍能达到88.74%。与实施例3相比,再生5次后的耐酸性负载纳米γ-Al2O3生物炭对HReO4的去除率为再生前的95.46%。
实施例9
一种耐酸性负载纳米γ-Al2O3生物炭和Al2O3在强酸溶液中的稳定性对比
取实施例3中的所制备的耐酸性负载纳米γ-Al2O3生物炭,在强酸性溶液(2 mol/LHCl)中进行稳定性对比。将耐酸性负载纳米γ-Al2O3生物炭和Al2O3颗粒各1 g置于2 mol/LHCl中,震荡2 h后回收并称取质量,烘干后再次投入同样浓度的盐酸溶液中去,如此循环5次。耐酸性负载纳米γ-Al2O3生物炭在循环过程中质量基本保持不变,第5次称取质量为0.99 g,且对Re(VII)的吸附率是未循环的95%以上;而Al2O3颗粒在首次投入强酸溶液后质量损失62.14%,第3次循环过程中质量损失100%。
以上所述仅为本发明的较佳实施列,凡依本发明申请专利范围所做的均等变化与修饰,皆应属于本发明的涵盖范围。
Claims (10)
1.一种耐酸性负载纳米γ-Al2O3生物炭的制备方法,其特征在于:包括如下步骤:
1)制粒:将洗净,干燥后的笋壳粉碎,过筛,制得笋壳颗粒,备用;
2)烘焙:取经步骤1)处理后的笋壳在管式炉中进行烘焙,并通入惰性气体,一段时间后得到烘焙炭;
3)载铝:取经步骤2)处理后的烘焙炭进行研磨,并与铝试剂和钾试剂均匀分散于乙醇溶液,将上述混合物置于密闭压力容器中保温一段时间;
4)炭化:将步骤3)中保温后的密闭压力容器冷却至室温,将得到的载铝烘焙炭干燥后,在惰性气体保护下进行炭化;
5)干燥:将步骤4)得到的产物洗涤至中性,干燥后得到耐酸性负载纳米γ-Al2O3生物炭。
2.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭制备的方法,其特征在于:所述步骤1)中笋壳粉碎后过20-100目筛,干燥温度为60-100℃。
3.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭制备的方法,其特征在于:所述步骤2)中惰性气体为氮气、氩气和二氧化碳中的一种,流速为50-150 mL/min。
4.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭制备的方法,其特征在于:所述步骤2)中烘焙温度为100-350℃,烘焙时间为0.5-3 h。
5.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭制备的方法,其特征在于:所述步骤3)中,铝试剂为硫酸铝、氯化铝、硝酸铝、偏铝酸钠中的一种或几种,钾试剂为氢氧化钾或乙酸钾,铝试剂和钾试剂的质量比为1:1-1:8。
6.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭制备的方法,其特征在于:所述步骤3)中,乙醇溶液的体积分数为20%-80%。
7.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭制备的方法,其特征在于:所述步骤3)中,密闭压力容器中保温温度为120-240℃,时间为3-24 h。
8.根据权利要求1所述的一种耐酸性负载纳米γ-Al2O3生物炭的制备方法,其特征在于:所述步骤4)中,炭化温度为500-800℃,炭化时间为1-3 h,惰性气体为氮气、氩气和二氧化碳中的一种,流速为50-150 mL/min。
9.如权利要求1-8任一项所述制备方法得到的耐酸性负载纳米γ-Al2O3生物炭,其特征在于:晶粒尺寸在0.341~1.52 nm,γ-Al2O3负载量为10~35wt%。
10.如权利要求9所述的耐酸性负载纳米γ-Al2O3生物炭的应用,其特征在于,用于高效选择性吸附分离酸性废液中稀散金属铼,具体方法包括以下步骤:
1)配置盐酸浓度为0.1~4 mol/L HCl的Re(VII)溶液,加入耐酸性纳米γ-Al2O3生物炭;
2)置于摇床充分振荡一段时间,取上清液检测Re(VII)的浓度。
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