CN106311131B - 氢氧化钠改性废砖、基于该废砖的复合材料及用其吸附水体重金属的方法 - Google Patents
氢氧化钠改性废砖、基于该废砖的复合材料及用其吸附水体重金属的方法 Download PDFInfo
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Abstract
本发明公开了氢氧化钠改性废砖、基于该废砖的复合材料及用其吸附去除水体重金属的方法,氢氧化钠改性废砖的制备方法包括:步骤S1,将废砖粉碎,过筛分级,选出0.5‑1.2mm粒径的砖粒;步骤S2,将砖粒用水洗涤、过滤,100‑110℃烘干;步骤S3,将步骤S2所得砖粒置于氢氧化钠溶液中超声浸泡改性;氢氧化钠溶液摩尔浓度为1‑10mol/L,氢氧化钠溶液体积为砖粒质量的10‑20倍。将改性废砖浸泡于四氯化钛的四氢呋喃溶液中,再向其中通入干燥的硫化氢气体,反应完成后过滤取出,烘干即得无定型二硫化钛负载的改性废砖。本发明复合材料通过将无定型二硫化钛负载于改性废砖上制成,对水体中重金属的吸附能力显著高于改性废砖、无定型二硫化钛单独吸附量之和。
Description
技术领域
本发明属于环境科学与工程领域,具体涉及氢氧化钠改性废砖、基于该废砖的复合材料及用其吸附水体重金属的方法。
背景技术
研究表明,不溶于水的金属硫化物可以用以去除水中阳离子,如林璋等硫化锌基纳米材料用以去除水中的阳离子染料(CN201210201118.1),容学德等利用硫化锌纳米微粒吸附去除水中的镉离子(广东化工,2013(2):13-15)。然而,现有文献报道的方法均是用晶型的纳米级材料进行吸附,首先晶型材料的比表面积较小,吸附量有限;其次,纳米级材料颗粒较小,吸附后难以分离,容易造成材料流失。
目前我国城市建筑垃圾中实体粘土砖约占总量的30-50%。粘土砖由粘土、页岩和煤矸石等原料混合经高温烧结而成,主要成分为石英(约占67%)、Al2O3(约占12%)以及Fe2O3(约占8%),且存在一定的机械强度和大量的孔隙,可以作为吸附剂或者载体被回收利用。因此,对建筑废转进行资源化利用作为一种新的处理途径,不仅可以为污水净化提供一种新型廉价的吸附材料或载体,对建筑行业和环境保护也都有巨大的经济和社会效益。但是,由于废砖的表面积较低(20m2/g左右),制约了其对污染物的吸附以及作为载体的固载量,限制了废砖的有效利用率,因此,需要增大废砖的表面积来提高废砖的回收和利用率。
发明内容
本发明的第一目的是提供一种氢氧化钠改性的废砖,以提高废砖的比表面积;
本发明的第二目的是提供一种基于上述改性废砖的复合材料,利用改性废砖作为载体负载无定型二硫化钛得到复合吸附剂;
本发明的第三目的是提供一种利用上述改性废砖以及基于改性废砖的复合材料吸附水体重金属的方法,用于吸附去除水体中Hg2+、Cd2+、Cr3+、Pb2+等重金属。
上述目的是通过如下技术方案实现的:
一种氢氧化钠改性废砖,通过如下方法制备而成:将废砖粉碎、洗涤、过滤、烘干后,置于氢氧化钠溶液中浸泡改性,再洗涤、烘干即得。
优选地,制备方法具体包括如下步骤:
步骤S1,将废砖粉碎,过筛分级,选出0.5-1.2mm粒径的砖粒;
步骤S2,将上述砖粒用水洗涤、过滤后,于100-110℃烘干;
步骤S3,将步骤S2所得砖粒置于氢氧化钠溶液中超声浸泡改性;所述氢氧化钠溶液的摩尔浓度为1-10mol/L,氢氧化钠溶液的体积为砖粒质量的10-20倍;
步骤S4,将改性后的砖粒洗涤至中性,100-110℃烘干即得。
优选地,步骤S3中,改性温度为40-50℃,超声频率为50-70KHz,超声时间为3-5h。
一种基于上述改性废砖的复合材料,通过如下方法制成:先将改性废砖浸泡于四氯化钛的四氢呋喃溶液中,再向其中通入干燥的硫化氢气体,最后过滤取出,烘干即得无定型二硫化钛负载的改性废砖。
优选地,制备方法具体包括:
步骤S1,将改性废砖浸泡于四氯化钛的四氢呋喃溶液中2-4小时;四氯化钛的浓度为0.06-0.1mol/L,体积为改性废砖质量的5-10倍;
步骤S2,再于25-30℃条件下通入干燥的硫化氢气体反应;
步骤S3,反应完成后过滤取出,烘干即得无定型二硫化钛负载的改性废砖。
优选地,步骤S3烘干条件为:30-40℃真空烘干。
上述复合材料在吸附净化水体中重金属方面的应用。
优选地,吸附净化水体中重金属的方法为:先将待处理的水体过滤,去除不溶性杂质,调节其pH至4-6,再将其以4-40BV/h的流速通过装填有所述复合材料的吸附柱床层即可。
优选地,所述复合材料使用后的脱附再生方法为:将浓度为3-4mol/L的盐酸溶液以0.5-5BV/h的流速通过吸附柱床层,时间为0.5-1.5h,脱附再生温度为20-40℃。
本发明的有益效果:
1、本发明提供的改性废砖比表面积显著增大;
2、本发明提供的复合材料通过将无定型二硫化钛负载于改性废砖上制备而成,吸附能力显著高于改性废砖、无定型二硫化钛单独使用时的吸附量之和,比现有技术具有显著的进步;
3、单独使用纳米二硫化钛时,吸附后二硫化钛不易分离,本发明复合材料克服了该缺陷;
4、本发明提供的改性废砖和基于该改性废砖的复合材料可以用于吸附净化水体中的重金属,且脱附再生后可以反复套用。
附图说明
图1为测试1、2、3对水体中二价镉离子的去除率(%)。
具体实施方式
下面结合附图和实施例具体介绍本发明的技术方案。
实施例1:氢氧化钠改性废砖的制备
制备方法具体包括如下步骤:
步骤S1,将废砖粉碎,过筛分级,选出0.5-1.2mm粒径的砖粒;
步骤S2,将上述砖粒用水洗涤、过滤后,于105℃烘干;
步骤S3,将步骤S2所得砖粒置于氢氧化钠溶液中超声浸泡改性;所述氢氧化钠溶液的摩尔浓度为5mol/L,氢氧化钠溶液的体积为砖粒质量的15倍;改性温度为45℃,超声频率为60KHz,超声时间为4h;
步骤S4,将改性后的砖粒洗涤至中性,105℃烘干即得。
比表面积从19.5m2/g提高到60.5m2/g,增加了2.1倍。
实施例2:氢氧化钠改性废砖的制备
制备方法具体包括如下步骤:
步骤S1,将废砖粉碎,过筛分级,选出0.5-1.2mm粒径的砖粒;
步骤S2,将上述砖粒用水洗涤、过滤后,于100℃烘干;
步骤S3,将步骤S2所得砖粒置于氢氧化钠溶液中超声浸泡改性;所述氢氧化钠溶液的摩尔浓度为1mol/L,氢氧化钠溶液的体积为砖粒质量的20倍;改性温度为50℃,超声频率为70KHz,超声时间为5h;
步骤S4,将改性后的砖粒洗涤至中性,100℃烘干即得。
比表面积从19.5m2/g提高到43.8m2/g,增加了1.2倍。
实施例3:氢氧化钠改性废砖的制备
制备方法具体包括如下步骤:
步骤S1,将废砖粉碎,过筛分级,选出0.5-1.2mm粒径的砖粒;
步骤S2,将上述砖粒用水洗涤、过滤后,于110℃烘干;
步骤S3,将步骤S2所得砖粒置于氢氧化钠溶液中超声浸泡改性;所述氢氧化钠溶液的摩尔浓度为10mol/L,氢氧化钠溶液的体积为砖粒质量的10倍;改性温度为40℃,超声频率为50KHz,超声时间为3h;
步骤S4,将改性后的砖粒洗涤至中性,110℃烘干即得。
比表面积从19.5m2/g提高到63.3m2/g,增加了2.3倍。
实施例4:基于改性废砖的复合材料的制备
先将改性废砖浸泡于四氯化钛的四氢呋喃溶液中,再向其中通入干燥的硫化氢气体,最后过滤取出,烘干即得无定型二硫化钛负载的改性废砖。
具体包括如下步骤:
步骤S1,将改性废砖浸泡于四氯化钛的四氢呋喃溶液中;四氯化钛溶液的浓度为0.08mol/L,体积为改性废砖质量的8倍;
步骤S2,28℃条件下向其中通入干燥的硫化氢气体反应;
步骤S3,过滤取出,35℃真空烘干即得无定型二硫化钛负载的改性废砖。
实施例5:基于改性废砖的复合材料的制备
先将改性废砖浸泡于四氯化钛的四氢呋喃溶液中,再向其中通入干燥的硫化氢气体,最后过滤取出,烘干即得无定型二硫化钛负载的改性废砖。
具体包括如下步骤:
步骤S1,将改性废砖浸泡于四氯化钛的四氢呋喃溶液中;四氯化钛溶液的浓度为0.1mol/L,体积为改性废砖质量的5倍;
步骤S2,25℃条件下向其中通入干燥的硫化氢气体,反应;
步骤S3,过滤取出,30℃真空烘干即得无定型二硫化钛负载的改性废砖。
实施例6:基于改性废砖的复合材料的制备
先将改性废砖浸泡于四氯化钛的四氢呋喃溶液中,再向其中通入干燥的硫化氢气体,最后过滤取出,烘干即得无定型二硫化钛负载的改性废砖。
具体包括如下步骤:
步骤S1,将改性废砖浸泡于四氯化钛的四氢呋喃溶液中;四氯化钛溶液的浓度为0.06mol/L,体积为改性废砖质量的10倍;
步骤S2,30℃条件下向其中通入干燥的硫化氢气体,反应;
步骤S3,过滤取出,40℃真空烘干即得无定型二硫化钛负载的改性废砖。
实施例7:对比实施例
复合材料:取100g实施例1制备的改性废砖,按照实施例4方法制备得复合材料(105.2g,经计算可知该复合材料中无定型二硫化钛占5.2g)。
对比A:仅100g实施例1制备的改性废砖。
对比B:仅5.2g纯无定型二硫化钛,不负载在载体上。
实施例8:应用与效果实施例
测定本发明基于该废砖的复合材料对水体中二价镉离子的吸附能力。
水体中二价镉离子的浓度为80mg/L。
测试方法为:
先将待处理的水体过滤,去除不溶性杂质,调节其pH至5.5。
测试1,复合材料:取100LpH为5.5的水体以20BV/h的流速通过装填有复合材料(实施例7中所述复合材料,105.2g)的吸附柱床层。47.5小时通过完毕。
测试2,对比A:取100LpH为5.5的水体通过装填有改性废砖(实施例7中的对比A所示100g改性废砖)的吸附柱床层。47.5小时通过完毕。
测试3,对比B:将实施例7中的对比B所示5.2g无定型二硫化钛添加进100LpH为5.5的水体中,搅拌47.5小时。
测试1、2、3中材料对于100L水体中二价镉离子的去除率如下表和图1。
测试1 | 测试2 | 测试3 | |
二价镉离子去除率(%) | 98.6 | 18.4 | 46.5 |
测试1的二价镉离子去除率远大于测试2、3的去除率之和,证明将无定型二硫化钛负载在改性废砖后形成的复合材料对二价镉离子的去除率显著提高。
本领域技术人员知道,理论上,二硫化钛负载在改性废砖后必然会占据改性废砖上的吸附位点,复合材料的吸附去除效果应低于二硫化钛和改性废砖吸附效果之和。这说明本发明相对于现有技术具有突出的实质性特点和显著的进步。
复合材料使用后的脱附再生方法为:将浓度为3-4mol/L的盐酸溶液以0.5-5BV/h的流速通过吸附柱床层,时间为0.5-1.5h,脱附再生温度为20-40℃。
实施例9:应用实例
废水改为含Hg2+、Cr3+、Pb2+等金属离子的废水后,去除率稍有差异,但仍达90%以上。
上述实施例的作用仅在于说明本发明的实质性内容,但并不以此限定本发明的保护范围。本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和保护范围。
Claims (4)
1.一种基于改性废砖的复合材料,其特征在于,通过如下制备方法制备:
步骤S1,将改性废砖浸泡于四氯化钛的四氢呋喃溶液中2-4小时;四氯化钛的浓度为0.06-0.1mol/L,溶液体积为改性废砖质量的5-10倍;
步骤S2,再于25-30℃条件下通入干燥的硫化氢气体反应;
步骤S3,反应完成后过滤取出,30-40℃真空烘干即得;
其中,所述改性废砖通过如下制备方法制备:
步骤S1,将废砖粉碎,过筛分级,选出0.5-1.2mm粒径的砖粒;
步骤S2,将上述砖粒用水洗涤、过滤后,于100-110℃烘干;
步骤S3,将步骤S2所得砖粒置于氢氧化钠溶液中超声浸泡改性;所述氢氧化钠溶液的摩尔浓度为1-10mol/L,氢氧化钠溶液的体积为砖粒质量的10-20倍;改性温度为40-50℃,超声频率为50-70KHz,超声时间为3-5h;
步骤S4,将改性后的砖粒洗涤至中性,100-110℃烘干即得。
2.权利要求1所述的复合材料在吸附净化水体中重金属方面的应用。
3.根据权利要求2所述的应用,其特征在于,吸附净化水体中重金属的方法为:先将待处理的水体过滤,去除不溶性杂质,调节其pH至4-6,再将其以4-40BV/h的流速通过装填有所述复合材料的吸附柱床层即可。
4.根据权利要求3所述的应用,其特征在于,所述复合材料使用后的脱附再生方法为:将浓度为3-4mol/L的盐酸溶液以0.5-5BV/h的流速通过吸附柱床层,时间为0.5-1.5h,脱附再生温度为20-40℃。
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