CN111514853A - 一种碳酸钙-废弃煤基活性炭复合吸附剂的制备方法 - Google Patents
一种碳酸钙-废弃煤基活性炭复合吸附剂的制备方法 Download PDFInfo
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Abstract
一种碳酸钙‑废弃煤基活性炭复合吸附剂的制备方法,涉及制药废水中四环素类抗生素去除吸附剂制备技术领域。首先利用废弃煤资源制备废弃煤基多孔活性炭,然后将废弃煤基多孔活性炭、氯化钙和碳酸钠混合通过超声反应器进行反应,制备获得碳酸钙‑废弃煤基活性炭复合吸附剂。本发明利用废弃煤资源以最新发展的超声波湿法球磨组合反应法制备性能优良的多元复合吸附材料。并对吸附性能进行了测试,筛选出性能优良的吸附材料。本发明所制备的碳酸钙‑废弃煤基活性炭复合吸附剂可以用于去除制药废水中四环素类抗生素污水废水环境治理中,并将富集四环素类抗生素进行资源的回收利用,合成一些其它类抗生素及其衍生物,从而有效保护环境,节约资源和能源。
Description
技术领域
本发明涉及制药废水中四环素类抗生素去除吸附剂制备技术领域,具体是涉及一种碳酸钙-废弃煤基活性炭复合吸附剂的制备方法。
背景技术
吸附是通过多孔性固体物质跟流体混合物接触,使流体中某一组分或多个组分在固体表面处产生富集进而以分离的一种方法。固体称为吸附剂,被吸附的物质称为吸附质。因为吸附净化法处理效率高,设备简单,操作方便,且能实现自动控制,因此吸附操作已广泛应用于有机化工、石油化工、环境工程等生产领域,成为一种必不可少的操作单元。
活性炭由于其丰富的孔结构及巨大的比表面积,可有效地去除常规水处理工艺无法解决的溶解性有机物(DOM)。因此,在微污染水深度处理方面获得广泛应用,且发展前景十分广阔。
由于制药废水中四环素的残留量较高,致使该废水在生化处理之前,必须消减其所残留的四环素。人或动物往往不能将服用的抗生素完全吸收,导致大量的抗生素以代谢物甚至原态排入环境中造成的污染,称之为抗生素污染。危害:抗生素的使用会导致病原微生物产生耐药性,使得抗生素能杀死细菌的有效剂量不断增加。低剂量的抗生素长期排入环境中,会造成敏感菌耐药性的增强。并且,耐药基因可以在环境中扩展和演化,对生态环境及人类健康造成潜在威胁。除了能引起细菌的抗药性,抗生素对其它生物也可能产生一定的毒性。
本发明利用废弃煤资源制备煤基活性炭复合吸附剂,期望可以用于去除四环素类抗生素污水废水环境治理中。
发明内容
本发明要解决的技术问题是提出一种碳酸钙-废弃煤基活性炭复合吸附剂的制备方法,以制备可以用于去除四环素类抗生素污水废水环境治理的吸附材料。
为了实现上述目的,本发明所采用的技术方案为:一种碳酸钙-废弃煤基活性炭复合吸附剂的制备方法,首先利用废弃煤资源制备废弃煤基多孔活性炭,然后将废弃煤基多孔活性炭、氯化钙和碳酸钠混合通过超声反应器进行反应,制备获得碳酸钙-废弃煤基活性炭复合吸附剂。
作为本发明的碳酸钙-废弃煤基活性炭复合吸附剂的制备方法的优选技术方案,具体步骤如下:
1)、依次对废弃煤资源进行粉碎、过筛、洗涤、浮选获得炭料,然后烘干、球磨得到较高活性的废弃煤基多孔活性炭;这种方法既能将低品位的或废弃的煤资源处理掉,减小污染,还能制备活性炭,将资源合理充分的再利用。既减少了对原生资源的开采,又节约了大量的能源。
2)、将废弃煤基多孔活性炭、氯化钙和碳酸钠加入至反应容器中,加入水搅拌溶解,然后加入氨水调节溶液的pH值至4~13,充分搅拌后,将反应容器转移至超声反应器中;
3)、开启超声波800W功能,反应20min,反应结束后水洗至不含离子,烘干;
4)、将烘干后的样品放入球磨机中加入适量乙醇进一步球磨20分钟,得到碳酸钙-废弃煤基活性炭复合吸附剂。
作为本发明的碳酸钙-废弃煤基活性炭复合吸附剂的制备方法的进一步优选技术方案,碳酸钙-废弃煤基活性炭复合吸附剂中碳酸钙与废弃煤基活性炭的复合比例为1:0.1~2。所述废弃煤资源为低品位煤或者废弃的无烟煤、褐煤、泥煤、煤焦油沥青烟道炭黑。
与现有技术相比,本发明的有益效果表现在:
1)、本发明以碳酸钙-废弃煤基活性炭复合吸附剂在微观结构与表界面物理化学性能影响的因素,利用吸附性能实验测试装置,对碳酸钙-废弃煤基活性炭复合吸附剂吸附去除制药废水中四环素类抗生素进行实验测试,深入探讨去除制药废水中四环素类抗生素在碳酸钙-废弃煤基活性炭复合吸附剂多孔介质内复杂的表面物理化学状态和相互作用机制。
2)、本发明利用废弃煤资源以最新发展的超声波湿法球磨组合反应法制备性能优良的多元复合吸附材料。采用仪器表征手段XRD,SEM对其结构进行表征,并对吸附性能进行了测试,筛选出性能优良的吸附材料。
3)、本发明所制备的碳酸钙-废弃煤基活性炭复合吸附剂可以用于去除制药废水中四环素类抗生素污水废水环境治理中,并将富集四环素类抗生素进行资源的回收利用,合成一些其它类抗生素及其衍生物,从而有效保护环境,节约资源和能源。
附图说明
以下结合实施例和附图对本发明的碳酸钙-废弃煤基活性炭复合吸附剂的制备方法作出进一步的详述。
图1是实施例1~4制备各系列复合吸附剂的XRD图。
图2是实施例1中以碳酸钙与废弃煤基活性炭的复合比例为2:1制备复合吸附剂的低、中、高倍率SEM图。
图3是实施例1~4制备各系列复合吸附剂的吸附残余四环素百分比曲线图。
图4是实施例1~4制备各系列复合吸附剂的吸附量曲线图。
具体实施方式
实施例1
碳酸钙-废弃煤基活性炭复合吸附剂的制备方法,步骤如下:
1)、依次对废弃无烟煤进行粉碎、过筛、洗涤、浮选获得炭料,然后烘干、球磨得到较高活性的废弃煤基多孔活性炭。
2)、按照制备产物目标摩尔比将废弃煤基多孔活性炭、氯化钙和碳酸钠加入至反应容器中,加入水搅拌溶解,然后加入氨水调节溶液的pH值至12,充分搅拌后,将反应容器转移至超声反应器中。
3)、开启超声波800W功能,反应20min,反应结束后水洗至不含离子,烘干。
4)、将烘干后的样品放入球磨机中加入适量乙醇进一步球磨20分钟,得到碳酸钙-废弃煤基活性炭复合吸附剂,其中碳酸钙与废弃煤基活性炭的复合比例为2:1。
实施例2
控制制备的碳酸钙-废弃煤基活性炭复合吸附剂中碳酸钙与废弃煤基活性炭的复合比例为3:1,制备步骤同实施例1。
实施例3
控制制备的碳酸钙-废弃煤基活性炭复合吸附剂中碳酸钙与废弃煤基活性炭的复合比例为1:1,制备步骤同实施例1。
实施例4
控制制备的碳酸钙-废弃煤基活性炭复合吸附剂中碳酸钙与废弃煤基活性炭的复合比例为1:2,制备步骤同实施例1。
图1是实施例1~4制备各系列复合吸附剂的XRD图。由图1易知,对照PDF标准卡在2θ=23.04°,29.40°,36.00°,39.40°,43.16°,47.48°和48.50°位置附近的各衍射峰处均出现较强的的特征衍射峰和所对应的衍射面分别为(012),(104),(110),(11-3),(202),(018)和(11-6)。4种样品的主要特征衍射峰与(PDF No:41-1475,05-0586)的有关数据,可以确定制备的碳酸钙-废弃煤基活性炭复合吸附剂的晶型为方解石型,实施例1制备的碳酸钙-废弃煤基活性炭复合吸附剂(2:1)的组分结晶度相对较好,对应的XRD特征衍射峰强度的尖锐。通过对复合材料样品的XRD分析,样品的衍射强峰与基本相对应,衍射谱图与其它衍射峰出峰位置相比较有明显的差异。XRD衍射图有明显的衍射峰,而且都比较尖锐,说明合成的复合吸附剂在物相上与实验设计目标物相吻合。
图2是实施例1中以碳酸钙与废弃煤基活性炭的复合比例为2:1制备复合吸附剂的低、中、高倍率SEM图。由图2易知,吸附剂样品孔道结构明显,孔径分布主要在1μm以内,大孔、中孔、微孔都有分布,大孔和中孔比例较小,主要以中微孔分布占据主导位置。微孔分布在改性活性碳表面和孔道壁。碳酸钙-废弃煤基活性炭复合吸附剂呈现多级多尺度分布,继而有利于制药废水中四环素类抗生素污染物的去除。
图3是实施例1~4制备各系列复合吸附剂的吸附残余四环素百分比曲线图。其中,碳酸钙-废弃煤基活性炭复合吸附剂样品用量为40mg,吸附时间为80min。制药废水中四环素类抗生素溶液体积为120mL,初始浓度均为100mg/L。由图3可知,实施例1制备的碳酸钙-废弃煤基活性炭复合吸附剂(2:1)的吸附效果最好,去除率达到99.1%,且所有不同组成的系列产品在随时间的延长,吸附去除效果越好,当吸附时间为70min后,四环素类抗生素去除率不再明显变化。
图4为日光照条件下,不同组成的系列碳酸钙-废弃煤基活性炭复合吸附剂对去除制药废水中四环素类抗生素溶液吸附量与去除时间、物质组成的曲线。其中,碳酸钙-废弃煤基活性炭复合吸附剂材料用量为30mg,吸附时间为105min。制药废水中四环素类抗生素溶液体积为400mL。由图4可知,实施例1制备的碳酸钙-废弃煤基活性炭复合吸附剂(2:1)的吸附效果最好,吸附量达到142mg/g,且所有不同组成的系列产品在随时间的延长,吸附去除效果越好,在吸附时间达到50分钟后,随着时间的增加,吸附量基本上达到稳定,说明吸附过程主要在50分钟内完成,而且吸附效果很好。
由此可知,本发明所制备的碳酸钙-废弃煤基活性炭复合吸附剂可以用于去除制药废水中四环素类抗生素溶液的工业污水废水的环境治理中。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (5)
1.一种碳酸钙-废弃煤基活性炭复合吸附剂的制备方法,其特征在于,首先利用废弃煤资源制备废弃煤基多孔活性炭,然后将废弃煤基多孔活性炭、氯化钙和碳酸钠混合通过超声反应器进行反应,制备获得碳酸钙-废弃煤基活性炭复合吸附剂。
2.如权利要求1所述的制备方法,其特征在于,具体步骤如下:
1)、依次对废弃煤资源进行粉碎、过筛、洗涤、浮选获得炭料,然后烘干、球磨得到较高活性的废弃煤基多孔活性炭;
2)、将废弃煤基多孔活性炭、氯化钙和碳酸钠加入至反应容器中,加入水搅拌溶解,然后加入氨水调节溶液的pH值至4~13,充分搅拌后,将反应容器转移至超声反应器中;
3)、开启超声波800W功能,反应20min,反应结束后水洗至不含离子,烘干;
4)、将烘干后的样品放入球磨机中加入适量乙醇进一步球磨20分钟,得到碳酸钙-废弃煤基活性炭复合吸附剂。
3.如权利要求2所述的制备方法,其特征在于,碳酸钙-废弃煤基活性炭复合吸附剂中碳酸钙与废弃煤基活性炭的复合比例为1:0.1~2。
4.如权利要求2所述的制备方法,其特征在于,所述废弃煤资源为低品位煤或者废弃的无烟煤、褐煤、泥煤、煤焦油沥青烟道炭黑。
5.如权利要求1或2或3或4所述方法制备的碳酸钙-废弃煤基活性炭复合吸附剂在吸附去除制药废水中四环素类抗生素的应用。
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