CN107915215B - 一种生物炭的制备方法及其应用 - Google Patents
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Abstract
本发明公开了生物材料制备领域的一种生物炭的制备方法及其应用。该方法具体步骤为:先将洗净的香蕉皮在含有造孔剂的溶液中浸泡并冻干,然后在惰性气氛下煅烧,之后在含氮气体气氛下球磨并过筛,最后经过酸洗、水洗和离心收集得到生物炭。本发明在香蕉皮碳化前加入造孔剂,使碳化后的材料具有更加丰富的孔径;对碳化后的材料进一步在含氮气体下进行球磨,不仅可以提高其比表面积,还可以在生物炭中引入氮源;制备的生物炭材料稳定性强,可以应用于大气中颗粒物和有机物的过滤、水中有机物的吸附以及作为超级电容器电极材料,且可重复使用。
Description
技术领域
本发明属于生物材料制备领域,具体涉及一种生物炭的制备方法及其应用。
背景技术
香蕉皮中富含糖类、蛋白质、脂肪及各类无机元素,并且含有很多孔隙和纤维状结构,这种纤维状结构通过一定的加工和碳化,可以形成天然的介孔(2-50nm)和大孔(>50nm),成为一种非常好的吸附材料和过滤材料。
专利“CN106147781A”(一种用于修复重金属污染土壤固化剂的制备方法)公开了一种通过碳化后的香蕉皮和酸化海泡石混合的土壤固化剂。但是该方法中对香蕉皮的处理程度还不够,3%的氢氧化钠溶液浓度较低,仅能对香蕉皮有一定的活化,无法对香蕉皮在高温下有效造孔。
专利“CN102895952B”(一种选择性吸附金离子的多孔碳材料及其制备方法和应用)公开了一种通过粉碎机粉碎香蕉皮并高温碳化得到的多孔碳材料。但是该碳化温度较低,且无其他扩孔处理,香蕉皮的孔径仍然有限。
可见,目前基于香蕉皮制备得到的生物炭还存在一定的局限性。
发明内容
本发明的目的是提出一种生物炭的制备方法及其应用,具体技术方案如下:
一种生物炭的制备方法,包括如下步骤:
(1)将洗净的香蕉皮在含有造孔剂的溶液中浸泡,之后冻干处理;
(2)在惰性气体气氛下,将冻干后的香蕉皮煅烧;
(3)在含氮气体气氛下,将煅烧后的物质进行球磨,之后过筛处理;
(4)将筛下物酸洗、水洗至pH=6~7,离心收集得到生物炭。
步骤(1)中所述造孔剂为氢氧化钠、碳酸氢铵、尿素、聚甲基丙烯酸甲酯或淀粉中的一种或多种,溶液为水、乙醇、乙酸或丙酮中的一种或多种,造孔剂的浓度为5~20wt%。
步骤(1)中香蕉皮在溶液中的浓度为100~1000mg/ml。
步骤(1)中所述浸泡温度为10~50℃,时间为0.5~10h;冻干处理温度为-51℃,时间为12~24h。
步骤(2)中所述惰性气体为氩气、氦气、氮气或氖气中的一种或多种,惰性气体的气流速度为50~200sccm;所述煅烧温度为500~1000℃,煅烧时间为1~10h。
步骤(3)中所述含氮气体为氮气、氨气或二氧化氮中的一种或多种,含氮气体的气流速度为50~500sccm;所述球磨转速为30~80rpm,时间为4~20h,磨球直径为10~50mm,球料质量比为2:1~10:1。
步骤(3)中过筛处理为过100~200目筛。
步骤(3)中所述酸为稀盐酸、稀硝酸、稀硫酸或稀氢氟酸中的一种,浓度为1~3mol/L。
所制备的生物炭在大气中颗粒物和有机物的过滤、水中有机物的吸附以及超级电容器电极材料中的应用。
本发明的有益效果为:
本发明通过在香蕉皮碳化前加入造孔剂,调控孔道结构和尺寸,使碳化后的材料具有更加丰富的孔径;通过对碳化后的材料进一步在氮气下进行球磨,不仅可以提高其比表面积,还可以在生物炭中引入氮源;制备的生物炭材料稳定性强,可以应用于大气中颗粒物和有机物的过滤、水中有机物的吸附以及作为超级电容器电极材料,且可重复使用。
附图说明
图1为实施例1得到的生物炭的扫描电镜(SEM)图。
图2为实施例2得到的生物炭的扫描电镜(SEM)图。
图3为实施例3得到的生物炭的扫描电镜(SEM)图。
具体实施方式
以下实施例便于更好地理解本发明。
实施例1
生物炭的制备方法,包括如下步骤:
(1)将香蕉皮表面洗净,在10wt%的氢氧化钠溶液中50℃浸泡10h,溶液中香蕉皮的浓度为1000mg/mL,之后在-51℃下冻干24h;
(2)在气流速度为200sccm的Ar气氛下,将步骤(1)处理后的香蕉皮于1000℃煅烧5h;
(3)在气流速度为50sccm的氮气气氛下,将煅烧后得到的碳化物质用20mm直径的磨球球磨4h,球料比为5:1,转速为30rpm,之后过200目筛;
(4)将筛下物在1M盐酸中酸洗、水洗至pH=7,离心收集得到生物炭。
图1为实施例1得到的生物炭的扫描电镜(SEM)图。该生物炭比表面积大,约为1000cm2/g,孔道丰富,大孔、介孔占80%,适合用于对大气中的颗粒物的过滤,对PM2.5的截留率可以达到99.5%以上。
PM2.5截留实验:将多孔生物炭负载在纤维上,压片成膜,截取半径为2cm的圆片固定在测试装置上,用自制的颗粒物发生装置产生约100μg/m3的PM2.5,气体流速为5L/min,通过激光尘埃粒子计数器测定过滤膜前后的颗粒物浓度,并用压差表测定前后压差,最后计算分级过滤效率。
实施例2
生物炭的制备方法,包括如下步骤:
(1)将香蕉皮表面洗净,在5wt%的碳酸氢铵溶液中40℃浸泡0.5h,溶液中香蕉皮的浓度为100mg/mL,之后在-51℃下冻干24h;
(2)在气流速度为50sccm的Ar气氛下,将步骤(1)处理后的香蕉皮于500℃煅烧10h;
(3)在气流速度为300sccm的氮气气氛下,将步骤(2)中煅烧后得到的碳化物质用10mm直径的磨球球磨10h,球料比为10:1,转速为50rpm,之后过100目筛;
(4)将筛下物在2M盐酸中酸洗、水洗至pH=7,离心收集得到生物炭。
图2为实施例2得到的生物炭的扫描电镜(SEM)图。该生物炭的氮含量丰富,氮元素含量可以达到10%以上,作为超级电容器电极材料可以使超级电容器的比电容达到200F/g。
超级电容器电极材料的制备及测试:将富氮生物炭与炭黑、PVDF按8:1:1的比例溶于DMF溶液中,形成10wt%的溶液,搅拌12h,之后滴涂在压片后的泡沫镍上,负载量为10mg/cm2,接着封装超级电容器,在1A/g的电流密度下测定电容。
实施例3
生物炭的制备方法,包括以下步骤:
(1)将香蕉皮表面洗净,在20wt%的尿素溶液中10℃浸泡3h,溶液中香蕉皮的浓度为800mg/mL,之后在-51℃下冻干12h;
(2)在气流速度为100sccm的N2气氛下,将步骤(1)处理后的香蕉皮于800℃煅烧4h;
(3)在气流速度为200sccm的氨气气氛下,将步骤(2)中煅烧后得到的碳化物质用10mm直径的磨球球磨8h,球料比为10:1,转速为60rpm,之后过100目筛;
(4)将筛下物在2M硝酸中酸洗、水洗至pH=7,离心收集得到生物炭。
图3为实施例3得到的生物炭的扫描电镜(SEM)图。该生物炭比表面积大,孔径约为800cm2/g,孔道丰富,大孔、介孔占90%,氮含量丰富,氮元素含量可以达到10%以上,适合用于对大气中有机物的过滤及对水中有机物的吸附,如对苯酚的吸附量在30min后可以达到500mg/g,3次吸附-解吸后吸附量仍然能够达到80%以上。
苯酚吸附实验:称取100mg富氮多孔生物炭于烧杯中,室温下加入pH=6,浓度为100mg/L的苯酚溶液,磁力搅拌30min后取上清液过0.45μm滤膜,采用液相色谱法测定吸附前后浓度。
Claims (2)
1.一种生物炭的制备方法,其特征在于,包括如下步骤:
(1)将洗净的香蕉皮在含有浓度为5~20wt%氢氧化钠、碳酸氢铵、尿素、聚甲基丙烯酸甲酯或淀粉中的一种或多种造孔剂的水、乙醇、乙酸或丙酮中的一种或多种溶液中浸泡,香蕉皮在溶液中的浓度为100~1000mg/ml,浸泡温度为10~50℃,时间为0.5~10h,之后冻干处理;冻干处理温度为-51℃,时间为12~24h;
(2)在惰性气体气氛氮气、氨气或二氧化氮中的一种或多种下,将冻干后的香蕉皮煅烧,气流速度为50~200sccm;所述煅烧温度为500~1000℃,煅烧时间为1~10h;
(3)在气流速度为50~500sccm含氮气体气氛下,将煅烧后的物质进行球磨,球磨转速为30~80rpm,时间为4~20h,磨球直径为10~50mm,球料质量比为2:1~10:1,之后100~200目筛过筛处理;
(4)将筛下物在浓度为1~3mol/L稀盐酸、稀硝酸、稀硫酸或稀氢氟酸中的一种酸洗、水洗至pH=6~7,离心收集得到生物炭;
步骤(3)中所述含氮气体为氮气、氨气或二氧化氮中的一种或多种。
2.一种权利要求1所制备的生物炭在大气中颗粒物和有机物的过滤、水中有机物的吸附以及超级电容器电极材料中的应用。
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