CN113289601B - 一种泡沫碳催化剂的制备方法及应用 - Google Patents
一种泡沫碳催化剂的制备方法及应用 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 94
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- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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Abstract
一种泡沫碳催化剂的制备方法及应用,它涉及一种催化剂的制备方法及应用。本发明的目的是要解决现有方法制备的泡沫碳耗时长,大部分碳源无法负载在模板上,导致碳源的利用不充分和对污染物的降解效率低的问题。方法:一、泡沫模板的预处理;二、配置碳源分散体系;三、制备泡沫碳;泡沫碳催化剂在高级氧化体系、光催化体系或电化学体系中使用,用于降解去除水中的污染物。通过本发明制备的泡沫碳催化剂比表面积高、吸附催化能力强、耐热、化学稳定、易与水体分离,可重复使用,在水体中污染物的去除,维护水质安全方面具有良好的前景。本发明可获得一种泡沫碳催化剂。
Description
技术领域
本发明涉及一种催化剂的制备方法及应用。
背景技术
泡沫碳具有三维多孔结构,具有巨大的表面积,是一种水处理领域常见的吸附材料。除了良好的吸附性能外,泡沫碳还具有质量轻、耐热性好、导电性好等优点,因此它也很适合作为污水处理的催化剂,如光催化剂、电催化剂等。与普通的粉末碳催化剂相比,泡沫碳催化剂的显著优势之一是易于从水中分离,使用过程中损失量少,故泡沫碳催化剂更容易实现重复利用,废弃后的处理处置也比粉末碳简单。此外,泡沫碳的形状可以在制备中人为进行调节,因此可根据实际使用条件制备出不同形状的泡沫碳。
为了得到均质的泡沫碳材料,在制备碳源溶液时,通常利用凝胶化反应使碳源聚合为胶体,并不断的搅拌使其均匀的分散在溶液中。该过程耗时很长,并且碳源的利用也很不充分,大部分碳源以溶质的形式存在溶剂中而无法负载在模板上进而制备泡沫碳。
发明内容
本发明的目的是要解决现有方法制备的泡沫碳耗时长,大部分碳源无法负载在模板上,导致碳源的利用不充分和对污染物的降解效率低的问题,而提供一种泡沫碳催化剂的制备方法及应用。
一种泡沫碳催化剂的制备方法,是按以下步骤完成的:
一、泡沫模板的预处理:
将泡沫模板浸入到恒温碱液中,再用超纯水将泡沫模板冲洗至中性,最后干燥,得到预处理后的泡沫模板;
二、配置碳源分散体系:
将交联剂加入到缓冲溶液中,得到交联剂溶液;向搅拌中的交联剂溶液中加入碳源,持续搅拌,得到含有碳源的交联剂溶液;
步骤二中所述的交联剂与碳源的摩尔比为1:(1~20);
步骤二中所述的含有碳源的交联剂溶液中碳源的浓度为0.5g/L~2.5g/L;
三、制备泡沫碳:
将预处理后的泡沫模板浸入到含有碳源的交联剂溶液中,再取出干燥;将干燥的泡沫模板放入管式炉中,再进行碳化,得到泡沫碳催化剂。
泡沫碳催化剂在高级氧化体系、光催化体系或电化学体系中使用,用于降解去除水中的污染物。
本发明的有益效果:
本发明利用交联剂控制碳源凝胶化的速度,加快“碳-交联剂”复合体负载在泡沫模板上的时间,进而制备泡沫碳催化剂,其具有以下优点:
一、本发明制备过程简单,制备泡沫催化剂的催化性能良好且容易与水分离,不造成水体二次污染且可以重复使用,节能环保;
二、本发明反应速度可通过调节交联剂的种类和使用量,控制反应进程,在宏观上节约了试验时间,并且不同反应速度影响泡沫碳的微观形态与表面粗糙度,可在使用碳源量相同的情况下,构造出更多的反应位点,节约了碳源;
三、本发明使用条件广泛,泡沫碳本身具有催化性和导电性,可以在高级氧化体系与电化学反应体系中发挥作用,此外若交联剂为金属,可形成金属-碳(氮)复合体系,提高催化效率,例如在光催化剂体系中,金属的掺杂可对电子捕获、掺杂能级形成起到重要作用;
本发明采用模板法制备泡沫碳,通过交联剂控制碳源凝胶化反应的速度,调节反应的进程,此外交联剂与碳还可以形成复合催化剂,强化泡沫碳催化剂的使用效果;通过本发明制备的泡沫碳催化剂比表面积高、吸附催化能力强、耐热、化学稳定、易与水体分离,可重复使用,在水体中污染物的去除,维护水质安全方面具有良好的前景;
四、本发明制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体有较好的效果,90min内污染物去除率可以达到89.3%。
本发明可获得一种泡沫碳催化剂。
附图说明
图1为实施例一制备的泡沫碳催化剂的SEM图;
图2为实施例二制备的泡沫碳催化剂的SEM图;
图3为实施例三制备的泡沫碳催化剂的SEM图;
图4为实施例四利用实施例一制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体的效果图;
图5为实施例五利用实施例二制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体的效果图;
图6为实施例六利用实施例三制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体的效果图。
具体实施方式
以下实施例进一步说明本发明的内容,但不应理解为对本发明的限制。在不背离本发明实质的情况下,对本发明方法、步骤或条件所作的修改和替换,均属于本发明的范围。
具体实施方式一:本实施方式一种泡沫碳催化剂的制备方法,是按以下步骤完成的:
一、泡沫模板的预处理:
将泡沫模板浸入到恒温碱液中,再用超纯水将泡沫模板冲洗至中性,最后干燥,得到预处理后的泡沫模板;
二、配置碳源分散体系:
将交联剂加入到缓冲溶液中,得到交联剂溶液;向搅拌中的交联剂溶液中加入碳源,持续搅拌,得到含有碳源的交联剂溶液;
步骤二中所述的交联剂与碳源的摩尔比为1:(1~20);
步骤二中所述的含有碳源的交联剂溶液中碳源的浓度为0.5g/L~2.5g/L;
三、制备泡沫碳:
将预处理后的泡沫模板浸入到含有碳源的交联剂溶液中,再取出干燥;将干燥的泡沫模板放入管式炉中,再进行碳化,得到泡沫碳催化剂。
本实施方式的有益效果:
本实施方式利用交联剂控制碳源凝胶化的速度,加快“碳-交联剂”复合体负载在泡沫模板上的时间,进而制备泡沫碳催化剂,其具有以下优点:
一、本实施方式制备过程简单,制备泡沫催化剂的催化性能良好且容易与水分离,不造成水体二次污染且可以重复使用,节能环保;
二、本实施方式反应速度可通过调节交联剂的种类和使用量,控制反应进程,在宏观上节约了试验时间,并且不同反应速度影响泡沫碳的微观形态与表面粗糙度,可在使用碳源量相同的情况下,构造出更多的反应位点,节约了碳源;
三、本实施方式使用条件广泛,泡沫碳本身具有催化性和导电性,可以在高级氧化体系与电化学反应体系中发挥作用,此外若交联剂为金属,可形成金属-碳(氮)复合体系,提高催化效率,例如在光催化剂体系中,金属的掺杂可对电子捕获、掺杂能级形成起到重要作用;
本实施方式采用模板法制备泡沫碳,通过交联剂控制碳源凝胶化反应的速度,调节反应的进程,此外交联剂与碳还可以形成复合催化剂,强化泡沫碳催化剂的使用效果;通过本实施方式制备的泡沫碳催化剂比表面积高、吸附催化能力强、耐热、化学稳定、易与水体分离,可重复使用,在水体中污染物的去除,维护水质安全方面具有良好的前景;
四、本实施方式制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体有较好的效果,90min内污染物去除率可以达到89.3%。
本实施方式可获得一种泡沫碳催化剂。
具体实施方式二:本实施方式与具体实施方式一不同点是:步骤一中所述的恒温碱液为90℃~100℃的碱性溶液,所述的碱性溶液为氢氧化钠溶液或氢氧化钾溶液;所述的碱性溶液的pH值为11.4~11.8。其它步骤与具体实施方式一相同。
具体实施方式三:本实施方式与具体实施方式一或二之一不同点是:步骤一中所述的干燥的温度为50℃~60℃,干燥的时间为4h~6h。其它步骤与具体实施方式一或二相同。
具体实施方式四:本实施方式与具体实施方式一至三之一不同点是:步骤一中所述的泡沫模板为聚氨酯泡沫板、沸石泡沫、酚醛树脂泡沫或氧化铝泡沫板。其它步骤与具体实施方式一至三相同。
本实施方式中泡沫模板的厚度根据使用的需要进行裁剪。
具体实施方式五:本实施方式与具体实施方式一至四之一不同点是:步骤二中所述的交联剂为过渡金属离子溶液、过氧化氢和甲基丙稀酰乙基磺基甜菜碱中的一种或其中几种的混合物;所述的过渡金属离子溶液中过渡金属为铁、锰、钒、钴或铜。其它步骤与具体实施方式一至四相同。
具体实施方式六:本实施方式与具体实施方式一至五之一不同点是:步骤二中所述的缓冲溶液的pH值为7~9,由缓冲物质和水配制而成;所述的缓冲物质为磷酸二氢钾与磷酸氢二钾的混合物、磷酸二氢钠与磷酸氢二钠的混合物、硼酸与硼砂的混合物或三羟甲基氨基甲烷与氢氧化钠的混合物。其它步骤与具体实施方式一至五相同。
具体实施方式七:本实施方式与具体实施方式一至六之一不同点是:步骤二中所述的碳源为儿茶酚、多巴胺、透明质酸、壳聚糖、纤维素、尿素和多巴中的一种或几种的混合。其它步骤与具体实施方式一至六相同。
具体实施方式八:本实施方式与具体实施方式一至七之一不同点是:步骤三中将预处理后的泡沫模板浸入到含有碳源的交联剂溶液中的时间为15min~360min;步骤三中所述的干燥为在烘箱中干燥或者是冷冻干燥;在烘箱中干燥的温度为80℃~120℃,干燥的时间为4h~6h;所述的冷冻干燥的温度为-40℃~-60℃,冷冻干燥的时间为18h~36h;步骤三中将干燥的泡沫模板放入管式炉中,再进行碳化,碳化时管式炉中的气氛为氩气、氦气、氧气、氮气或真空氛围;步骤三中干燥的泡沫模板放入管式炉中,以2℃/min~5℃/min的升温速率将管式炉升温至300℃~450℃,再在300℃~450℃下碳化30min~60min。其它步骤与具体实施方式一至七相同。
具体实施方式九:本实施方式是泡沫碳催化剂在高级氧化体系、光催化体系或电化学体系中使用,用于降解去除水中的污染物。
具体实施方式十:本实施方式与具体实施方式一至九之一不同点是:泡沫碳催化剂在高级氧化体系中使用需要添加氧化剂,所述的氧化剂为臭氧、过硫酸氢钠、过硫酸氢钾、过硫酸钾等中的一种或多种的组合;泡沫碳催化剂在光催化体系中使用需要外设可见光源;泡沫碳催化剂在电化学体系中使用需要将泡沫碳催化剂进一步加工成电极。其它步骤与具体实施方式一至九相同。
具体实施方式十一:本实施方式与具体实施方式十的不同点是:所述的泡沫碳催化剂在光催化体系中使用需要外设500W的Xe灯,泡沫碳催化剂与500W的Xe灯结合使用,通过光催化去除水中的污染物。其它步骤与具体实施方式十相同。
具体实施方式十二:本实施方式与具体实施方式十或十一的不同点是:所述的污染物为染料、兽药、有机农药和食品添加剂中的一种或多种的混合物。其它步骤与具体实施方式十或十一相同。
下面结合附图和实施例对本发明进行详细的说明。
实施例一:一种泡沫碳催化剂的制备方法是按以下步骤完成的:
一、泡沫模板的预处理:
将聚氨酯泡沫板浸入到温度为100℃的氢氧化钠溶液中,再用超纯水将泡沫模板冲洗至中性,最后在55℃下干燥6h,得到预处理后的聚氨酯泡沫板;
步骤一中所述的聚氨酯泡沫板切割成2cm*2cm*2cm的立方体;
步骤一中所述的氢氧化钠溶液的pH值为11.5;
二、配置碳源分散体系:
将五水硫酸铜加入到缓冲溶液中,得到交联剂溶液;向搅拌中的交联剂溶液中加入多巴胺,持续搅拌,得到含有碳源的交联剂溶液;
步骤二中所述的含有碳源的交联剂溶液中多巴胺的浓度为1.5g/L,五水硫酸铜的浓度为0.34g/L;
步骤二中所述的缓冲溶液的pH值为8.2,由磷酸二氢钾与磷酸氢二钾配置而成;
三、制备泡沫碳:
将预处理后的聚氨酯泡沫板浸入到含有碳源的交联剂溶液中30min,取出后在温度为 80℃下干燥6h;将干燥的泡沫模板放入管式炉中,向管式炉中通入氮气,氮气的流速为 150mL/min,再在氮气气氛下将管式炉以2℃/min的升温速率升温至350℃,再在350℃下进行碳化40min,得到泡沫碳催化剂。
图1为实施例一制备的泡沫碳催化剂的SEM图;
实施例二:一种泡沫碳催化剂的制备方法是按以下步骤完成的:
一、泡沫模板的预处理:
将聚氨酯泡沫板浸入到温度为100℃的氢氧化钠溶液中,再用超纯水将泡沫模板冲洗至中性,最后在55℃下干燥6h,得到预处理后的聚氨酯泡沫板;
步骤一中所述的聚氨酯泡沫板切割成2cm*2cm*2cm的立方体;
步骤一中所述的氢氧化钠溶液的pH值为11.5;
二、配置碳源分散体系:
将五水硫酸铜和双氧水加入到缓冲溶液中,得到交联剂溶液;向搅拌中的交联剂溶液中加入多巴胺,持续搅拌,得到含有碳源的交联剂溶液;
步骤二中所述的含有碳源的交联剂溶液中多巴胺的浓度为2g/L,五水硫酸铜的浓度为0.64g/L,双氧水的浓度为2mL/L,双氧水的质量分数为30%;
步骤二中所述的缓冲溶液的pH值为8,由磷酸二氢钾与磷酸氢二钾配置而成;
三、制备泡沫碳:
将预处理后的聚氨酯泡沫板浸入到含有碳源的交联剂溶液中30min,取出后在温度为 120℃下干燥4h;将干燥的泡沫模板放入管式炉中,向管式炉中通入氮气,氮气的流速为 150mL/min,再在氮气气氛下将管式炉以2℃/min的升温速率升温至350℃,再在350℃下进行碳化40min,得到泡沫碳催化剂。
图2为实施例二制备的泡沫碳催化剂的SEM图;
实施例三:一种泡沫碳催化剂的制备方法是按以下步骤完成的:
一、泡沫模板的预处理:
将聚氨酯泡沫板浸入到温度为100℃的氢氧化钠溶液中,再用超纯水将泡沫模板冲洗至中性,最后在55℃下干燥6h,得到预处理后的聚氨酯泡沫板;
步骤一中所述的聚氨酯泡沫板切割成2cm*2cm*2cm的立方体;
步骤一中所述的氢氧化钠溶液的pH值为11.5;
二、配置碳源分散体系:
将无水硫酸铜和硫酸铁加入到缓冲溶液中,得到交联剂溶液;向搅拌中的交联剂溶液中加入多巴胺,持续搅拌,得到含有碳源的交联剂溶液;
步骤二中所述的含有碳源的交联剂溶液中多巴胺的浓度为2g/L,五水硫酸铜的浓度为0.32g/L,硫酸铁的浓度为0.12g/L;
步骤二中所述的缓冲溶液的pH值为7,由磷酸二氢钾与磷酸氢二钾配置而成;
三、制备泡沫碳:
将预处理后的聚氨酯泡沫板浸入到含有碳源的交联剂溶液中30min,取出后在温度为 -40℃下干燥24h;将干燥的泡沫模板放入管式炉中,向管式炉中通入氮气,氮气的流速为200mL/min,再在氮气气氛下将管式炉以3℃/min的升温速率升温至400℃,再在400℃下进行碳化35min,得到泡沫碳催化剂。
图3为实施例三制备的泡沫碳催化剂的SEM图;
实施例四:用实施例一制备的泡沫碳催化剂与氧化剂结合处理被染料污染的水体是按以下步骤完成的:
向1L被染料污染的水体中加入0.12g过硫酸氢钠和15mg实施例一制备的泡沫碳催化剂,降解0min~90min,亚甲基蓝的降解情况如图4所示;
所述被染料污染的水体中含有15mg/L的亚甲基蓝。
图4为实施例四利用实施例一制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体的效果图;
从图4可知,实施例一制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体有较好的效果,90min内污染物去除率达到84.2%。
实施例五:用实施例二制备的泡沫碳催化剂与氧化剂结合处理被染料污染的水体是按以下步骤完成的:
向1L被染料污染的水体中加入0.12g过硫酸氢钠和15mg实施例二制备的泡沫碳催化剂,降解0min~90min,亚甲基蓝的降解情况如图5所示;
所述被染料污染的水体中含有15mg/L的亚甲基蓝。
图5为实施例五利用实施例二制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体的效果图;
从图5可知,实施例二制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体有较好的效果,90min内污染物去除率达到79.4%。
实施例六:用实施例三制备的泡沫碳催化剂与氧化剂结合处理被染料污染的水体是按以下步骤完成的:
向1L被染料污染的水体中加入0.12g过硫酸氢钠和15mg实施例二制备的泡沫碳催化剂,降解0min~90min,亚甲基蓝的降解情况如图6所示;
所述被染料污染的水体中含有15mg/L的亚甲基蓝。
图6为实施例六利用实施例三制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体的效果图。
从图6可知,实施例三制备的泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体有较好的效果,90min内污染物去除率达到89.3%。
Claims (1)
1.利用泡沫碳催化剂与氧化剂结合处理被染料污染的水体的方法,其特征在于泡沫碳催化剂与过硫酸氢钠结合降解被亚甲基蓝染料污染的水体有较好的效果,90min内污染物去除率达到89.3%,该方法具体是按以下步骤完成的:
向1L被染料污染的水体中加入0.12g过硫酸氢钠和15mg泡沫碳催化剂,降解90min;
所述被染料污染的水体中含有15mg/L的亚甲基蓝;
所述泡沫碳催化剂的制备方法是按以下步骤完成的:
一、泡沫模板的预处理:
将聚氨酯泡沫板浸入到温度为100℃的氢氧化钠溶液中,再用超纯水将泡沫模板冲洗至中性,最后在55℃下干燥6h,得到预处理后的聚氨酯泡沫板;
步骤一中所述的聚氨酯泡沫板切割成2cm*2cm*2cm的立方体;
步骤一中所述的氢氧化钠溶液的pH值为11.5;
二、配置碳源分散体系:
将五水硫酸铜和硫酸铁加入到缓冲溶液中,得到交联剂溶液;向搅拌中的交联剂溶液中加入多巴胺,持续搅拌,得到含有碳源的交联剂溶液;
步骤二中所述的含有碳源的交联剂溶液中多巴胺的浓度为2g/L,五水硫酸铜的浓度为0.32g/L,硫酸铁的浓度为0.12g/L;
步骤二中所述的缓冲溶液的pH值为7,由磷酸二氢钾与磷酸氢二钾配置而成;
三、制备泡沫碳:
将预处理后的聚氨酯泡沫板浸入到含有碳源的交联剂溶液中30min,取出后在温度为-40℃下干燥24h;将干燥的泡沫模板放入管式炉中,向管式炉中通入氮气,氮气的流速为200mL/min,再在氮气气氛下将管式炉以3℃/min的升温速率升温至400℃,再在400℃下进行碳化35min,得到泡沫碳催化剂。
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