CN107754864A - 植物纤维负载改性纳米二氧化钛复合材料及其制备与应用 - Google Patents
植物纤维负载改性纳米二氧化钛复合材料及其制备与应用 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 34
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Abstract
本发明提供了一种植物纤维负载改性纳米二氧化钛复合材料及其制备方法,通过本发明方法制备负载改性二氧化钛的复合材料,可充分改善二氧化钛光响应范围窄、量子效率低以及存在的固载化问题,最终制备出的相互镶嵌的具有微纳结构的复合材料可以用于净化甲醛等有机气体;另外,本发明以植物纤维为主要原料,来源十分广泛,在生产过程中无污染;本发明为生产负载改性二氧化钛的复合材料提供了一种简单可行的方法,具有巨大的发展前景。
Description
(一)技术领域
本发明属于半导体光催化技术领域,具体涉及一种植物纤维负载改性纳米二氧化钛复合材料及其制备方法,以及作为强吸附能力光催化剂的应用。
(二)背景技术
室内环境中挥发性有机化合物(VOCs)的存在严重影响人类的健康,其中以甲醛这种气体污染持续时间长,危害大,它已被世界卫生组织(WHO)和美国环境保护局(EPA)定为人体潜在危险致癌物和重要环境污染物。
光催化反应,就是在光的作用下进行的化学反应。光化学反应需要分子吸收特定波长的电磁辐射,受激产生分子激发态,然后会发生化学反应生成新的物质,或者变成引发热反应的中间化学产物。光化学反应的活化能来源于光子的能量,在太阳能的利用中光电转化以及光化学转化一直是十分活跃的研究领域。
1972年Fujishima和Honda发表了关于二氧化钛电极上光分解水的论文,由此研究者对纳米二氧化钛材料的光催化性质开始了深入的研究。研究表明,纳米二氧化钛能将污染物、臭气、细菌、微生物、甲醛、甲苯和二甲苯等有害有机物彻底分解成无害的二氧化碳和水,且不产生二次污染。
纳米二氧化钛是一种重要的无机半导体材料,其具有独特的物理化学性质,例如比表面积大、活性高、热导性好、优异的颜色效应以及紫外线屏蔽等功能,在化妆品、功能陶瓷和气敏传感器件等方面具有广阔的应用前景。纳米二氧化钛以其高催化活性、强氧化能力、不易溶解、良好的稳定性及价廉无毒等优势而被公认为是最具开发前途和应用潜力的环保型光催化材料,其理论和应用研究日益蓬勃开展起来。
二氧化钛是间接带隙半导体,只能吸收波长小于387nm的紫外线,因此不能充分利用太阳能,即光响应范围窄;纯二氧化钛的光生电子和空穴很容易发生复合,导致光量子效率低;大多数的二氧化钛以粉末为主,在实际应用中存在易团聚失活以及难分离回收的问题,即纯二氧化钛存在固载化问题。
(三)发明内容
为改进二氧化钛存在的光响应范围窄,量子效率低以及固载化问题,本发明提供一种植物纤维负载改性纳米二氧化钛复合材料,充分利用天然植物纤维来源充分的优势,改性二氧化钛能够使光响应范围变宽以及提高光量子效率的特点,并通过由植物纤维负载改性纳米二氧化钛来解决二氧化钛的固载化问题,有利于半导体光催化技术及相关领域的进步。
本发明的技术方案如下:
一种植物纤维负载改性纳米二氧化钛复合材料,按如下方法制备得到:
(1)制备植物纤维:
选取天然植物枝条,经打抛、烘干、碎化、纯化处理,得到植物纤维;
具体的,所述天然植物枝条选自竹子、芦苇、稻草、小麦秸秆中的一种或两种以上任意比例的混合物;
所述打抛、烘干、碎化、纯化处理的操作方法为:将所述天然植物枝条进行打抛(以去除木质素等非纤维成分),接着用水浸渍,升温至120℃保温1h后,冷却至室温,用去离子水清洗,然后置于100℃的烘箱中烘干,取出粉碎过筛,接着进行纯化(以进一步去除果胶质、树胶质和其他杂质),即:将粉碎过筛后的固体物质浸渍于沸水中1min,然后依次用5g/L的H2O2水溶液、4g/L的Na2SiO3水溶液进行氧漂,再经水洗、沸水洗、去离子水冲洗,最后放入100℃的烘箱中烘干,得到植物纤维;
(2)制备改性二氧化钛纳米溶胶:
2-a、室温下,将钛酸四丁酯逐滴加到异丙醇中,以300-400r/min的速率搅拌25-35min,用浓硝酸(市售,浓度68wt%)调节pH至2.5-3.5(优选3),得到溶液A;所述钛酸四丁酯与异丙醇的体积比为1:4.2-6;
2-b、将二次蒸馏水和异丙醇混合,搅拌均匀,得到溶液B;所述二次蒸馏水与异丙醇的体积比为1:1.1-1.8;所述搅拌的时间为5-15min,优选10min;
2-c、将硝酸银溶液逐滴加到乙二胺溶液中,搅拌,得到溶液C;所述硝酸银溶液的浓度为2-4wt%,优选3wt%;所述乙二胺溶液的浓度为2-4wt%,优选3wt%;所述硝酸银溶液与乙二胺溶液的体积比为1:1.2-2;所述搅拌的时间为5-15min,优选为10min;
2-d、搅拌条件下,将溶液B、溶液C分别滴加到溶液A中,得到改性纳米二氧化钛溶胶;所述溶液A与溶液B、溶液C的体积比为1:0.23-0.32:0.08-0.13;
所述“溶液A”、“溶液B”、“溶液C”没有特殊的含义,标记为“A”、“B”、“C”只是用于区分不同操作步骤中提到的溶液;
(3)制备复合材料:
3-a、将步骤(1)所得植物纤维浸没于步骤(2)所得改性纳米二氧化钛溶胶中15-25min,之后取出,用去离子水洗涤,于95-110℃干燥10-13h,接着在惰性气体(例如:氮气)保护下,于500-600℃焙烧1.5-2.5h,得到的焙烧物即完成一次负载过程;
3-b、将3-a得到的焙烧物替代所述的植物纤维按3-a方法重复负载过程2-4次,最终得到负载改性纳米二氧化钛的植物纤维,之后经氮元素掺杂,再于惰性气体保护下经450~550℃热处理1.5~2.5h,得到成品复合材料;
所述氮元素掺杂为:在WSPS-13.56-1000固态射频电源中,在频率为13.56MHz,输出功率为1000W,供电电压为220V,效率为65%,散热方式为风冷的条件下,采用微波等离子体掺杂方法,以氮气为气源,掺杂时间为15-25min。
本发明中,所述室温为20~30℃。
本发明制得的植物纤维负载改性纳米二氧化钛复合材料可作为强吸附能力光催化剂进行应用。例如:可用于甲醛等有毒气体的吸附去除。
本发明的优点在于:通过本发明方法制备负载改性二氧化钛的复合材料,可充分改善二氧化钛光响应范围窄、量子效率低以及存在的固载化问题,最终制备出的相互镶嵌的具有微纳结构的复合材料可以用于净化甲醛等有机气体。另外,本发明以植物纤维为主要原料,来源十分广泛,在生产过程中无污染。本发明为生产负载改性二氧化钛的复合材料提供了一种简单可行的方法,具有巨大的发展前景。
(四)附图说明
图1:植物纤维结构示意图;
图2:未经处理的植物纤维图;
图3:经过打抛、烘干、碎化、纯化处理后的植物纤维图;
图4:负载改性二氧化钛后的植物纤维示意图。
(五)具体实施方式
以下结合具体实施例用于说明本发明,但不用来限制本发明的范围。
实施例1植物纤维负载改性纳米二氧化钛复合材料的制备方法
(1)选取竹子、苇、稻草、小麦秸秆等中的一种或几种的混合物,经打抛处理后去除木质素等非纤维成分,将得到的纤维素组分浸渍蒸馏水,放入烘箱,缓慢加热到120℃,一小时后取出,待其冷却到室温后,用去离子水清洗,然后放入烘箱,缓慢加热到100℃,一小时后取出,粉碎过筛,得到植物纤维。
(2)将步骤(1)所得的植物纤维进行纯化,进一步去除植物纤维中的果胶质、树胶质和其他杂质。首先植物纤维浸渍在沸水中1min,然后用5g/L的H2O2和4g/L的Na2SiO3进行氧漂,然后进行水洗,用沸水洗2min,然后用去离子水冲洗3次,然后放入烘箱,缓慢加热到100℃,一小时后取出。
(3)将5mL的钛酸四丁酯逐滴加到22mL的异丙醇里,室温下剧烈搅拌30分钟,并用浓硝酸调节pH直至pH=3,得到溶液A;将3.0mL二次水和3.3mL异丙醇混合,搅拌10分钟,得到溶液B;将1.0mL的3wt%的硝酸银溶液逐滴加入到1.2mL 3wt%的乙二胺溶液中,搅拌10分钟,得到溶液C。在剧烈搅拌下,将6.3mL溶液B,2.2mL溶液C分别通过恒压漏斗逐滴加到27mL溶液A中,得到改性纳米二氧化钛溶胶。
(4)将步骤(2)得到的植物纤维放入步骤(3)得到的改性纳米二氧化钛溶胶中,浸渍20分钟,取出,用去离子水洗涤,100℃干燥12h,在氮气的保护下,在550℃温度下焙烧2h。
(5)重复步骤(4)三次
(6)在WSPS-13.56-1000固态射频电源中采用微波等离子体掺杂方法,以氮气为气源,对步骤(5)得到的复合材料进行氮元素掺杂,掺杂时间为20min。
(7)最后将上述所得复合材料置于管式炉中以500℃惰性气体保护热处理2小时。
(8)将步骤(7)所得复合材料和纯二氧化钛粉末、一盆绿萝至于相同密闭环境下(甲醛浓度为0.1㎎/m3),经检测,3h后,本发明所在环境甲醛浓度为0.62㎎/m3,纯二氧化钛粉末所在环境甲醛浓度为0.75㎎/m3,绿萝所在环境甲醛浓度为0.92㎎/m3。经比较,本发明去除甲醛及其他有毒气体的效率高于纯二氧化钛粉末以及绿色植物。
实施例2植物纤维负载改性纳米二氧化钛复合材料的制备方法
(1)选取竹子、苇、稻草、小麦秸秆等中的一种或几种的混合物,经打抛处理后去除木质素等非纤维成分,将得到的纤维素组分浸渍蒸馏水,放入烘箱,缓慢加热到120℃,一小时后取出,待其冷却到室温后,用去离子水清洗,然后放入烘箱,缓慢加热到100℃,一小时后取出,粉碎过筛,得到植物纤维。
(2)将步骤(1)所得的植物纤维进行纯化,进一步去除植物纤维中的果胶质、树胶质和其他杂质。首先植物纤维浸渍在沸水中1min,然后用5g/L的H2O2和4g/L的Na2SiO3进行氧漂,然后进行水洗,用沸水洗2min,然后用去离子水冲洗3次,然后放入烘箱,缓慢加热到100℃,一小时后取出。
(3)将5mL的钛酸四丁酯逐滴加到25mL的异丙醇里,室温下剧烈搅拌30分钟,并用浓硝酸调节pH直至pH=3,得到溶液A;将3.5mL二次水和5.2mL异丙醇混合,搅拌10分钟,得到溶液B;将1.23mL的3wt%的硝酸银溶液逐滴加入到1.85mL 3wt%的乙二胺溶液中,搅拌10分钟,得到溶液C。在剧烈搅拌下,将8.7mL溶液B,3.08mL溶液C分别通过恒压漏斗逐滴加到30mL溶液A中,得到改性纳米二氧化钛溶胶。
(4)将步骤(2)得到的植物纤维放入步骤(3)得到的改性纳米二氧化钛溶胶中,浸渍20分钟,取出,用去离子水洗涤,100℃干燥12h,在氮气的保护下,在550℃温度下焙烧2h。
(5)重复步骤(4)三次
(6)在WSPS-13.56-1000固态射频电源中采用微波等离子体掺杂方法,以氮气为气源,对步骤(5)得到的复合材料进行氮元素掺杂,掺杂时间为20min。
(7)最后将上述所得复合材料置于管式炉中以500℃惰性气体保护热处理2小时。
(8)将步骤(7)所得复合材料和纯二氧化钛粉末、一盆绿萝至于相同密闭环境下(甲醛浓度为0.1㎎/m3),经检测,3h后,本发明所在环境甲醛浓度为0.58㎎/m3,纯二氧化钛粉末所在环境甲醛浓度为0.75㎎/m3,绿萝所在环境甲醛浓度为0.92㎎/m3。经比较,本发明去除甲醛及其他有毒气体的效率高于纯二氧化钛粉末以及绿色植物。
实施例3植物纤维负载改性纳米二氧化钛复合材料的制备方法
(1)选取竹子、苇、稻草、小麦秸秆等中的一种或几种的混合物,经打抛处理后去除木质素等非纤维成分,将得到的纤维素组分浸渍蒸馏水,放入烘箱,缓慢加热到120℃,一小时后取出,待其冷却到室温后,用去离子水清洗,然后放入烘箱,缓慢加热到100℃,一小时后取出,粉碎过筛,得到植物纤维。
(2)将步骤(1)所得的植物纤维进行纯化,进一步去除植物纤维中的果胶质、树胶质和其他杂质。首先植物纤维浸渍在沸水中1min,然后用5g/L的H2O2和4g/L的Na2SiO3进行氧漂,然后进行水洗,用沸水洗2min,然后用去离子水冲洗3次,然后放入烘箱,缓慢加热到100℃,一小时后取出。
(3)将5mL的钛酸四丁酯逐滴加到30mL的异丙醇里,室温下剧烈搅拌30分钟,并用浓硝酸调节pH直至pH=3,得到溶液A;将4.0mL二次水和7.2mL异丙醇混合,搅拌10分钟,得到溶液B;将1.5mL的3wt%的硝酸银溶液逐滴加入到3.0mL 3wt%的乙二胺溶液中,搅拌10分钟,得到溶液C。在剧烈搅拌下,将11.2mL溶液B,4.5mL溶液C分别通过恒压漏斗逐滴加到35mL溶液A中,得到改性纳米二氧化钛溶胶。
(4)将步骤(2)得到的植物纤维放入步骤(3)得到的改性纳米二氧化钛溶胶中,浸渍20分钟,取出,用去离子水洗涤,100℃干燥12h,在氮气的保护下,在550℃温度下焙烧2h。
(5)重复步骤(4)三次
(6)在WSPS-13.56-1000固态射频电源中采用微波等离子体掺杂方法,以氮气为气源,对步骤(5)得到的复合材料进行氮元素掺杂,掺杂时间为20min。
(7)最后将上述所得复合材料置于管式炉中以500℃惰性气体保护热处理2小时。
(8)将步骤(7)所得复合材料和纯二氧化钛粉末、一盆绿萝至于相同密闭环境下(甲醛浓度为0.1㎎/m3),经检测,3h后,本发明所在环境甲醛浓度为0.57㎎/m3,纯二氧化钛粉末所在环境甲醛浓度为0.75㎎/m3,绿萝所在环境甲醛浓度为0.92㎎/m3。经比较,本发明去除甲醛及其他有毒气体的效率高于纯二氧化钛粉末以及绿色植物。
以上所述,仅是本发明的较佳实施例而已,并非对本发明的技术方案作任何形式上的限制。凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明的技术方案的范围内。
Claims (5)
1.一种植物纤维负载改性纳米二氧化钛复合材料,其特征在于,按如下方法制备得到:
(1)制备植物纤维:
选取天然植物枝条,经打抛、烘干、碎化、纯化处理,得到植物纤维;
所述天然植物枝条选自竹子、芦苇、稻草、小麦秸秆中的一种或两种以上任意比例的混合物;
(2)制备改性二氧化钛纳米溶胶:
2-a、室温下,将钛酸四丁酯逐滴加到异丙醇中,以300-400r/min的速率搅拌25-35min,用浓硝酸调节pH至2.5-3.5,得到溶液A;所述钛酸四丁酯与异丙醇的体积比为1:4.2-6;
2-b、将二次蒸馏水和异丙醇混合,搅拌均匀,得到溶液B;所述二次蒸馏水与异丙醇的体积比为1:1.1-1.8;
2-c、将硝酸银溶液逐滴加到乙二胺溶液中,搅拌,得到溶液C;所述硝酸银溶液的浓度为2-4wt%;所述乙二胺溶液的浓度为2-4wt%;所述硝酸银溶液与乙二胺溶液的体积比为1:1.2-2;
2-d、搅拌条件下,将溶液B、溶液C分别滴加到溶液A中,得到改性纳米二氧化钛溶胶;所述溶液A与溶液B、溶液C的体积比为1:0.23-0.32:0.08-0.13;
(3)制备复合材料:
3-a、将步骤(1)所得植物纤维浸没于步骤(2)所得改性纳米二氧化钛溶胶中15-25min,之后取出,用去离子水洗涤,于95-110℃干燥10-13h,接着在惰性气体保护下,于500-600℃焙烧1.5-2.5h,得到的焙烧物即完成一次负载过程;
3-b、将3-a得到的焙烧物替代所述的植物纤维按3-a方法重复负载过程2-4次,最终得到负载改性纳米二氧化钛的植物纤维,之后经氮元素掺杂,再于惰性气体保护下经450~550℃热处理1.5~2.5h,得到成品复合材料。
2.如权利要求1所述的植物纤维负载改性纳米二氧化钛复合材料,其特征在于,步骤(1)中,所述打抛、烘干、碎化、纯化处理的操作方法为:
将所述天然植物枝条进行打抛,接着用水浸渍,升温至120℃保温1h后,冷却至室温,用去离子水清洗,然后置于100℃的烘箱中烘干,取出粉碎过筛,接着进行纯化,即:将粉碎过筛后的固体物质浸渍于沸水中1min,然后依次用5g/L的H2O2水溶液、4g/L的Na2SiO3水溶液进行氧漂,再经水洗、沸水洗、去离子水冲洗,最后放入100℃的烘箱中烘干,得到植物纤维。
3.如权利要求1所述的植物纤维负载改性纳米二氧化钛复合材料,其特征在于,步骤(3)中,所述氮元素掺杂为:在WSPS-13.56-1000固态射频电源中,在频率为13.56MHz,输出功率为1000W,供电电压为220V,效率为65%,散热方式为风冷的条件下,采用微波等离子体掺杂方法,以氮气为气源,掺杂时间为15-25min。
4.如权利要求1所述的植物纤维负载改性纳米二氧化钛复合材料作为强吸附能力光催化剂的应用。
5.如权利要求4所述的应用,其特征在于,所述植物纤维负载改性纳米二氧化钛复合材料用于甲醛的吸附去除。
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