CN107684886B - 一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法 - Google Patents
一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法 Download PDFInfo
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Abstract
本发明公开了一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,将废棉织物放入反应釜中水热炭化,取出剩余物质与壳聚糖混合,加入醋酸溶液使其完全溶解得到透明溶胶,同时加入环氧氯丙烷、石墨烯、纳米TiO2后充分搅拌,静置,倒入模具中冷冻,将冷冻好的凝胶材料冷冻干燥后得到气凝胶。将气凝胶升温至350‑550℃,持续加热得到复合碳气凝胶。本发明解决了传统碳气凝胶的制备方法成本高毒害大的技术问题,是一种以天然高分子和废弃物为原料制备碳气凝胶的方法。
Description
技术领域
本发明涉及碳气凝胶材料制备技术领域,特别是涉及一种掺杂 TiO2的棉纤维复合碳气凝胶的制备方法。
背景技术
碳气凝胶是一种新型轻质纳米多空无定形碳素材料,具有比表面积高、质量密度低、孔隙率高等特点,在力学、声学、电学、热学和光学等领域都具有潜在的应用价值。目前碳气凝胶中常规的方法是利用有机气凝胶间苯二酚-甲醛气凝胶炭化后得到的产物,其前驱体大多来自石油工业,原料成本较高,对环境毒害较大。因此利用天然有机聚合物或者可再生的工业废弃物制备碳气凝胶有重要的意义和前景,具有来源丰富、价格低廉和环境友好的优点。
发明内容
本发明就是针对上述存在的缺陷而提供一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法。本发明解决了传统碳气凝胶的制备方法成本高毒害大的技术问题,是一种以天然高分子和废弃物为原料制备碳气凝胶的方法。
本发明的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法技术方案为,包括以下步骤:
(1)将废棉织物加入去离子水中,转移至水热反应釜中碳化2-4h; (2)将炭化后的产物取出,与壳聚糖混合,加入去离子水混合均匀后得到混合物,逐滴加入醋酸溶液,使壳聚糖完全溶解得到透明溶胶; (3)向溶胶中加入环氧氯丙烷、石墨烯粉末、纳米TiO2粉末,然后充分搅拌使各物质均匀混合后静置形成混合凝胶后倒入模具中;
(4)将盛有凝胶的模具放入冰箱中冷冻;
(5)取出冷冻好的凝胶,真空冷冻干燥后得到复合气凝胶材料;
(6)将气凝胶材料升温,持续加热保温,得到复合碳气凝胶。
步骤(1)中,将废棉织物剪成碎条加入去离子水中,固液比为 10-260g/L,优选为10-120g/L。
步骤(1)中,碳化温度为260-350℃。
步骤(2)中,棉织物碳化后与壳聚糖混合,加入去离子水使壳聚糖的浓度为20-40g/L。
步骤(2)中,冰醋酸的加入量为混合物质量的1%-2%。
步骤(3)中加入按溶胶体积10%环氧氯丙烷;石墨烯粉末采用改进的Hummers法制备,加入10-20g/L石墨烯;纳米TiO2采用硫酸钛为钛源利用水热法于80℃合成,加入0.5-12g/L纳米TiO2。
步骤(3)中搅拌时间为4-6h,静置时间为2-3h。
步骤(4)中凝胶冷冻的时间为24h。
步骤(5)中冷冻好的凝胶,置于-50—-10℃的真空冷冻干燥仪中干燥24h得到复合气凝胶材料。
步骤(5)具体为,将气凝胶材料以5℃/min的速度升温至 350-550℃,持续加热2h后保温30分钟,得到复合碳气凝胶。
本发明的有益效果为:
1.利用主要成分为纤维素的废弃棉织物和天然高分子物质壳聚糖作为碳气凝胶的原料,成本低廉,绿色环保。
2.废弃棉织物水热炭化后可以得到纳米碳纤维,有助于增强碳气凝胶的强度。
3.石墨烯纳米碳材料和纳米TiO2粉末的添加有助于增强碳气凝胶的疏水性和光敏性,可以增强碳气凝胶的光催化降解能力。
附图说明:
图1为实施例1中的掺杂TiO2的棉纤维复合碳气凝胶置于蒲公英上的照片;
图2为实施例2中的掺杂TiO2的棉纤维复合碳气凝胶上放置50g的砝码照片;
图3为实施例3中的掺杂TiO2的棉纤维复合碳气凝胶的SEM图;
图4为实施例3中的掺杂TiO2的棉纤维复合碳气凝胶的TEM图;
图5为实施例3中的掺杂TiO2的棉纤维复合碳气凝胶的拉曼光谱;
图6为实施例3中的掺杂TiO2的棉纤维复合碳气凝胶对四种染料的降解速度。
具体实施方式:
为了更好地理解本发明,下面用具体实例来详细说明本发明的技术方案,但是本发明并不局限于此。
实施例1
取1g碎布条加入50ml去离子水中,同时转移至水热反应釜中,在280℃下加热4h,得到液体,冷却后,加入1.5g壳聚糖到上述溶液,加入适量去离子水,磁力搅拌得到混合物,逐滴加入混合物质量 2%的冰醋酸至粘稠溶胶,加入5ml环氧氯丙烷,0.75g石墨烯,25mg纳米TiO2,混合凝胶体积约50ml置于磁力搅拌器上均匀搅拌4h,静置2h,将该凝胶倒入准备好的模具中冷冻24h。将冻好的凝胶置于-50 —-10℃的真空冷冻干燥仪中干燥24h得到气凝胶,将气凝胶置于铝坩埚中以5℃/min的速度升温至550℃加热2h,并保温半小时后,即可得到掺杂TiO2的棉纤维复合碳气凝胶。由图1可知,制备好的碳气凝胶可以放置在蒲公英上,说明该气凝胶非常轻盈。分别将0.15g该气凝胶置于50mL初始浓度为20mg/L的罗丹明和结晶紫溶液中进行光催化降解反应,整个光催化反应在光催化反应器中进行。以汞灯为光源,前30min黑暗条件下进行吸附,然后打开汞灯进行光催化降解。打开光源后60分钟内罗丹明的降解率达到91%,40分钟内结晶紫的降解率达到95%。
实施例2:
取1.5g碎布条加入50ml去离子水中,同时转移至水热反应釜中,在300℃下加热3h,得到液体,冷却后,加入1.5g壳聚糖到上述溶液,加入适量去离子水,磁力搅拌得到混合物,逐滴加入混合物质量 2%的冰醋酸至粘稠溶胶,同时加入4ml环氧氯丙烷,0.75g石墨烯, 40mg纳米TiO2,混合凝胶体积约40ml置于磁力搅拌器上均匀搅拌4h,静置2h,将该凝胶倒入准备好的模具中冷冻24h。将冻好的凝胶置于 -50—-10℃的真空冷冻干燥仪中干燥24h得到气凝胶,将气凝胶置于铝坩埚中以5℃/min的速度升温至450℃加热2h,并保温半小时后,即可得到掺杂TiO2的棉纤维复合碳气凝胶。由图2可知,将50g砝码放置在碳气凝胶上面对该气凝胶没有任何影响,说明制备的碳气凝胶有一定的强度,可以支持约333倍于自身重量的物质。分别将0.15g 该气凝胶置于50mL初始浓度为20mg/L的活性艳红X-3B和活性艳蓝K-NR溶液中进行光催化降解反应,整个光催化反应在光催化反应器中进行。以汞灯为光源,前30min黑暗条件下进行吸附,然后打开汞灯进行光催化降解。打开光源后90分钟内活性艳红X-3B的降解率达到95%,130分钟内活性艳蓝K-NR的降解率达到90%。
实施例3:
取3g碎布条加入50ml去离子水中,同时加入转移至水热反应釜中,在350℃下加热2h,得到液体,冷却后,加入1.0g壳聚糖到上述溶液,加入适量去离子水,磁力搅拌得到混合物,逐滴加入混合物质量2%的冰醋酸至粘稠溶胶,同时加入4ml环氧氯丙烷,0.5g石墨烯,80mg纳米TiO2,混合凝胶体积约40ml置于磁力搅拌器上均匀搅拌5h,静置2h,将该凝胶倒入准备好的模具中冷冻24h。将冻好的凝胶置于-50—-10℃的真空冷冻干燥仪中干燥24h得到气凝胶,将气凝胶置于铝坩埚中以5℃/min的速度升温至350℃加热2h,并保温半小时后,即可得到掺杂TiO2的棉纤维复合碳气凝胶。对掺杂TiO2的棉纤维复合碳气凝胶的光催化性能的评价方法:整个光催化反应在光催化反应器中进行,以汞灯为光源,分别将50mL 20mg/L的活性艳红X-3B、罗丹明、活性艳蓝K-NR、结晶紫四种染料加入光催化试管中,分别加入0.15g碳气凝胶样品,前30min黑暗条件下进行吸附,然后打开汞灯进行光催化降解。每隔10分钟取样利用紫外可见分光光度计测量吸光度。记录吸光度随时间的变化关系。结果如图6所示。
由图3可知,本实施例制备碳气凝胶内部呈现出大小不一的分级孔结构。
由图4可知,废弃棉织物经水热炭化以后可以得到纳米碳纤维。
由图5可知,碳气凝胶的拉曼光谱在1355cm-1和1582cm-1处对应的是典型的碳材料的D带(sp3杂化)和G带(sp2杂化),说明样品为无定形碳结构。
由图6可知,碳气凝胶对于染料的降解速度较快。
Claims (10)
1.一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,包括以下步骤:
(1)将废棉织物加入去离子水中,固液比为10-260g/L,转移至水热反应釜中碳化2-4h;
(2)将炭化后的产物取出,与壳聚糖混合,加入去离子水混合均匀后得到混合物,逐滴加入冰醋酸,使壳聚糖完全溶解得到透明溶胶;
(3)向溶胶中加入环氧氯丙烷、石墨烯粉末、纳米TiO2粉末,然后充分搅拌使各物质均匀混合后静置形成混合凝胶后倒入模具中;
(4)将盛有凝胶的模具放入冰箱中冷冻;
(5)取出冷冻好的凝胶,真空冷冻干燥后得到复合气凝胶材料;
(6)将气凝胶材料升温,持续加热保温,得到复合碳气凝胶。
2.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(1)中,将废棉织物剪成碎条加入去离子水中。
3.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(1)中,碳化温度为260-350℃。
4.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(2)中,棉织物碳化后与壳聚糖混合,加入去离子水使壳聚糖的浓度为20-40g/L。
5.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(2)中,冰醋酸的加入量为混合物质量的1%-2%。
6.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(3)中加入按溶胶体积10%的环氧氯丙烷;石墨烯粉末采用改进的Hummers法制备,每L溶胶加入10-20g石墨烯;纳米TiO2采用硫酸钛为钛源利用水热法于80℃合成,每L溶胶加入加入0.5-12g纳米TiO2。
7.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(3)中搅拌时间为4-6h,静置时间为2-3h。
8.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(4)中凝胶冷冻的时间为24h。
9.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(5)中冷冻好的凝胶,置于-50—-10℃的真空冷冻干燥仪中干燥24h得到复合气凝胶材料。
10.根据权利要求1所述的一种掺杂TiO2的棉纤维复合碳气凝胶的制备方法,其特征在于,步骤(5)具体为,将气凝胶材料以5℃/min的速度升温至350-550℃,持续加热2h后保温30分钟,得到复合碳气凝胶。
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