CN110371946A - 一种萘炔碳材料、制备方法及应用 - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005997 Calcium carbide Substances 0.000 claims abstract description 17
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 claims abstract description 17
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- XGCWMXCKMIUJAU-UHFFFAOYSA-N 1,2,3,4,5,6,7,8-octabromonaphthalene Chemical compound BrC1=C(Br)C(Br)=C(Br)C2=C(Br)C(Br)=C(Br)C(Br)=C21 XGCWMXCKMIUJAU-UHFFFAOYSA-N 0.000 claims description 7
- 241001537210 Perna Species 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
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- 238000000227 grinding Methods 0.000 claims 2
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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Abstract
本发明公开了一种萘炔碳材料、制备方法及应用,其包括如下步骤:将碳化钙与全卤代萘混合得到混合物,所述碳化钙与全卤代萘摩尔比为4~16:1,然后将所述混合物一次或多次地加入到球磨机中,在真空或常压惰性气体保护条件下球磨反应1~10h得反应产物,反应温度为常温,球磨速率为400~700r/min,将所述的反应产物先用稀硝酸洗涤,再用苯或甲苯洗涤得洗涤产物,将所述的洗涤产物用旋转蒸发仪在120℃下真空干燥,然后研磨成粉,得到粉末状萘炔碳材料,制备所得萘炔具有萘环间通过1个炔基连接的超广域共轭结构的碳骨架,在制备电催化产氧催化剂、光催化助催化剂、空穴传输材料和锂离子电池负极材料上具有良好的应用前景。
Description
技术领域
本发明属于新型碳纳米材料制备技术领域,尤其涉及一种萘炔碳材料、制备方法及应用。
背景技术
碳元素在地球上的丰度为第14位,主要以碳酸钙形式存在,其他存在形式包括碳纤维、石墨、金刚石、焦炭、炭黑、活性碳等。在过去的几十年中,富勒烯、碳纳米管、石墨烯等被相继发现。
新型碳材料研究是材料科学领域的重要分支。并因其新颖的合成技术、创新性的表征方法、有指导意义的结构性质关系、以及巨大的应用潜力,对科研界与人类生活产生了重大影响,也为能源、环境、催化等领域提供了巨大助力。
炔碳材料是碳原子聚集在一起形成的链,这些碳原子通过双键或者交替的单键和三键连接在一起,被认为是世界上最强韧的材料,强度比钢高200多倍。现有炔碳制备方法中以碳化钙、草酸或盐酸为原料在高温或高压条件下制备炔碳,缺少以碳化钙和全卤代萘为原料在常温下制备具有超广域共轭结构萘炔碳材料的方法。
发明内容
本发明所要解决的技术问题在于:缺少以碳化钙和全卤代萘为原料在常温下制备萘炔碳材料的方法,提供了一种萘炔碳材料、制备方法及应用。
本发明是通过以下技术方案解决上述技术问题的,本发明的一种萘炔碳材料的制备方法,包括如下步骤:
(1)将碳化钙与全卤代萘混合得到混合物,所述碳化钙与全卤代萘摩尔比为4~16:1,然后将所述混合物一次或多次地加入到球磨机的球磨罐中,在真空或常压惰性气体保护条件下球磨反应1~10h得反应产物,反应温度为常温,球磨速率为400~700r/min;
(2)将所述的反应产物先用稀硝酸洗涤,再用苯或甲苯洗涤得洗涤产物;
(3)将所述的洗涤产物用旋转蒸发仪在120℃下真空干燥,然后研磨成粉,得到粉末状萘炔碳材料;
所述的萘炔碳材料具有超广域共轭结构;
所述的萘炔碳材料结构中萘环通过炔基连接。
所述步骤(1)中,球磨机选自震动式球磨机、搅拌式球磨机、滚筒式球磨机和行星式球磨机中的任一种。
所述步骤(1)中,碳化钙与全卤代萘摩尔比为8~12:1。
所述步骤(1)中,全卤代萘选自全氯萘、全溴萘中的至少一种。
所述步骤(1)中,球磨机中磨球与混合物的质量比为10~100:1。
所述步骤(1)中,碳化钙及全卤代萘为预先粉碎的150~200目的粉末;
惰性气氛选自氮气、氩气中的任一种;
球磨机中磨球与混合物的质量比为30~60:1。
所述的萘炔碳材料结构中萘环通过1个炔基连接。
一种由所述的萘炔碳材料的制备方法制备得到的萘炔碳材料。
一种所述的萘炔碳材料在制备能量储存与传递材料上的应用。
一种所述的萘炔碳材料在制备电催化产氧催化剂、光催化助催化剂上的应用。
该方法以碳化钙和全卤代萘为原料,通过机械化学作用使二者在温和条件下直接反应,从而高效合成新型萘炔碳材料——萘炔(Naphyne),本方法反应条件温和、设备简单、工艺简便,原料廉价易得。
本发明方法制备所得萘炔是萘环通过1个炔基连接的超广域共轭结构的碳骨架,质地均匀,结构独特,物化性质优良,在制备电催化产氧催化剂、光催化助催化剂、空穴传输材料和锂离子电池负极材料上具有良好的应用前景,并且具有良好的超电容性能,可作为超级电容器电极材料的优良备选,在能量储存与传递领域具有良好的应用前景。
附图说明
图1为萘炔的化学结构式;
图2为实施例1所制备萘炔的扫描电镜图;
图3为实施例1所制备萘炔的透射电镜图;
图4为实施例1所制备萘炔的EDS元素分析图;
图5为实施例1所制备萘炔的X射线光电子能谱的碳谱拟合图;
图6为实施例1所制备萘炔的X射线衍射图(XRD);
图7为实施例1所制备萘炔电极材料的CV图谱;
图8为实施例1所制备萘炔电极材料的GCD图谱;
图9为实施例2所制备萘炔的扫描电镜图;
图10为实施例2所制备萘炔的透射电镜图;
图11为实施例2所制备萘炔的拉曼图;
图12为实施例3所制备萘炔的扫描电镜图;
图13为实施例3所制备萘炔的透射电镜图。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1:
本实施例提供一种萘炔的制备方法,包括如下步骤:
(1)按照碳化钙和全氯萘(C10Cl8)摩尔比为12:1,分别称取碳化钙和全氯萘,置于真空球磨罐中,并控制球料质量比为30:1。密封球磨罐,并将其抽至1kPa的真空度,然后将其置于行星式球磨机上。以650转/分钟的球磨速率通过行星式球磨机球磨4小时。运行过程中为防止机器过热,每运行30分钟停止5分钟。反应完成后,打开球磨罐,原来的灰色粉末变为漆黑色,证明碳材料的生成;取部分漆黑色的反应产物置入烧杯中,以稀硝酸处理并测定滤液中氯离子含量,由此确定全氯萘的脱氯率为95.89%。
(2)步骤(1)的反应产物经酸洗、苯洗后再于120℃真空干燥5小时,即可得到本发明所述的萘炔,称重并计算其表观碳收率为106%。
所得萘炔的化学结构式如图1所示,可知,制备所得萘炔是萘环通过1个炔基连接的超广域共轭结构的碳骨架。
所得萘炔的扫描电镜测试结果(图2)表明,用该方法制备的萘炔具有良好的孔结构,属于多孔材料,且多片状褶皱存在。
所得萘炔的透射电镜测试结果(图3)表明,该炔碳材料具有良好的层状结构。
所得萘炔的EDS元素分析(图4)表明,样品除了表面污染所带入的氧元素及极微量的氯元素残留外,仅由碳元素组成,碳含量高达98.57%。
样品的X射线光电子能谱的碳谱拟合(图5)证明样品中的碳元素之间存在sp2和sp杂化,且含量之比接近10:8。
所得萘炔的X射线衍射分析(图6)表明,萘炔碳材料具有一定的晶状结构。
将所得萘炔置于泡沫镍上,制成超级电容器电极材料,并对其进行超电容性能测试。实验所得其CV图谱(图7)与GCD图谱(图8),证实所得萘炔具备出色的超电容性能,且其比容可达154F/g。
实施例2:
本实施例提供一种萘炔的制备方法,其包括如下步骤:
(1)按照碳化钙和全溴萘(C10Br8)摩尔比为8:1分别称取碳化钙和全溴萘,置于真空球磨罐中,并控制球料质量比为50:1。密封球磨罐,并将其抽至1kPa的真空度,然后将其置于行星式球磨机上。以500转/分钟的球磨速率在行星式球磨机上球磨10小时。运行过程中为防止机器过热,每运行30分钟停止5分钟。反应完成后,打开球磨罐,原来的灰色粉末变为漆黑色,证明碳材料的生成。取部分漆黑色的反应产物移入烧杯中,以稀硝酸处理并测定滤液中溴离子含量,由此确定全溴萘的脱溴率为96%。
(2)步骤(1)的反应产物经酸洗、苯洗后再于120℃真空干燥5小时,即可得到本发明所述的萘炔,称重并计算其表观碳收率为98%。
所得萘炔的扫描电镜测试结果(图9)表明,用该方法制备的萘炔具有良好的孔结构,属于多孔材料。
所得萘炔的透射电镜测试结果(图10)表明,该萘炔碳材料具有良好的孔隙结构。
所得萘炔的拉曼图样(图11)说明样品中的结构呈现高度有序化,缺陷极少。
实施例3:
本实施例提供一种萘炔的制备方法,其包括如下步骤:
(1)按照摩尔比为碳化钙:全氯萘(C10Cl8):全溴萘(C10Br8)=4:1:1分别称取碳化钙、全氯萘、全溴萘,置于真空球磨罐中,并控制球料质量比为60:1。密封球磨罐,并将其抽至1kPa的真空度,然后将其置于搅拌式球磨机上。以400转/分钟的球磨速率在搅拌式球磨机上运行1小时。反应完成后,打开球磨罐,原来的灰色粉末变为漆黑色,证明碳材料的生成。
(2)步骤(1)的反应产物经酸洗、苯洗后再于120℃真空干燥5小时,即可得到本发明所述的萘炔,称重并计算其表观碳收率为95%。
所得萘炔的扫描电镜测试结果(图12)表明,用该方法制备的萘炔具有良好的孔结构,属于多孔材料。
所得萘炔的透射电镜测试结果(图13)表明,该炔碳材料具有良好的层状结构。所得萘炔的结构性计算证明,其能带呈现窄带直接隙,同时证明其具备半导体的相关特性。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种萘炔碳材料的制备方法,其特征在于,包括如下步骤:
(1)将碳化钙与全卤代萘混合得到混合物,所述碳化钙与全卤代萘摩尔比为4~16:1,然后将所述混合物一次或多次地加入到球磨机的球磨罐中,在真空或常压惰性气体保护条件下球磨反应1~10h得反应产物,反应温度为常温,球磨速率为400~700r/min;
(2)将所述的反应产物先用稀硝酸洗涤,再用苯或甲苯洗涤得洗涤产物;
(3)将所述的洗涤产物用旋转蒸发仪在120℃下真空干燥,然后研磨成粉,得到粉末状萘炔碳材料;
所述的萘炔碳材料具有超广域共轭结构;所述萘炔碳材料结构中萘环通过炔基连接。
2.根据权利要求1所述的一种萘炔碳材料的制备方法,其特征在于,所述步骤(1)中,球磨机选自震动式球磨机、搅拌式球磨机、滚筒式球磨机和行星式球磨机中的任一种。
3.根据权利要求1所述的一种萘炔碳材料的制备方法,其特征在于,所述步骤(1)中,碳化钙与全卤代萘摩尔比为8~12:1。
4.根据权利要求1所述的一种萘炔碳材料的制备方法,其特征在于,所述步骤(1)中,全卤代萘选自全氯萘、全溴萘中的至少一种。
5.根据权利要求1所述的一种萘炔碳材料的制备方法,其特征在于,所述步骤(1)中,球磨机中磨球与混合物的质量比为10~100:1。
6.根据权利要求1所述的一种萘炔碳材料的制备方法,其特征在于,所述步骤(1)中,碳化钙及全卤代萘为预先粉碎的150~200目的粉末;
惰性气氛选自氮气、氩气中的任一种。
7.根据权利要求1所述的一种萘炔碳材料的制备方法,其特征在于,所述的萘炔碳材料结构中萘环通过1个炔基连接。
8.一种由权利要求1~7任一项所述的萘炔碳材料的制备方法制备得到的萘炔碳材料。
9.一种如权利要求8所述的萘炔碳材料在制备能量储存与传递材料上的应用。
10.一种如权利要求8所述的萘炔碳材料在制备电催化产氧催化剂、光催化助催化剂上的应用。
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