CN106947250B - 一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法 - Google Patents
一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法 Download PDFInfo
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- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 title claims abstract description 31
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 25
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 5
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
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Abstract
本发明涉及一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法。包括以下步骤：三氧化钨的制备，三氧化钨/聚苯胺的制备，三氧化钨/聚苯胺/石墨烯的制备。本发明的有益效果是三氧化钨/聚苯胺/石墨烯复合材料的制备方法简便新颖。
Description
技术领域
本发明涉及一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法，属于材料合成领域。
技术背景
近年来，石墨烯与导电高分子及过渡金属氧化物复合材料已经引起了研究工作者越来越多的关注，已经成为电化学研究的前言领域之一。三氧化钨是稳定的n型半导体材料，已经被广泛的应用在气体传感器和电化学催化等方面。近几年已经有部分研究将三氧化钨应用在电化学储能方面，研究表明三氧化钨与石墨烯气凝胶复合材料能表现出极好的电容性能。聚苯胺，高分子化合物的一种，具有特殊的电学、光学性质，经掺杂后可具有导电性，稳定性好。石墨烯是从石墨材料中剥离出来、由碳原子组成的只有一层原子厚度的二维晶体，石墨烯既是最薄的材料，也是最强韧的材料，同时它还具有很好的弹性。每个碳原子均为sp2杂化，并贡献剩余一个p轨道上的电子形成大π键，π电子可以自由移动，赋予石墨烯良好的导电性。因此本实验通过逐步合成的方法合成三氧化钨/聚苯胺/石墨烯复合材料。
发明内容
本发明的目的是在于提供一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法。
本发明所述一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法，包括以下步骤：
a、三氧化钨的制备：称取磷钨酸溶于的乙醇中，在室温下干燥完全后在空气条件下煅烧4h；
b、三氧化钨/聚苯胺的制备：将0.2g步骤a中所制备的三氧化钨超声分散在10mL1mol L-1的盐酸溶液中，加入苯胺单体，然后迅速加入10mL溶有过硫酸铵的1mol L-1的盐酸溶液，室温下迅速晃动30s，静置4h后将生成物离心，洗涤，冷冻干燥；
c、三氧化钨/聚苯胺/石墨烯的制备：将0.2g步骤b中所制备的三氧化钨/聚苯胺超声分散在10mL 1mg mL-1的氧化石墨烯的分散液中，加入0.9mL的浓盐酸，然后加入锌粉超声30min，紧接着加入1mL浓盐酸除去过量的锌粉，最后将生成物离心，洗涤，冷冻干燥。
进一步，所述步骤a中磷钨酸的量为1～5g，煅烧温度为200～500℃。
进一步，所述步骤b中苯胺单体的量为0.1～0.5mL，过硫酸铵的量为0.1～0.4g。
进一步，所述步骤c中加入锌粉的量为40～100mg。
本发明的有益效果是：三氧化钨/聚苯胺/石墨烯复合材料的制备方法简便新颖。
具体实施方式
现在结合具体实施例对本发明做进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例一：
三氧化钨/聚苯胺/石墨烯复合材料的制备方法，包括以下步骤：
(1)称取1g磷钨酸溶于的乙醇中，在室温下干燥完全后在空气条件下350℃煅烧4h。
(2)将0.2g步骤(1)中所制备的三氧化钨超声分散在10mL 1mol L-1的盐酸溶液中，加入0.3mL苯胺单体，然后迅速加入10mL溶有0.18g过硫酸铵的1mol L-1的盐酸溶液，室温下迅速晃动30s，静置4h后将生成物离心，洗涤，冷冻干燥。
(3)将0.2g步骤(2)中所制备的三氧化钨/聚苯胺超声分散在10mL 1mg mL-1的氧化石墨烯的分散液中，加入0.9mL的浓盐酸，然后加入80mg锌粉超声30min，紧接着加入1mL浓盐酸除去过量的锌粉，最后将生成物离心，洗涤，冷冻干燥。
Claims (4)
1.一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法，其特征在于：步骤如下：
a、三氧化钨的制备：称取磷钨酸溶于的乙醇中，在室温下干燥完全后在空气条件下煅烧4h；
b、三氧化钨/聚苯胺的制备：将0.2g步骤a中所制备的三氧化钨超声分散在10mL 1molL-1的盐酸溶液中，加入苯胺单体，然后迅速加入10mL溶有过硫酸铵的1mol L-1的盐酸溶液，室温下迅速晃动30s，静置4h后将生成物离心，洗涤，冷冻干燥；
c、三氧化钨/聚苯胺/石墨烯的制备：将0.2g步骤b中所制备的三氧化钨/聚苯胺超声分散在10mL 1mg mL-1的氧化石墨烯的分散液中，加入0.9mL的浓盐酸，然后加入锌粉超声30min，紧接着加入1mL浓盐酸除去过量的锌粉，最后将生成物离心，洗涤，冷冻干燥。
2.根据权利要求1所述一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法，其特征是：所述步骤a中磷钨酸的量为1～5g，煅烧温度为200～500℃。
3.根据权利要求1所述一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法，其特征是：所述步骤b中苯胺单体的量为0.1～0.5mL，过硫酸铵的量为0.1～0.4g。
4.根据权利要求1所述一种三氧化钨/聚苯胺/石墨烯复合材料的制备方法，其特征是：所述步骤c中加入锌粉的量为40～100mg。
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| Graphenated polyaniline-doped tungsten oxide nanocompositesensor for real time determination of phenanthrene;Oluwakemi等;《Electrochimica Acta》;20140104;138-148页 |
| Preparation of polyaniline grafted graphene oxide–WO3 nanocomposite and its application as a chromium(III) chemi-sensor;Anish Khan等;《RSC Adv.》;20151113;第5卷;105169-105178页 |
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