CN110078105A - 一种碳-氢氧化铝纳米粒子的制备方法 - Google Patents
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000012065 filter cake Substances 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims abstract description 8
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- 239000000047 product Substances 0.000 claims abstract description 5
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 4
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 4
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- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract 2
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- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
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- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
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- 239000000463 material Substances 0.000 description 7
- 239000011852 carbon nanoparticle Substances 0.000 description 6
- 238000010189 synthetic method Methods 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000408529 Libra Species 0.000 description 1
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- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QLRJIUFLNIZNQZ-UHFFFAOYSA-G [C+4].[OH-].[Al+3].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [C+4].[OH-].[Al+3].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] QLRJIUFLNIZNQZ-UHFFFAOYSA-G 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XFBXDGLHUSUNMG-UHFFFAOYSA-N alumane;hydrate Chemical compound O.[AlH3] XFBXDGLHUSUNMG-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 carbon-hydroxide Aluminum Chemical compound 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
本发明公开了一种碳‑氢氧化铝纳米粒子的制备方法，包括以下步骤：取石墨放入到装有高氯酸HClO4的三口烧瓶中，沸腾状态下回流；将三口烧瓶冷却至60‑80℃，加入Al(CH3COO)3和聚乙烯醇PVA，用NaOH调节pH值，搅拌，冷却后得到黑色悬浊液；将所述悬浊液超声，抽滤，得到滤饼；将滤饼真空干燥研磨，得到产品即碳‑氢氧化铝纳米粒子。本发明成本低、简便、快速，实现了大规模的生产绿色环保稳定的碳‑氢氧化铝纳米粒子复合材料。
Description
技术领域
本发明涉及碳-氢氧化铝纳米粒子的制备方法。
背景技术
不同的碳纳米材料具有不同的功能，如石墨碳纳米颗粒具有强大的吸附能力，该类碳纳米颗粒还具有很好的相容性、增敏效应和易于表面功能化等优点。目前，碳纳米颗粒的制备方法可以分为两类：自上而下法和自下而上法。自上而下法即从较大的碳结构剥落制备碳纳米颗粒的物理方法，主要包括：电弧放电法、激光刻蚀法、电化学法、酸回煮法。自下而上法即由分子前驱体制备碳纳米颗粒的化学方法，主要包括：支持合成法、有机物碳化法。这些合成方法各自存在一定的不足，碳纳米颗粒的形貌、产量以及质量难以达到精确控制，不能达到大规模的简单合成。对于其生长机制也缺乏探讨，特别是由于合成方法的限制使其在应用方面的研究尚处于起步阶段。
氢氧化铝是一种应用前景好的高聚物基复合材料的无机阻燃填料，其市场用量十分庞大。但是氢氧化铝与高分子材料的相容性、分散性均很差，往高分子材料中添加氢氧化铝常常严重影响材料的力学性能和加工性能。因此，必须对其进行表面改性处理，以改善其与高聚物基料的相容性，使填充材料的力学性能不下降，甚至使材料的部分力学性能有所提高。
发明内容
本发明为了克服上述的不足，提供了一种碳-氢氧化铝纳米粒子的制备方法，其制备过程成本低、简便、快速。
本发明的技术方案如下：
一种碳-氢氧化铝纳米粒子的制备方法，包括以下步骤：
(1)取1-2g石墨放入到装有3-5M、150ml的高氯酸HClO4的三口烧瓶中，在室温下200rpm下搅拌24h，然后在100-120℃沸腾状态下回流24h；
(2)将三口烧瓶冷却至60-80℃，加入1-2g Al(CH3COO)3和1-5毫升聚乙烯醇PVA(5mg/ml)，用NaOH(3M)调节pH至9-11，在300rpm下搅拌6h，冷却至室温，得到黑色悬浊液；
(3)将悬浊液在80-120W、30-50KHz超声3-6h，抽滤，用去离子水洗涤滤饼至质量不变；
(4)将滤饼在50-80℃下真空干燥8-10h，对干燥后的滤饼进行研磨，得到产品即碳-氢氧化铝纳米粒子。
本发明的有益效果是：
本发明具有可连续生产，环境污染少等优点，在制备碳-氢氧化铝纳米粒子时更为经济、便捷和环保。
附图说明
本发明将通过例子并参照附图的方式说明，其中：
图1是原料石墨和碳-氢氧化铝纳米粒子样品UV图；
图2是碳-氢氧化铝纳米粒子样品粒径测试图；
图3是原料石墨的SEM图；
图4是碳-氢氧化铝纳米粒子样品TEM图。
具体实施方式
本说明书中公开的任一特征，除非特别叙述，均可被其他等效或具有类似目的的替代特征加以替换。即，除非特别叙述，每个特征只是一系列等效或类似特征中的一个例子而已。
一种碳-氢氧化铝纳米粒子的制备方法，包括以下步骤：
(1)取1-2g石墨放入到装有3-5M、150ml的高氯酸HClO4的三口烧瓶中，在室温下200rpm下搅拌24h，然后在100-120℃沸腾状态下回流24h；
(2)将三口烧瓶冷却至60-80℃，加入1-2g Al(CH3COO)3和1-5毫升聚乙烯醇PVA(5mg/ml)，用NaOH(3M)调节pH至9-11，在300rpm下搅拌6h，冷却至室温，得到黑色悬浊液；
(3)将悬浊液在80-120W、30-50KHz超声3-6h，抽滤，用去离子水洗涤滤饼至质量不变；
(4)将滤饼在50-80℃下真空干燥8-10h，对干燥后的滤饼进行研磨，得到产品即碳-氢氧化铝纳米粒子。
将上述得到的碳-氢氧化铝纳米粒子样品通过紫外可见分光光度计(UV)(T6北京普析通用仪器有限公司)进行紫外表征的分析(见图1)。如图1所示，曲线(虚)为原料石墨的UV曲线；曲线(实)是在530-550nm处出现了明显的C/Al(OH)3的特征峰；进一步证实了产品就是碳-氢氧化铝纳米粒子。
将上述得到的碳-氢氧化铝纳米粒子样品通过纳米粒度分析仪(NANOPHOXParticle Size Analysis)进行分析(见图2)，测试范围：1-10000nm，浓度范围：ppm-70vol.％，光源：氦氖激光、波长632.8nm，激光功率：10mw，温度：15-40℃，湿度20-70％无冷凝。如图2所示，碳-氢氧化铝纳米粒子粒径小于5nm，由此可得，成功制备了碳-氢氧化铝纳米粒子。
对碳-氢氧化铝纳米粒子的样品通过日本日立公司生产的S4800型扫描电镜SEM(见图3)和日立Libra 120型透射电镜TEM(见图4)进行分析。图3是原料石墨的SEM图，石墨呈片层状；图4是碳-氢氧化铝纳米粒子的TEM图，从图4可以看到图中分布颗粒状的碳包覆氢氧化铝纳米颗粒；与图3比较可以知道石墨的片层结构已经被破坏，纳米级的碳-氢氧化铝粒子已经制备成功。
本发明并不局限于前述的具体实施方式。本发明扩展到任何在本说明书中披露的新特征或任何新的组合，以及披露的任一新的方法或过程的步骤或任何新的组合。
Claims (1)
1.一种碳-氢氧化铝纳米粒子的制备方法，其特征在于，包括以下步骤：
(1)取1-2g石墨放入到装有3-5M、150ml的高氯酸HClO4的三口烧瓶中，在室温下200rpm下搅拌24h，然后在100-120℃沸腾状态下回流24h；
(2)将三口烧瓶冷却至60-80℃，加入1-2g Al(CH3COO)3和1-5毫升聚乙烯醇PVA(5mg/ml)，用NaOH(3M)调节pH至9-11，在300rpm下搅拌6h，冷却至室温，得到黑色悬浊液；
(3)将悬浊液在80-120W、30-50KHz超声3-6h，抽滤，用去离子水洗涤滤饼至质量不变；
(4)将滤饼在50-80℃下真空干燥8-10h，对干燥后的滤饼进行研磨，得到产品即碳-氢氧化铝纳米粒子。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05105425A (ja) * | 1991-10-16 | 1993-04-27 | Matsushita Electric Works Ltd | 酸化アルミニウム粉末の製造方法 |
| KR20150006713A (ko) * | 2013-07-09 | 2015-01-19 | 삼성전기주식회사 | 인쇄회로기판용 절연필름 및 이를 이용한 제품 |
| CN105152164A (zh) * | 2015-08-21 | 2015-12-16 | 合肥工业大学 | 一种石墨烯薄片的制备方法 |
| CN108502908A (zh) * | 2018-04-10 | 2018-09-07 | 宁波工程学院 | 一种碳包覆氢氧化铝纳米复合材料的制备方法 |
| CN108658105A (zh) * | 2018-04-10 | 2018-10-16 | 宁波工程学院 | 一种碳包覆氢氧化镁纳米复合材料的制备方法 |
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- 2019-04-22 CN CN201910322529.8A patent/CN110078105A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05105425A (ja) * | 1991-10-16 | 1993-04-27 | Matsushita Electric Works Ltd | 酸化アルミニウム粉末の製造方法 |
| KR20150006713A (ko) * | 2013-07-09 | 2015-01-19 | 삼성전기주식회사 | 인쇄회로기판용 절연필름 및 이를 이용한 제품 |
| CN105152164A (zh) * | 2015-08-21 | 2015-12-16 | 合肥工业大学 | 一种石墨烯薄片的制备方法 |
| CN108502908A (zh) * | 2018-04-10 | 2018-09-07 | 宁波工程学院 | 一种碳包覆氢氧化铝纳米复合材料的制备方法 |
| CN108658105A (zh) * | 2018-04-10 | 2018-10-16 | 宁波工程学院 | 一种碳包覆氢氧化镁纳米复合材料的制备方法 |
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