CN112591736A - Novel method for dispersing carbon nano-tubes with assistance of cellulose - Google Patents
Novel method for dispersing carbon nano-tubes with assistance of cellulose Download PDFInfo
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- CN112591736A CN112591736A CN202011484328.7A CN202011484328A CN112591736A CN 112591736 A CN112591736 A CN 112591736A CN 202011484328 A CN202011484328 A CN 202011484328A CN 112591736 A CN112591736 A CN 112591736A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 48
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 48
- 229920002678 cellulose Polymers 0.000 title claims abstract description 24
- 239000001913 cellulose Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 235000010980 cellulose Nutrition 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 6
- 229920001046 Nanocellulose Polymers 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 2
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 2
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 239000002109 single walled nanotube Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 239000002270 dispersing agent Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 150000004676 glycans Chemical class 0.000 abstract 1
- 229920001282 polysaccharide Polymers 0.000 abstract 1
- 239000005017 polysaccharide Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 3
- 238000007385 chemical modification Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 229920000875 Dissolving pulp Polymers 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明涉及一种纤维素辅助分散碳纳米管的新方法，属于材料技术领域。本发明采用天然多糖纤维素作为碳纳米管分散剂，在冰浴中通过温和的搅拌，短时间内实现碳纳米管在NaOH/尿素溶液中均匀稳定的分散。采用此制备方法操作简单，无需任何原料的预处理，易于规模化生产；且以纤维素作为原料，成本低廉，对环境无污染；本发明制备过程不会破坏碳纳米管的电子结构，有效地保护了其固有性质。
The invention relates to a new method for cellulose-assisted dispersion of carbon nanotubes, and belongs to the technical field of materials. The present invention adopts natural polysaccharide cellulose as carbon nanotube dispersant, and realizes uniform and stable dispersion of carbon nanotubes in NaOH/urea solution in a short time by gentle stirring in an ice bath. The preparation method is simple to operate, does not need any pretreatment of raw materials, and is easy to produce on a large scale; and cellulose is used as a raw material, which has low cost and no pollution to the environment; the preparation process of the invention does not destroy the electronic structure of carbon nanotubes, and effectively preserve its inherent properties.
Description
Technical Field
The invention belongs to the technical field of materials, and relates to a novel method for dispersing carbon nanotubes with the assistance of cellulose.
Background
Since the discovery of carbon nanotubes, carbon nanotubes have exhibited great application potential in the fields of catalysis, energy storage and conversion, flexible electronics, and the like due to their superior properties such as excellent electrical conductivity, ultra-high mechanical strength, and high thermal stability, and are considered as one of the core materials of next-generation ultra-light structural materials. However, since it has a large specific surface area and aspect ratio, the carbon nanotubes may be aggregated and entangled due to strong van der waals forces. The formation of such aggregates can seriously affect the subsequent processability and useful life of the carbon nanotubes. Therefore, effective dispersion of aggregated carbon nanotubes is a key technology for promoting the development of carbon nanotube-based materials.
At present, the dispersion method of carbon nanotubes mainly includes four methods: physical dispersion, chemical modification, surfactant dispersion, and polymer exfoliation. However, they have their own drawbacks. Physical methods require strong energy processes such as ultrasound to disperse carbon nanotubes, but the dispersion effect is poor despite simple processes, and the carbon nanotubes tend to aggregate quickly; chemical modification can destroy the electronic structure of the carbon nano tube and influence the conductivity and mechanical property of the carbon nano tube; the surfactant method may cause weak interfacial adhesion between the carbon nanotubes and the substrate material. The polymer stripping method is considered as one of the most potential carbon nanotube dispersion methods, and DNA, protein, chitosan, etc. can be used as a dispersing agent.
Nanocellulose has proven to be a highly efficient carbon nanotube dispersant because it has similar spatial dimensions as carbon nanotubes and is an amphiphilic molecule. However, the process of dispersing carbon nanotubes by cellulose reported at present is very complicated, and the cellulose and the carbon nanotubes need to be modified respectively first, and then the carbon nanotubes are dispersed by a strong physical process, so that the production period is long, the cost is high, and the large-scale application is not facilitated. Based on the problems, the invention provides a novel method for dispersing carbon nanotubes with the assistance of cellulose. The key points of the preparation method are as follows: dissolving cellulose and carbon nano tubes into NaOH/urea solution together, and stirring at ice bath temperature to obtain uniform and stable carbon nano tube dispersion liquid.
Disclosure of Invention
The invention utilizes cellulose, a rich natural biomass resource, as a carbon nano tube dispersing agent, and realizes the high-efficiency dispersion of the carbon nano tube in the NaOH/urea solution through a simple and mild stirring process in an ice bath.
The purpose of the invention is realized by the following technical scheme.
A novel method for dispersing carbon nano tubes with the assistance of cellulose is characterized by comprising the following steps:
(1) adding cellulose and carbon nano tubes into 11 wt% NaOH/4 wt% urea solution according to a fixed proportion;
(2) placing the mixed solution in an ice bath, and stirring at the rotating speed of 1000 rpm/min for 5 min;
(3) and centrifuging the obtained solution to remove insoluble substances to obtain uniform and stable carbon nanotube dispersion liquid.
Preferably, the ratio of cellulose to carbon nanotubes in step (1) is greater than 3: 1.
Preferably, the cellulose in the step (1) can be microcrystalline cellulose, nano cellulose fiber, bamboo fiber, hemp fiber, cellulose derivatives and the like, and the concentration of the cellulose is 1% -8%.
Preferably, the carbon nanotube species in step (1) may be single-walled carbon nanotubes, double-walled carbon nanotubes, or multi-walled carbon nanotubes.
Preferably, the mixture in step (1) is stirred in an ice bath.
Compared with the prior art, the invention has the following advantages:
(1) the method is simple to operate, does not need any pretreatment of raw materials, and is easy for large-scale production;
(2) the invention takes cellulose as raw material, has low cost and no pollution to the environment;
(3) the preparation process of the invention does not damage the electronic structure of the carbon nano tube, and effectively protects the inherent property of the carbon nano tube.
Drawings
FIG. 1 is a pictorial representation of a product of example 1 in accordance with the present invention.
FIG. 2 is a chart of the UV-Vis spectrum of the product of example 1 of the present invention.
Detailed Description
For a better understanding of the invention, it will be explained further below with reference to the embodiment examples and the accompanying drawings. It should be noted that the embodiments are only used for further explaining the invention, and the scope of the invention to be claimed is not limited to the scope shown in the embodiments.
Examples 1
Adding 3 g of cellulose and 0.2 g of carbon nano tube into 45 g of 11 wt% NaOH/4 wt% urea solution; then, the mixed solution is placed in an ice bath and stirred for 5min at the rotating speed of 1000 rpm/min; and centrifuging the obtained solution at the rotating speed of 3000 rpm/min for 3 min, and removing insoluble substances to obtain uniform and stable carbon nanotube dispersion liquid. Fig. 1 shows a physical diagram of the obtained carbon nanotube dispersion, and the solution did not precipitate even when left at room temperature for 1 day. Meanwhile, we performed an absorbance test on the solution to examine the dispersibility of the carbon nanotubes. As shown in fig. 2, at 290 nm, the carbon nanotube dispersion showed a broad peak, demonstrating monodispersity of the carbon nanotubes in solution.
Claims (5)
1. A novel method for dispersing carbon nano tubes with the assistance of cellulose is characterized by comprising the following steps:
(1) adding cellulose and carbon nano tubes into 11 wt% NaOH/4 wt% urea solution according to a fixed proportion;
(2) placing the mixed solution in an ice bath, and stirring at the rotating speed of 1000 rpm/min for 5 min;
(3) the solution obtained above was centrifuged to remove insoluble matter, and a uniform and stable carbon nanotube dispersion was obtained.
2. The method of claim 1, wherein the mass ratio of the cellulose to the carbon nanotubes in step (1) is greater than 3: 1.
3. The method of claim 1, wherein the cellulose in step (1) is microcrystalline cellulose, nanocellulose fiber, bamboo fiber, hemp fiber, cellulose derivative, etc., and the concentration of cellulose is 1-8%.
4. The method of claim 1, wherein the carbon nanotubes used in step (1) are selected from the group consisting of single-walled carbon nanotubes, multi-walled carbon nanotubes, and combinations thereof.
5. The method of claim 1, wherein the mixture in step (2) is stirred in an ice bath.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011484328.7A CN112591736B (en) | 2020-12-16 | 2020-12-16 | A method for cellulose-assisted dispersion of carbon nanotubes |
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| CN202011484328.7A CN112591736B (en) | 2020-12-16 | 2020-12-16 | A method for cellulose-assisted dispersion of carbon nanotubes |
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| CN112591736A true CN112591736A (en) | 2021-04-02 |
| CN112591736B CN112591736B (en) | 2022-12-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612312A (en) * | 2022-11-08 | 2023-01-17 | 浙江天浩新材料股份有限公司 | High-stability nano-cellulose dye dispersion liquid and preparation method thereof |
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| CN1482159A (en) * | 2003-07-25 | 2004-03-17 | 武汉大学 | A kind of solvent composition and its preparation method and application |
| CN101485962A (en) * | 2008-11-06 | 2009-07-22 | 青岛大学 | Simple method for dispersing carbon nano-tube |
| US20090202764A1 (en) * | 2007-11-26 | 2009-08-13 | Porcher Industries | RFL film or adhesive dip coating comprising carbon nanotubes and yarn comprising such a coating |
| US20100143234A1 (en) * | 2008-12-04 | 2010-06-10 | Sony Corporation | Methods of preparing and purifying carbon nanotubes, carbon nanotubes, and an element using the same |
| US20150069666A1 (en) * | 2012-05-30 | 2015-03-12 | Soongsil University Research Consortium Techno-Park | Method for preparing carbon nanotube fiber reinforced wtih carbon precursor |
| CN107207260A (en) * | 2015-02-25 | 2017-09-26 | 东丽株式会社 | The manufacture method of carbon nano tube dispersion liquid and conductive film |
| CN108745219A (en) * | 2018-06-20 | 2018-11-06 | 四川大学 | A kind of cellulose microsphere preparation method of novel high intensity and even intensity |
| CN109251342A (en) * | 2018-07-12 | 2019-01-22 | 南京林业大学 | A kind of nano-cellulose/carbon nano-tube/poly dimethyl siloxane conductive composite film and preparation method thereof |
| CN109796007A (en) * | 2019-02-19 | 2019-05-24 | 昆明理工大学 | Micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube |
| CN111554942A (en) * | 2020-05-07 | 2020-08-18 | 上海理工大学 | Silver-loaded cellulose/carbon nanotube composite material and preparation method and application thereof |
-
2020
- 2020-12-16 CN CN202011484328.7A patent/CN112591736B/en not_active Expired - Fee Related
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482159A (en) * | 2003-07-25 | 2004-03-17 | 武汉大学 | A kind of solvent composition and its preparation method and application |
| US20090202764A1 (en) * | 2007-11-26 | 2009-08-13 | Porcher Industries | RFL film or adhesive dip coating comprising carbon nanotubes and yarn comprising such a coating |
| CN101485962A (en) * | 2008-11-06 | 2009-07-22 | 青岛大学 | Simple method for dispersing carbon nano-tube |
| US20100143234A1 (en) * | 2008-12-04 | 2010-06-10 | Sony Corporation | Methods of preparing and purifying carbon nanotubes, carbon nanotubes, and an element using the same |
| US20150069666A1 (en) * | 2012-05-30 | 2015-03-12 | Soongsil University Research Consortium Techno-Park | Method for preparing carbon nanotube fiber reinforced wtih carbon precursor |
| CN107207260A (en) * | 2015-02-25 | 2017-09-26 | 东丽株式会社 | The manufacture method of carbon nano tube dispersion liquid and conductive film |
| CN108745219A (en) * | 2018-06-20 | 2018-11-06 | 四川大学 | A kind of cellulose microsphere preparation method of novel high intensity and even intensity |
| CN109251342A (en) * | 2018-07-12 | 2019-01-22 | 南京林业大学 | A kind of nano-cellulose/carbon nano-tube/poly dimethyl siloxane conductive composite film and preparation method thereof |
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| CN115612312B (en) * | 2022-11-08 | 2024-01-09 | 浙江天浩新材料股份有限公司 | High-stability nano cellulose dye dispersion liquid and preparation method thereof |
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| CN112591736B (en) | 2022-12-20 |
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