CN108640566B - Preparation method of carbon nanotube/cellulose light wave-absorbing foam - Google Patents
Preparation method of carbon nanotube/cellulose light wave-absorbing foam Download PDFInfo
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- CN108640566B CN108640566B CN201810367882.3A CN201810367882A CN108640566B CN 108640566 B CN108640566 B CN 108640566B CN 201810367882 A CN201810367882 A CN 201810367882A CN 108640566 B CN108640566 B CN 108640566B
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- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/28—Polysaccharides or derivatives thereof
- C04B26/285—Cellulose or derivatives thereof
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- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
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Abstract
The invention relates to a preparation method of carbon nanotube/cellulose light wave-absorbing foam, which specifically comprises the preparation of carbon nanotube water dispersion and cellulose water solution; and mixing the two solutions by processes such as ultrasonic stirring to obtain uniform dispersion liquid, and placing the uniform dispersion liquid in a mold for freeze drying to obtain the carbon nano tube/cellulose light wave-absorbing foam. The invention adopts nontoxic and easily obtained raw materials, has simple preparation process, controllable process, low cost and good repeatability, and the obtained wave-absorbing foam has the advantages of width, strength, lightness, thinness and adjustable dielectric property, and is suitable for the fields of electromagnetic wave absorption/shielding and the like.
Description
Technical Field
The invention belongs to the technical field of carbon nano functional material manufacturing, and relates to a preparation method of carbon nano tube/cellulose light wave-absorbing foam.
Background
The foam material has the advantages of strong designability, light weight, simple process and the like, and is widely concerned and researched in the field of electromagnetic wave absorption/shielding. Patent CN103923337 discloses a PMI composite foam wave-absorbing material, which is prepared by mixing a wave-absorbing agent and foamable PMI resin particles with a specific binder and then foaming the mixture. However, the process is complicated, the types of the required materials are more than 10, and the density of the prepared foam is high, so that the practical application of the foam is limited. Patent CN201710250796.X discloses a light broadband PMI foam and a preparation method thereof, the light broadband PMI foam has good wave absorbing performance, but the preparation process is complex and is difficult to apply on a large scale.
The carbon nano tube has the characteristics of excellent electric conductivity, heat conductivity, high specific strength, low density and the like, is used as a composite material reinforcement, and is widely applied to the fields of composite material reinforcement, heat conductivity, catalysis, supercapacitors, electromagnetic shielding, sensors and the like. In particular, in the field of electromagnetic wave absorption/shielding, materials such as carbon nanotube-reinforced PDC ceramics, carbon nanotube-reinforced resin-based composite materials, carbon nanotube/nanoparticle composite wave absorbers, carbon nanotube films, and the like have been widely studied. Multiwall carbon nanotube/waterborne polyurethane foams (Zhong Zhang, et al. Lightweight and Anisotropic porous MWCNT/WPU Composites for ultra high Performance Electromagnetic interference Shield, adv. Funct. Mater.2016,26, 303-doped 310) were prepared by Zhong Zhang et al, and the Electromagnetic shielding Performance of the resulting foams was up to 50 dB.
Because the carbon nano tube has high conductivity, the existing carbon nano tube foam material mostly shows electromagnetic shielding performance. The wave-absorbing performance is rarely reported, and how to develop the light carbon nanotube foam material with adjustable electromagnetic wave-absorbing/shielding performance and simple preparation process is very important for the practical application.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of carbon nanotube/cellulose light wave-absorbing foam, aiming at the defects of complex preparation process, high density, difficult regulation and control of electromagnetic wave absorption/shielding performance and the like of the existing wave-absorbing foam. The method takes environment-friendly cellulose and carbon nano tubes as raw materials, and has the advantages of easy adjustment of electromagnetic wave absorption/shielding performance, simple preparation process, low cost and the like.
Technical scheme
A preparation method of carbon nano tube/cellulose light wave-absorbing foam is characterized by comprising the following steps:
step 1: placing 0.1-3 g of carbon nano tube in 97-99.9 ml of deionized water, and performing ultrasonic dispersion for 0.5-6 h to obtain a uniformly dispersed carbon nano tube water dispersion liquid;
placing 0.1-1.5 g of cellulose in 98.5-99.9 ml of deionized water, and carrying out ultrasonic treatment for 0.5-3 h to obtain a cellulose aqueous solution;
step 2: placing the carbon nano tube water dispersion in a cellulose water solution, and carrying out ultrasonic treatment for 1-3 h to obtain a mixed solution; the volume of the carbon nano tube water dispersion liquid is 10-90 ml, and the volume of the cellulose water solution is 10-90 ml;
and step 3: placing the mixed solution in a mold, cooling to-60 ℃ at a speed of 3-10 ℃/min, pre-freezing for 3-10 h, drying for 20-40 h under a vacuum condition of 0.1Pa, and demolding to obtain the carbon nanotube/cellulose light wave-absorbing foam;
the proportion is measured in each part.
The carbon nano tube is a single-wall carbon nano tube, a double-wall carbon nano tube, a multi-wall carbon nano tube or an aminated multi-wall carbon nano tube.
The cellulose is nano cellulose fiber or carboxymethyl cellulose.
Advantageous effects
The invention provides a preparation method of carbon nanotube/cellulose light wave-absorbing foam, which specifically comprises the preparation of carbon nanotube water dispersion and cellulose water solution; and mixing the two solutions by processes such as ultrasonic stirring to obtain uniform dispersion liquid, and placing the uniform dispersion liquid in a mold for freeze drying to obtain the carbon nano tube/cellulose light wave-absorbing foam. The invention adopts nontoxic and easily obtained raw materials, has simple preparation process, controllable process, low cost and good repeatability, and the obtained wave-absorbing foam has the advantages of width, strength, lightness, thinness and adjustable dielectric property, and is suitable for the fields of electromagnetic wave absorption/shielding and the like.
Drawings
FIG. 1 is SEM photograph and optical photograph of carbon nanotube/cellulose light wave-absorbing foam in example 1
FIG. 2(a) electromagnetic wave absorption performance of light carbon nanotube/cellulose wave-absorbing foam in example 1
FIG. 2(b) electromagnetic shielding performance of the carbon nanotube/cellulose light wave-absorbing foam in example 2
FIG. 3 is a flow chart of a preparation process of carbon nanotube/cellulose light wave-absorbing foam
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1
Putting 3g of multi-walled carbon nano-tube into 97ml of deionized water, and ultrasonically dispersing for 3h to obtain a uniformly dispersed multi-walled carbon nano-tube water dispersion liquid; putting 1g of nano cellulose fiber into 99ml of deionized water, and carrying out ultrasonic treatment for 1h to obtain a nano cellulose fiber aqueous solution; putting 10ml of multi-walled carbon nanotube aqueous dispersion into 70ml of nano cellulose fiber aqueous solution, and carrying out ultrasonic treatment for 1.5h to obtain a mixed solution; placing the mixed solution in a cubic mold, pre-freezing at 5 deg.C/min to-60 deg.C for 6h, and drying under 0.1Pa vacuum for 30 h. And demolding to obtain the carbon nano tube/cellulose light wave-absorbing foam. When the thickness of the prepared foam is changed within the range of 5.3-6.8 mm, the prepared foam has excellent wave absorbing performance (EAB is 4.2GHz, and has the capacity of absorbing more than 99% of electromagnetic waves within the range of 8.2-12.4 GHz) of effectively absorbing and covering all frequency bands within the range of X wave band, and the strongest absorption can reach-27 dB. The electromagnetic reflection coefficient is shown in fig. 2 a.
Example 2
Placing 1.5g of single-walled carbon nanotubes in 98.5ml of deionized water, and ultrasonically dispersing for 5 hours to obtain uniformly dispersed single-walled carbon nanotube water dispersion; putting 0.5g of carboxymethyl cellulose in 99.5ml of deionized water, and carrying out ultrasonic treatment for 1 hour to obtain a carboxymethyl cellulose aqueous solution; putting 50ml of single-walled carbon nanotube aqueous dispersion into 20ml of carboxymethyl cellulose aqueous solution, and carrying out ultrasonic treatment for 2 hours to obtain a mixed solution; placing the mixed solution in a cuboid mold, pre-freezing at 3 deg.C/min to-60 deg.C for 8h, and drying under 0.1Pa vacuum condition for 40 h. And demolding to obtain the carbon nano tube/cellulose light wave-absorbing foam. The prepared foam has the electromagnetic wave shielding performance of more than 37dB in an X wave band. Its electromagnetic shielding performance is shown in fig. 2 b.
Example 3
Placing 2g of aminated carbon nanotube in 98ml of deionized water, and ultrasonically dispersing for 4 hours to obtain a uniformly dispersed aminated carbon nanotube water dispersion; putting 1.5g of carboxymethyl cellulose in 98.5ml of deionized water, and carrying out ultrasonic treatment for 2 hours to obtain a carboxymethyl cellulose aqueous solution; placing 30ml of single-walled carbon nanotube aqueous dispersion in 50ml of carboxymethyl cellulose aqueous solution, and carrying out ultrasonic treatment for 2 hours to obtain a mixed solution; placing the mixed solution in a cuboid mold, pre-freezing at 3 deg.C/min to-60 deg.C for 6h, and drying under 0.1Pa vacuum for 36 h. And demolding to obtain the carbon nano tube/cellulose light wave-absorbing foam. The prepared foam has excellent wave-absorbing performance in X.
Example 4
Putting 1g of double-walled carbon nanotube into 99ml of deionized water, and ultrasonically dispersing for 3 hours to obtain uniformly dispersed double-walled carbon nanotube water dispersion; putting 1.2g of nano cellulose fiber into 98.8ml of deionized water, and carrying out ultrasonic treatment for 3h to obtain a carboxymethyl cellulose aqueous solution; putting 40ml of single-walled carbon nanotube aqueous dispersion into 40ml of nanocellulose fiber aqueous solution, and carrying out ultrasonic treatment for 3 hours to obtain a mixed solution; placing the mixed solution in a cuboid mold, pre-freezing at 5 deg.C/min to-60 deg.C for 6h, and drying under 0.1Pa vacuum condition for 32 h. And demolding to obtain the carbon nano tube/cellulose light wave-absorbing foam. The prepared foam has excellent wave-absorbing performance in Ku.
Claims (1)
1. A preparation method of carbon nano tube/cellulose light wave-absorbing foam is characterized by comprising the following steps:
step 1: placing 0.1-3 g of carbon nano tube in 97-99.9 ml of deionized water, and performing ultrasonic dispersion for 0.5-6 h to obtain a uniformly dispersed carbon nano tube water dispersion liquid;
placing 0.1-1.5 g of cellulose in 98.5-99.9 ml of deionized water, and carrying out ultrasonic treatment for 0.5-3 h to obtain a cellulose aqueous solution;
step 2: placing the carbon nano tube water dispersion in a cellulose water solution, and carrying out ultrasonic treatment for 1-3 h to obtain a mixed solution; the volume of the carbon nano tube water dispersion liquid is 10-90 ml, and the volume of the cellulose water solution is 10-90 ml;
and step 3: placing the mixed solution in a mold, cooling to-60 ℃ at a speed of 3-10 ℃/min, pre-freezing for 3-10 h, drying for 20-40 h under a vacuum condition of 0.1Pa, and demolding to obtain the carbon nanotube/cellulose light wave-absorbing foam;
the proportion is measured by each part;
the carbon nano tube is a single-wall carbon nano tube, a double-wall carbon nano tube, a multi-wall carbon nano tube or an aminated multi-wall carbon nano tube;
the cellulose is nano cellulose fiber or carboxymethyl cellulose.
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| CN113527753B (en) * | 2020-04-15 | 2023-10-20 | 吴娜 | Bio-based foam material prepared at normal pressure and preparation method and application thereof |
| TW202144183A (en) * | 2020-05-11 | 2021-12-01 | 日商松下電器產業股份有限公司 | Laminated sheet for electromagnetic wave shielding |
| CN113698639A (en) * | 2021-08-30 | 2021-11-26 | 武汉纺织大学 | Carbon nano tube composite material electromagnetic shielding film and preparation method thereof |
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