CN103834064B - A kind of bacteria cellulose/ferrite composite wave-suction material and preparation method thereof - Google Patents
A kind of bacteria cellulose/ferrite composite wave-suction material and preparation method thereof Download PDFInfo
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- CN103834064B CN103834064B CN201410057366.2A CN201410057366A CN103834064B CN 103834064 B CN103834064 B CN 103834064B CN 201410057366 A CN201410057366 A CN 201410057366A CN 103834064 B CN103834064 B CN 103834064B
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Abstract
The invention discloses a kind of bacteria cellulose/ferrite composite wave-suction material and preparation method thereof.Relate to a kind of absorbing material technology of preparing.Comprise: take molysite and be dissolved in ethylene glycol, and one or more adding in zinc salt, nickel salt, magnesium salts, mantoquita and cobalt salt, ultrasonic disperse is carried out after being added by bacteria cellulose, add anhydrous sodium acetate and dispersion agent again, mechanical stirring, puts into reactor by mixture after powder dissolves completely, naturally cools to room temperature after having reacted, with dry after deionized water wash, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.Preparation process environmental protection of the present invention, simple, easy to operate, cost is low, and the absorbing material absorption of electromagnetic wave obtained is strong, absorption band is wide, has good mechanical properties and ultra-thin, ultralight advantage.
Description
Technical field
The present invention relates to absorbing material field, refer to the preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material especially.
Background technology
Along with the develop rapidly of electronic industry and widely using of more and more electronic product, electromangnetic spectrum, stealthy technique obtain further development in recent years, and people also receive more concern and attention to the research of absorbing material.And the detection of the various defense system in the world, tracking, attacking ability strengthen day by day, the viability, penetration ability etc. of sea, land and sky arms and services military target receive serious threat; Therefore as improving weapons system existence, prominent anti-, especially the stealthy technique of one of the effective means of striking capabilities, becomes most important, the most effective Tactical means just gradually.Absorbing material technology is then stealthy technique optimal selection, the electromagnetic wave energy projecting surface can absorb by it, can not the secondary electromagnetic radiation that causes because of reflection electromagnetic wave of product and interference, and electromagnetic wave energy can be made to be converted into heat energy or other forms of energy.And now science and technology development also cause the impact of electromagenetic wave radiation on environment, human body increasing.Therefore, the research and development of absorbing material are for military or civilianly all have very important meaning.Absorbing material mainly contains electromagnetic wave absorbing material, metal fine powder, conduction high polymer and nano wave-absorbing material etc.Wherein electromagnetic wave absorbing material---ferrite, absorbs the advantage such as strong, wide, the good frequency response characteristic of absorption band, cost are low and preparation technology is simple owing to having and receives and pay close attention to widely and approve.
At military aspect, the performance of modernized war to absorbing material proposes more and more higher requirement, and the absorbing material of general traditional sense has been difficult to meet thin, light, wide, strong composite request.In civilian, its snappiness, the focus that ultra-thin, pattern polytropy becomes the research of recent absorbing material.Therefore, develop a kind of there is good mechanical properties, ultra-thin, ultralight and to absorb strong, that absorption band is wide absorbing material be that tool grows a lot the absorbing material of new generation of potentiality.
Bacteria cellulose is a kind of natural biopolymer, has hyperfine reticulated structure, is combined into the thick fibrous bundle of 40 ~ 60 nanometers by the fento of diameter 3 ~ 4 nanometer, and is intertwined to form flourishing hyperfine network structure.This nano level superfine fiber, to the extremely strong winding binding ability of object and tension intensity, can more have the object of absorbing property by active adsorption, greatly improve the absorbing property of matrix material.The characteristic of the high purity of bacteria cellulose, high-crystallinity, high-polymerization degree and numberator height orientation, makes it have excellent mechanical property.And the Young's modulus of bacteria cellulose is more than the several times to ten times of general vegetable fibre, has high-tensile and durability, be therefore also more suitable for using in the form polytropy of absorbing material and some particular surroundingss.
This patent adopts solvent-thermal method to add the bacteria cellulose with ultra-fine fiber construction in the ferritic preparation process of electromagnetic wave absorbing material, prepares bacterial cellulose three-dimensional network internal and is evenly distributed with ferritic composite wave-suction material.Preparation process environmental protection of the present invention, simple, easy to operate, cost is low, and the composite wave-suction material absorption of electromagnetic wave obtained is strong, absorption band is wide, has good mechanical properties and ultra-thin, ultralight advantage.
Summary of the invention
The object of this invention is to provide a kind of bacteria cellulose/ferrite composite wave-suction material and preparation method thereof.Relate to a kind of absorbing material technology of preparing.Preparation process environmental protection of the present invention, simple, easy to operate, cost is low, the composite wave-suction material absorption of electromagnetic wave obtained is strong, absorption band is wide, has good mechanical properties and ultra-thin, ultralight advantage.
Of the present inventionly disclose a kind of bacteria cellulose/ferrite composite wave-suction material, be made up of bacteria cellulose and ferrite composite material, the mass ratio of bacteria cellulose and ferrite composite material is 0.1 ~ 1:1, and wherein ferrite composite material is made up of one or more in molysite and zinc salt, nickel salt, magnesium salts, mantoquita and cobalt salt.Its preparation method, comprising:
(1) taking molysite, to be dissolved in concentration be in the ethylene glycol of 90 ~ 99.9wt%, and add one or more in zinc salt, nickel salt, magnesium salts, mantoquita and cobalt salt, wherein Zn
2+, Ni
2+, Mg
2+, Cu
2+, Co
2+mole number or several mole number sum and Fe
3+the ratio of mole number be 1:2, added by bacteria cellulose and carry out ultrasonic disperse 30 ~ 120 minutes, the gross weight of molysite, zinc salt, nickel salt, magnesium salts, mantoquita and cobalt salt and the mass ratio of bacteria cellulose are 1:0.1 ~ 1;
(2) to add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 8 ~ 12:1, volume accounts for the dispersion agent of ethylene glycol volume 2 ~ 4%, dissolving 60 DEG C ~ 100 DEG C of heating, and 15 ~ 30min, treats that powder dissolves completely and obtain mixture;
(3) said mixture is put into reactor, at 140 ~ 180 DEG C of reaction 9 ~ 15h, after react, naturally cool to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacteria cellulose/ferrite composite wave-suction material.
As preferred technical scheme:
Wherein, the preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as above, described molysite, zinc salt, nickel salt, magnesium salts, mantoquita, cobalt salt are iron, zinc, nickel, magnesium, copper, the muriate of cobalt, nitrate, acetate, the vitriol of solubility.
The preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as above, described dispersion agent is one or more in polyoxyethylene glycol, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate.
The preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as above, described drying means is oven dry, seasoning or lyophilize.
The preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as above, described bacteria cellulose/ferrite composite wave-suction material refers to that the bacterial cellulose three-dimensional network internal that solvent-thermal method obtains is evenly distributed with ferrite molecule.
Compared with prior art, the invention has the beneficial effects as follows:
This patent adopts solvent-thermal method to add the bacteria cellulose with ultra-fine fiber construction preparing in the ferritic process of excellent magnetic absorbing material, effectively combine both advantages---strong wave absorbtion and excellent mechanical property, prepare and can absorb different frequency bands hertzian wave, and the composite wave-suction material of applied range, diversification of forms.Preparation process environmental protection of the present invention, simple, easy to operate, cost is low, and the composite wave-suction material absorption of electromagnetic wave obtained is strong, absorption band is wide, has good mechanical properties and ultra-thin, ultralight advantage.
Accompanying drawing explanation
Fig. 1 is the absorption usefulness of bacteria cellulose/ferrite composite wave-suction material prepared by different embodiment.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1:
Taking molysite, to be dissolved in concentration be in the ethylene glycol of 90wt%, and add zinc salt, wherein Zn
2+mole number be 1:2 with the ratio of the mole number of Fe3+, added by bacteria cellulose and carry out ultrasonic disperse 30 minutes, the gross weight of molysite, zinc salt and the mass ratio of bacteria cellulose are 1:1;
Add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 8:1, volume accounts for the dispersion agent of ethylene glycol volume 2%, dissolving 60 DEG C of heating, and 30min treats that powder dissolves completely and obtains mixture;
Said mixture is put into reactor, at 140 DEG C of reaction 15h, after react, naturally cools to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.
Embodiment 2:
Taking molysite, to be dissolved in concentration be in the ethylene glycol of 95wt%, and add magnesium salts, wherein Mg
2+mole number be 1:2 with the ratio of the mole number of Fe3+, added by bacteria cellulose and carry out ultrasonic disperse 60 minutes, the gross weight of molysite and magnesium salts and the mass ratio of bacteria cellulose are 1:0.8;
Add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 9:1, volume accounts for the dispersion agent of ethylene glycol volume 2%, dissolving 70 DEG C of heating, and 25min treats that powder dissolves completely and obtains mixture;
Said mixture is put into reactor, at 150 DEG C of reaction 13h, after react, naturally cools to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.
Embodiment 3:
Taking molysite, to be dissolved in concentration be in the ethylene glycol of 98wt%, and add nickel salt and mantoquita, wherein Ni
2+, Cu
2+mole number sum be 1:2 with the ratio of the mole number of Fe3+, added by bacteria cellulose and carry out ultrasonic disperse 90 minutes, the gross weight of molysite, nickel salt and mantoquita and the mass ratio of bacteria cellulose are 1:0.6;
Add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 10:1, volume accounts for the dispersion agent of ethylene glycol volume 3%, dissolving 80 DEG C of heating, and 20min treats that powder dissolves completely and obtains mixture;
Said mixture is put into reactor, at 160 DEG C of reaction 10h, after react, naturally cools to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.
Embodiment 4:
Taking molysite, to be dissolved in concentration be in the ethylene glycol of 99wt%, and add zinc salt and cobalt salt, wherein Zn
2+, Co
2+mole number sum and Fe
3+the ratio of mole number be 1:2, added by bacteria cellulose and carry out ultrasonic disperse 120 minutes, the gross weight of molysite, zinc salt and cobalt salt and the mass ratio of bacteria cellulose are 1:0.5;
Add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 11:1, volume accounts for the dispersion agent of ethylene glycol volume 3%, dissolving 90 DEG C of heating, and 15min treats that powder dissolves completely and obtains mixture;
Said mixture is put into reactor, at 170 DEG C of reaction 10h, after react, naturally cools to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.
Embodiment 5:
Taking molysite, to be dissolved in concentration be in the ethylene glycol of 99.5wt%, and add nickel salt, magnesium salts, mantoquita and cobalt salt, wherein Ni
2+, Mg
2+, Cu
2+, Co
2+mole number sum be 1:2 with the ratio of the mole number of Fe3+, added by bacteria cellulose and carry out ultrasonic disperse 120 minutes, the gross weight of molysite, nickel salt, magnesium salts, mantoquita and cobalt salt and the mass ratio of bacteria cellulose are 1:0.1;
Add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 12:1, volume accounts for the dispersion agent of ethylene glycol volume 4%, dissolving 100 DEG C of heating, and 15min treats that powder dissolves completely and obtains mixture;
Said mixture is put into reactor, at 180 DEG C of reaction 9h, after react, naturally cools to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.
Experimental example 1: the test of bacteria cellulose/ferrite composite wave-suction material electromagnet shield effect
Employing vector network analyzer is tested, and range of frequency is 600MHz ~ 18GHz, and test thickness is 3mm.Test result is shown in Fig. 1.
Can find out according to result (accompanying drawing 1), the electromagnet shield effect of the matrix material of different embodiment all increases with the increase of frequency.And the electromagnet shield effect of the 18Hz of bacteria cellulose/ferrite composite wave-suction material prepared by 3 embodiments all can reach more than 29dB, especially when the absorbing material adopting embodiment 5 to prepare, effect is best, far away higher than similar matrix material disclosed in prior art.
We are found by the sample reflection loss of research performation example 5 and the relation of frequency, and most high-selenium corn peak is along with the reduction of thickness of sample is to high-frequency mobile.When the thickness of sample is 6mm, reflectance peak is about-14dB; When the thickness of sample is 4mm, reflectance peak is about-19dB; And when the thickness of sample is 2mm, the peak value of reflectivity can reach-25dB.This is better than composite wave-suction material disclosed in prior art far away, has good mechanical properties and ultra-thin, ultralight advantage, has huge market application foreground.
Claims (5)
1. a preparation method for bacteria cellulose/ferrite composite wave-suction material, is characterized in that:
(1) taking molysite, to be dissolved in concentration be in the ethylene glycol of 90 ~ 99.9wt%, and add one or more in zinc salt, nickel salt, magnesium salts, mantoquita and cobalt salt, wherein Zn
2+, Ni
2+, Mg
2+, Cu
2+, Co
2+mole number or several mole number sum and Fe
3+the ratio of mole number be 1:2, added by bacteria cellulose and carry out ultrasonic disperse 30 ~ 120 minutes, a kind of weight in molysite, zinc salt, nickel salt, magnesium salts, mantoquita and cobalt salt or the mass ratio of several gross weights and bacteria cellulose are 1:0.1 ~ 1;
(2) to add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 8 ~ 12:1, volume accounts for the dispersion agent of ethylene glycol volume 2 ~ 4%, be heated to 60 DEG C ~ 100 DEG C, keep 15 ~ 30min, treat that powder dissolves completely and obtain mixture, described dispersion agent is one or more in polyoxyethylene glycol, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate;
(3) said mixture is put into reactor, at 140 ~ 180 DEG C of reaction 9 ~ 15h, after react, naturally cool to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacteria cellulose/ferrite composite wave-suction material.
2. the preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as claimed in claim 1, is characterized in that: described molysite, zinc salt, nickel salt, magnesium salts, mantoquita, cobalt salt are iron, zinc, nickel, magnesium, copper, the muriate of cobalt, nitrate, acetate, the vitriol of solubility.
3. the preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as claimed in claim 1, is characterized in that: described drying means is oven dry, seasoning or lyophilize.
4. a preparation method for bacteria cellulose/ferrite composite wave-suction material, is characterized in that:
(1) taking molysite, to be dissolved in concentration be in the ethylene glycol of 99.5wt%, and add nickel salt, magnesium salts, mantoquita and cobalt salt, wherein Ni
2+, Mg
2+, Cu
2+, Co
2+mole number sum and Fe
3+the ratio of mole number be 1:2, added by bacteria cellulose and carry out ultrasonic disperse 120 minutes, the gross weight of molysite, nickel salt, magnesium salts, mantoquita and cobalt salt and the mass ratio of bacteria cellulose are 1:0.1;
(2) to add respectively again and Fe
3+the ratio of mole number be the anhydrous sodium acetate of 12:1, volume accounts for one or more in the polyoxyethylene glycol of ethylene glycol volume 4%, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, is heated to 100 DEG C, keeps 15min to treat that powder dissolves completely and obtain mixture;
(3) said mixture is put into reactor, at 180 DEG C of reaction 9h, after react, naturally cool to room temperature, with drying after deionized water wash 2 ~ 5 times, obtain bacterial cellulose three-dimensional network internal and be evenly distributed with ferritic composite wave-suction material.
5. the preparation method of a kind of bacteria cellulose/ferrite composite wave-suction material as described in any one of claim 1-3, it is characterized in that: described bacteria cellulose/ferrite composite wave-suction material refers to what solvent-thermal method obtained, bacterial cellulose three-dimensional network internal is evenly distributed with ferrite molecule.
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| CN104532407B (en) * | 2014-12-24 | 2016-07-20 | 暨南大学 | A kind of carbon nano-fiber based on carbonization Bacterial cellulose and compositions thereof and application |
| CN104774346B (en) * | 2015-04-30 | 2017-10-20 | 武汉艾特米克超能新材料科技有限公司 | A kind of light porous suction ripple film and preparation method thereof |
| CN109207122A (en) * | 2018-06-28 | 2019-01-15 | 滁州市经纬装备科技有限公司 | A kind of preparation method for the flexible material absorbing radar signal |
| CN109082119B (en) * | 2018-07-02 | 2021-04-02 | 东营欣邦电子科技有限公司 | Cellulose modified polyimide corona-resistant film and preparation method thereof |
| CN111944204B (en) * | 2020-07-24 | 2022-03-08 | 南京理工大学 | Fe3O4Magnetic bacterial cellulose and preparation method thereof |
| CN112225950B (en) * | 2020-10-28 | 2022-04-22 | 北京航空航天大学 | Preparation method of environment-friendly Fe @ C composite wave-absorbing material |
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