CN103319749A - Composite wave-absorbing material and preparation method thereof - Google Patents
Composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite wave-absorbing material, comprising main materials and auxiliary agents, wherein the main materials include a nanometer ferriferrous oxide particle and nanometer cellulose, the auxiliary agents include oleic acid and potassium persulphate, the mass percentage of the main materials in the wave-absorbing material is 60 to 85%, and the mass percentage of the auxiliary agents in the wave-absorbing material is 4 to 15%. A preparation method for the composite wave-absorbing material comprises the following steps: (1) preparing a nanometer cellulose solution; (2) adding potassium persulphate for a reaction; (3) adding oleic acid-coated nanometer ferriferrous oxide into a uniformly mixed solution obtained in the previous step; (4) allowing a mixed liquor obtained in the previous step to undergo a reaction at a temperature of 60 DEG C for 6 h, cooling to room temperature after completion of the reaction and transferring the reacted mixed liquor to a centrifuge tube for centrifugation; (5) adding purified water into a supernatant obtained in the previous step and carrying out centrifugation again; and (6) adding purified water into a precipitate obtained in the previous step, carrying out full mixing with stirring, carrying out centrifugation again and drying and grinding a precipitate obtained after centrifugation. Compared with a conventional wave-absorbing material, the wave-absorbing material provided by the invention has the advantages of low density, a wide absorption frequency band and enhanced wave-absorbing performance.
Description
Technical field
The invention belongs to chemical material class technical field, specifically a kind of composite wave-suction material and preparation method thereof.
Background technology
Absorbing material is comprised of absorption agent and body material two portions, and be that a class can absorb, the hertzian wave of the incident that decays, and electromagnetic energy be converted to the energy of other form, such as mechanical energy, electric energy and heat energy, thereby with the used up class functional materials of electromagnetic energy.The absorbing material of excellent property should possess two requirements simultaneously: the one, and can make the hertzian wave of incident enter to greatest extent material internal, have the wave resistance matching properties, even incident electromagnetic wave is minimum at the reflection coefficient on material medium surface; The 2nd, with the electromagnetic wave attenuation that enters.
Traditional ferrite wave-absorbing material performance is best, and it has the characteristics such as the frequency range of absorption is high, specific absorption is high, matching thickness is thin, but its weak point is that relative density is large and absorption band is narrow.The inorganic-inorganic composite manufacture can effectively improve Fe
3O
4The narrow defective of absorption band, generally adopt barium titanate or special alloy etc., but still can not change the large defective of its relative density, be unsuitable for practical application.And organic interpolation can effectively make novel material make the design of material more reasonable satisfying under the condition of impedance matching by regulating electromagnetic parameter, and performance is more optimized.Composite organic-inorganic material adopts the method for chemical plating more at present, exists power consumption large, the shortcomings such as complicated operation.But composite organic-inorganic material is the development trend of absorbing material, is to wideband, Composite, and advance in low-dimensional and intelligent aspect.Low-dimensional materials (such as fiber) rely on wide, compatible good, the many-sided advantages such as specific absorption is high, light specific gravity of its absorption band, are important supplement of Wave suction composite material.But at present for the research of fiber-like absorbing material still in the starting stage, industry also needs the absorbing material that density is less, absorbing property is stronger.
Summary of the invention
For solving the defective of existing absorbing material, the present invention has developed composite wave-suction material of a kind of new composition and preparation method thereof, realizes that the absorbing property of absorbing material strengthens the purpose that the existing absorbing material of density ratio is little.
For achieving the above object, the technical solution used in the present invention is, the composite wave-suction material of the new composition that the present invention develops, comprise major ingredient and auxiliary agent, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 60～85%, the mass percent of auxiliary agent in absorbing material is 4～15%.Natural cellulose is that a kind of wide material sources, aboundresources, cost are low, the renewable polymeric materials that density is light, and matrix material prepared therefrom can effectively improve Fe
3O
4The nanoparticle absorption band is narrow, and the defective that density is large satisfies the technical parameter of absorbing material needed " thin, light, wide, strong ", and for new approach has been opened up in the development of absorbing material, simultaneously, also the reproducible utilization for waste fiber provides new thinking.
The mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 10～30%, and nano-cellulose is 50～75%.
The mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 1～5%, Potassium Persulphate is 3～10%.Select the quality proportioning of suitable major ingredient, auxiliary agent, can access the material that production cost is low, have each regulation parameter of absorbing material.
In addition, the method for preparing this composite wave-suction material is also disclosed, comprise the steps, (1) takes by weighing nano-cellulose, its mass percent in absorbing material is 50～75%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 3～10%; The effect of Potassium Persulphate is to make cellulose surface produce a large amount of free radicals in order to be combined with the nano ferriferrous oxide particle.
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 10～30%, the mass percent of oleic acid in absorbing material is 1～5%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 60～85%; What adopt is the liquid phase compounding technology, less demanding, simple and easy to operate to instrument, the advantage that less energy-consumption is arranged, and this absorbing material makes take the new constituent nano-cellulose as raw material, nano-cellulose belongs to the polyose macromolecular compound, and the liquid phase compounding technology is comparatively suitable in numerous preparation absorbing material methods.
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.Add the centrifugal thoroughly wash-out of ionic liquid quilt residual in the mixture that repeatedly guarantees of purified water.
When preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that nano-cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.Select suitable temperature, can make Mierocrystalline cellulose ion liquid dissolving not only soon but also abundant.
When adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.Under this temperature, the purpose of reaction 0.5h be make cellulose surface produce a large amount of free radicals in case with the nano ferriferrous oxide ionic bond.
Centrifugal speed in described step (4), (5), (6) is 1600 r/min.Centrifugal under this centrifugal speed, supernatant liquor is better separated with throw out.
Drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.Two kinds of methods all can obtain absorbing material, all can make the performance of absorbing material reach best.
When in the described step (6) throw out being ground, grind and stopped when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m.Use the Mierocrystalline cellulose of new composition as major ingredient, even it is to belong to macromolecular compound, also it can be worn into the powder of 300 sieve fineness, be convenient to utilize.
To sum up, beneficial effect of the present invention is with present composite organic-inorganic material (Fe
3O
4/ polypyrrole, PVC/Fe
3O
4) compare, it is raw material that the present invention adopts natural waste wood fiber and ferriferrous oxide nano-particle, prepares novel Fe
3O
4The nano combined absorbing material of/Mierocrystalline cellulose.Wherein, natural cellulose is that a kind of wide material sources, aboundresources, cost are low, the renewable polymeric materials that density is light, and matrix material prepared therefrom can effectively improve Fe
3O
4The nanoparticle absorption band is narrow, and the defective that density is large satisfies the technical parameter of absorbing material needed " thin, light; wide, strong ", for new approach has been opened up in the development of absorbing material, simultaneously, also the reproducible utilization for waste fiber provides new thinking, and with Fe
3O
4Nanoparticle embedding Fufen under electrostatic attraction and van der Waals interaction is dispersed in the cellulosic matrix, and the density of mixture is reduced to 1.26 g/cm
3The matching thickness of sample is 2mm, to compare absorption band wide with inorganic wave-absorbing material, can reach 6～18GHz, and wave-sucking performance is the strongest at the 17GHz place, and reflectivity is-13dB that general reflectivity is less, the performance that absorbing material is described is better, employing liquid phase compounding technology is simple to operate, less demanding to plant and instrument, power consumption is low, and this composite wave-suction material utilizes dielectric loss and magnetic loss to interact and produces wave-absorbing effect, is suitable for electromagnetic shielding material.On the other hand, the decrease of the improvement of technology and material relative density has determined that this matrix material is suitable for being applied to practical application and production.
Embodiment
Below in conjunction with specific embodiment the present invention is made further instruction.
Embodiment one: below nanometer four iron oxide particles, the nano-cellulose used all be the finished product of buying according to directly, nano ferriferrous oxide is available from receive nanotechnology development corporation, Ltd. in Jiang Suhai; Nano-cellulose is available from trade limited liability company of Chinese National Travel Agency.
This experiment of ionic liquid of below using adopts homemade ionic liquid 1-butyl-3-Methylimidazole villaumite ([Bmim] Cl) also to utilize known technology to prepare, it utilizes following methods to make, get respectively 500mLN-Methylimidazole (available from becoming medical chemistry company limited in Wuhan benefit China) and 800mL n-propylcarbinyl chloride (available from rising chemical industry company limited in the Yancheng City dragon), both are added in the 2000mL flask mix, with mixing solutions reflux in 110 ℃ oil bath pan, impose simultaneously induction stirring, continuity along with the reaction times, the color of the solution is deepened, viscosity increases gradually, behind the backflow 24h, withdrawing fluid fades away, thereby judges that reaction finishes.Then steam with Rotary Evaporators n-propylcarbinyl chloride excessive in the reaction solution is removed, be cooled to room temperature, namely obtain ([Bmim] Cl) ionic liquid.
The composite wave-suction material of a kind of new composition that the present invention leaves, comprise major ingredient and auxiliary agent, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 60%, the mass percent of auxiliary agent in absorbing material is 10%.
The mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 10%, and nano-cellulose is 50%.
The mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 1%, Potassium Persulphate is 3%.
The method for preparing absorbing material of the present invention, comprise the steps, (1) take by weighing nano-cellulose, its mass percent in absorbing material is 50%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 5%;
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 10%, the mass percent of oleic acid in absorbing material is 5%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 60%;
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.
When preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that Mierocrystalline cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.
When adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.
Centrifugal speed in described step (4), (5), (6) is 1600 r/min.
Drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.
When in the described step (6) throw out being ground, grind and stopped when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m
It is 1.27kg/m that Wave suction composite material of the present invention is detected its density
3, absorption band reaches 6～18GHz, and this material is the strongest at the wave-sucking performance of 17GHz, and reflectivity is-13dB.
Embodiment two: the composite wave-suction material of a kind of new composition that the present invention leaves, comprise major ingredient and auxiliary agent, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 85%, the mass percent of auxiliary agent in absorbing material is 4%.
The mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 30%, and nano-cellulose is 55%.
The mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 1%, Potassium Persulphate is 3%.
The method for preparing absorbing material of the present invention, comprise the steps, (1) take by weighing nano-cellulose, its mass percent in absorbing material is 55%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 3%;
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 30%, the mass percent of oleic acid in absorbing material is 1%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 85%;
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.
When preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that Mierocrystalline cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.
When adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.
Centrifugal speed in described step (4), (5), (6) is 1600 r/min.
Drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.
When in the described step (6) throw out being ground, grind and stopped when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m.
It is 1.29kg/m that Wave suction composite material of the present invention is detected its density
3, absorption band reaches 6～18GHz, and is the strongest at the 17GHz wave-sucking performance, and reflectivity is-13dB.
Embodiment three: the composite wave-suction material of a kind of new composition that the present invention leaves, comprise major ingredient and auxiliary agent, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 85%, the mass percent of auxiliary agent in absorbing material is 11%.
The mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 10%, and nano-cellulose is 75%.
The mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 1%, Potassium Persulphate is 10%.
The method for preparing absorbing material of the present invention, comprise the steps, (1) take by weighing nano-cellulose, its mass percent in absorbing material is 75%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 10%;
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 10%, the mass percent of oleic acid in absorbing material is 1%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 85%;
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.
When preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that Mierocrystalline cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.
When adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.
Centrifugal speed in described step (4), (5), (6) is 1600 r/min.
Drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.
When in the described step (6) throw out being ground, grind and stopped when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m.
It is 1.31kg/m that Wave suction composite material of the present invention is detected its density
3, absorption band reaches 6～18GHz, reaches the strongest at the 17GHz wave-sucking performance, and reflectivity is-12dB.
Embodiment four: the composite wave-suction material of a kind of new composition that the present invention leaves, comprise major ingredient and auxiliary agent, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 70%, the mass percent of auxiliary agent in absorbing material is 15%.
The mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 20%, and nano-cellulose is 50%.
The mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 5%, Potassium Persulphate is 10%.
The method for preparing absorbing material of the present invention, comprise the steps, (1) take by weighing nano-cellulose, its mass percent in absorbing material is 50%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 10%;
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 20%, the mass percent of oleic acid in absorbing material is 5%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 70%;
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.
When preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that Mierocrystalline cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.
When adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.
Centrifugal speed in described step (4), (5), (6) is 1600 r/min.
Drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.
When in the described step (6) throw out being ground, grind and stopped when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m.
It is 1.32kg/m that Wave suction composite material of the present invention is detected its density
3, absorption band reaches 6～18GHz, reaches wave-sucking performance at 17GHz the strongest, and reflectivity is-13dB.
Embodiment five: the composite wave-suction material of a kind of new composition that the present invention leaves, comprise major ingredient and auxiliary agent, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 70%, the mass percent of auxiliary agent in absorbing material is 9%.
The mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 20%, and nano-cellulose is 50%.
The mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 3%, Potassium Persulphate is 6%.
The method for preparing absorbing material of the present invention, comprise the steps, (1) take by weighing nano-cellulose, its mass percent in absorbing material is 50%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 6%;
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 20%, the mass percent of oleic acid in absorbing material is 3%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 70%;
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.
When preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that Mierocrystalline cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.
When adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.
Centrifugal speed in described step (4), (5), (6) is 1600 r/min.
Drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.
When in the described step (6) throw out being ground, grind and stopped when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m.
It is 1.32kg/m that Wave suction composite material of the present invention is detected its density
3, absorption band reaches 6～18GHz, reaches wave-sucking performance at 17GHz the strongest, reflectivity-11dB.
Below be the comparative figure of each parameter of Wave suction composite material of the present invention and existing absorbing material, to further specify beneficial effect of the present invention.
| The absorbing material composition | Mean density (kg/m 3） | Absorption band (GHz) | Reflecting effect |
| Organic and inorganic composite wave-suction material: alpha-feooh/polyaniline nano-composite material | 4.76 | 2～18 | This absorbing material is the strongest at the 12GHz wave-sucking performance, and reflectivity is-10dB |
| Inorganic wave-absorbing material: Z 250 | 5.5 | 8～18 | This absorbing material is the strongest at the 15GHz wave-sucking performance, and reflectivity is-25dB |
| Absorbing material of the present invention | 1.26 | 6～18 | This absorbing material is the strongest in 17GH left and right sides receptivity, reflectivity-13dB |
Obtain conclusion according to above-mentioned test-results, when the absorbing property of generally weighing absorbing material is strong, poor, utilize reflectivity to weigh, the absolute value of reflectivity is less, reflectivity is higher, absorbing property is poorer, by above-mentioned test-results as can be known, the density ratio of absorbing material of the present invention is existing all little, therefore can be used in the various structures, and purposes is wide, absorption band than inorganic-organic composite material is wide, wave-sucking performance than inorganic wave-absorbing material is strong, and is comprehensive, is preferably absorbing material of absorbing property index.
The present invention prepares Powdered Fe by the liquid phase recombining process
3O
4The nano combined absorbing material of/Mierocrystalline cellulose, Fe in this matrix material
3O
4The even embedding Fufen of nanoparticle is dispersed in the cellulosic substrates, has stronger microwave absorbing effect, is all dielectric loss and magnetic loss and interacts.The density of matrix material is 1.26kg/m
3, far below traditional inorganic wave-absorbing material and organic and inorganic composite wave-suction material, absorption band is 6～18GHz, reaches reflection potential at 17GHz the strongest, can reach-13dB, is higher than the composite organic-inorganic material of present report, has good absorbing property.
The above is not the restriction to content of the present invention, all any modifications of doing on flesh and blood of the present invention, is equal to and replaces and simple modifications etc., all should be included within protection scope of the present invention.
Claims (9)
1. composite wave-suction material, comprise major ingredient and auxiliary agent, it is characterized in that, major ingredient comprises nano ferriferrous oxide particle, nano-cellulose, auxiliary agent comprises oleic acid, Potassium Persulphate, and the mass percent of major ingredient in absorbing material is 60～85%, the mass percent of auxiliary agent in absorbing material is 4～15%.
2. composite wave-suction material according to claim 1 is characterized in that, the mass percent of each composition in absorbing material is respectively in the described major ingredient, and the nano ferriferrous oxide particle is 10～30%, and nano-cellulose is 50～75%.
3. composite wave-suction material according to claim 1 is characterized in that, the mass percent of each composition in absorbing material is respectively in the described auxiliary agent, and oleic acid is 1～5%, Potassium Persulphate is 3～10%.
4. method for preparing the described composite wave-suction material of claim 1, it is characterized in that, the method comprises the steps, (1) takes by weighing nano-cellulose, its mass percent in absorbing material is 50～75%, nano-cellulose is dissolved in 1-butyl-3-Methylimidazole villaumite ionic liquid to form mass concentration be 1～3% cellulose solution;
(2) upwards add Potassium Persulphate in the nano-cellulose homogeneous phase solution in step, the mass percent of Potassium Persulphate in composite wave-suction material is 3～10%;
(3) add the nano ferriferrous oxide particle with Coated with Oleic Acid in the solution that upwards step mixes, the mass percent of nano ferriferrous oxide particle in absorbing material is 10～30%, the mass percent of oleic acid in absorbing material is 1～5%, and nano ferriferrous oxide particle and nano-cellulose altogether the mass percent in absorbing material be 60～85%;
(4) upper step mixed solution reacts 6h under 60 ℃ of conditions, reaction is cooled to room temperature after finishing, and then reacted mixed solution is transferred in the centrifuge tube, and centrifuge tube is inserted centrifugal 10min in the refrigeration whizzer, centrifuging temperature is-20 ℃～-40 ℃, collects supernatant liquor;
(5) upwards add purified water in the supernatant liquor in step, stir supernatant liquor can be dissolved in the purified water fully, centrifugal 10min then, abandoning supernatant collecting precipitation thing;
(6) upwards go on foot the throw out adding purified water that obtains and also stir fully mixing, centrifugal 10min repeats this step at least 5 times again, and the drying precipitate after centrifugal, grinding had both been got the composite wave-suction material finished product.
5. the method for preparing composite wave-suction material according to claim 4, it is characterized in that, when preparing cellulose solution in the described step (1), adopt magnetic stirring apparatus that Mierocrystalline cellulose and 1-butyl-3-Methylimidazole villaumite ionic liquid are stirred, the temperature of stirring is 60 ℃.
6. the method for preparing composite wave-suction material according to claim 4 is characterized in that, when adding Potassium Persulphate in the nanofiber cellulose solution in the described step (2), temperature maintains 60 ℃ always, and the time of Potassium Persulphate and fibrin reaction is 0.5h.
7. the method for preparing composite wave-suction material according to claim 4 is characterized in that, the centrifugal speed in described step (4), (5), (6) is 1600 r/min.
8. the method for preparing composite wave-suction material according to claim 4 is characterized in that, the drying step in the described step (6) be with throw out in vacuum drying oven 60 ℃ of dry 12h or in freeze drier-45 ℃ of dry 12h.
9. the method for preparing composite wave-suction material according to claim 4 is characterized in that, when in the described step (6) throw out being ground, grinds and stops when fineness reaches the 300 mesh sieve period of the day from 11 p.m. to 1 a.m.
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