CN108912402A - A kind of sepiolite composite absorber and the preparation method and application thereof - Google Patents
A kind of sepiolite composite absorber and the preparation method and application thereof Download PDFInfo
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- CN108912402A CN108912402A CN201810523495.4A CN201810523495A CN108912402A CN 108912402 A CN108912402 A CN 108912402A CN 201810523495 A CN201810523495 A CN 201810523495A CN 108912402 A CN108912402 A CN 108912402A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
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Abstract
The invention discloses a kind of sepiolite composite absorbers, by sepiolite and magnetic Fe3O4Composition, the magnetic Fe3O4It is supported in the network structure and nano pore of sepiolite, magnetic Fe3O4Mass ratio with sepiolite is 1：(3~6).Sepiolite composite absorber of the present invention has unique fibrous structure and high-specific surface area, possesses significant electrical polarization characteristics and high natural resonance magnetic loss, have the advantages that absorption band is wide, density is low and weather resistance is good；The preparation method of sepiolite composite absorber of the present invention, process conditions are mild, and easy to operate, production cost is low, are conducive to industrialized production；The present invention has wideband, lightweight, the strong characteristic for inhaling wave using the sepiolite composite wave-suction material that sepiolite composite absorber is prepared, and the surface density of composite wave-suction material is in 1.0kg/m2Within, absorption band is wide, and reflectance test is the result shows that be greater than 7.3GHz better than -10dB bandwidth.
Description
Technical field
The invention belongs to functional material preparation technical fields, and in particular to a kind of sepiolite composite absorber and its preparation side
Method and application.
Background technique
The development of military radar stealth technology and civilian anti-electromagnetic-radiation perturbation technique, which proposes absorbing material, to be compeled to be essential
It asks.Incoming electromagnetic wave energy can be converted into the energy of thermal energy or other forms and make electromagnetic wave loss decaying by absorbing material, be inhaled
Wave material reaches the radar detection characteristic signal that military target is effectively reduced by filling powder absorbent, meanwhile, electricity can be improved
Sub- device product Electromagnetic Compatibility and improvement periphery electromagnetic environment, have very important technology and economical and practical value.Closely
Nian Lai, the absorber material studied both at home and abroad mainly include magnetic metal and its alloy, conductive carbon material, conduction high polymer, iron
Oxysome etc..Currently, have been achieved for rapid progress to the research of wave absorbing agent, but that generally there are still absorption bands is narrow, density is big
And weather resistance it is poor the disadvantages of.
Summary of the invention
The sepiolite composite absorber and its preparation side that the purpose of the present invention is to provide a kind of absorption bands is wide, density is small
Method and application.
This sepiolite composite absorber provided by the invention, by sepiolite and magnetic Fe3O4Composition, the magnetic Fe3O4
It is supported in the network structure and nano pore of sepiolite, magnetic Fe3O4Mass ratio with sepiolite is 1：(3~6).
The present invention provides the preparation method of the sepiolite composite absorber, includes the following steps：
(1) it is prepared by predetermined ratio and contains Fe2+And Fe3+Mixing salt solution；
(2) it disperses sepiolite in mixing salt solution obtained by step (1), is stirred under an inert atmosphere, before obtaining
Drive liquid solution；
(3) lye is added into precursor solution obtained by step (2), adjusts PH to 9~12,40~80 DEG C at a temperature of
Crystallizing treatment is carried out, magnetic Fe is made3O4It is supported in the network structure and nano pore of sepiolite, will be precipitated obtained by Crystallizing treatment
It is washed, it is dry, obtain the sepiolite composite absorber.
Preferably, in the step (1), Fe in mixing salt solution2+、Fe3+Concentration is 0.05~0.2mol/L, and Fe2+、
Fe3+Molar concentration rate is 1：(1~2).
Preferably, in the step (1), Fe2+、Fe3+Salting liquid be one or both of nitrate, sulfate.
Preferably, in the step (2), the sepiolite is handled by purification & isolation, through broken, levigate to 200 mesh excessively
Sieve, grade >=80% of sepiolite.
Preferably, in the step (2), the inert atmosphere is one or both of high pure nitrogen, high-purity argon gas, is led to
The angle of incidence terminates from starting to be dissolved to reaction, and mixing time is 0.5~2h.
Preferably, in the step (3), lye be NaOH solution or ammonium hydroxide, the NaOH solution concentration be 0.05~
0.1mol/L, ammonium hydroxide mass percent concentration are 20~40%.
Preferably, in the step (3), the Crystallizing treatment time is 1~3h.
The present invention also provides the applications of the sepiolite composite absorber, and sepiolite composite absorber is used to prepare Hai Pao
Stone composite wave-suction material, the sepiolite composite wave-suction material include by weight percentage：Sepiolite composite absorber 50~
70%, epoxy resin 24~40%, epoxy hardener 6~10%.
Preferably, the preparation process of the sepiolite composite wave-suction material is：Under mechanical agitation, sepiolite is answered
Absorbent is closed than uniformly to mix with epoxy resin by design weight；The epoxy hardener of predetermined ratio is added, continues stirring curing
10~40min adds nonessential organic solvent and adjusts viscosity and nonessential auxiliary agent adjusting dispersibility and levelability, mixture is applied
It overlays on aluminium sheet, after baking is cooling to obtain the final product.
Preferably, the mechanical stirring disperses integration apparatus using vertical mixing, and revolving speed is 1000~1500r/min.
Preferably, the epoxy resin is bisphenol A epoxide resin, cycloaliphatic epoxy resin, one in bisphenol F epoxy resin
Kind is a variety of；The epoxy hardener is poly- phthalein amine curing agent, in low molecule amine curing agent, cashew nut oil modified curing agent
It is one or more.
Preferably, the nonessential organic solvent is one of benzene class, alcohols, ketone or a variety of；It is described nonessential to help
Agent is one of coalescing agent, levelling agent, defoaming agent, dispersing agent, promotor or a variety of.
Preferably, the surface of the aluminium sheet reaches Sa2.5 grades through sandblasting or mechanical grinding processing.
Preferably, the baking temperature is 40~50 DEG C, and baking time is 1~2h, and cooling time is 0.5~1h.
Sepiolite is a kind of aqueous rich magnesium silicate clay mineral with layer chain structure, has unique network of fibers
Structure and nano pore structure, theoretical specific surface area are up to greatly 900m2/ g, density are only 2~2.5g/cm3, meanwhile, sepiolite sheet
Body has the excellent environment weatherabilities such as high-low temperature resistant, salt spray resistance, UV resistant, oil resistivity, assigns sepiolite and is preparing electromagnetism
Huge advantage in terms of wave absorbent.
Compared with prior art, advantageous effects of the invention：
(1) sepiolite composite absorber of the present invention, weatherability good sepiolite low using density will be received as raw material
Rice magnetic Fe3O4Be supported in the unique fibrous-network structure of sepiolite and nano pore, have unique fibrous structure and
High-specific surface area possesses significant electrical polarization characteristics and high natural resonance magnetic loss, and sepiolite composite absorber, which has, to be absorbed
The advantage that bandwidth, density are low and weather resistance is good.
(2) preparation method of sepiolite composite absorber of the present invention, process conditions are mild, easy to operate, are produced into
This is low, is conducive to industrialized production.
(3) application of sepiolite composite absorber of the present invention, the sepiolite composite wave-suction material being prepared have
Wideband, lightweight, the strong characteristic for inhaling wave, the surface density of composite absorber is in 1.0kg/m2Within, absorption band is wide, and reflectivity is surveyed
Test result shows to be greater than 7.3GHz better than -10dB (90% absorbs) bandwidth.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained sepiolite composite absorber of the embodiment of the present invention.
Fig. 2 is 4~6 gained sepiolite composite wave-suction material of embodiment and 1~2 absorbing material of comparative example in 8~18GHz frequency
The absorbing property figure of section.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, rather than whole embodiments, based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses, present invention will be further explained below with reference to the attached drawings and specific examples.
Embodiment 1
The present invention provides a kind of preparation method of sepiolite composite absorber, includes the following steps：
(1) 7.0g FeSO is weighed respectively4·7H2O and 20.2g Fe (NO3)·9H2O, and be dissolved in and gone equipped with 1000mL
Mixing salt solution is made in the four-hole boiling flask of ionized water；
(2) it disperses 29.0g sepiolite in mixing salt solution, in a nitrogen atmosphere stirring at normal temperature 30min, obtains forerunner
Liquid solution；
(3) it is slowly added to the NaOH solution that concentration is 0.05mol/L into precursor solution, PH to 10 is adjusted, at 80 DEG C
Thermostat water bath in Crystallizing treatment 1h, stand 30min after remove suspension, make magnetic Fe3O4It is supported on the network knot of sepiolite
In structure and nano pore, precipitating deionized water obtained by Crystallizing treatment and dehydrated alcohol are washed and filtered afterwards three times, filter residue is 60
It is dry under DEG C vacuum, the sepiolite composite absorber is obtained, scanning electron microscope (SEM) photograph is as shown in Figure 1, nano-magnetic Fe3O4Load
In the fibrous-network structure and nano pore of sepiolite.
Embodiment 2
The present invention provides a kind of preparation method of sepiolite composite absorber, includes the following steps：
(1) 14.0g FeSO is weighed respectively4·7H2O and 30.3g Fe (NO3)·9H2O, and be dissolved in and gone equipped with 1000mL
Mixing salt solution is made in the four-hole boiling flask of ionized water；
(2) it disperses 46.4g sepiolite in mixing salt solution, in a nitrogen atmosphere stirring at normal temperature 30min, obtains forerunner
Liquid solution；
(3) it is slowly added to the NaOH solution that concentration is 0.075mol/L into precursor solution, PH to 11 is adjusted, at 80 DEG C
Thermostat water bath in Crystallizing treatment 2h, stand 30min after remove suspension, make magnetic Fe3O4It is supported on the network knot of sepiolite
In structure and nano pore, precipitating deionized water obtained by Crystallizing treatment and dehydrated alcohol are washed and filtered afterwards three times, filter residue is 60
It is dry under DEG C vacuum, obtain the sepiolite composite absorber.
Embodiment 3
The present invention provides a kind of preparation method of sepiolite composite absorber, includes the following steps：
(1) 7.0g FeSO is weighed respectively4·7H2O and 20.2g Fe (NO3)·9H2O, and be dissolved in and gone equipped with 1000mL
Mixing salt solution is made in the four-hole boiling flask of ionized water；
(2) it disperses 17.4g sepiolite in mixing salt solution, in a nitrogen atmosphere stirring at normal temperature 30min, obtains forerunner
Liquid solution；
(3) it is slowly added to the ammonium hydroxide that concentration is 40wt% into precursor solution, PH to 12 is adjusted, in 60 DEG C of thermostatted water
Crystallizing treatment 3h in bath removes suspension after standing 30min, makes magnetic Fe3O4It is supported on the network structure and nanometer of sepiolite
In duct, precipitating deionized water obtained by Crystallizing treatment and dehydrated alcohol are washed and filtered afterwards three times, filter residue is under 60 DEG C of vacuum
It is dry, obtain the sepiolite composite absorber.
Embodiment 4
1 gained sepiolite composite absorber of embodiment is used to prepare sepiolite composite wave-suction material, preparation process is：It adopts
Disperse integration apparatus with vertical mixing, by 50g sepiolite composite absorber, 40g bisphenol A epoxide resin in 1000r/min item
1h is dispersed with stirring under part；Be added 10g low molecule amine curing agent, continue stirring curing 20min, addition 7g xylene solvent and
0.2g coalescing agent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using spraying process, it is cooling after 50 DEG C of baking 1h
0.5h to get.The performance parameter of sepiolite composite wave-suction material obtained by the present embodiment is as shown in the table：
Embodiment 5
2 gained sepiolite composite absorber of embodiment is used to prepare sepiolite composite wave-suction material, preparation process is：It adopts
Disperse integration apparatus with vertical mixing, by 75g sepiolite composite absorber, 40g cycloaliphatic epoxy resin in 1500r/min item
1h is dispersed with stirring under part；The poly- phthalein amine hardener of 10g is added, continues stirring curing 20min, adds 7g n-butanol solvent and 0.1g stream
Flat agent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using spraying process, after 40 DEG C of baking 1.5h, cooling 0.5h,
To obtain the final product.The performance parameter of sepiolite composite wave-suction material obtained by the present embodiment is as shown in the table：
Embodiment 6
3 gained sepiolite composite absorber of embodiment is used to prepare sepiolite composite wave-suction material, preparation process is：It adopts
Disperse integration apparatus with vertical mixing, by 110g sepiolite composite absorber, 40g bisphenol F epoxy resin in 2000r/min item
0.5h is stirred under part；10g low molecule amine hardener is added, continues stirring curing 20min, adds 8g dimethylbenzene and n-butanol is molten
Agent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using roll coating process, after 50 DEG C of baking 1.5h, cooling 1.0h, i.e.,
?.The performance parameter of sepiolite composite wave-suction material obtained by the present embodiment is as shown in the table：
Comparative example 1
Integration apparatus is dispersed using vertical mixing, by 50g flaky carbonyl iron powder, 40g bisphenol A epoxide resin in 1000r/
1h is dispersed with stirring under the conditions of min；10g low molecule amine curing agent is added, continues stirring curing 20min, addition 7g dimethylbenzene is molten
Agent, and using spraying process by mixture be coated in 180mm ╳ 180mm aluminium sheet on, after 50 DEG C of baking 1h, cool down 0.5h to get.
The performance parameter of composite wave-suction material obtained by this comparative example is as shown in the table：
Comparative example 2
Integration apparatus is dispersed using vertical mixing, by 50g sheet iron aluminum silicon powder, 40g bisphenol A epoxide resin in 1000r/
1h is dispersed with stirring under the conditions of min；10g low molecule amine curing agent is added, continues stirring curing 20min, addition 7g dimethylbenzene is molten
Agent, and using spraying process by mixture be coated in 180mm ╳ 180mm aluminium sheet on, after 50 DEG C of baking 1h, cool down 0.5h to get.
The performance parameter of composite wave-suction material obtained by this comparative example is as shown in the table：
Fig. 2 is 4~6 gained sepiolite composite wave-suction material of embodiment and 1~2 absorbing material of comparative example in 8~18GHz frequency
The absorbing property figure of section, figure it is seen that the resulting sepiolite of the present invention is multiple compared to absorbing material in comparative example 1~2
Closing absorbing material has lower surface density (≤1.0kg/m2) and broader effective suction wavestrip it is wide (>=7.3GHz).
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example.To those of ordinary skill in the art, obtained improvement and change in the case where not departing from the technology of the present invention concept thereof
It changes and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of sepiolite composite absorber, which is characterized in that by sepiolite and magnetic Fe3O4Composition, the magnetic Fe3O4Load
In the network structure and nano pore of sepiolite, magnetic Fe3O4Mass ratio with sepiolite is 1：(3~6).
2. a kind of preparation method of sepiolite composite absorber according to claim 1, which is characterized in that including following step
Suddenly：
(1) it is prepared by predetermined ratio and contains Fe2+And Fe3+Mixing salt solution；
(2) it disperses sepiolite in mixing salt solution obtained by step (1), is stirred under an inert atmosphere, obtains presoma
Solution；
(3) lye is added into precursor solution obtained by step (2), adjusts PH to 9~12,40~80 DEG C at a temperature of carry out
Crystallizing treatment makes magnetic Fe3O4It is supported in the network structure and nano pore of sepiolite, precipitating obtained by Crystallizing treatment is carried out
Washing, it is dry, obtain the sepiolite composite absorber.
3. the preparation method of sepiolite composite absorber according to claim 2, which is characterized in that in the step (1), mix
Close Fe in salting liquid2+、Fe3+Concentration is 0.05~0.2mol/L, and Fe2+、Fe3+Molar concentration rate is 1：(1~2).
4. the preparation method of sepiolite composite absorber according to claim 2, which is characterized in that in the step (1), Fe2 +、Fe3+Salting liquid be one or both of nitrate, sulfate.
5. the preparation method of sepiolite composite absorber according to claim 2, which is characterized in that in the step (2), sea
Afrodite is handled by purification & isolation, through broken, levigate to 200 meshes excessively, grade >=80% of sepiolite；The inert atmosphere is
One or both of high pure nitrogen, high-purity argon gas.
6. the preparation method of sepiolite composite absorber according to claim 2, which is characterized in that in the step (3), alkali
Liquid be NaOH solution or ammonium hydroxide, the NaOH solution concentration be 0.05~0.1mol/L, ammonium hydroxide mass percent concentration be 20~
40%.
7. the preparation method of sepiolite composite absorber according to claim 2, which is characterized in that brilliant in the step (3)
Changing the processing time is 1~3h.
8. a kind of application of sepiolite composite absorber according to claim 1, which is characterized in that by sepiolite composite absorption
Agent is used to prepare sepiolite composite wave-suction material, and the sepiolite composite wave-suction material includes by weight percentage：Sepiolite is multiple
Close absorbent 50~70%, epoxy resin 24~40%, epoxy hardener 6~10%.
9. the application of sepiolite composite absorber according to claim 8, which is characterized in that the sepiolite composite wave-absorbing material
The preparation process of material is：Under mechanical agitation, by sepiolite composite absorber and epoxy resin by design weight than uniform
Mixing；The epoxy hardener of predetermined ratio is added, continues stirring 10~40min of curing, adds nonessential organic solvent and adjust and glue
Degree and nonessential auxiliary agent adjust dispersibility and levelability, and mixture is coated in aluminium sheet using spraying, roller coating or brush coating process
On, after baking is cooling to obtain the final product.
10. the application of sepiolite composite absorber according to claim 8, which is characterized in that the epoxy resin is bisphenol-A
One of epoxy resin, cycloaliphatic epoxy resin, bisphenol F epoxy resin are a variety of；The epoxy hardener is poly- phthalein amine
One of curing agent, low molecule amine curing agent, cashew nut oil modified curing agent are a variety of；The nonessential organic solvent is benzene
One of class, alcohols, ketone are a variety of；The nonessential auxiliary agent is coalescing agent, levelling agent, defoaming agent, dispersing agent, promotion
One of agent is a variety of.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110108772A (en) * | 2019-05-29 | 2019-08-09 | 中南大学 | A kind of modified meerschaum modified electrode and the preparation method and application thereof |
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Application publication date: 20181130 |