CN115746767A - Glue with wave absorbing function and preparation method thereof - Google Patents
Glue with wave absorbing function and preparation method thereof Download PDFInfo
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- CN115746767A CN115746767A CN202211583694.7A CN202211583694A CN115746767A CN 115746767 A CN115746767 A CN 115746767A CN 202211583694 A CN202211583694 A CN 202211583694A CN 115746767 A CN115746767 A CN 115746767A
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- wave absorbing
- glue
- iron powder
- carbonyl iron
- wave
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- 239000003292 glue Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 74
- 239000006096 absorbing agent Substances 0.000 claims abstract description 87
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 78
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000003822 epoxy resin Substances 0.000 claims abstract description 23
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000003755 preservative agent Substances 0.000 claims abstract description 8
- 230000002335 preservative effect Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 238000004945 emulsification Methods 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 22
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 16
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 230000003213 activating effect Effects 0.000 claims description 11
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 9
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 8
- 150000003512 tertiary amines Chemical class 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 19
- 239000010410 layer Substances 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002250 absorbent Substances 0.000 description 10
- 230000002745 absorbent Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 7
- -1 carbonium anions Chemical class 0.000 description 5
- 230000001804 emulsifying effect Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
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- 238000004471 energy level splitting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The invention relates to glue, in particular to glue with a wave-absorbing function and a preparation method thereof, wherein the glue comprises the following raw materials in parts by weight: 50-80 parts of epoxy resin, 5-10 parts of hydrogen-containing silicone oil, 2-4 parts of preservative, 5-10 parts of solvent, 3-8 parts of curing agent and 25-40 parts of wave absorbing agent; the preparation method of the wave absorbing agent comprises the following steps: 1) Carrying out high-shear emulsification dispersion on carbonyl iron powder, then carrying out ultrasonic treatment, and drying to prepare pretreated carbonyl iron powder; 2) Mixing the pretreated carbonyl iron powder prepared in the step 1) with oleylamine, and calcining for 2-3h at 550-700 ℃ to obtain the catalyst. This application has the advantage that improves the wave absorption performance who inhales ripples glue.
Description
Technical Field
The invention relates to the field of glue, in particular to glue with a wave absorbing function and a preparation method thereof.
Background
With the development of modern society, scientific technology and electronic industry are also developing at a high speed, various digital and high-frequency electronic and electrical equipment generate a large amount of electromagnetic waves with different wavelengths and frequencies during working, the electromagnetic waves can generate electromagnetic wave interference and radiation frequency interference, the interference can not only influence the performance of electronic products, but also cause serious harm to human beings and other organisms due to electromagnetic wave pollution; therefore, wave-absorbing materials are needed to be adopted for the preparation of some electronic products which are easy to be radiated by electromagnetic waves, so that the electromagnetic waves are inhibited, and the harm of the electromagnetic waves to the electronic products is reduced; the existing wave-absorbing material needs to be cut and processed when in use, so that the processing difficulty is increased, wave-absorbing glue is produced at the same time, the wave-absorbing glue can be used for adhering a substrate, and the wave-absorbing glue can also be used through direct compression molding, so that the difficulty of subsequent cutting and processing is reduced.
In the above-described related art, the inventors consider that: the wave-absorbing performance of the existing wave-absorbing glue needs to be improved.
Disclosure of Invention
In order to improve the wave absorbing performance of the wave absorbing glue, the application provides the glue with the wave absorbing function and the preparation method thereof.
First aspect, the application provides a glue with inhale ripples function adopts following technical scheme:
the glue with the wave absorbing function comprises the following raw materials in parts by weight: 50-80 parts of epoxy resin, 5-10 parts of hydrogen-containing silicone oil, 2-4 parts of preservative, 5-10 parts of solvent, 3-8 parts of curing agent and 25-40 parts of wave absorbing agent; the preparation method of the wave absorbing agent comprises the following steps:
1) Carrying out high-shear emulsification and dispersion on carbonyl iron powder, then carrying out ultrasonic treatment, and drying to prepare pretreated carbonyl iron powder;
2) Mixing the pretreated carbonyl iron powder prepared in the step 1) with oleylamine, and calcining at 550-700 ℃ for 2-3h to obtain the iron-based catalyst.
By adopting the technical scheme, the glue prepared from the epoxy resin has the characteristics of low toxicity, small volatility, strong cohesiveness and good toughness, and the prepared glue has good wave-absorbing performance by adding the wave-absorbing agent into the glue prepared from the epoxy resin; by carrying out high-shear emulsification and dispersion on the carbonyl iron powder, the particle size of the carbonyl iron powder is reduced in the process, so that after the carbonyl iron powder is added into the epoxy resin, the adhesive property of the glue prepared from the epoxy resin cannot be influenced on the premise of improving the wave absorption property of the glue; but the reduction of the particle size of the carbonyl iron powder can promote the direct contact among the carbonyl iron powder particles, so that the carbonyl iron powder particles are aggregated, and then the carbonyl iron powder particles emulsified by high shear are subjected to ultrasonic dispersion to prepare the nano-scale carbonyl iron powder; the oleylamine and the pretreated carbonyl iron powder are mixed, the oleylamine covers the pretreated carbonyl iron powder, a carbon layer is formed on the surface of the pretreated carbonyl iron powder by the oleylamine through calcination, the carbonyl iron powder can be protected by the carbon layer, the agglomeration and oxidation of the carbonyl iron powder can be effectively prevented, meanwhile, the carbon layer belongs to a resistance-shaped wave-absorbing material, and the carbon layer has the characteristics of light weight, thin material, good oxidation resistance and the like, and also has a macroscopic quantum tunnel effect and a quantum size effect, so that the carbon particles can generate electron energy level splitting, the atom and electron motion can be intensified, the electron energy is converted into heat energy, and meanwhile, hysteresis damage, domain wall resonance effect and other attenuation electromagnetic waves are generated, so that the carbon layer has a good wave-absorbing effect; carbonyl iron powder belongs to a magnetic medium wave-absorbing material and can achieve the wave-absorbing effect through resonance and hysteresis loss; through the common cooperation of carbon layer and carbonyl iron powder, the wave absorbing agent who makes has composite construction, still has good wave absorbing effect simultaneously, cooperates other raw materials simultaneously for the glue of preparation has good gluey stickness simultaneously, still has good wave absorbing performance.
Optionally, the mass ratio of the pretreated carbonyl iron powder to the oleylamine in the step 2) is (25-35) to (2-4).
By adopting the technical scheme, the mass ratio of the pretreated carbonyl iron powder to the oleylamine is limited, and when the oleylamine is low in mass, the coating effect on the pretreated carbonyl iron powder is insufficient, so that the wave absorbing performance of the prepared wave absorbing agent is influenced; when the amount of oleylamine is large, after high-temperature calcination, the thickness of a coating carbon layer formed on the surface of carbonyl iron powder is uneven, adhesion is easy to occur, the wave absorbing performance of a subsequent wave absorbing agent is influenced, and the wave absorbing performance of the prepared glue is reduced.
Optionally, before mixing the pretreated carbonyl iron powder with oleylamine in step 2), the pretreated carbonyl iron powder is first placed in 3-aminopropyltriethoxysilane for impregnation, and then taken out and dried.
By adopting the technical scheme, the carbonyl iron powder has the advantages of good magnetic conductivity, large saturation magnetization, good temperature stability and the like; but after the carbonyl iron powder is subjected to high-speed shearing emulsification, the particles are smaller, the specific surface area is larger, the activity of the material surface is higher, and the carbonyl iron powder is easy to generate oxidation reaction with oxygen in the air when being mixed with oleylamine and calcined, so that the wave absorbing performance of the carbonyl iron powder is reduced.
Optionally, the mass ratio of the pretreated carbonyl iron powder to the 3-aminopropyltriethoxysilane is (7-9) to (1-3).
By adopting the technical scheme, the mass ratio of the 3-aminopropyltriethoxysilane to the pretreated carbonyl iron powder is adjusted, so that the 3-aminopropyltriethoxysilane can pretreat the carbonyl iron powder to form a uniform and compact silane coating layer; however, when the amount of the 3-aminopropyltriethoxysilane is too much, silane coating layers formed by the 3-aminopropyltriethoxysilane on the pretreated carbonyl iron powder are multi-layered, and mutual sliding is easily generated among the multi-layered silane coating layers, so that the coating effect of the subsequent oleylamine on the pretreated carbonyl iron powder is influenced, and the wave absorbing performance of the prepared wave absorbing agent is reduced.
Optionally, the wave absorbing agent is soaked in an activating agent for 5-8min before use, and the activating agent is composed of at least one of sulfuric acid and nitric acid and water according to a mass ratio of (6-8) to (1-3).
By adopting the technical scheme, sulfuric acid or nitric acid is used for impregnating the wave absorbent, and both the sulfuric acid and the nitric acid have etching effects, so that abundant pore structures can be etched on the surface of the prepared wave absorbent, and electromagnetic waves can be repeatedly reflected and scattered in the pore structures so as to consume the energy of the electromagnetic waves, so that the consumption effect of the wave absorbent on the electromagnetic waves is improved, and the prepared glue has a better wave absorbing effect.
Optionally, the wave absorbing agent consists of sulfuric acid, nitric acid and water according to a mass ratio of (4-5) to (2-3) to (1-3).
By adopting the technical scheme, the nitric acid can remove inorganic components and ash on the surface of the wave absorbent while etching the wave absorbent, and carboxyl functional groups are formed on the surface of the wave absorbent, so that the contents of carboxyl and phenolic groups on the surface of the wave absorbent are improved, and the binding force between the subsequent wave absorbent and epoxy resin and other raw materials is improved; compared with nitric acid, the sulfuric acid has stronger etching effect and is quicker; the activating agent is prepared by compounding sulfuric acid, nitric acid and water, the carbon layer on the surface of the wave absorbent is etched, and meanwhile, the stability of the wave absorbent in combination with epoxy resin and other raw materials in the follow-up process is improved, so that the prepared glue has better wave-absorbing performance.
Optionally, the curing agent consists of methyltetrahydrophthalic anhydride and tertiary amine 2,4, 6-tris (dimethylaminomethyl) phenol according to the mass ratio of (6-9) to (3-4).
By adopting the technical scheme, methyltetrahydrophthalic anhydride and tertiary amine 2,4, 6-tri (dimethylaminomethyl) phenol are compounded to form a curing agent, the tertiary amine 2,4, 6-tri (dimethylaminomethyl) phenol reacts with the methyltetrahydrophthalic anhydride to generate carbonium anions, the carbonium anions can react with an epoxy group of epoxy resin to generate alkoxy anions, the alkoxy anions can react with anhydride in the methyltetrahydrophthalic anhydride to continuously generate carbonium anions, and the epoxy resin is cured by the reaction; by adjusting the mass ratio of the methyltetrahydrophthalic anhydride to the tertiary amine 2,4, 6-tris (dimethylaminomethyl) phenol, the curing of the epoxy resin is promoted together, the curing rate of the epoxy resin is improved, the prepared glue has higher drying speed, and meanwhile, the wave absorbing agent is favorably and quickly fixed in the epoxy resin, the sedimentation of the wave absorbing agent is reduced, and the wave absorbing performance of the prepared glue is improved.
In a second aspect, the application provides a preparation process of glue with a wave-absorbing function:
a preparation process of glue with a wave absorbing function comprises the following steps: mixing the wave absorbing agent with epoxy resin, hydrogen-containing silicone oil, antiseptic, solvent and curing agent.
By adopting the technical scheme, the wave absorbing agent is mixed with other raw materials, the prepared glue water is coated, the epoxy resin is crosslinked into a network structure under the curing action of heating and curing agents, and meanwhile, the wave absorbing agent is inserted into the network structure, so that the prepared glue water has good adhesive property and good wave absorbing performance while the prepared glue water has a reinforcing effect on the network structure.
Optionally, before being mixed with other raw materials, the wave absorber is modified to prepare a modified wave absorber, and the preparation method of the modified wave absorber comprises the following steps: uniformly mixing the wave absorbing agent, the polyurethane prepolymer and 1, 4-butanediol to obtain the polyurethane prepolymer; the mass ratio of the wave absorbing agent to the polyurethane prepolymer to the 1, 4-butanediol is (10-12) to (5-7) to (1-2).
By adopting the technical scheme, the polyurethane prepolymer and the 1, 4-butanediol are mixed with the wave absorbing agent firstly, so that the polyurethane prepolymer and the 1, 4-butanediol wrap the wave absorbing agent firstly, and then are mixed with the epoxy resin and other raw materials, and in the curing process of the glue, the polyurethane prepolymer generates a polyurethane network structure under the chain extension action of the 1, 4-butanediol, so that the wave absorbing agent is wrapped more tightly, and the protection effect on the wave absorbing agent is further improved; meanwhile, under the curing and heating effects of the curing agent, epoxy groups and hydroxyl groups in the epoxy resin can react with isocyanate groups in a polyurethane system, an interpenetrating network structure is generated through cross-linking combination, the effects of toughening and bonding force enhancement of the prepared glue are achieved by utilizing the high elasticity and wear resistance of the polyurethane and the high viscosity of the epoxy resin, and meanwhile, the fixing effect of the prepared glue on the wave absorbing agent is improved by matching with other raw materials, the stability of the wave absorbing agent in the glue is also improved, so that the prepared glue has better wave absorbing performance.
In summary, the present application has the following beneficial effects:
through emulsifying carbonyl iron powder through high shear, prepare into tiny granule, then through ultrasonic dispersion, reduce the gathering of tiny granule, then through the mixture of oleylamine and preliminary treatment carbonyl iron powder, make oleylamine generate the carbon-layer on preliminary treatment carbonyl iron powder in high temperature calcination, the carbon-layer can also effectively prevent the reunion and the oxidation of carbonyl iron powder when carrying out the protection to preliminary treatment carbonyl iron powder, and make the carbon-layer and the cooperation of carbonyl iron powder generate the wave-absorbing agent that has composite construction, under the resistance of carbon-layer is inhaled the wave and is inhaled the effect with the magnetic medium of carbonyl iron powder and inhale the wave, improve the ripples effect of the glue of preparing jointly.
Detailed Description
The present application will be described in further detail with reference to examples;
the raw materials of the examples and comparative examples of the present application were all generally commercially available unless otherwise specified.
The solvent used in the present application is ethylene glycol monoethyl ether acetate;
the preparation method of the polyurethane prepolymer comprises the following steps: putting dihydroxy polyether and toluene diisocyanate into a flask together, and continuously reacting for 4 hours at 80 ℃ to obtain the polyether polyol; the molar ratio of-OH in the dihydroxy polyether to-NCO in the toluene diisocyanate is 1;
the epoxy resin used in the present application is bisphenol a epoxy resin;
preparation example
Wave absorber preparation example 1
The preparation method of the wave absorbing agent in the preparation example comprises the following steps:
1) Taking carbonyl iron powder, putting the carbonyl iron powder into a high-shear emulsifying machine for high-shear emulsifying dispersion for 40min, taking out, putting into an ultrasonic machine for ultrasonic dispersion for 20min, taking out, drying, and preparing into pretreated carbonyl iron powder;
2) Mixing the pretreated carbonyl iron powder prepared in the step 1) with oleylamine, and calcining at 650 ℃ for 2.5 hours to obtain the catalyst; the mass ratio of the used pretreatment carbonyl iron powder to oleylamine is 25.
Wave absorber preparation example 2
The preparation method of the wave absorbing agent in the preparation example is different from that in the preparation example 1 of the wave absorbing agent in that the mass ratio of the pretreated carbonyl iron powder to the oleylamine in the step 2) is 35.
Wave absorber preparation example 3
The difference between the preparation method of the wave absorbing agent in the preparation example and the preparation example 1 of the wave absorbing agent is that the mass ratio of the pretreated carbonyl iron powder to the oleylamine in the step 2) is 30.
Wave absorber preparation example 4
The preparation method of the wave absorbing agent in the preparation example comprises the following steps:
1) Taking carbonyl iron powder, putting the carbonyl iron powder into a high-shear emulsifying machine for high-shear emulsifying dispersion for 40min, taking out, putting into an ultrasonic machine for ultrasonic dispersion for 20min, taking out, and drying to prepare pretreated carbonyl iron powder;
2) Putting the pretreated carbonyl iron powder prepared in the step 1) into 3-aminopropyltriethoxysilane for dipping, taking out, drying, mixing with oleylamine, and calcining at 650 ℃ for 2.5 hours to obtain the catalyst; the mass ratio of the used pretreatment carbonyl iron powder to the oleylamine is 30; the mass ratio of the used pretreated carbonyl iron powder to the 3-aminopropyltriethoxysilane is 7.
Wave absorber preparation example 5
The preparation method of the wave absorbing agent in the preparation example is different from that in the preparation example 4 of the wave absorbing agent in that the mass ratio of the pretreated carbonyl iron powder to the 3-aminopropyltriethoxysilane in the step 2) is 9.
Wave absorber preparation example 6
The difference between the preparation method of the wave absorbing agent in the preparation example and the preparation method of the wave absorbing agent in the preparation example 4 is that the mass ratio of the pretreated carbonyl iron powder used in the step 2) to the 3-aminopropyltriethoxysilane is 8.
Examples
Example 1
The glue with the wave absorbing function in the embodiment is prepared from the following raw materials: 50kg of bisphenol A epoxy resin, 5kg of hydrogen-containing silicone oil, 2kg of preservative, 5kg of solvent, 3kg of curing agent and 25kg of wave absorbing agent, wherein the wave absorbing agent is prepared from the wave absorbing agent preparation example 1; the curing agent consists of methyltetrahydrophthalic anhydride and tertiary amine 2,4, 6-tri (dimethylaminomethyl) phenol with the mass ratio of 6;
the preparation method of the glue with the wave absorbing function in the embodiment comprises the following steps:
and (3) putting the wave absorbing agent, the epoxy resin, the hydrogen-containing silicone oil, the preservative, the solvent and the curing agent in parts by weight into a stirring barrel, and uniformly mixing to obtain the epoxy resin wave absorbing agent.
Example 2
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 1 in that the glue with the wave absorbing function comprises the following raw materials: 80kg of bisphenol A epoxy resin, 10kg of hydrogen-containing silicone oil, 4kg of preservative, 10kg of solvent, 8kg of curing agent and 40kg of wave absorbing agent.
Example 3
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 1 in that the preparation raw materials of the glue with the wave absorbing function comprise: 60kg of bisphenol A epoxy resin, 8kg of hydrogen-containing silicone oil, 3kg of preservative, 7kg of solvent, 5kg of curing agent and 30kg of wave absorbing agent.
Example 4
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 3 in that the wave absorbing agent is soaked in the activating agent for 6min before being mixed with other raw materials, and then is taken out and dried; the activating agent is composed of sulfuric acid and water according to a mass ratio of 6.
Example 5
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 4 in that the used activating agent consists of sulfuric acid and water according to a mass ratio of 8.
Example 6
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 4 in that the used activating agent is composed of sulfuric acid and water according to a mass ratio of 7.
Example 7
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 4 in that the used activating agent consists of nitric acid and water according to a mass ratio of 7.
Example 8
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 4 in that the used activating agent is composed of sulfuric acid, nitric acid and water according to a mass ratio of 4.5.
Example 9
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 8 in that the wave absorbing agent is modified before being mixed with other raw materials, and the modification treatment comprises the following steps: putting the wave absorbing agent, the polyurethane prepolymer and the 1, 4-butanediol into a mixing barrel and uniformly mixing to obtain the polyurethane prepolymer; the mass ratio of the wave absorbing agent to the polyurethane prepolymer to the 1, 4-butanediol is (11).
Example 10
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 9 in that the curing agent consists of methyl tetrahydrophthalic anhydride and tertiary amine 2,4, 6-tris (dimethylaminomethyl) phenol in a mass ratio of 9.
Example 11
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 10 in that the curing agent consists of methyl tetrahydrophthalic anhydride and tertiary amine 2,4, 6-tris (dimethylaminomethyl) phenol according to a mass ratio of 7.
Example 12
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 6 in that the wave absorbing agent is prepared in the wave absorbing agent preparation example 2.
Example 13
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 6 in that the wave absorbing agent is prepared in the wave absorbing agent preparation embodiment 3.
Example 14
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 6 in that the wave absorbing agent is prepared in the wave absorbing agent preparation embodiment 4.
Example 15
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 6 in that the wave absorbing agent is prepared in the wave absorbing agent preparation example 5.
Example 16
The preparation process of the glue with the wave absorbing function in the embodiment is different from that in the embodiment 6 in that the wave absorbing agent is prepared in the wave absorbing agent preparation example 6.
Comparative example
Comparative example 1
The difference between the preparation process of the glue with the wave absorbing function in the comparative example and the preparation process in the example 1 is that the wave absorbing agent is carbonyl iron powder.
Comparative example 2
The difference between the preparation process of the glue with the wave absorbing function in the comparative example and the preparation process in the example 1 is that the wave absorbing agent is a carbon nano tube.
Comparative example 3
The difference between the preparation process of the glue with the wave absorbing function in the comparative example and the preparation process in the example 1 is that the preparation method of the wave absorbing agent comprises the following steps: mixing carbonyl iron powder and oleylamine, and calcining at 550-700 ℃ for 2-3h to obtain the catalyst.
Detection method
Respectively preparing the glue with the wave absorbing function according to the preparation processes of the glue with the wave absorbing function in the embodiments 1 to 16 and the comparative examples 1 to 3, taking the same mass of glue, pressing for 2 hours at 80 ℃ to prepare rectangular sheets with the thickness of 2mm and 120mm multiplied by 120mm, testing the shielding effect of the rectangular sheets at the frequency of 1GHz, and recording data to obtain a table 1;
table 1 shielding effectiveness of glues with wave absorbing function in examples 1-16 and comparative examples 1-3
As can be seen by combining examples 1 to 8 and table 1, a carbon layer is formed on the surface of carbonyl iron powder by oleylamine, the carbon layer and the carbonyl iron powder are compounded to generate a wave absorber with a core-shell structure, nitric acid, sulfuric acid and water are prepared into an activator according to a ratio of 4.5;
as can be seen by combining examples 9 to 11 and table 1, the polyurethane prepolymer and 1, 4-butanediol are mixed with the wave absorbing agent, the mass ratio of the wave absorbing agent to the polyurethane prepolymer to the 1, 4-butanediol is set to be 11; by combining examples 12-16, comparative examples 1-3 and table 1, it can be seen that the mass ratio of the carbonyl iron powder to the oleylamine is adjusted, so that the oleylamine can form a carbon layer on the surface of the carbonyl iron powder during the preparation process of the wave absorber, the generated wave absorber has a composite structure, and the electromagnetic waves can be consumed through the coordination of the composite structure; when the carbonyl iron powder is coated, the phenomenon that the thickness of a generated carbon layer is uneven due to excessive oleylamine, so that the adhesion of the wave absorbing agent is caused, and the wave absorbing performance of the prepared wave absorbing agent is influenced is also prevented; in the preparation process of the wave absorbing agent, the pretreated carbonyl iron powder is impregnated by 3-aminopropyltriethoxysilane, the mass ratio of the pretreated carbonyl iron powder to the 3-aminopropyltriethoxysilane is adjusted, so that the pretreated carbonyl is uniformly wrapped by the 3-aminopropyltriethoxysilane, the oxidation of the pretreated carbonyl iron powder in subsequent calcination is prevented, and the phenomenon that the wave absorbing performance of the prepared wave absorbing agent is influenced due to the fact that a wrapping layer formed by the 3-aminopropyltriethoxysilane is too thick and the connection between subsequent oleylamine and the carbonyl iron powder is not tight enough is avoided, and the wave absorbing performance of the prepared glue is further reduced.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The utility model provides a glue with inhale ripples function which characterized in that: the composite material comprises the following raw materials in parts by weight: 50-80 parts of epoxy resin, 5-10 parts of hydrogen-containing silicone oil, 2-4 parts of preservative, 5-10 parts of solvent, 3-8 parts of curing agent and 25-40 parts of wave absorbing agent; the preparation method of the wave absorbing agent comprises the following steps:
1) Carrying out high-shear emulsification and dispersion on carbonyl iron powder, then carrying out ultrasonic treatment, and drying to prepare pretreated carbonyl iron powder;
2) Mixing the pretreated carbonyl iron powder prepared in the step 1) with oleylamine, and calcining for 2-3h at 550-700 ℃ to obtain the catalyst.
2. The glue with the wave absorbing function according to claim 1, wherein: before the pretreated carbonyl iron powder and oleylamine are mixed in the step 2), the pretreated carbonyl iron powder is firstly placed into 3-aminopropyltriethoxysilane for dipping, and then taken out and dried.
3. The glue with the wave absorbing function according to claim 2, characterized in that: the mass ratio of the pretreated carbonyl iron powder to the 3-aminopropyltriethoxysilane is (7-9) to (1-3).
4. The glue with the wave absorbing function according to claim 1, characterized in that: the mass ratio of the pretreated carbonyl iron powder to the oleylamine in the step 2) is (25-35) to (4-8).
5. The glue with the wave absorbing function according to claim 2, characterized in that: the wave absorbing agent is soaked in an activating agent for 5-8min before use, and the activating agent is composed of at least one of sulfuric acid and nitric acid and water according to a mass ratio of (6-8) to (1-3).
6. The glue with the wave absorbing function according to claim 5, characterized in that: the wave absorbing agent consists of sulfuric acid, nitric acid and water according to a mass ratio of (4-5) to (2-3) to (1-3).
7. The glue with the wave absorbing function according to claim 1, characterized in that: the curing agent consists of methyl tetrahydrophthalic anhydride and tertiary amine 2,4, 6-tri (dimethylaminomethyl) phenol according to the mass ratio of (6-9) to (3-4).
8. The preparation method of the glue with the wave absorbing function according to claim 1, characterized by comprising the following steps: the method comprises the following steps: mixing the wave absorbing agent with epoxy resin, hydrogen-containing silicone oil, preservative, solvent and curing agent.
9. The preparation method of the glue with the wave absorbing function according to claim 8, characterized in that: the wave absorbing agent is modified before being mixed with other raw materials to prepare the modified wave absorbing agent, and the preparation method of the modified wave absorbing agent comprises the following steps: uniformly mixing the wave absorbing agent, the polyurethane prepolymer and 1, 4-butanediol to obtain the polyurethane prepolymer; the mass ratio of the wave absorbing agent to the polyurethane prepolymer to the 1, 4-butanediol is (10-12) to (5-7) to (1-2).
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| CN101185973A (en) * | 2007-12-07 | 2008-05-28 | 北京科技大学 | Method for preparing spherical nano iron powder |
| CN104479341A (en) * | 2014-12-08 | 2015-04-01 | 哈尔滨工程大学 | Preparation method of anisotropic variable-modulus polyurethane-base composite damping material |
| CN104788938A (en) * | 2015-04-13 | 2015-07-22 | 重庆大学 | High-damping and high-strength magneto-rheological elastomer and preparation method thereof |
| CN112744870A (en) * | 2019-10-30 | 2021-05-04 | 洛阳尖端技术研究院 | Aluminum oxide-carbonyl iron microsphere wave absorbing agent and preparation method thereof |
| CN114381228A (en) * | 2022-02-26 | 2022-04-22 | 东莞市恒尔朗实业有限公司 | Magnetic conductive adhesive for winding sheet type common mode inductor and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101185973A (en) * | 2007-12-07 | 2008-05-28 | 北京科技大学 | Method for preparing spherical nano iron powder |
| CN104479341A (en) * | 2014-12-08 | 2015-04-01 | 哈尔滨工程大学 | Preparation method of anisotropic variable-modulus polyurethane-base composite damping material |
| CN104788938A (en) * | 2015-04-13 | 2015-07-22 | 重庆大学 | High-damping and high-strength magneto-rheological elastomer and preparation method thereof |
| CN112744870A (en) * | 2019-10-30 | 2021-05-04 | 洛阳尖端技术研究院 | Aluminum oxide-carbonyl iron microsphere wave absorbing agent and preparation method thereof |
| CN114381228A (en) * | 2022-02-26 | 2022-04-22 | 东莞市恒尔朗实业有限公司 | Magnetic conductive adhesive for winding sheet type common mode inductor and preparation method thereof |
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