CN117143475A - Preparation method of wave-absorbing coating - Google Patents
Preparation method of wave-absorbing coating Download PDFInfo
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- CN117143475A CN117143475A CN202311093821.XA CN202311093821A CN117143475A CN 117143475 A CN117143475 A CN 117143475A CN 202311093821 A CN202311093821 A CN 202311093821A CN 117143475 A CN117143475 A CN 117143475A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 40
- 238000000576 coating method Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 106
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 229920001971 elastomer Polymers 0.000 claims abstract description 13
- 239000000806 elastomer Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- 238000012216 screening Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 13
- 229920002635 polyurethane Polymers 0.000 claims description 8
- 239000004814 polyurethane Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 4
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- -1 iron-silicon-aluminum Chemical compound 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 229910002796 Si–Al Inorganic materials 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 229920002050 silicone resin Polymers 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 13
- 239000011358 absorbing material Substances 0.000 abstract description 11
- 238000011068 loading method Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 23
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 229910000702 sendust Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000005670 electromagnetic radiation Effects 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
-
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08K2201/01—Magnetic additives
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Paints Or Removers (AREA)
Abstract
A preparation method of the wave-absorbing paint comprises the following steps: s1, preparing raw materials: screening the modified wave-absorbing powder to obtain modified wave-absorbing powder I, modified wave-absorbing powder II and modified wave-absorbing powder III of three grades of-80 to +150 meshes, 325 to +400 meshes and-2300 meshes respectively, and proportioning the modified wave-absorbing powder I, the modified wave-absorbing powder II and the modified wave-absorbing powder III to obtain graded modified wave-absorbing powder; uniformly mixing the grading modified wave-absorbing powder with a high polymer elastomer to obtain a mixture; s2, stirring slurry: adding the mixture into a stirrer, and then adding solvent and auxiliary components to prepare the wave-absorbing coating. According to the preparation method of the wave-absorbing coating, the particle size distribution of the modified wave-absorbing powder is changed through the particle grading, so that the graded modified wave-absorbing powder with higher loose loading and tap density is obtained, and the graded modified wave-absorbing powder is mixed with the high polymer elastomer to prepare the wave-absorbing coating, so that the wave-absorbing coating is easy to process into wave-absorbing materials with various shapes, and has excellent wave-absorbing performance.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing materials, and particularly relates to a preparation method of wave-absorbing paint.
Background
Since the beginning of the 20 th century, various electronic technologies and microwaves have been vigorously developed, bringing great convenience to human life. At the same time, these electronic facilities generate a great deal of electromagnetic radiation pollution during normal operation, which leads to an increasing deterioration of the living environment. Electromagnetic radiation can interfere electromagnetic sensitive equipment and instruments.
How to solve the problems of electromagnetic radiation and electromagnetic interference has been gradually paid attention to the whole society. The development of new absorbing materials, which are functional materials that absorb incident electromagnetic waves and convert them into energy such as thermal energy for loss, has been widely recognized as an effective approach to solve such problems. The wave absorbing material is applied to various electronic facilities and can absorb electromagnetic radiation pollution, so that the effects of eliminating electromagnetic pollution and purifying living environment are realized.
The object of the invention is therefore: the novel wave-absorbing paint is developed, the wave-absorbing performance of the wave-absorbing paint is improved through particle grade matching and modification of wave-absorbing materials, the preparation method is simple, the wave-absorbing paint can be prepared in a large scale, and the wave-absorbing paint has wide application scenes in the field of wave-absorbing materials.
Disclosure of Invention
The invention aims to: in order to overcome the defects, the invention aims to provide a preparation method of a wave-absorbing coating, which is reasonable in design, and is characterized in that soft magnetic alloy powder is modified by a liquid phase hydrolysis method to prepare modified wave-absorbing powder with higher saturation induction intensity and lower loss, the particle size distribution of the modified wave-absorbing powder is changed by particle grading, the graded modified wave-absorbing powder with higher loose packing and tap density is prepared, and the graded modified wave-absorbing powder is mixed with a high polymer elastomer to prepare the wave-absorbing coating, so that the wave-absorbing coating is easy to process into wave-absorbing materials with various shapes and has excellent wave-absorbing performance.
The invention aims at realizing the following technical scheme:
a preparation method of the wave-absorbing paint comprises the following steps:
s1, preparing raw materials: screening the modified wave-absorbing powder to obtain modified wave-absorbing powder I, modified wave-absorbing powder II and modified wave-absorbing powder III of which the grades are respectively-80 to +150 meshes, 325 to +400 meshes and-2300 meshes, wherein the mass percentages of the modified wave-absorbing powder I, the modified wave-absorbing powder II and the modified wave-absorbing powder III are 5-10: 1-5: 1-5, proportioning to obtain graded modified wave-absorbing powder; uniformly mixing the grading modified wave-absorbing powder and the high polymer elastomer, wherein the mass ratio of the grading modified wave-absorbing powder to the high polymer elastomer is 10-20:1-5, obtaining a mixture;
s2, stirring slurry: adding the mixture into a stirrer, and then adding a solvent and an auxiliary agent component, wherein the mass ratio of the solvent to the mixture to the auxiliary agent component is 50-100: 10-50: and 0.5-5, stirring to uniformly mix the materials, and preparing the wave-absorbing coating.
The preparation method of the wave-absorbing coating is reasonable in design, the modified wave-absorbing powder is screened into three-level powder with narrower particle size distribution, and the particle size distribution of the modified wave-absorbing powder is changed through particle grading, so that the graded modified wave-absorbing powder with higher loose loading and tap density is obtained. The graded modified wave-absorbing powder is mixed with the polymer elastomer to prepare the wave-absorbing paint, the polymer elastomer plays roles of filler and binder in the wave-absorbing paint, so that the graded modified wave-absorbing powder can be uniformly distributed in the wave-absorbing paint, and the wave-absorbing paint is easy to process into wave-absorbing materials with various shapes. The preparation method of the wave-absorbing coating is simple, can be used for large-scale preparation, and has wide application scenes in the field of wave-absorbing materials.
Further, the preparation method of the wave-absorbing coating comprises the following steps: adding soft magnetic alloy powder into a mixed solution of polyvinylpyrrolidone and absolute ethyl alcohol under the conditions of 40-60 ℃ and stirring, stirring for 10-30min, then dropwise adding tetrabutyl titanate, stirring for 10-30min, then adding a mixed solution of deionized water and absolute ethyl alcohol, dropwise adding acetic acid to adjust the pH, stirring for 0.5-2h, after the reaction is finished, washing with water and absolute ethyl alcohol for multiple times respectively, and drying for 10-16h at 40-60 ℃ to obtain modified wave-absorbing powder.
The soft magnetic alloy powder can be made of Sendai Style alloy powder, and the main component is Fe9.6-Si5.4-Al.
In order to improve the performance of the wave-absorbing coating, the wave-absorbing powder needs higher saturated magnetic induction intensity and lower loss, the invention adopts liquid phase hydrolysis, a layer of uniform and compact titanium oxide film is coated on the surface of the soft magnetic alloy powder, the reaction system is stable and uniform, the optimization of hydrolysis polycondensation reaction is realized by controlling the pH value of the solution, the insulation effect of the soft magnetic alloy powder is effectively improved, the high-frequency eddy current loss is effectively restrained, and the comprehensive performance of the wave-absorbing powder is improved.
Further, in the preparation method of the wave-absorbing coating, the ratio of the mass of polyvinylpyrrolidone to the volume of absolute ethyl alcohol in the mixed solution of polyvinylpyrrolidone and absolute ethyl alcohol is 5-10: 1000; the volume ratio of deionized water to absolute ethyl alcohol in the mixed solution of deionized water and absolute ethyl alcohol is 1-5:10; acetic acid is added dropwise to adjust the pH to 4-6.
Further, in the preparation method of the wave-absorbing coating, the mass ratio of polyvinylpyrrolidone in the mixed solution of the iron-silicon-aluminum soft magnetic alloy, polyvinylpyrrolidone and absolute ethyl alcohol is 80-150: 1, a step of; the mass ratio of the tetrabutyl titanate to the Fe-Si-Al soft magnetic alloy is 1-20: 100; the mass ratio of deionized water in the mixed solution of the iron-silicon-aluminum soft magnetic alloy and deionized water and absolute ethyl alcohol is 100: 10-50.
Further, the preparation method of the wave-absorbing coating comprises the steps of screening modified wave-absorbing powder, and specifically comprises the following steps: and (3) screening the modified wave-absorbing powder through a 150-mesh analysis screen, taking out the oversize product to obtain modified wave-absorbing powder I, screening the undersize product to continuously pass through a 325-mesh analysis screen and a 400-mesh analysis screen, taking out the undersize product to obtain modified wave-absorbing powder II, screening the undersize product to continuously pass through a 2300-mesh analysis screen, and taking out the undersize product to obtain modified wave-absorbing powder III.
Further, according to the preparation method of the wave-absorbing coating, the loose packing density of the graded modified wave-absorbing powder is 1-5g/cm 3 Tap density of 1-5g/cm 3 。
Further, in the method for preparing the wave-absorbing coating, the molecular elastomer is at least one of polyurethane, acrylic acid, organosilicon and epoxy resin.
Further, in the preparation method of the wave-absorbing coating, the solvent is one of cyclohexanone, cycloheptane, methyl isopropyl ketone, acetone, dimethyl carbonate, DMF and propylene glycol methyl ether; the auxiliary agent component is at least one of dispersing agent, defoaming agent, leveling agent and surfactant.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the preparation method of the wave-absorbing coating, a layer of uniform and compact titanium oxide film is coated on the surface of the soft magnetic alloy powder by adopting a liquid phase hydrolysis method, the hydrolysis polycondensation reaction is optimized by controlling the pH value of the solution, the insulation effect of the soft magnetic alloy powder is effectively improved, the high-frequency eddy current loss is effectively inhibited, and the modified wave-absorbing powder with higher saturated magnetic induction intensity and lower loss is prepared;
(2) According to the preparation method of the wave-absorbing coating, the modified wave-absorbing powder is screened into three-stage powder with narrower particle size distribution, and the particle size distribution of the modified wave-absorbing powder is changed through particle grading, so that the graded modified wave-absorbing powder with higher loose loading and tap density is obtained. The grading modified wave-absorbing powder is mixed with the high polymer elastomer to prepare the wave-absorbing paint, the high polymer elastomer plays roles of a filler and a binder in the wave-absorbing paint, so that the grading modified wave-absorbing powder can be uniformly distributed in the wave-absorbing paint, and the wave-absorbing paint is easy to process into wave-absorbing materials with various shapes;
(3) The preparation method of the wave-absorbing coating is simple, can be used for large-scale preparation, and has wide application fields in the field of wave-absorbing materials.
Detailed Description
In the following, the technical solutions in the examples of the present invention will be clearly and completely described in combination with specific experimental data, namely, comparative example 1, comparative example 2, comparative example 3, example 1, example 2, and example 3, and it is apparent that the described examples are only some examples of the present invention, but not all examples. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The following comparative example 1, example 1 and example 2 provide a wave-absorbing powder, and the raw materials used in comparative example 1, example 1 and example 2 are all commercially available common raw materials.
Comparative example 1
The wave-absorbing powder of comparative example 1 was a sendust alloy powder.
Example 1
The wave-absorbing powder of example 1 was prepared by the steps of:
(1) Adding 6 g polyvinylpyrrolidone into 1L absolute ethyl alcohol, and continuously stirring until the solution is transparent to prepare a mixed solution of polyvinylpyrrolidone and absolute ethyl alcohol;
(2) Adding 0.12L deionized water into 0.5L absolute ethyl alcohol, and continuously stirring to prepare a mixed solution of deionized water and absolute ethyl alcohol;
(3) 600g of the sendust alloy powder is added into a mixed solution of polyvinylpyrrolidone and absolute ethyl alcohol under the conditions of a temperature of 55 ℃ and stirring, 50g of tetrabutyl titanate is added dropwise after stirring for 15min, a mixed solution of deionized water and absolute ethyl alcohol is added after stirring for 20min, acetic acid is added dropwise to adjust the pH to about 5.5, stirring is carried out for 0.5-2h, the reaction is finished, and the mixture is washed with water and absolute ethyl alcohol for multiple times and then dried for 12h at 60 ℃ to obtain the wave-absorbing powder of the embodiment 1.
Example 2
The wave-absorbing powder of example 2 was prepared as follows: taking the wave-absorbing powder of the embodiment 1, a 150-mesh analysis screen, taking out the oversize product to obtain modified wave-absorbing powder I, selecting the undersize product to continuously pass through a 325-mesh analysis screen and a 400-mesh analysis screen, taking out the undersize product to obtain modified wave-absorbing powder II, selecting the undersize product to continuously pass through a 2300-mesh analysis screen, taking out the undersize product to obtain modified wave-absorbing powder III, and mixing the modified wave-absorbing powder I, the modified wave-absorbing powder II and the modified wave-absorbing powder III according to the mass percentage of 6:1.8:2.2, the wave-absorbing powder of example 2 was obtained.
The wave-absorbing powders of comparative example 1, example 1 and example 2 were tested for bulk density and tap density, respectively, and the test results are shown in table 1.
TABLE 1 apparent density and tap Density of wave-absorbing powder
| Bulk density (g/cm 3) | Tap density (g/cm 3) | |
| Comparative example 1 | 0.478 | 1.334 |
| Example 1 | 0.524 | 1.578 |
| Comparative example 2 | 1.678 | 3.227 |
Wave absorbing performance test: the electromagnetic parameters of the wave-absorbing powder of comparative example 1, example 1 and example 2 are tested, the testing instrument is a vector analyzer, and the testing frequency band is 0.5-18 GHz.
In the test, the wave-absorbing powders of comparative example 1, example 1 and example 2 were manufactured and tested on the same collar, namely, paraffin and the wave-absorbing powders of comparative example 1, example 1 and example 2 were prepared in a ratio of 1: 1. is fully and uniformly mixed to form a concentric ring with the thickness of about 2.5 and mm, the inner diameter of about 3.0 and mm and the outer diameter of about 7.0 and mm.
The test result of the wave absorbing performance is as follows: generally, the material is considered to have an effective absorption band when RL < -10 dB. In comparative example 1, RLmin is-12.54 dB at 0.81 GHz, and the effective wave-absorbing bandwidth is less than 0.2GHz; in the embodiment 1, at the frequency of 1.34 GHz, RLmin is-15.89 dB, and the effective absorption bandwidth can reach 0.4GHz; example 2 at 4.38 GHz, RLmin is-22.47 dB, and the effective absorption bandwidth can reach 2.1GHz.
The test result of the wave absorbing performance shows that: the particle size distribution of the wave-absorbing powder is changed through the particle grading, so that the wave-absorbing performance of the wave-absorbing powder is improved to a certain extent but not much. A layer of uniform and compact titanium oxide film is coated on the surface of the wave-absorbing powder by a liquid phase hydrolysis method, and compared with comparative example 1 and example 1, the microwave loss minimum value RLmin, the effective bandwidth and the like of the wave-absorbing powder are obviously improved, which shows that the wave-absorbing performance of the wave-absorbing powder is enhanced by the treatment.
The following comparative examples 2, 3 and 3 provide a wave-absorbing coating, and the raw materials used in comparative examples 2, 3 and 3 are all common raw materials in the commercial industry.
Comparative example 2
The wave-absorbing coating of comparative example 2 was prepared by the steps of:
s1, preparing raw materials: uniformly mixing the sendust alloy powder and polyurethane, wherein the mass ratio of the sendust alloy powder to the polyurethane is 80:20, obtaining a mixture;
s2, stirring slurry: adding the mixture into a stirrer, and then adding a solvent DMF and an auxiliary component (dispersant BYK-110: defoamer BYK-141: flatting agent BYK-330 is 6:1:1), wherein the mass ratio of the solvent DMF to the mixture to the auxiliary component is 100:70:2, stirring and uniformly mixing the materials to prepare the wave-absorbing coating of the comparative example 2.
Comparative example 3
The wave-absorbing coating of comparative example 3 was prepared by the steps of:
s1, preparing raw materials: the wave-absorbing powder of example 1 was uniformly mixed with polyurethane, and the mass ratio of the sendust alloy powder to polyurethane was 80:20, obtaining a mixture;
s2, stirring slurry: adding the mixture into a stirrer, and then adding a solvent DMF and an auxiliary component (dispersant BYK-110: defoamer BYK-141: flatting agent BYK-330 is 6:1:1), wherein the mass ratio of the solvent DMF to the mixture to the auxiliary component is 100:70:2, stirring the mixture to uniformly mix the mixture, thereby preparing the wave-absorbing coating of comparative example 3.
Example 3
The wave-absorbing coating of example 3 was prepared comprising the steps of:
s1, preparing raw materials: the wave-absorbing powder of example 2 was uniformly mixed with polyurethane, and the mass ratio of the sendust alloy powder to polyurethane was 80:20, obtaining a mixture;
s2, stirring slurry: adding the mixture into a stirrer, and then adding a solvent DMF and an auxiliary component (dispersant BYK-110: defoamer BYK-141: flatting agent BYK-330 is 6:1:1), wherein the mass ratio of the solvent DMF to the mixture to the auxiliary component is 100:70:2, stirring and uniformly mixing the materials to prepare the wave-absorbing coating of example 3.
There are many ways in which the invention may be practiced, and what has been described above is merely a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that modifications may be made without departing from the principles of the invention, and such modifications are intended to be within the scope of the invention.
Claims (8)
1. The preparation method of the wave-absorbing coating is characterized by comprising the following steps:
s1, preparing raw materials: screening the modified wave-absorbing powder to obtain modified wave-absorbing powder I, modified wave-absorbing powder II and modified wave-absorbing powder III of which the grades are respectively-80 to +150 meshes, 325 to +400 meshes and-2300 meshes, wherein the mass percentages of the modified wave-absorbing powder I, the modified wave-absorbing powder II and the modified wave-absorbing powder III are 5-10: 1-5: 1-5, proportioning to obtain graded modified wave-absorbing powder; uniformly mixing the grading modified wave-absorbing powder and the high polymer elastomer, wherein the mass ratio of the grading modified wave-absorbing powder to the high polymer elastomer is 10-20:1-5, obtaining a mixture;
s2, stirring slurry: adding the mixture into a stirrer, and then adding a solvent and an auxiliary agent component, wherein the mass ratio of the solvent to the mixture to the auxiliary agent component is 50-100: 10-50: and 0.5-5, stirring to uniformly mix the materials, and preparing the wave-absorbing coating.
2. The method for preparing the wave-absorbing coating according to claim 1, wherein the preparation of the modified wave-absorbing powder comprises the following steps: adding soft magnetic alloy powder into a mixed solution of polyvinylpyrrolidone and absolute ethyl alcohol under the conditions of 40-60 ℃ and stirring, stirring for 10-30min, then dropwise adding tetrabutyl titanate, stirring for 10-30min, then adding a mixed solution of deionized water and absolute ethyl alcohol, dropwise adding acetic acid to adjust the pH, stirring for 0.5-2h, after the reaction is finished, washing with water and absolute ethyl alcohol for multiple times respectively, and drying for 10-16h at 40-60 ℃ to obtain modified wave-absorbing powder.
3. The method for preparing the wave-absorbing coating according to claim 2, wherein the ratio of the mass of polyvinylpyrrolidone to the volume of absolute ethyl alcohol in the mixed solution of polyvinylpyrrolidone and absolute ethyl alcohol is 5-10: 1000; the volume ratio of deionized water to absolute ethyl alcohol in the mixed solution of deionized water and absolute ethyl alcohol is 1-5:10; acetic acid is added dropwise to adjust the pH to 4-6.
4. The method for preparing the wave-absorbing coating according to claim 3, wherein the mass ratio of polyvinylpyrrolidone in the mixed solution of the iron-silicon-aluminum soft magnetic alloy, polyvinylpyrrolidone and absolute ethyl alcohol is 80-150: 1, a step of; the mass ratio of the tetrabutyl titanate to the Fe-Si-Al soft magnetic alloy is 1-20: 100; the mass ratio of deionized water in the mixed solution of the iron-silicon-aluminum soft magnetic alloy and deionized water and absolute ethyl alcohol is 100: 10-50.
5. The method for producing a wave-absorbing coating according to claim 1, wherein the wave-absorbing coating is a film; the screening of the modified wave-absorbing powder comprises the following specific contents: and (3) screening the modified wave-absorbing powder through a 150-mesh analysis screen, taking out the oversize product to obtain modified wave-absorbing powder I, screening the undersize product to continuously pass through a 325-mesh analysis screen and a 400-mesh analysis screen, taking out the undersize product to obtain modified wave-absorbing powder II, screening the undersize product to continuously pass through a 2300-mesh analysis screen, and taking out the undersize product to obtain modified wave-absorbing powder III.
6. The method for producing a wave-absorbing coating according to claim 1, which is characterized in thatCharacterized in that the bulk density of the graded modified wave-absorbing powder is 1-5g/cm 3 Tap density of 1-5g/cm 3 。
7. The method for producing a wave-absorbing coating according to claim 1, wherein the molecular elastomer is at least one of polyurethane, acrylic acid, silicone, and epoxy resin.
8. The method for preparing the wave-absorbing coating according to claim 1, wherein the solvent is one of cyclohexanone, cycloheptane, methyl isopropyl ketone, acetone, dimethyl carbonate, DMF and propylene glycol methyl ether; the auxiliary agent component is at least one of dispersing agent, defoaming agent, leveling agent and surfactant.
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