CN114686071B - Wave-absorbing coating composition, wave-absorbing coating, wave-absorbing material and preparation method thereof - Google Patents
Wave-absorbing coating composition, wave-absorbing coating, wave-absorbing material and preparation method thereof Download PDFInfo
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- CN114686071B CN114686071B CN202011602787.0A CN202011602787A CN114686071B CN 114686071 B CN114686071 B CN 114686071B CN 202011602787 A CN202011602787 A CN 202011602787A CN 114686071 B CN114686071 B CN 114686071B
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 67
- 239000011248 coating agent Substances 0.000 title claims abstract description 33
- 238000000576 coating method Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000008199 coating composition Substances 0.000 title claims abstract description 24
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical class [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims abstract description 45
- 239000011162 core material Substances 0.000 claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 15
- 239000006096 absorbing agent Substances 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 11
- 239000002518 antifoaming agent Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910021389 graphene Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000003973 paint Substances 0.000 claims description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 5
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 claims description 4
- 238000006467 substitution reaction Methods 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 6
- 239000007864 aqueous solution Substances 0.000 claims 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims 2
- 229920000178 Acrylic resin Polymers 0.000 claims 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- HLPKYOCVWVMBMR-UHFFFAOYSA-N azane benzylbenzene Chemical compound N.N.C=1C=CC=CC=1CC1=CC=CC=C1 HLPKYOCVWVMBMR-UHFFFAOYSA-N 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 abstract description 40
- 230000006835 compression Effects 0.000 abstract description 10
- 238000007906 compression Methods 0.000 abstract description 10
- 238000004132 cross linking Methods 0.000 abstract description 5
- 238000003892 spreading Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000013530 defoamer Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005470 impregnation Methods 0.000 description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229920001732 Lignosulfonate Polymers 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 229920003235 aromatic polyamide Polymers 0.000 description 2
- 229910001622 calcium bromide Inorganic materials 0.000 description 2
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 description 2
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- LUMVCLJFHCTMCV-UHFFFAOYSA-M potassium;hydroxide;hydrate Chemical compound O.[OH-].[K+] LUMVCLJFHCTMCV-UHFFFAOYSA-M 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910000547 2024-T3 aluminium alloy Inorganic materials 0.000 description 1
- 241000256837 Apidae Species 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 125000006416 CBr Chemical group BrC* 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- AZIQALWHRUQPHV-UHFFFAOYSA-N prop-2-eneperoxoic acid Chemical compound OOC(=O)C=C AZIQALWHRUQPHV-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 230000003313 weakening effect Effects 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
-
- 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
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/04—Polymer mixtures characterised by other features containing interpenetrating networks
Abstract
The invention provides a wave-absorbing coating composition, a wave-absorbing coating, a wave-absorbing material and a preparation method thereof. The wave-absorbing coating composition comprises: 60-90 parts by weight of resin component, 10-40 parts by weight of wave absorber, 3-10 parts by weight of curing agent, 10-15 parts by weight of brominated calcium lignin sulfonate, 200 parts by weight of solvent and 4-11 parts by weight of auxiliary agent. On one hand, the resin component and the brominated calcium lignosulfonate form a network interpenetrating structure, and on the other hand, the compressive strength retention rate and the shear strength retention rate of the wave-absorbing material are effectively improved by controlling the introduction amount of the brominated calcium lignosulfonate. Meanwhile, the types and the amounts of other components are beneficial to improving the structure and the crosslinking density of the wave-absorbing coating and the spreading degree and uniformity of the wave-absorbing coating on the honeycomb core material wall, so that the mechanical property of the wave-absorbing material is improved, and the retention rate of the compression strength and the retention rate of the shear strength are further improved.
Description
Technical Field
The invention relates to the technical field of wave-absorbing paint, in particular to a wave-absorbing paint composition, a wave-absorbing paint, a wave-absorbing material and a preparation method thereof.
Background
Up to now, oily honeycomb epoxy resin-based wave-absorbing composite materials are studied to a certain extent in China, but most of the problems of low retention rate of high-temperature compression strength, low retention rate of low-temperature compression strength, low retention rate of compression strength after water resistance, low retention rate of high-temperature shear strength and the like exist.
Disclosure of Invention
The invention mainly aims to provide a wave-absorbing coating composition, a wave-absorbing coating, a wave-absorbing material and a preparation method thereof, so as to solve the problems of low compressive strength retention rate and low shear strength retention rate of an oily honeycomb epoxy resin-based wave-absorbing composite material in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a wave-absorbing coating composition comprising: 60-90 parts by weight of resin component, 10-40 parts by weight of wave absorber, 3-10 parts by weight of curing agent, 10-15 parts by weight of brominated calcium lignin sulfonate, 200 parts by weight of solvent and 4-11 parts by weight of auxiliary agent.
Further, the resin component is selected from one or more of aqueous epoxy resin, aqueous polyurethane resin and aqueous acrylate resin.
Further, the curing agent is selected from one or more of dicyandiamide, m-xylylenediamine, diaminodiphenylmethane and adipic acid dihydrazide.
Further, the wave absorber is selected from any one or more of graphene, multi-wall carbon tubes, single-wall carbon tubes, conductive graphite and carbon black.
Further, the auxiliary agent comprises 1-2 parts by weight of flatting agent, 1-4 parts by weight of defoaming agent and 2-5 parts by weight of dispersing agent, wherein the flatting agent is selected from any one or more of JRC-2420 flatting agent, organosilicon flatting agent Tech-2778, F66 flatting agent and 101 water-based flatting agent, the defoaming agent is selected from any one or more of M5600 defoamer, BASF defoamer M02190, hualae-2330 defoamer, D312 defoamer and Hualae-2330 defoamer, the dispersing agent is selected from any one or more of Greesol DP1060H dispersing agent, DP1020 dispersing agent, dispersing agent-9366, KYC-9201 dispersing agent and GBK-PEI3Y006 dispersing agent, and the solvent is selected from any one or more of water, ethanol and acetone.
According to another aspect of the present invention, there is provided a wave-absorbing coating material prepared by mixing a wave-absorbing coating composition, which is the above-mentioned wave-absorbing coating composition.
According to still another aspect of the present invention, there is provided a method for producing a wave-absorbing material, the method comprising: step S1, adopting wave-absorbing paint to impregnate a honeycomb core material to obtain an impregnated honeycomb core material; and S2, curing the impregnated honeycomb core material to obtain the wave-absorbing material, wherein the wave-absorbing coating is the upper wave-absorbing coating.
Further, the preparation method also comprises a preparation process of the brominated calcium lignin sulfonate, and the preparation process comprises the following steps: substitution reaction of calcium lignosulfonate in sodium hydroxide and/or potassium hydroxide water solution, liquid bromine and 30% hydrogen peroxide water solution to obtain brominated calcium lignosulfonate, wherein the substitution reaction temperature is 70-100 ℃, and the concentration of the sodium hydroxide and/or potassium hydroxide water solution is preferably 0.1-0.2 mol.L -1 。
Further, the curing comprises the steps of raising the temperature of the impregnated honeycomb core material from 25 ℃ to 110-120 ℃ within 1h, preserving heat at 110-120 ℃ for 25-50 min, and then continuing to raise the temperature of the impregnated honeycomb core material to 150-80 ℃ within 1h, preserving heat for 1-2 h to obtain the wave-absorbing material.
According to a further aspect of the present invention there is provided a wave-absorbing material obtainable by the process as hereinbefore described.
By applying the technical scheme of the invention, on one hand, the resin component and the brominated calcium lignosulfonate form a network interpenetrating structure, and on the other hand, the brominated calcium lignosulfonate provides a benzene ring and introduces a strong polar bond C-Br, so that the mechanical property of the wave-absorbing material is improved, and the compressive strength retention rate and the shear strength retention rate of the wave-absorbing material are effectively improved by controlling the introduction amount of the brominated calcium lignosulfonate. Meanwhile, the types and the amounts of other components are beneficial to improving the structure and the crosslinking density of the wave-absorbing coating and the spreading degree and uniformity of the wave-absorbing coating on the honeycomb core material wall, so that the mechanical property of the wave-absorbing material is improved, and the retention rate of the compression strength and the retention rate of the shear strength are further improved.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present invention will be described in detail with reference to examples.
As analyzed by the background art, the oily honeycomb epoxy resin-based wave-absorbing composite material in the prior art has the problems of low compressive strength retention rate and low shear strength retention rate, and in order to solve the problems, the invention provides a wave-absorbing coating composition, a wave-absorbing coating, a wave-absorbing material and a preparation method thereof.
In one exemplary embodiment of the present application, there is provided a wave-absorbing coating composition comprising: 60-90 parts by weight of resin component, 10-40 parts by weight of wave absorber, 3-10 parts by weight of curing agent, 10-15 parts by weight of brominated calcium lignin sulfonate, 200 parts by weight of solvent and 4-11 parts by weight of auxiliary agent.
On one hand, the resin component and the calcium lignosulfonate form a network interpenetrating structure, and the brominated calcium lignosulfonate provides a benzene ring, so that the mechanical property of the wave-absorbing material is improved by adding the brominated calcium lignosulfonate because the benzene ring is a rigid group, and the compressive strength retention rate and the shear strength retention rate of the wave-absorbing material are effectively improved by controlling the introduction amount of the brominated calcium lignosulfonate. On the other hand, the types and the amounts of other components are beneficial to improving the structure and the crosslinking density of the wave-absorbing coating and the spreading degree and the uniformity of the wave-absorbing coating on the honeycomb core material wall, so that the mechanical property of the wave-absorbing material is also improved, and the retention rate of the compression strength and the retention rate of the shear strength are further improved.
In order to improve the film forming property of the resin component, it is preferable that the resin component is selected from one or more of an aqueous epoxy resin, an aqueous urethane resin, and an aqueous acrylate resin.
In order to further improve the mechanical properties, heat resistance and water resistance of the wave-absorbing material and to optimize the curing temperature and crosslinking density of the wave-absorbing material, it is preferable that the curing agent is selected from one or more of dicyandiamide, m-xylylenediamine, diaminodiphenylmethane and adipic dihydrazide, on the basis of ensuring successful curing of the resin component in the wave-absorbing coating composition.
In order to further enhance the wave absorbing effect of the wave absorbing material, the wave absorbing agent is preferably selected from any one or more of graphene, multi-wall carbon tubes, single-wall carbon tubes, conductive graphite and carbon black.
In one embodiment of the present application, the above auxiliary agent comprises 1 to 2 parts by weight of a leveling agent, 1 to 4 parts by weight of a defoaming agent, 2 to 5 parts by weight of a dispersing agent, preferably any one or more of a JRC-2420 leveling agent, a silicone leveling agent Tech-2778, an F66 leveling agent, a 101 aqueous leveling agent, preferably any one or more of a M5600 defoaming agent, a BASF defoaming agent M02190, a Hualae-2330 defoaming agent, a D312 defoaming agent, a Hualae-2330 defoaming agent, preferably any one or more of a greenol DP1060H dispersing agent, a DP1020 dispersing agent, a dispersing agent-9366, a KYC-9201 dispersing agent, a GBK-PEI3Y006 dispersing agent, preferably any one or more of water, ethanol, acetone.
In order to improve the synergistic effect of the components in the wave-absorbing coating composition, it is preferable to add an auxiliary agent into the wave-absorbing coating composition, wherein the addition amount of the dispersing agent influences the dispersion degree of the wave-absorbing agent, so that the dispersing agent can keep a suspension state in slurry for even 72 hours, thereby improving the local uniformity of the wave-absorbing material, and further improving the mechanical property, the compressive strength retention rate and the shear strength retention rate of the wave-absorbing material. The leveling agent influences the spreading degree and uniformity of the wave-absorbing coating on the honeycomb core material wall, so that the mechanical property, the compressive strength retention rate and the shear strength retention rate of the wave-absorbing coating are improved. The defoaming agent eliminates bubbles in the wave-absorbing coating, thereby preventing the occurrence of voids in the wave-absorbing coating and further reducing the probability of weakening the mechanical properties of the wave-absorbing material. Preferably, the solvent further improves the dispersibility of each component in the wave-absorbing coating composition in the solvent.
In another exemplary embodiment of the present application, there is provided a wave-absorbing coating prepared by mixing a wave-absorbing coating composition, which is the wave-absorbing coating composition described above.
The wave-absorbing coating prepared from the wave-absorbing coating composition has excellent mechanical properties, high compressive strength retention and high shear strength retention when being used for wave-absorbing materials.
In yet another exemplary embodiment of the present application, there is provided a method of preparing a wave-absorbing material, the method comprising: step S1, adopting wave-absorbing paint to impregnate a honeycomb core material to obtain an impregnated honeycomb core material; and S2, curing the impregnated honeycomb core material to obtain the wave-absorbing material, wherein the wave-absorbing coating is the wave-absorbing coating.
The wave-absorbing coating is adsorbed on the honeycomb core material by impregnation, and then the wave-absorbing material is obtained by curing. The obtained wave-absorbing material has high compressive strength retention rate and high shear strength retention rate, and the preparation method is simple and has lower preparation cost. The honeycomb core material is aramid honeycomb, and the lattice shape of the honeycomb is regular hexagon.
In order to further improve the preparation efficiency of the wave-absorbing material, the wave-absorbing material is preferably obtained by controlling the following specific parameters: preferably, the curing comprises raising the temperature of the impregnated honeycomb core material from 25 ℃ to 110-120 ℃ within 1h, keeping the temperature at 110-120 ℃ for 25-50 min, and then continuously raising the temperature of the impregnated honeycomb core material to 150-80 ℃ within 1h, keeping the temperature for 1-2 h to obtain the wave-absorbing material. Preferably, the impregnation is performed for a plurality of times, preferably each time, the impregnation is performed for 5-10 min, preferably, the next impregnation is performed after the pre-curing is performed for 30-40 min after each time of impregnation, preferably, the pre-curing is performed to raise the temperature of the impregnated honeycomb core material from 25 ℃ to 120 ℃ within 1h, and the heat is preserved for 30-40 min at 120 ℃ to obtain the impregnated honeycomb core material. Thereby the wave-absorbing coating is fully solidified, and the wave-absorbing material with excellent mechanical property, high compressive strength retention rate and high shear strength retention rate is obtained.
In yet another exemplary embodiment of the present application, a wave-absorbing material is provided, which is obtained by the aforementioned preparation method.
The wave-absorbing material obtained by the preparation method has excellent mechanical property, high compressive strength retention rate and high shear strength retention rate, so that the wave-absorbing material can be widely applied to the field of wave-absorbing materials.
The advantageous effects of the present application will be described below with reference to specific examples and comparative examples.
Preparation of brominated calcium lignosulfonate:
preparation of calcium Lignin sulfonate bromide example 1
Firstly, drying calcium lignosulfonate to absolute dryness at 110 ℃, then weighing the calcium lignosulfonate into a reaction kettle, and adding the calcium lignosulfonate into a reaction kettle according to the mass ratio of 1:20, wherein the molar concentration is 0.1 mol.L -1 Stirring in water bath at 80deg.C until completely dissolved, dropwise adding liquid bromine and 30% hydrogen peroxide water solution for reaction, introducing the mixed solution into isopropanol for precipitation, washing and filtering for three times after the reaction is finished, drying, pulverizing, and sieving to obtain brominated calcium lignin sulfonate powder.
Preparation example 2 of calcium Bromide Lignosulfonate
Firstly, drying calcium lignosulfonate at 110 ℃ to absolute dryness, then weighing the calcium lignosulfonate into a reaction kettle, and adding the molar concentration into the reaction kettle according to the mass ratio of 1:20The degree of the reaction is 0.2 mol.L -1 Stirring in water bath at 70deg.C until completely dissolved, dropwise adding liquid bromine and 30% hydrogen peroxide water solution for reaction, introducing the mixed solution into isopropanol for precipitation, washing and filtering for three times after the reaction is finished, drying, pulverizing, and sieving to obtain brominated calcium lignin sulfonate powder.
Preparation example 3 of calcium Bromide Lignosulfonate
Firstly, drying calcium lignosulfonate to absolute dryness at 110 ℃, then weighing the calcium lignosulfonate to a reaction kettle, and adding the calcium lignosulfonate into a reaction kettle according to the mass ratio of 1:20, wherein the molar concentration is 0.15 mol.L -1 Stirring in water bath at 100deg.C until completely dissolving, dropwise adding liquid bromine and 30% hydrogen peroxide water solution to react, introducing the mixed solution into isopropanol to precipitate, washing and filtering for three times after the reaction is completed, drying, pulverizing, and sieving to obtain brominated calcium lignin sulfonate powder.
The following preparation examples of the wave-absorbing material and the brominated calcium lignin sulfonate used in the comparative examples were brominated calcium lignin sulfonate obtained in any one or more of preparation examples 1 to 3 of brominated calcium lignin sulfonate.
Preparation of the wave-absorbing material:
preparation of wave-absorbing Material example 1
50 parts by weight of NPEW-114 waterborne epoxy resin (Shanxi Aojia building Co., ltd.), 3 parts by weight of M-xylylenediamine, 10 parts by weight of brominated calcium lignin sulfonate, 40 parts by weight of graphene, 5 parts by weight of Greesol DP1060H dispersant, 2 parts by weight of JRC-2420 leveling agent, 4 parts by weight of M5600 defoamer and 200 parts by weight of water were mixed to obtain a wave-absorbing coating.
Soaking the wave-absorbing coating and the hexagonal aramid honeycomb core material for 5 times to obtain the dry densification degree of 52kg/m 3 And (3) soaking for 10min each time, raising the temperature of the soaked material to 120 ℃ from 25 ℃ within 1h after each time of soaking, and pre-curing for 30min at 120 ℃ and then carrying out next soaking to obtain the soaked honeycomb core material. Raising the temperature of the impregnated honeycomb core material from 25 ℃ to 120 ℃ within 1h, and keeping the temperature at 120 ℃ for 30min, and continuing to impregnate the honeybees within 1hAnd heating the nest core material to l80 ℃ and preserving heat for 1.5 hours to obtain the wave-absorbing material.
Preparation of wave-absorbing Material example 2
Preparation of the wave-absorbing material example 2 is different from preparation of the wave-absorbing material example 1 in that,
60 parts by weight of aqueous epoxy resin (NPEW-114 Shanxio auspicious building Co., ltd.), 10 parts by weight of M-xylylenediamine, 15 parts by weight of brominated calcium lignin sulfonate, 10 parts by weight of graphene, 2 parts by weight of Greesol DP1060H dispersant, 1 part by weight of JRC-2420 flatting agent, 1 part by weight of M5600 defoamer and 200 parts by weight of water are mixed to obtain a wave-absorbing coating, and finally the wave-absorbing material is obtained.
Preparation of wave-absorbing Material example 3
Preparation of the wave-absorbing material example 3 is different from preparation of the wave-absorbing material example 1 in that,
90 parts by weight of a water-based epoxy resin (NPEW-114 Shanxio auspicious building Co., ltd.), 5 parts by weight of M-xylylenediamine, 10 parts by weight of brominated calcium lignosulfonate, 25 parts by weight of graphene, 3 parts by weight of Greesol DP1060H dispersant, 1.5 parts by weight of JRC-2420 leveling agent, 2 parts by weight of M5600 defoamer and 200 parts by weight of water are mixed to obtain a wave-absorbing coating, and finally the wave-absorbing material is obtained.
Example 4
Example 4 was different from example 1 in that an aqueous hydroxyacrylate resin WX-3200 (New Material technology Co., ltd., bay of Fleecefield) was used to obtain a wave-absorbing material.
Example 5
Example 5 differs from example 1 in that the curing agent is adipic acid dihydrazide, and the wave-absorbing material is finally obtained.
Example 6
Example 6 differs from example 1 in that the wave-absorbing agent is a multiwall carbon tube, and the wave-absorbing material is finally obtained.
Example 7
Example 7 differs from example 1 in that the solvent is ethanol, and the wave-absorbing material is finally obtained.
Example 8
Example 8 differs from example 1 in that the leveling agent is an F66 leveling agent, the dispersant is a DP1020 dispersant, the defoamer is a D312 defoamer, and finally the wave absorbing material is obtained.
Example 9
Example 9 differs from example 1 in that the impregnated honeycomb core material was raised from 25 ℃ to 110 ℃ within 1h, and after heat preservation at 110 ℃ for 50min, the impregnated honeycomb core material was continued to be raised to 150 ℃ and heat preservation for 1h within 1h, finally the wave-absorbing material was obtained.
Example 10
Example 10 differs from example 1 in that the impregnated honeycomb core material was raised from 25 ℃ to 115 ℃ within 1h, and after heat preservation at 115 ℃ for 25min, the impregnated honeycomb core material was continued to be raised to 170 ℃ and heat preservation for 2h within 1h, finally the wave-absorbing material was obtained.
Example 11
Example 11 differs from example 1 in that the impregnated honeycomb core material was raised from 25 ℃ to 105 ℃ within 1h, and after heat preservation at 105 ℃ for 25min, the impregnated honeycomb core material was continued to be raised to 145 ℃ and heat preservation for 2h within 1h, finally the wave-absorbing material was obtained.
Comparative example 1
Comparative example 1 differs from example 1 in that the brominated calcium lignosulfonate was replaced with calcium lignosulfonate, and finally a wave-absorbing material was obtained.
Comparative example 2
Comparative example 2 is different from example 1 in that 50 parts by weight of NPEW-114 aqueous epoxy resin (auspicious building company of san xi, inc.), 2 parts by weight of M-xylylenediamine, 5 parts by weight of brominated calcium lignosulfonate, 5 parts by weight of graphene, 1 part by weight of greenol DP1060H dispersant, 1 part by weight of JRC-2420 leveling agent, 2 parts by weight of M5600 defoamer and 200 parts by weight of water were mixed, and finally a wave absorbing material was obtained.
The high temperature compression strength retention, the compression strength retention after water resistance, the low temperature compression strength retention, the high temperature shear strength retention of the wave-absorbing materials obtained in examples 1 to 11, comparative example 1, comparative example 2 described above were respectively tested, and the test results are shown in table 1.
Specifically, the stabilized honeycomb cores were tested for room temperature compressive strength and modulus according to test method ASTM C365M-05. Sample standard dimensions 50mm (L) 50mm (W) 12.7mm (T). The stabilized honeycomb compression test specimen was coated with a 0.5mm thick 2024-T3 aluminum sheet with a J-116A (0.2 mm thick) film. The honeycomb cores were tested for compressive strength after 15 minutes incubation at 175 ℃ according to test method ASTM C365. The honeycomb core samples were tested for compressive strength after 24h immersion in water at 23 ℃ according to test method ASTM C365.
The honeycomb core material was tested for L-direction and W-direction normal temperature shear strength and modulus according to test method ASTM C273. The standard dimensions of the test specimens were as follows: the L-direction shear was 150mm (L) ×50mm (W) ×12.7mm (T). The W shear was 150mm (W) 50mm (L) 12.7mm (T). The sample was prepared using J-116A (0.2 mm thick) film. The honeycomb cores were tested for L-direction shear strength at 150℃for 15min in accordance with test method ASTM C365.
TABLE 1
From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:
on one hand, the resin component and the calcium lignosulfonate form a network interpenetrating structure, and the brominated calcium lignosulfonate provides a benzene ring, so that the mechanical property of the wave-absorbing material is improved by adding the brominated calcium lignosulfonate because the benzene ring is a rigid group, and the compressive strength retention rate and the shear strength retention rate of the wave-absorbing material are effectively improved by controlling the introduction amount of the brominated calcium lignosulfonate. On the other hand, the types and the amounts of other components are beneficial to improving the structure and the crosslinking density of the wave-absorbing coating and the spreading degree and the uniformity of the wave-absorbing coating on the honeycomb core material wall, so that the mechanical property of the wave-absorbing material is also improved, and the retention rate of the compression strength and the retention rate of the shear strength are further improved.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A wave absorbing coating composition, characterized in that the wave absorbing coating composition comprises: 60-90 parts by weight of a resin component, 10-40 parts by weight of a wave absorber, 3-10 parts by weight of a curing agent, 10-15 parts by weight of calcium bromolignin sulfonate, 200 parts by weight of a solvent and 4-11 parts by weight of an auxiliary agent;
the resin component and the brominated calcium lignin sulfonate form a network interpenetrating structure;
the curing agent is selected from any one or more of dicyandiamide, m-xylylenediamine, diamine diphenyl methane and adipic acid dihydrazide;
the resin component is selected from any one or more of aqueous epoxy resin, aqueous polyurethane resin and aqueous acrylic resin;
the preparation process of the brominated calcium lignosulfonate comprises the following steps:
carrying out substitution reaction on calcium lignosulfonate in sodium hydroxide and/or potassium hydroxide aqueous solution, liquid bromine and 30% hydrogen peroxide aqueous solution to obtain the brominated calcium lignosulfonate, wherein the temperature of the substitution reaction is 70-100 ℃, and the concentration of the sodium hydroxide and/or potassium hydroxide aqueous solution is 0.1-0.2mol.L -1 。
2. The wave absorbing coating composition of claim 1, wherein the wave absorbing agent is selected from any one or more of graphene, multi-walled carbon tubes, single-walled carbon tubes, conductive graphite, carbon black.
3. The wave-absorbing coating composition according to claim 1, wherein the auxiliary agent comprises 1-2 parts by weight of a leveling agent, 1-4 parts by weight of an antifoaming agent, and 2-5 parts by weight of a dispersing agent.
4. A wave-absorbing coating prepared by mixing a wave-absorbing coating composition, characterized in that the wave-absorbing coating composition is the wave-absorbing coating composition according to any one of claims 1 to 3.
5. A method for preparing a wave-absorbing material, the method comprising:
step S1, adopting wave-absorbing paint to impregnate a honeycomb core material to obtain an impregnated honeycomb core material;
and step S2, curing the impregnated honeycomb core material to obtain a wave-absorbing material, wherein the wave-absorbing coating is the wave-absorbing coating of claim 4.
6. The method according to claim 5, wherein the curing comprises raising the temperature of the impregnated honeycomb core material from 25 ℃ to 110-120 ℃ within 1h, keeping the temperature at 110-120 ℃ for 25-50 min, and then continuing to raise the temperature of the impregnated honeycomb core material to 150-180 ℃ within 1h, keeping the temperature for 1-2 h, so as to obtain the wave-absorbing material.
7. A wave-absorbing material, characterized in that it is obtained by the production method according to claim 5 or 6.
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