CN116925577A - Double-layer coated aluminum silver paste and preparation method thereof - Google Patents
Double-layer coated aluminum silver paste and preparation method thereof Download PDFInfo
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- CN116925577A CN116925577A CN202210335118.4A CN202210335118A CN116925577A CN 116925577 A CN116925577 A CN 116925577A CN 202210335118 A CN202210335118 A CN 202210335118A CN 116925577 A CN116925577 A CN 116925577A
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- Prior art keywords
- silver paste
- aluminum
- paste
- dispersion liquid
- aluminum silver
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- -1 aluminum silver Chemical compound 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 49
- 239000006185 dispersion Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 27
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000012046 mixed solvent Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 15
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000008247 solid mixture Substances 0.000 claims abstract description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 33
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 30
- 239000011248 coating agent Substances 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 17
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical group CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- XFCMNSHQOZQILR-UHFFFAOYSA-N 2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOC(=O)C(C)=C XFCMNSHQOZQILR-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 2
- FQMIAEWUVYWVNB-UHFFFAOYSA-N 3-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OC(C)CCOC(=O)C=C FQMIAEWUVYWVNB-UHFFFAOYSA-N 0.000 claims description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 2
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 claims description 2
- UUPWEGAONCOIFJ-UHFFFAOYSA-N CCCCC(CC)COC(=O)OOC(O)=O Chemical compound CCCCC(CC)COC(=O)OOC(O)=O UUPWEGAONCOIFJ-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- IBIOCBIKMYWYRA-UHFFFAOYSA-N carboxyoxy 2,2-diphenoxyethyl carbonate Chemical compound C1=CC=C(C=C1)OC(COC(=O)OOC(=O)O)OC2=CC=CC=C2 IBIOCBIKMYWYRA-UHFFFAOYSA-N 0.000 claims description 2
- BLCKNMAZFRMCJJ-UHFFFAOYSA-N cyclohexyl cyclohexyloxycarbonyloxy carbonate Chemical compound C1CCCCC1OC(=O)OOC(=O)OC1CCCCC1 BLCKNMAZFRMCJJ-UHFFFAOYSA-N 0.000 claims description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims description 2
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 2
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 33
- 239000000243 solution Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 125000003545 alkoxy group Chemical group 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 229910003849 O-Si Inorganic materials 0.000 description 3
- 229910003872 O—Si Inorganic materials 0.000 description 3
- 229910002808 Si–O–Si Inorganic materials 0.000 description 3
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000003021 water soluble solvent Substances 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
- C09C1/64—Aluminium
- C09C1/648—Aluminium treated with inorganic and organic, e.g. polymeric, compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The application belongs to the technical field of metal pigments, and particularly relates to double-layer coated aluminum silver paste and a preparation method thereof. The method of the application comprises the following steps: mixing and washing oily aluminum paste and an alcohol-water mixed solvent, filtering, and then re-dividing the obtained aluminum paste solid mixture into alcohol-water mixed solvent, and adjusting to be alkaline to obtain aluminum paste dispersion liquid; mixing and reacting the aluminum paste dispersion liquid, tetraethoxysilane and a silane coupling agent, and filtering to obtain a silicon dioxide coated aluminum paste solid; dispersing the silicon dioxide coated aluminum silver paste solid in benzene solvent to obtain silicon dioxide coated aluminum silver paste dispersion liquid; mixing methyl methacrylate, a cross-linking agent and an oil-soluble initiator to obtain a polymethyl methacrylate solution; and mixing the polymethyl methacrylate solution with the silicon oxide coated aluminum silver paste dispersion liquid under the protective atmosphere, heating for reaction, and filtering to obtain the double-layer coated aluminum silver paste. The method of the application can improve the corrosion resistance of the aluminum silver paste in water, and the surface glossiness and the adhesiveness of the aluminum silver paste.
Description
Technical Field
The application belongs to the technical field of metal pigments, and particularly relates to double-layer coated aluminum silver paste and a preparation method thereof.
Background
There are three production modes of aqueous aluminum paste. Firstly, the aluminum powder is directly ground in a ball mill under the action of an antioxidant, a dispersing agent and a water-soluble solvent, and the cost is low, but the effect is general, the corrosion resistance is poor and the aluminum powder is unstable. Secondly, the oily aluminum paste is used for replacement, the solvent oil is replaced by a high-boiling point water-soluble solvent in a distillation mode, and meanwhile, a dispersing agent and an antioxidant are added, so that a good metal appearance effect can be obtained, but the corrosion resistance is relatively poor, the stability is poor, and the universality is poor.
In order to meet the needs of aqueous systems, to prevent corrosion of the aluminum silver paste surface, it is necessary to modify the surface. For example, a dense film is coated on the surface of an aluminum sheet by using a conventional coating substance to prevent the aluminum sheet from corroding, but the conventional coating substance has the problems that the glossiness and the hiding power of the aluminum silver paste are reduced or the compatibility of the aluminum silver paste with resin is poor, and the adhesive force of the coated aluminum silver paste is reduced.
Disclosure of Invention
In order to solve the defect of the existing coated aluminum silver paste, the application provides a SiO 2 A preparation method of PMMA double-layer coated aluminum silver paste. In SiO 2 The silane coupling agent containing silicon oxygen group and vinyl group is introduced into the layer, alkoxy can be subjected to hydrolysis reaction, and is condensed with hydroxyl groups on the surface of metal aluminum to form an Al-O-Si covalent bond, and meanwhile, the alkoxy can be condensed with silanol after hydrolysis of tetraethoxysilane to form an Si-O-Si covalent bond. The vinyl group can be polymerized with the carbon-carbon double bond of MMA. Thus, the inorganic metal aluminum/SiO can be used 2 The layers/PMMA layers are tightly connected by chemical bonds.
The application provides a preparation method of double-layer coated aluminum silver paste, which comprises the following steps:
step 1, mixing and washing oily aluminum paste and an alcohol-water mixed solvent, removing the alcohol-water mixed solvent, and then re-dividing the obtained aluminum paste solid mixture into the alcohol-water mixed solvent, and adjusting pH to be alkaline to obtain an aluminum paste dispersion liquid;
step 2, mixing the aluminum silver paste dispersion liquid, ethyl orthosilicate and a silane coupling agent for reaction, and filtering to obtain SiO 2 Coating aluminum silver paste solids;
step 3, the SiO is processed 2 Dispersing the coated aluminum silver paste solid in benzene solvent to obtain SiO 2 Coating aluminum silver paste dispersion liquid;
mixing and dissolving methyl methacrylate, a cross-linking agent and an oil-soluble initiator to obtain a polymethyl methacrylate solution;
step 4, in the protective gasUnder the atmosphere, the polymethyl methacrylate solution and the SiO 2 Mixing the coated aluminum silver paste dispersion liquid, heating for reaction, and filtering to obtain the double-layer coated aluminum silver paste.
In another embodiment, in step 1, the alcohol of the alcohol-water mixed solvent is selected from one or more of methanol, ethanol, isopropanol and n-butanol, preferably isopropanol; the mass ratio of the alcohol-water mixed solvent to the water of the alcohol-water mixed solvent is (1-3) 1; the mass of the alcohol-water mixed solvent is 5-10 times of the mass of the oily aluminum silver paste.
In another embodiment, in the step 1, adjusting the pH to 8-10 by adopting alkali liquor, wherein the alkali liquor is one or more selected from ammonia water, sodium hydroxide aqueous solution, potassium hydroxide aqueous solution and sodium carbonate aqueous solution; preferably, the pH value is 8, and the alkali liquor is ammonia water.
In another embodiment, in step 2, the silane coupling agent is 3-methacryloxypropyl trimethoxysilane.
Specifically, in the step 3, the dosage of the oil-soluble initiator is 0.5% -1% of the total mass of the methyl methacrylate monomer.
In another embodiment, in step 3, the benzene solvent is selected from one or more of benzene, toluene, and xylene, preferably toluene; the mass of the benzene solvent is the SiO 2 5 to 10 times of the solid mass of the coated aluminum paste.
In another embodiment, in step 3, the cross-linking agent is selected from one or more of allyl methacrylate, trimethylolpropane triacrylate, triallyl isocyanurate, 1, 3-butanediol diacrylate, 1, 4-butanediol diacrylate, ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, preferably trimethylolpropane triacrylate.
In another embodiment, in step 3, the oil-soluble initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dibenzoyl peroxide, 2-ethylhexyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, diphenyloxyethyl peroxydicarbonate, bis (3, 5-trimethylacetyl) peroxide and cumyl peroxyneodecanoate, preferably azobisisobutyronitrile and dibenzoyl peroxide.
In another embodiment, the addition amount of the tetraethoxysilane is 10% -50% of the mass of the aluminum silver paste dispersion liquid; the addition amount of the silane coupling agent is 10-50% of the mass of the aluminum silver paste dispersion liquid.
In another embodiment, the addition amount of the methyl methacrylate is 5-35% of the mass of the SiO2 coated aluminum paste dispersion liquid, preferably 15-25%; the addition amount of the cross-linking agent is 0.5-1.5% of the mass of the methyl methacrylate monomer, and is preferably 0.8-1%.
In another embodiment, step 2 specifically includes: the ethyl orthosilicate and the silane coupling agent are mixed and then added into the aluminum silver paste dispersion liquid in a dropwise manner for mixed reaction, wherein the dropwise addition time is 2-6 h, the dropwise addition mixing temperature is 30-60 ℃, the mixing reaction temperature is 2-6 h, and the heat preservation temperature is 30-60 ℃.
In another embodiment, step 4 specifically includes: dropping the polymethyl methacrylate solution into the SiO under a protective atmosphere 2 Mixing the aluminum-coated silver paste dispersion liquid, and then heating for reaction; the dripping time is 1-5 h, and the dripping temperature is 60-80 ℃; the heat preservation temperature of the heating reaction is 80-90 ℃, and the heating reaction time is 2-5 h.
The second aspect of the application provides double-layer coated aluminum silver paste, which comprises the double-layer coated aluminum silver paste prepared by the preparation method.
Step 1 and step 2 are specifically inorganic SiO 2 The coating of the layer specifically comprises:
dispersing oily aluminum paste in an alcohol-water mixed solvent, uniformly stirring, carrying out suction filtration and separation on the obtained mixture, and removing the solvent to obtain a solid mixture. And dispersing the solid mixture in an alcohol-water mixed solvent again, and regulating the pH value of the system to 8 by using ammonia water to obtain an aluminum silver paste dispersion liquid. Uniformly mixing tetraethoxysilane and 3-methacryloxypropyl trimethoxysilane, then dripping the mixture into the aluminum silver paste dispersion for 2 to 6 hours, and dripping the mixture reverselyThe temperature should be kept between 30 and 60 ℃. After the dripping is finished, preserving heat for 2-6 h, and preserving heat at 30-60 ℃. Filtering after the reaction is finished, removing the solvent, and obtaining a filter cake which is SiO 2 Coating aluminum silver paste solid.
Step 3 and step 4 are specifically coating of an organic PMMA layer, specifically including:
SiO obtained in the step 2 is processed 2 Dispersing the coated aluminum silver paste solid in benzene solvent, stirring and dispersing uniformly to obtain SiO 2 Coating aluminum silver paste dispersion liquid. Introducing nitrogen and heating to 60-80 ℃. And mixing and dissolving methyl methacrylate, a cross-linking agent and an oil-soluble initiator to obtain a polymethyl methacrylate solution. The polymethyl methacrylate solution is then added dropwise to SiO 2 And (3) dropwise adding the aluminum paste into the aluminum paste coating dispersion liquid for 1-5 h, and keeping the temperature at 60-80 ℃. After the dripping is finished, the temperature is raised to 80-90 ℃ and the reaction is continued for 2-5 h. After the reaction is finished, cooling to room temperature, filtering to obtain SiO 2 And (3) preparing the PMMA double-layer coated aluminum silver paste, namely the double-layer coated aluminum silver paste.
In the prior art, siO is carried out on oily aluminum silver paste 2 Single layer cladding, although enhancing corrosion resistance, is due to SiO 2 The surface of the aluminum sheet is granular, so that the light is scattered, and the glossiness of the aluminum silver paste is obviously reduced; the oily aluminum paste is coated with polystyrene resin, the binding force between the polystyrene and the aluminum powder is very weak, the resin easily falls off from the surface of the aluminum powder under the action of high shear, and the protection effect on the aluminum powder is lost. In addition, the grain diameter of the aluminum powder is relatively large, and the conversion rate of in-situ polymerization monomers taking the aluminum powder as a matrix and the resin coating rate are not too high.
Based on the defects, the application provides a SiO 2 A preparation method of PMMA double-layer coated aluminum silver paste. In SiO 2 The silane coupling agent containing silicon oxygen group and vinyl group is introduced into the layer, alkoxy can be subjected to hydrolysis reaction, and is condensed with hydroxyl groups on the surface of metal aluminum to form an Al-O-Si covalent bond, and meanwhile, the alkoxy can be condensed with silanol after hydrolysis of tetraethoxysilane to form an Si-O-Si covalent bond. The vinyl group can be polymerized with the carbon-carbon double bond of MMA. Thus, the inorganic metal aluminum/SiO can be used 2 layer/PMMA layer is bonded by chemical bondIs tightly connected by the way of (a).
Detailed Description
The application provides double-layer coated aluminum-silver paste and a preparation method thereof, which are used for solving the technical defects that the glossiness and covering power of the aluminum-silver paste or the compatibility of the aluminum-silver paste with resin are reduced and the adhesive force of the coated aluminum-silver paste is reduced when the aluminum-silver paste is coated by conventional coating substances in the prior art.
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Wherein, the raw materials or reagents used in the following examples are all commercially available or self-made.
The test of each physical property in the embodiment of the application is carried out by the following method:
(1) Corrosion resistance test
Testing corrosion resistance of modified aluminum silver paste in alkaline system, adding 1g of SiO respectively into 250ml flask 2 The PMMA double-layer coated aluminum paste sample and 200g of sodium hydroxide solution with the concentration of 0.01mol/L are uniformly stirred, and the released hydrogen is collected by a glass tube with scales, and the test time is 1 week.
(2) Gloss test
1g of SiO is taken 2 1g of toluene solvent and 10g of acrylic resin are added into a PMMA double-layer coated aluminum silver paste sample, and the mixture is stirred uniformly. Then, a 50 μm bar was used to uniformly scrape the coating film on a special iron plate, and after drying, the gloss data of the coating film at 60℃was measured with a gloss meter.
(3) Adhesion test
1g of SiO is taken 2 1g of toluene solvent and 10g of acrylic resin are added into a PMMA double-layer coated aluminum silver paste sample, and the mixture is stirred uniformly. Then the steel plate is uniformly coated and scraped on a special iron plate through a 50 mu m wire rod, and after drying, the steel plate is subjected to a cross-cut test of paint films according to national standard GB/T9286-1998And (3) carrying out paint film adhesion test, wherein the test result is in 0-5 grades, the 0 grade is the best, and the 5 grade is the worst.
Example 1
The embodiment of the application provides double-layer coated aluminum silver paste, which comprises the following specific preparation methods:
into a four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 50g of oily aluminum paste was added. After adding 300g of a mixed solvent of isopropyl alcohol and water (200 g of isopropyl alcohol, 100g of water), stirring at room temperature for 1h, separating the obtained mixture by suction filtration, and removing the solvent to obtain an aluminum silver paste solid mixture. The obtained aluminum paste solid mixture system was redispersed in 300g of an alcohol-water solvent (200 g of isopropyl alcohol, 100g of water), and the pH of the system was adjusted to 8 with ammonia water to obtain an aluminum paste dispersion. 12.5g of tetraethoxysilane and 12.5g of 3-methacryloxypropyl trimethoxysilane are weighed and added into the aluminum silver paste dispersion liquid dropwise after being uniformly mixed, the dropwise adding time is 4 hours, and the dropwise adding temperature is kept at 50 ℃. After the dripping is finished, the temperature is kept for 4 hours, and the temperature is kept at 60 ℃. Filtering after the reaction is finished, removing the solvent, and obtaining a filter cake which is SiO 2 Coating aluminum silver paste solid.
The SiO obtained above was charged into a four-necked flask equipped with a stirrer, a thermometer and a reflux condenser 2 50g of coated aluminum silver paste solid, 300g of toluene is added, and the mixture is stirred and dispersed uniformly to obtain SiO 2 Coating aluminum silver paste dispersion liquid. 15g of methyl methacrylate, 0.075g of azobisisobutyronitrile, 0.03g of dibenzoyl peroxide and 0.075g of trimethylolpropane triacrylate were uniformly mixed to obtain a polymethyl methacrylate solution. Dropping the polymethyl methacrylate solution into a solution containing SiO 2 In a flask coated with the aluminum paste dispersion liquid, the dripping time is 4 hours, the dripping temperature is 68 ℃, and the stirring state is kept all the time in the dripping process. And after the dripping is finished, curing the polymer by adopting a gradual heating mode, heating to 75 ℃ and preserving heat for 1h, heating to 80 ℃ and preserving heat for 1h, heating to 85 ℃ and preserving heat for 1h, and finally heating to 90 ℃ and preserving heat for 1h. Cooling to room temperature after the reaction is finished, and filtering the product to obtain double-layer coated aluminum silver paste which is SiO 2 PMMA double-layer cladding aluminum silver paste.
Comparative example 1
This application disclosesThe comparative example provides coating of only one layer of SiO 2 The specific preparation method of the aluminum silver paste comprises the following steps:
into a four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 50g of oily aluminum paste was added. After adding 300g of a mixed solvent of isopropyl alcohol and water (200 g of isopropyl alcohol, 100g of water), stirring at room temperature for 1h, separating the obtained mixture by suction filtration, and removing the solvent to obtain an aluminum silver paste solid mixture. The obtained aluminum paste solid mixture was redispersed in 300g of an alcohol-water solvent (200 g of isopropyl alcohol, 100g of water), and the pH of the aluminum paste solid mixture system was adjusted to 8 with ammonia water to obtain an aluminum paste dispersion. 12.5g of tetraethoxysilane and 12.5g of 3-methacryloxypropyl trimethoxysilane are weighed and added into the aluminum silver paste dispersion liquid dropwise after being uniformly mixed, the dropwise adding time is 4 hours, and the dropwise adding temperature is kept at 50 ℃. After the dripping is finished, the temperature is kept for 4 hours, and the temperature is kept at 60 ℃. Filtering after the reaction is finished, removing the solvent, and obtaining a filter cake which is SiO 2 Coating aluminum silver paste solid, dispersing to obtain SiO 2 Coating aluminum silver paste.
Comparative example 2
The application provides an aluminum silver paste without adding 3-methacryloxypropyl trimethoxysilane, and the specific preparation method comprises the following steps:
into a four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 50g of oily aluminum paste was added. After adding 300g of a mixed solvent of isopropyl alcohol and water (200 g of isopropyl alcohol, 100g of water), stirring at room temperature for 1h, separating the obtained mixture by suction filtration, and removing the solvent to obtain an aluminum silver paste solid mixture. The obtained aluminum paste solid mixture was redispersed in 300g of an alcohol-water solvent (200 g of isopropyl alcohol, 100g of water), and the pH of the aluminum paste solid mixture system was adjusted to 8 with ammonia water to obtain an aluminum paste dispersion. 25g of ethyl orthosilicate is weighed and added into the aluminum silver paste dispersion liquid dropwise for 4 hours, and the temperature of the dropwise is kept at 50 ℃. After the dripping is finished, the temperature is kept for 4 hours, and the temperature is kept at 60 ℃. Filtering after the reaction is finished, removing the solvent, and obtaining a filter cake which is SiO without adding 3-methacryloxypropyl trimethoxy silane 2 Coating aluminum silver paste solid.
Four with stirring paddles, thermometer and reflux condenserThe prepared SiO without 3-methacryloxypropyl trimethoxysilane was added to a flask 2 50g of coated aluminum silver paste solid, 300g of toluene is added, and the mixture is stirred and dispersed uniformly. 15g of methyl methacrylate, 0.075g of azobisisobutyronitrile, 0.03g of dibenzoyl peroxide and 0.075g of trimethylolpropane triacrylate are weighed and uniformly mixed to obtain a polymethyl methacrylate solution. Dropping the polymethyl methacrylate solution into a solution containing SiO 2 In a coated aluminum silver paste dispersion liquid flask, dropwise adding is carried out for 4 hours, the dropwise adding temperature is 68 ℃, and the stirring state is kept all the time in the dropwise adding process. And after the dripping is finished, curing the polymer by adopting a gradual heating mode, heating to 75 ℃ and preserving heat for 1h, heating to 80 ℃ and preserving heat for 1h, heating to 85 ℃ and preserving heat for 1h, and finally heating to 90 ℃ and preserving heat for 1h. Cooling to room temperature after the reaction is finished, and filtering the product to obtain SiO 2 PMMA double-layer cladding aluminum silver paste.
The corrosion resistance, gloss and adhesion tests were carried out on the non-coated modified aluminum silver pastes of example 1, comparative examples 1 to 2 (i.e., commercially available oily aluminum silver pastes), and the test results are shown in the following table
TABLE 1
| Numbering device | Alkali corrosion hydrogen evolution amount/ml | Gloss level | Adhesion force |
| Example 1 | 4 | 85 | 0 |
| Comparative example 1 | 45 | 80 | 1 |
| Comparative example 2 | 20 | 84 | 2 |
| Unmodified aluminum silver paste | 200 | 88 | 3 |
From the above experimental results, example 1 has SiO 2 The PMMA double-layer coated aluminum silver paste has the best comprehensive performance, and only has one SiO layer 2 Comparative example 1 coated with SiO on the surface layer 2 The particles have a scattering effect on light, so that the glossiness is the worst. The aluminum surface is coated with a single layer of inorganic coating, and the corrosion resistance and glossiness obtained are limited because of SiO 2 The surface of the aluminum sheet is granular and has a scattering effect on light. Comparative example 2 has no 3-methacryloxypropyl trimethoxysilane, and therefore, the layers are simply coated and are not bonded together by chemical bonds, resulting in unsatisfactory adhesion. The unmodified aluminum paste has no polymer coating on the surface, so that the corrosion resistance is the worst under alkaline conditions.
In summary, the application is described in SiO 2 The silane coupling agent containing silicon oxygen group and vinyl group is introduced into the layer, alkoxy can be subjected to hydrolysis reaction, and is condensed with hydroxyl groups on the surface of metal aluminum to form an Al-O-Si covalent bond, and meanwhile, the alkoxy can be condensed with silanol after hydrolysis of tetraethoxysilane to form an Si-O-Si covalent bond. The vinyl group can be polymerized with the carbon-carbon double bond of MMA. Thus, the inorganic metal aluminum/SiO can be used 2 The layers/PMMA layers are tightly connected by chemical bonds.
The foregoing is merely a preferred embodiment of the present application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present application, which are intended to be comprehended within the scope of the present application.
Claims (10)
1. The preparation method of the double-layer coated aluminum paste is characterized by comprising the following steps of:
step 1, mixing and washing oily aluminum paste and an alcohol-water mixed solvent, removing the alcohol-water mixed solvent, and then re-dividing the obtained aluminum paste solid mixture into the alcohol-water mixed solvent, and adjusting pH to be alkaline to obtain an aluminum paste dispersion liquid;
step 2, mixing the aluminum silver paste dispersion liquid, ethyl orthosilicate and a silane coupling agent for reaction, and filtering to obtain SiO 2 Coating aluminum silver paste solids;
step 3, the SiO is processed 2 Dispersing the coated aluminum silver paste solid in benzene solvent to obtain SiO 2 Coating aluminum silver paste dispersion liquid;
mixing and dissolving methyl methacrylate, a cross-linking agent and an oil-soluble initiator to obtain a polymethyl methacrylate solution;
step 4, under a protective atmosphere, the polymethyl methacrylate solution and the SiO are mixed 2 Mixing the coated aluminum silver paste dispersion liquid, heating for reaction, and filtering to obtain the double-layer coated aluminum silver paste.
2. The method according to claim 1, wherein in step 1, the alcohol of the alcohol-water mixed solvent is selected from one or more of methanol, ethanol, isopropanol and n-butanol; the mass ratio of the alcohol-water mixed solvent to the water of the alcohol-water mixed solvent is (1-3) 1; the mass of the alcohol-water mixed solvent is 5-10 times of the mass of the oily aluminum silver paste.
3. The preparation method according to claim 1, wherein in step 1, the pH is adjusted to 8 to 10 with an alkali solution selected from one or more of aqueous ammonia, aqueous sodium hydroxide solution, aqueous potassium hydroxide solution and aqueous sodium carbonate solution.
4. The method according to claim 1, wherein in step 2, the silane coupling agent is 3-methacryloxypropyl trimethoxysilane.
5. The preparation method according to claim 1, wherein in the step 3, the benzene solvent is selected from one or more of benzene, toluene and xylene; the mass of the benzene solvent is the SiO 2 5 to 10 times of the solid mass of the coated aluminum paste.
6. The preparation method according to claim 1, wherein in the step 3, the crosslinking agent is selected from one or more of allyl methacrylate, trimethylolpropane triacrylate, triallyl isocyanurate, 1, 3-butanediol diacrylate, 1, 4-butanediol diacrylate, ethylene glycol dimethacrylate and diethylene glycol dimethacrylate; the oil-soluble initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, dibenzoyl peroxide, 2-ethylhexyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, diphenyloxyethyl peroxydicarbonate, bis (3, 5-trimethylacetyl) peroxide and cumyl peroxyneodecanoate.
7. The preparation method according to claim 1, wherein the addition amount of the tetraethoxysilane is 10% -50% of the mass of the aluminum silver paste dispersion; the addition amount of the silane coupling agent is 10-50% of the mass of the aluminum silver paste dispersion liquid; the addition amount of the methyl methacrylate is the SiO 2 5 to 35 percent of the mass of the dispersion liquid of the coated aluminum silver paste; the addition amount of the cross-linking agent is 0.5-1.5% of the mass of the methyl methacrylate monomer.
8. The preparation method according to claim 1, wherein step 2 specifically comprises: the ethyl orthosilicate and the silane coupling agent are mixed and then added into the aluminum silver paste dispersion liquid in a dropwise manner for mixed reaction, wherein the dropwise addition time is 2-6 h, the dropwise addition mixing temperature is 30-60 ℃, the mixing reaction temperature is 2-6 h, and the heat preservation temperature is 30-60 ℃.
9. The preparation method according to claim 1, wherein the step 4 specifically comprises: dropping the polymethyl methacrylate solution into the SiO under a protective atmosphere 2 Mixing the aluminum-coated silver paste dispersion liquid, and then heating for reaction; the dripping time is 1-5 h, and the dripping temperature is 60-80 ℃; the heat preservation temperature of the heating reaction is 80-90 ℃, and the heating reaction time is 2-5 h.
10. A double-layer coated aluminum paste, characterized by comprising the double-layer coated aluminum paste produced by the production method according to any one of claims 1 to 9.
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