CN117487490B - Waterproof weather-proof electronic epoxy pouring sealant and preparation method thereof - Google Patents
Waterproof weather-proof electronic epoxy pouring sealant and preparation method thereof Download PDFInfo
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- 239000000565 sealant Substances 0.000 title claims abstract description 60
- 239000004593 Epoxy Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000000843 powder Substances 0.000 claims abstract description 90
- 239000010445 mica Substances 0.000 claims abstract description 75
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 75
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003822 epoxy resin Substances 0.000 claims abstract description 27
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010453 quartz Substances 0.000 claims abstract description 13
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims abstract description 11
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 10
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 16
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- VCUDBOXVJZSMOK-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecane-1-thiol Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)S VCUDBOXVJZSMOK-UHFFFAOYSA-N 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 9
- 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 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 9
- 244000028419 Styrax benzoin Species 0.000 claims description 8
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 8
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 8
- 229960002130 benzoin Drugs 0.000 claims description 8
- 235000019382 gum benzoic Nutrition 0.000 claims description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000011532 electronic conductor Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 239000000945 filler Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 239000003085 diluting agent Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000012790 adhesive layer Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- MCTWTZJPVLRJOU-UHFFFAOYSA-O 1-methylimidazole Chemical compound CN1C=C[NH+]=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-O 0.000 description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical class N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- 239000012776 electronic material Substances 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000005028 tinplate Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 125000005073 adamantyl group Chemical group C12(CC3CC(CC(C1)C3)C2)* 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a waterproof weather-proof electronic epoxy pouring sealant, which comprises a component A and a component B; the component A is prepared from the following raw materials in parts by weight: 50-80 parts of epoxy resin, 6-10 parts of polypropylene glycol diglycidyl ether, 25-40 parts of modified alumina, 15-40 parts of modified mica powder and 5-15 parts of quartz powder; the component B is prepared from the following raw materials in parts by weight: 60-80 parts of methyl tetrahydrophthalic anhydride and 0.1-1 part of 2-methylimidazole; the prepared electronic epoxy pouring sealant is suitable for pouring and sealing non-precision electronic devices such as LEDs, transformers, industrial electronics, controllers and power modules, can improve the water-proof and moisture-proof properties, corrosion resistance, weather resistance and impact resistance of downstream customer electronic conductor products, and can improve the comprehensive service life of products.
Description
Technical Field
The invention relates to the field of pouring sealants, in particular to a waterproof weather-proof electronic epoxy pouring sealant and a preparation method thereof.
Background
The encapsulation is to fill jelly into devices with electronic elements and circuits in an artificial or mechanical mode, and solidify the jelly at room temperature or under the condition of heating, so that the thermosetting polymer insulating material with excellent performance is finally obtained. The purpose of encapsulation is mainly to strengthen the integrality of electronic devices, improve the waterproof dustproof performance of devices, improve the resistance of devices to incoming impact and vibration simultaneously, and can also achieve the purpose of confidentiality. Along with the rapid development of the electronic industry, the use amount of the pouring sealant is larger and larger, and the epoxy resin pouring sealant is widely used due to the advantages of excellent performance, simple process and the like.
The epoxy pouring sealant can be classified into a general pouring sealant, a heat-resistant pouring sealant, an impact-resistant pouring sealant and the like according to the performance classification. The pouring sealant for electronic encapsulation mainly adopts room-temperature curing and medium-temperature curing pouring sealant according to special requirements in the aspect of application of electronic devices, wherein the room-temperature curing type refers to that the curing agent contained in the pouring sealant can be cured and crosslinked at room temperature to form a hardened substance, and the pouring sealant has the advantages that no heating equipment is needed, the operation is simple during curing, but the use is not very convenient, the pouring sealant generally needs to be prepared at present, and the application is limited by a certain period of time, and can be classified into single-component glue, double-component glue, multi-component glue and the like according to the packaging form.
The epoxy pouring sealant comprises a main body part and an additive part, wherein the main body part comprises epoxy resin and a curing agent. The additive part is mainly added according to different performance requirements and mainly comprises diluents, fillers, pigments and the like.
Epoxy resin is the most basic component in pouring sealant, has a plurality of types, and can be selected according to different viscosity and performance requirements. It must have a low chloride ion content to reduce its candles to electronic devices, and at the same time it must have a high deformation temperature, good heat and chemical resistance. When in use, a single epoxy resin can be selected, and a mixture of several epoxy resins can be used.
The curing agent is an indispensable main body part in the pouring sealant formula, and the thermoplastic epoxy resin can be cured and crosslinked into a net structure to form insoluble and infusible macromolecules only after the curing agent is added into the epoxy resin, so that various different performances can be shown. The curing agent is various, the selection of the curing agent is required to be determined according to specific application, the curing agent for electronic encapsulation generally needs to be a room temperature curing agent or a medium temperature curing agent, and if the single-component pouring sealant is prepared, the latent curing agent needs to be used.
The diluent mainly has the function of reducing the viscosity of the whole component, and more filler can be used by adding the diluent, so that the shrinkage is reduced, and the aims of improving the performance and reducing the cost are fulfilled.
The filler is completely different from the epoxy resin in structure, so that the physical properties of the epoxy resin condensate, such as reducing the shrinkage rate of the condensate, reducing the thermal expansion coefficient of the epoxy resin, changing the electrical property and heat transfer property of the condensate, and the like, can be improved, and the addition of the filler can also reduce the cost. The filler commonly used in epoxy resins is mainly silica micropowder, alumina, calcium carbonate, some metal powders, etc.
The chinese patent document cn202310860046.X discloses a multi-component pouring sealant comprising bisphenol a type epoxy resin, modified boron nitride, filler, modified polyether curing agent, diluent, defoamer and curing agent, wherein the modified boron nitride is a grafting compound of hexagonal boron nitride and epoxidized soybean oil, and the modified polyether curing agent is prepared by introducing tertiary amine and adamantyl groups into an allyl polyether structure, and a manufacturing process thereof.
With the rapid development of the electronic industry, the performance requirements of the pouring sealant are higher and higher at present, and the performance of the traditional pouring sealant can not meet the requirements of the electronic conductor product on water resistance, moisture resistance, corrosion resistance and high weather resistance.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide the waterproof weather-resistant electronic epoxy pouring sealant and the preparation method thereof, and the prepared electronic epoxy pouring sealant is suitable for pouring and sealing of non-precision electronic devices such as LEDs, transformers, industrial electronics, controllers, power modules and the like, and can improve the waterproof moisture resistance, the corrosion resistance, the weather resistance and the impact resistance of electronic conductor products of downstream clients and prolong the comprehensive service life of products.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A waterproof weather-proof electronic epoxy pouring sealant comprises a component A and a component B; the component A is prepared from the following raw materials in parts by weight: 50-80 parts of epoxy resin, 6-10 parts of polypropylene glycol diglycidyl ether, 25-40 parts of modified alumina, 15-40 parts of modified mica powder and 5-15 parts of quartz powder; the component B is prepared from the following raw materials in parts by weight: 60-80 parts of methyl tetrahydrophthalic anhydride and 0.1-1 part of 2-methylimidazole.
Preferably, the preparation method of the modified mica powder comprises the following steps:
(1) Adding A171 into ethanol, regulating pH with hydrochloric acid solution, adding mica powder, stirring for reaction, filtering, washing and drying the product to obtain pretreated mica powder;
(2) Adding the pretreated mica powder into toluene, simultaneously adding octavinyl POSS and benzoyl peroxide, stirring for reaction, and filtering, washing and drying the product to obtain POSS grafted mica powder;
(3) Dispersing POSS grafted mica powder into toluene, dissolving perfluorodecanethiol into methanol, mixing the two mixed solutions, adding benzoin dimethyl ether, continuously introducing N 2, stirring for reaction under the condition of ultraviolet irradiation, steaming the product to obtain solid, washing with acetone, and freeze-drying to obtain the modified mica powder.
Preferably, in the step (1), the weight ratio of the mica powder to the A171 to the ethanol is 10:0.5 to 1:60 to 80 percent.
Preferably, in the step (1), the mass fraction of the hydrochloric acid solution is 10-20%, the pH is adjusted to 3-6, and the stirring reaction condition is that the stirring reaction is carried out for 1-3 hours at 60-80 ℃.
Preferably, in the step (2), the weight ratio of the pretreated mica powder to toluene to octavinyl POSS to benzoyl peroxide is 10: 50-80: 1.2 to 6.8:0.02 to 0.05.
Preferably, in the step (2), the stirring reaction condition is that the reaction is carried out for 3 to 6 hours at 70 to 90 ℃, and the drying condition is that the reaction is carried out for 0.5 to 2 hours at 110 to 130 ℃.
Preferably, in the step (3), the weight ratio of POSS grafted mica powder to perfluorodecanethiol to benzoin dimethyl ether is 10:4.3 to 8.7: 0.02-0.05, and stirring and reacting for 4-8 h.
Preferably, the preparation method of the modified alumina comprises the following steps: preparing 3-glycidoxypropyl triethoxysilane, deionized water and ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing, adding alumina into the mixed solution, stirring for reaction, and filtering, washing and drying the product to obtain the modified alumina.
Preferably, the weight ratio of the 3-glycidoxypropyl triethoxysilane, deionized water, ethanol and alumina is 5-10: 5-10: 80-90: 10; the sealed hydrolysis time is 2-3 h, and the alumina is added into the mixed solution and stirred for reaction for 1-3 h.
The invention also claims a preparation method of the waterproof weather-proof electronic epoxy pouring sealant, which comprises the following steps: uniformly mixing epoxy resin, polypropylene glycol diglycidyl ether, modified alumina, modified mica powder and quartz powder to obtain a component A; and uniformly mixing methyl tetrahydrophthalic anhydride and 2-methylimidazole to obtain a component B.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention provides a waterproof weather-proof electronic epoxy pouring sealant, which is prepared by taking epoxy resin as a base adhesive, polypropylene glycol diglycidyl ether as a diluent, modified alumina, modified mica powder and quartz powder as inorganic fillers to obtain a component A, taking methyl tetrahydrophthalic anhydride as a curing agent and 2-methylimidazole as a curing accelerator to obtain a component B; the prepared electronic epoxy pouring sealant is suitable for pouring and sealing non-precision electronic devices such as LEDs, transformers, industrial electronics, controllers and power modules, can improve the water-proof and moisture-proof properties, corrosion resistance, weather resistance and impact resistance of downstream customer electronic conductor products, and can improve the comprehensive service life of products.
2) The invention provides a waterproof weather-proof electronic epoxy pouring sealant, wherein the added inorganic filler is modified mica powder, quartz powder and modified alumina, the particle size distribution of the selected inorganic filler is wider, the mosaic structure among the powder is more perfect, the integrity of the flaky structure of mica is higher, and the inside of the pouring sealant is provided with a better physical shielding and isolating effect after solidification, so that the shielding and isolating effect of the electronic material after pouring is obviously improved, and the waterproof and dampproof capabilities of the electronic material after pouring are improved; the gaps among the powder bodies with different particle diameters are smaller, so that a more complete heat conduction channel can be formed, and the solidification heat conduction efficiency of the pouring sealant is improved; meanwhile, the special flake structure of the mica can also play a role in resisting ultraviolet aging, so that the short plate with poor weather resistance of the epoxy resin is reinforced, and the whole service life of the encapsulated electronic material is prolonged.
3) The invention provides modified mica powder, which is prepared by firstly using a silane coupling agent A171 to modify the mica powder, consuming hydrophilic hydroxyl on the surface of the powder, introducing double bonds on the surface of the mica powder, then using benzoyl peroxide as an initiator to enable octavinyl POSS to react with vinyl on the surface of the pretreated mica powder to realize surface graft polymerization, obtaining POSS grafted mica powder, and finally using benzoin dimethyl ether as a photoinitiator to enable perfluoro decanethiol to react with POSS grafted mica powder to generate mercapto-alkene under the irradiation of inert atmosphere and ultraviolet light to obtain modified mica powder; because a large number of nonpolar groups are introduced on the surface of the mica powder, the surface of the mica powder has lipophilicity, so that the mica powder is more uniformly dispersed in an epoxy pouring sealant system, the addition amount of the filler can be increased, and the heat conductivity coefficient of a product can be improved; through grafting POSS on the surface of mica powder, the silicon-oxygen bond on the cage-type silsesquioxane can form a hydrogen bond effect with O atoms in the epoxy resin, so that the precipitation of modified mica powder is reduced, the bonding and fixing effect of filler particles is improved, and the introduction of organosilicon can also effectively improve the heat resistance, weather resistance and mechanical property of pouring sealant after curing and forming; the perfluorodecanethiol also introduces the fluorocarbon chain segment into the system, so that the hydrophobicity, shielding performance and insulating performance of the pouring sealant can be effectively improved, meanwhile, the fluorocarbon chain segment can realize self-repairing through reorientation, the shock resistance of the system is improved, and the pouring sealant can play roles of water resistance, moisture resistance, insulation, corrosion resistance, temperature resistance, wear resistance and the like after being cured.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples. Of course, the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Unless otherwise specified, both chemical reagents and materials in the present invention are purchased through a market route or synthesized from raw materials purchased through a market route.
The epoxy resin is bisphenol A epoxy resin, japanese Mitsubishi bisphenol A epoxy resin JER1256;
the alumina is spherical alumina with the density of 4.0g/mL and the median diameter D50 of 15-25 mu m;
the median diameter D50 of the quartz powder is 30-50 mu m;
the median diameter D50 of the mica powder is 60-80 mu m.
The invention will be further illustrated by the following examples.
Example 1
A preparation method of waterproof weather-proof electronic epoxy pouring sealant comprises the following steps:
(1) Adding 1g of A171 into 60g of ethanol, regulating the pH to 4 by using 15wt% hydrochloric acid solution, then adding 10g of mica powder, stirring at 80 ℃ for reaction for 3 hours, and filtering, washing and drying the product to obtain pretreated mica powder;
(2) 10g of pretreated mica powder is added into 60g of toluene, 6.8g of octavinyl POSS and 0.05g of benzoyl peroxide are added at the same time, the mixture is stirred and reacted for 6 hours at 90 ℃, the product is filtered and washed, and then the product is dried for 2 hours at 130 ℃ to obtain POSS grafted mica powder;
(3) Dispersing 10g of POSS grafted mica powder into 50g of toluene, dissolving 8.7g of perfluorodecanethiol into 30g of methanol, mixing the two mixed solutions, adding 0.05g of benzoin dimethyl ether, continuously introducing N 2, stirring under the condition of ultraviolet irradiation for reaction for 8 hours, steaming the product to obtain solid, washing 3 times with acetone, and freeze-drying to obtain modified mica powder;
(4) Preparing 10g of 3-glycidoxypropyl triethoxysilane, 10g of deionized water and 90g of ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing for 3 hours, adding 10g of aluminum oxide into the mixed solution, stirring and reacting for 3 hours, and filtering, washing and drying the product to obtain modified aluminum oxide;
(5) Uniformly mixing 80g of epoxy resin, 10g of polypropylene glycol diglycidyl ether, 40g of modified alumina, 40g of modified mica powder and 15g of quartz powder to obtain a component A; 80g of methyltetrahydrophthalic anhydride and 1g of 2-methylimidazole are uniformly mixed to obtain a component B.
Example 2
A preparation method of waterproof weather-proof electronic epoxy pouring sealant comprises the following steps:
(1) Adding 0.5g of A171 into 60g of ethanol, regulating the pH to 4 by using 15wt% hydrochloric acid solution, then adding 10g of mica powder, stirring at 60 ℃ for reaction for 1h, and filtering, washing and drying the product to obtain pretreated mica powder;
(2) 10g of pretreated mica powder is added into 60g of toluene, 1.2g of octavinyl POSS and 0.02g of benzoyl peroxide are added at the same time, the mixture is stirred and reacted for 3 hours at 70 ℃, the product is filtered and washed, and then dried for 0.5 hour at 110 ℃ to obtain POSS grafted mica powder;
(3) Dispersing 10g of POSS grafted mica powder into 50g of toluene, dissolving 4.3g of perfluorodecanethiol into 30g of methanol, mixing the two mixed solutions, adding 0.02g of benzoin dimethyl ether, continuously introducing N 2, stirring under the condition of ultraviolet irradiation for reaction for 4 hours, steaming the product to obtain solid, washing 3 times with acetone, and freeze-drying to obtain modified mica powder;
(4) Preparing 5g of 3-glycidoxypropyl triethoxysilane, 5g of deionized water and 80g of ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing for 2 hours, adding 10g of aluminum oxide into the mixed solution, stirring and reacting for 1 hour, and filtering, washing and drying the product to obtain modified aluminum oxide;
(5) Uniformly mixing 50g of epoxy resin, 6g of polypropylene glycol diglycidyl ether, 25g of modified alumina, 15g of modified mica powder and 5g of quartz powder to obtain a component A; 60g of methyltetrahydrophthalic anhydride and 0.1-methylimidazole are uniformly mixed to obtain a component B.
Example 3
A preparation method of waterproof weather-proof electronic epoxy pouring sealant comprises the following steps:
(1) Adding 0.8g of A171 into 60g of ethanol, regulating the pH to 4 by using 15wt% hydrochloric acid solution, then adding 10g of mica powder, stirring at 70 ℃ for reaction for 2 hours, and filtering, washing and drying the product to obtain pretreated mica powder;
(2) 10g of pretreated mica powder is added into 60g of toluene, 4.2g of octavinyl POSS and 0.03g of benzoyl peroxide are added at the same time, the mixture is stirred and reacted for 4 hours at 80 ℃, the product is filtered and washed, and then the product is dried for 1 hour at 120 ℃ to obtain POSS grafted mica powder;
(3) Dispersing 10g of POSS grafted mica powder into 50g of toluene, dissolving 6.3g of perfluorodecanethiol into 30g of methanol, mixing the two mixed solutions, adding 0.03g of benzoin dimethyl ether, continuously introducing N 2, stirring and reacting for 5h under the condition of ultraviolet irradiation, steaming the product to obtain solid, washing 3 times with acetone, and freeze-drying to obtain modified mica powder;
(4) Preparing 7g of 3-glycidoxypropyl triethoxysilane, 8g of deionized water and 85g of ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing for 2.5h, adding 10g of alumina into the mixed solution, stirring and reacting for 2h, filtering, washing and drying the product to obtain modified alumina;
(5) Uniformly mixing 65g of epoxy resin, 8g of polypropylene glycol diglycidyl ether, 32g of modified alumina, 28g of modified mica powder and 10g of quartz powder to obtain a component A; 70g of methyltetrahydrophthalic anhydride and 0.5g of 2-methylimidazole are uniformly mixed to obtain a component B.
Comparative example 1
The preparation method of the epoxy pouring sealant comprises the following steps:
(1) Adding 0.5g of A171 into 60g of ethanol, regulating the pH to 4 by using 15wt% hydrochloric acid solution, then adding 10g of mica powder, stirring at 60 ℃ for reaction for 1h, and filtering, washing and drying the product to obtain pretreated mica powder;
(2) 10g of pretreated mica powder is added into 60g of toluene, 1.2g of octavinyl POSS and 0.02g of benzoyl peroxide are added at the same time, the mixture is stirred and reacted for 3 hours at 70 ℃, the product is filtered and washed, and then dried for 0.5 hour at 110 ℃ to obtain POSS grafted mica powder;
(3) Preparing 5g of 3-glycidoxypropyl triethoxysilane, 5g of deionized water and 80g of ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing for 2 hours, adding 10g of aluminum oxide into the mixed solution, stirring and reacting for 1 hour, and filtering, washing and drying the product to obtain modified aluminum oxide;
(4) Uniformly mixing 50g of epoxy resin, 6g of polypropylene glycol diglycidyl ether, 25g of modified alumina, 15gPOSS g of grafted mica powder and 5g of quartz powder to obtain a component A; 60g of methyltetrahydrophthalic anhydride and 0.1-methylimidazole are uniformly mixed to obtain a component B.
Comparative example 2
The preparation method of the epoxy pouring sealant comprises the following steps:
(1) Adding 0.5g of A171 into 60g of ethanol, regulating the pH to 4 by using 15wt% hydrochloric acid solution, then adding 10g of mica powder, stirring at 60 ℃ for reaction for 1h, and filtering, washing and drying the product to obtain pretreated mica powder;
(2) Preparing 5g of 3-glycidoxypropyl triethoxysilane, 5g of deionized water and 80g of ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing for 2 hours, adding 10g of aluminum oxide into the mixed solution, stirring and reacting for 1 hour, and filtering, washing and drying the product to obtain modified aluminum oxide;
(3) Uniformly mixing 50g of epoxy resin, 6g of polypropylene glycol diglycidyl ether, 25g of modified alumina, 15g of pretreated mica powder and 5g of quartz powder to obtain a component A; 60g of methyltetrahydrophthalic anhydride and 0.1-methylimidazole are uniformly mixed to obtain a component B.
Pouring the epoxy pouring sealants prepared in the examples 1-3 and the comparative examples 1-2 into a polytetrafluoroethylene mold for testing, curing for 24 hours at room temperature after leveling, preparing a test sample with the thickness of about 2mm, and testing tensile strength, elongation and the like; and taking the roughened clean tinplate as a base material, taking the epoxy pouring sealant prepared in the examples 1-3 and the comparative examples 1-2, coating the pouring sealant on the surface of the tinplate by using an 80-mesh wire rod to prepare a glue layer test sample with the thickness of 25-30 mu m, curing for 24 hours at the room temperature of 25+/-2 ℃ under the relative humidity RH of 48+/-2%, and testing the impact resistance, ageing resistance, water resistance and moisture resistance of the organosilicon modified epoxy pouring sealant by referring to the evaluation method of the coating.
The performance test of the modified epoxy pouring sealant comprises that the elongation at break is referred to GB/T1040.1-2018, section 1 of determination of Plastic tensile Property: the general rule is that the sample preparation is measured by a universal pulling machine; impact resistance was measured with an impact tester with reference to GB/T1732-2020, paint film impact resistance measurement; the method for testing the flexibility of the adhesive layer by using a QTX type paint film flexibility tester is used for testing, and the larger the measured data is, the worse the flexibility of the adhesive layer is; the ageing resistance is described in GB/T2423.24-2022 part 2 of environmental test: test method test S: simulating solar radiation on the ground, measuring by using a KK-SN-150 xenon lamp aging resistance test box (irradiating by using a xenon lamp for 1000 hours under the condition of 85 ℃ and relative humidity RH of 85 percent of damp heat) according to solar radiation test and weather aging test rules; the waterproof performance of the surface of the epoxy pouring sealant is expressed by the contact angle (WCA) of water on the surface of the adhesive layer, and the water drop size is 5 mu L by using a JC-2000C1 static contact angle measuring instrument; the larger the WCA, the better the water repellency of the surface of the adhesive layer and the better the moisture resistance; the thermal conductivity is measured by referring to GB 3399-1982 Heat protection plate method for test method for thermal conductivity of plastics, and the larger the thermal conductivity is, the better the thermal conductivity is. The experimental test results are shown in table 1.
Table 1 epoxy pouring sealant performance test results
In the comparative example 1, perfluoro decyl mercaptan is not grafted to POSS grafted mica powder, the prepared epoxy pouring sealant has poor moisture resistance and reduced impact resistance; in comparative example 2, the mica powder is not modified by POSS and perfluorodecanethiol, and the prepared epoxy pouring sealant has poor mechanical properties such as impact resistance, flexibility, elongation at break and the like, and the heat conductivity coefficient of the mica powder is also reduced due to poor dispersibility of the mica powder in an epoxy resin matrix.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (9)
1. The waterproof weather-proof electronic epoxy pouring sealant is characterized by comprising a component A and a component B; the component A is prepared from the following raw materials in parts by weight: 50-80 parts of epoxy resin, 6-10 parts of polypropylene glycol diglycidyl ether, 25-40 parts of modified alumina, 15-40 parts of modified mica powder and 5-15 parts of quartz powder; the component B is prepared from the following raw materials in parts by weight: 60-80 parts of methyl tetrahydrophthalic anhydride and 0.1-1 part of 2-methylimidazole;
The preparation method of the modified mica powder comprises the following steps:
(1) Adding A171 into ethanol, regulating pH with hydrochloric acid solution, adding mica powder, stirring for reaction, filtering, washing and drying the product to obtain pretreated mica powder;
(2) Adding the pretreated mica powder into toluene, simultaneously adding octavinyl POSS and benzoyl peroxide, stirring for reaction, and filtering, washing and drying the product to obtain POSS grafted mica powder;
(3) Dispersing POSS grafted mica powder into toluene, dissolving perfluorodecanethiol into methanol, mixing the two mixed solutions, adding benzoin dimethyl ether, continuously introducing N 2, stirring for reaction under the condition of ultraviolet irradiation, steaming the product to obtain solid, washing with acetone, and freeze-drying to obtain the modified mica powder.
2. The waterproof weather-resistant electronic epoxy pouring sealant according to claim 1, wherein in the step (1), the weight ratio of mica powder to A171 to ethanol is 10:0.5 to 1:60 to 80 percent.
3. The waterproof weather-proof electronic epoxy pouring sealant according to claim 1, wherein in the step (1), the mass fraction of the hydrochloric acid solution is 10-20%, the pH is adjusted to 3-6, and the stirring reaction condition is that stirring reaction is carried out for 1-3 hours at 60-80 ℃.
4. The waterproof weather-resistant electronic epoxy pouring sealant according to claim 1, wherein in the step (2), the weight ratio of the pretreated mica powder to toluene to octavinyl POSS to benzoyl peroxide is 10: 50-80: 1.2 to 6.8:0.02 to 0.05.
5. The waterproof weather-proof electronic epoxy pouring sealant according to claim 1, wherein in the step (2), the stirring reaction condition is 70-90 ℃ for 3-6 h, and the drying condition is 110-130 ℃ for 0.5-2 h.
6. The waterproof weather-resistant electronic epoxy pouring sealant according to claim 1, wherein in the step (3), the weight ratio of POSS grafted mica powder to perfluorodecanethiol to benzoin dimethyl ether is 10:4.3 to 8.7: 0.02-0.05, and stirring and reacting for 4-8 h.
7. The waterproof weather-resistant electronic epoxy pouring sealant according to claim 1, wherein the preparation method of the modified alumina comprises the following steps: preparing 3-glycidoxypropyl triethoxysilane, deionized water and ethanol into a mixed solution, uniformly stirring, then sealing and hydrolyzing, adding alumina into the mixed solution, stirring for reaction, and filtering, washing and drying the product to obtain the modified alumina.
8. The waterproof weather-proof electronic epoxy pouring sealant according to claim 7, wherein the weight ratio of 3-glycidoxypropyl triethoxysilane, deionized water, ethanol and alumina is 5-10: 5-10: 80-90: 10; the sealed hydrolysis time is 2-3 h, and the alumina is added into the mixed solution and stirred for reaction for 1-3 h.
9. A method for preparing the waterproof weather-resistant electronic epoxy pouring sealant according to any one of claims 1 to 8, which is characterized by comprising the following steps: uniformly mixing epoxy resin, polypropylene glycol diglycidyl ether, modified alumina, modified mica powder and quartz powder to obtain a component A; and uniformly mixing methyl tetrahydrophthalic anhydride and 2-methylimidazole to obtain a component B.
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| KR20090032434A (en) * | 2007-09-28 | 2009-04-01 | 한국산업기술평가원(관리부서:요업기술원) | Pet hybrid nano-composite comprising poss and method for manufacturing the same |
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| CN116574472A (en) * | 2023-06-08 | 2023-08-11 | 北京高盟新材料股份有限公司 | High-low temperature aging resistant two-component epoxy pouring sealant and preparation method thereof |
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