CN116179130A - Anti-yellowing flame-retardant epoxy resin electronic pouring sealant and preparation method thereof - Google Patents
Anti-yellowing flame-retardant epoxy resin electronic pouring sealant and preparation method thereof Download PDFInfo
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- CN116179130A CN116179130A CN202310089846.6A CN202310089846A CN116179130A CN 116179130 A CN116179130 A CN 116179130A CN 202310089846 A CN202310089846 A CN 202310089846A CN 116179130 A CN116179130 A CN 116179130A
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- epoxy resin
- yellowing
- component
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- bisphenol
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 66
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 66
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000003063 flame retardant Substances 0.000 title claims abstract description 42
- 239000000565 sealant Substances 0.000 title claims abstract description 38
- 238000004383 yellowing Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims abstract description 26
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims abstract description 20
- 125000002723 alicyclic group Chemical group 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 16
- 239000003085 diluting agent Substances 0.000 claims abstract description 15
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 12
- 239000007822 coupling agent Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 150000008064 anhydrides Chemical class 0.000 claims description 8
- 239000012745 toughening agent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 238000004382 potting Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920000768 polyamine Polymers 0.000 claims description 2
- DWSWCPPGLRSPIT-UHFFFAOYSA-N benzo[c][2,1]benzoxaphosphinin-6-ium 6-oxide Chemical compound C1=CC=C2[P+](=O)OC3=CC=CC=C3C2=C1 DWSWCPPGLRSPIT-UHFFFAOYSA-N 0.000 claims 2
- 229920006332 epoxy adhesive Polymers 0.000 abstract description 2
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 description 30
- 238000001723 curing Methods 0.000 description 26
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 23
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 9
- 239000004593 Epoxy Substances 0.000 description 9
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 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 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 6
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- RUNBDQGENXJZOO-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) 7-oxabicyclo[4.1.0]hept-5-ene-3,4-dicarboxylate Chemical compound C1C2OC2=CC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 RUNBDQGENXJZOO-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000002715 modification method Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 150000003512 tertiary amines Chemical class 0.000 description 3
- 244000179970 Monarda didyma Species 0.000 description 2
- 235000010672 Monarda didyma Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000013007 heat curing Methods 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- XFUOBHWPTSIEOV-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) cyclohexane-1,2-dicarboxylate Chemical compound C1CCCC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 XFUOBHWPTSIEOV-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 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 1
- 238000005286 illumination Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 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
- 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
- C09J11/06—Non-macromolecular additives organic
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of epoxy adhesives, in particular to the field of IPC C09J163, and more particularly relates to a yellowing-resistant flame-retardant epoxy resin electronic pouring sealant and a preparation method thereof. The components comprise: a component A and a component B, wherein the component A comprises: 80-130 parts of epoxy resin, 10-20 parts of reactive diluent, 10-20 parts of filler, 5-10 parts of flexibilizer and 5-15 parts of flame retardant; the component B comprises the following components: 50-80 parts of curing agent and 5-15 parts of accelerator. 3. The epoxy resin comprises bisphenol A epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, wherein the weight ratio of the bisphenol A epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1: (1-2): and (5-8), the hardness and yellowing resistance of the prepared pouring sealant can be improved.
Description
Technical Field
The invention relates to the technical field of epoxy adhesives, in particular to the field of IPC C09J163, and more particularly relates to a yellowing-resistant flame-retardant epoxy resin electronic pouring sealant and a preparation method thereof.
Background
Potting adhesives are leading edge technology in the field of electronic assembly, which can effectively protect electronic devices under extremely challenging environmental conditions, improve mechanical strength, and impart excellent electrical insulation. Electronic pouring sealants are widely used in a variety of industries, various consumer electronics, and in automotive, aerospace, and other industries where electronic assembly is often involved. At present, epoxy resin pouring sealant, organic silicon pouring sealant and polyurethane pouring sealant are mainly used. The organosilicon pouring sealant is high in price and poor in scratch resistance. Polyurethane pouring sealant is easy to foam due to poor high temperature resistance, and meanwhile, the ageing resistance and the ultraviolet resistance are not strong enough. The epoxy resin pouring sealant has excellent high temperature resistance and electrical insulation capability, the production process is simple and convenient, the stability before and after solidification is high, the product yield is high, and the epoxy resin pouring sealant is widely applied. However, the current epoxy electronic pouring sealant has color yellowing under the condition of large heat, so that the electric performance, the thermal performance and the protective performance are deteriorated.
CN105907346a discloses an epoxy electronic pouring sealant and a preparation method thereof, which is prepared by mixing E-51 bisphenol A epoxy resin, an epoxy diluent, an epoxy toughening agent, a curing agent, a filler and an auxiliary agent. The epoxy electronic pouring sealant adopts bisphenol A type epoxy resin as main resin, and selects the types and the addition amount of the accelerator and the filler to select the optimal formula. The prepared epoxy pouring sealant has good heat conductivity, flame retardance, small internal stress of products and various performances superior to those of similar pouring sealants abroad, and is suitable for pouring and sealing high-power electronic elements. However, the epoxy electronic pouring sealant uses a more aromatic epoxy resin bisphenol A structure, is easy to oxidize to generate carbonyl formation and development Huang Jituan, and reduces yellowing resistance to a certain extent.
Disclosure of Invention
In order to overcome the defects in the background art, the invention provides the yellowing-resistant flame-retardant epoxy resin electronic pouring sealant and the preparation method thereof, and the prepared pouring sealant is excellent in mechanical property and has better yellowing resistance and flame retardance through using different types of epoxy resins and adjusting the proportion of components.
In order to achieve the purpose of the invention, the first aspect of the invention provides a yellowing-resistant flame-retardant epoxy resin electronic pouring sealant, which comprises the following components in parts by weight: a component A and a component B, wherein the component A comprises: 80-130 parts of epoxy resin, 10-20 parts of reactive diluent, 10-20 parts of filler, 5-10 parts of flexibilizer and 5-15 parts of flame retardant; the component B comprises the following components: 50-80 parts of curing agent and 5-15 parts of accelerator.
The applicant found that the epoxy resin comprises bisphenol a epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, wherein the weight ratio of the bisphenol a epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1: (1-2): and (5-8), the hardness and yellowing resistance of the prepared pouring sealant can be improved, and the higher mechanical property and insulating property are brought by the larger steric hindrance of ether groups and benzene rings in the bisphenol A epoxy resin, but the higher viscosity of the bisphenol A epoxy resin influences the dispersion property of the system. The dilution effect of bisphenol F epoxy resin on bisphenol A epoxy resin is quite obvious, and when the consumption of bisphenol F is too large, the viscosity of the mixed resin system is too low, so that the workability is greatly reduced, and the effect of reducing the viscosity is difficult to achieve. Bisphenol F epoxy resin and bisphenol A epoxy resin both contain more benzene ring structures, carbonyl formation is generated by easy oxidation, huang Jituan is reduced in yellowing resistance, and benzene rings are not contained in the molecular structure of alicyclic epoxy resin, so that the epoxy resin has good weather resistance and ultraviolet radiation resistance, meanwhile, as the epoxy groups of the alicyclic epoxy resin are directly connected to the alicyclic, a compact rigid molecular structure can be formed, an interpenetrating network structure is formed between the epoxy resin and bisphenol A epoxy resin after curing, the interval of crosslinking points is further reduced, the infiltration amount of oxygen is reduced, and the flame retardant property of pouring sealant is effectively improved.
Preferably, the epoxy resin comprises bisphenol A epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, wherein the weight ratio of the bisphenol A epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1: (1-2): (5-8).
Further preferably, the epoxy resin comprises bisphenol a epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, wherein the weight ratio of the bisphenol a epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1:1.5:7.
preferably, the bisphenol a epoxy resin comprises an epoxy value between 0.2 and 0.6.
Preferably, bisphenol a epoxy resins include E51, E44, E42, E20, wherein the numbers represent epoxy values.
Further preferably, the bisphenol a epoxy resin comprises E51, available from northeast tall and erect rubber products limited.
Preferably, the bisphenol F epoxy resin comprises F51, NPEF-170, EPALOY 8220 and EPALOY 8230.
Further preferably, the bisphenol F epoxy resin comprises F51 (available from Jinan Bai Chemie Co., ltd.).
Preferably, the alicyclic epoxy resin comprises at least one of 4, 5-epoxy tetrahydrophthalic acid diglycidyl ester, hexahydrophthalic acid diglycidyl ester, hydrogenated bisphenol a epoxy resin.
Further preferably, the cycloaliphatic epoxy resin comprises 4, 5-epoxy tetrahydrophthalic acid diglycidyl ester, available from North Chemie, inc.
The reactive diluent comprises one of butyl glycidyl ether, ethylene glycol diglycidyl ether and phenyl glycidyl ether.
Preferably, the reactive diluent comprises butyl glycidyl ether (CAS: 2426-08-6).
Preferably, the weight ratio of the epoxy resin to the reactive diluent to the filler is 1: (0.1-0.2): (0.1-0.2).
Further preferably, the weight ratio of the epoxy resin to the reactive diluent to the filler is 1:0.15:0.18.
the filler comprises a modified inorganic powder material.
Preferably, the mesh number of the modified inorganic powder material is 800-2000 mesh.
Preferably, the modified inorganic powder material comprises at least one of silica, aluminum hydroxide, aluminum oxide, magnesium hydroxide, wollastonite.
Further preferably, the modified inorganic powder material comprises silica having a mesh size of 2000 mesh, available from gold pure silicon materials limited in the forward region of bergamot.
The modified inorganic powder material is modified by a coupling agent.
Preferably, the coupling agent comprises KH550, KH560, KH570.
Further preferably, the coupling agent comprises KH550.
Preferably, the modification method comprises: adding 2-4 parts of coupling agent into 96-98 parts of solvent, stirring at 70-90 ℃ for 4-6h, and filtering to obtain the final product.
Further preferably, the modification method includes: adding 4 parts of coupling agent into 98 parts of solvent, stirring for 5 hours at 90 ℃, and filtering to obtain the modified inorganic powder material.
The toughening agent comprises one of polyester and polyether.
Preferably, the toughening agent comprises a polyester comprising dibutyl phthalate (CAS: 84-74-2).
The applicant found that when the flame retardant comprises aluminum hydroxide and DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), the flame retardant efficiency can be improved, the addition amount of the small molecular flame retardant can be reduced, and the DOPO can react with epoxy groups due to the P-H bond structure with higher activity in the molecule, so that a large amount of nonflammable gas CO is generated in the combustion process 2 、NH 3 、N 2 And H 2 And diluting active free radicals by O and the like, thereby reducing the reaction rate, absorbing heat and reducing the temperature of a matrix to realize the flame-retardant effect. On the other hand, DOPO groups are decomposed to generate phosphoric acid and polymetaphosphoric acid when the polymer matrix burns, matrix moisture is removed, matrix char formation is promoted to form a refractory insulating carbon layer, meanwhile, decomposition products polymetaphosphoric acid glass body covers the surface of the epoxy resin, oxygen and heat are isolated from being transferred to the inside of the matrix, but DOPO has lower dispersion performance in an epoxy resin system, the addition of aluminum hydroxide can effectively improve the dispersibility of DOPO, possibly the polarity of the aluminum hydroxide is higher, the compatibility of the DOPO with a high-molecular epoxy resin material is better, and DOPO can be dispersed among the aluminum hydroxide, so that the porosity of the surface of the material can be reduced, and the passing rate of oxygen in the resin in the combustion process is reduced.
Further studies have found that the weight ratio of aluminum hydroxide to DOPO is 1: (0.2-0.5), the yellowing resistance of the pouring sealant can be improved, the heat conduction performance of aluminum hydroxide is possibly higher, DOPO can absorb the heat in the system under a specific proportion, and the internal photo-thermal balance is achieved, so that the yellowing caused by photo-thermal is reduced.
Preferably, the flame retardant comprises aluminum hydroxide and DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), wherein the weight ratio of the aluminum hydroxide to the DOPO is 1: (0.2-0.5).
Further preferably, the flame retardant comprises aluminum hydroxide, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), the weight ratio of the aluminum hydroxide to DOPO being 1:0.3.
preferably, the aluminum hydroxide is purchased from Hebei Qingjiang New Material technologies Co.
Preferably, the DOPO is purchased from the fagadol chemical company, inc.
The curing agent comprises one of an aromatic amine curing agent, an anhydride curing agent, a polyamide curing agent and an aliphatic polyamine curing agent.
Preferably, the curing agent comprises an anhydride curing agent, wherein the anhydride curing agent comprises methyltetrahydrophthalic anhydride and methylhexahydrophthalic anhydride, and the weight ratio of the methyltetrahydrophthalic anhydride to the methylhexahydrophthalic anhydride is 1: (0.3-0.6).
Further preferably, the curing agent comprises an anhydride curing agent, wherein the anhydride curing agent comprises methyltetrahydrophthalic anhydride (CAS: 11070-44-3) and methylhexahydrophthalic anhydride (CAS: 25550-51-0), and the weight ratio of the methyltetrahydrophthalic anhydride to the methylhexahydrophthalic anhydride is 1:0.5.
the accelerator comprises a tertiary amine accelerator, a substituted urea accelerator and one of phenolic accelerators.
Preferably, the accelerator comprises a tertiary amine accelerator comprising at least one of 2,4, 6-tris (dimethylaminomethyl) phenol, benzyl dimethylamine, triethylamine, triethanolamine.
Further preferably, the accelerator comprises a tertiary amine accelerator comprising 2,4, 6-tris (dimethylaminomethyl) phenol, triethylamine, wherein the weight ratio of 2,4, 6-tris (dimethylaminomethyl) phenol to triethylamine is 1: (0.3-0.8).
Preferably, the accelerator comprises 2,4, 6-tris (dimethylaminomethyl) phenol (CAS: 90-72-2), triethylamine (CAS: 121-44-8), and the weight ratio of the 2,4, 6-tris (dimethylaminomethyl) phenol to the triethylamine is 1:0.5.
the invention provides a preparation method of a yellowing-resistant flame-retardant epoxy resin electronic pouring sealant, which comprises the following steps:
s1, uniformly stirring epoxy resin, an active diluent, a filler, a toughening agent and a flame retardant to prepare a component A;
s2, uniformly mixing a curing agent and an accelerator to prepare a component B;
s3, mixing the component A and the component B, and heating and curing.
Preferably, the weight ratio of the component A to the component B is 1: (0.1-0.3).
Further preferably, the weight ratio of the component A to the component B is 1:0.25.
the temperature of the heating and curing is 50-75 ℃, and the time of the heating and curing is 1-3h.
Preferably, the temperature of the heat curing is 60 ℃, and the time of the heat curing is 2 hours.
The beneficial effects are that:
1. when the flame retardant comprises aluminum hydroxide and DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), the flame retardant efficiency can be improved, and the addition amount of the micromolecular flame retardant can be reduced.
2. Aluminum hydroxide and DOPO in a weight ratio of 1: (0.2-0.5), the yellowing resistance of the pouring sealant can be improved.
3. The epoxy resin comprises bisphenol A epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, wherein the weight ratio of the bisphenol A epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1: (1-2): (5-8)
In this case, the hardness and yellowing resistance of the prepared pouring sealant can be improved.
Detailed Description
Example 1
The yellowing-resistant flame-retardant epoxy resin electronic pouring sealant comprises the following components in parts by weight: a component A and a component B, wherein the component A comprises: 100 parts of epoxy resin, 15 parts of reactive diluent, 18 parts of filler, 7 parts of toughening agent and 10 parts of flame retardant; the component B comprises the following components: 70 parts of curing agent and 12 parts of accelerator.
The epoxy resin comprises bisphenol A epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, wherein the weight ratio of the bisphenol A epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1:1.5:7.
the bisphenol A epoxy resin comprises E51, purchased from Hebei Zhuozheng rubber and plastic products Co.
The bisphenol F epoxy resin included F51 (available from Jinan Bai Chemicals Co., ltd.).
The cycloaliphatic epoxy resin comprises 4, 5-epoxy tetrahydrophthalic acid diglycidyl ester, available from North Chengfeng chemical Co.
The reactive diluent includes butyl glycidyl ether (CAS: 2426-08-6).
The filler comprises a modified inorganic powder material.
The modified inorganic powder material comprises silicon dioxide with the mesh number of 2000 mesh, and is purchased from gold pure silicon materials limited company in Shunde district of the bergamot.
The modified inorganic powder material is modified by a coupling agent, wherein the coupling agent comprises KH550.
The modification method comprises the following steps: adding 4 parts of coupling agent into 98 parts of solvent, stirring for 5 hours at 90 ℃, and filtering to obtain the modified inorganic powder material.
The toughening agent includes a polyester including dibutyl phthalate (CAS: 84-74-2).
The flame retardant comprises aluminum hydroxide and DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), wherein the weight ratio of the aluminum hydroxide to the DOPO is 1:0.3.
the aluminum hydroxide is purchased from Hebei Qingjiang new material science and technology Co.
The DOPO was purchased from Weifang Dakang chemical Co.
The curing agent comprises an anhydride curing agent, wherein the anhydride curing agent comprises methyltetrahydrophthalic anhydride (CAS: 11070-44-3) and methylhexahydrophthalic anhydride (CAS: 25550-51-0), and the weight ratio of the methyltetrahydrophthalic anhydride to the methylhexahydrophthalic anhydride is 1:0.5.
the accelerator comprises 2,4, 6-tris (dimethylaminomethyl) phenol (CAS: 90-72-2), triethylamine (CAS: 121-44-8), wherein the weight ratio of the 2,4, 6-tris (dimethylaminomethyl) phenol to the triethylamine is 1:0.5.
a preparation method of yellowing-resistant flame-retardant epoxy resin electronic pouring sealant comprises the following steps:
s1, uniformly stirring epoxy resin, an active diluent, a filler, a toughening agent and a flame retardant at 500rpm to prepare a component A;
s2, uniformly mixing the curing agent and the accelerator at 500rpm to prepare a component B;
s3, mixing the component A and the component B at 500rpm, and heating for curing.
The weight ratio of the component A to the component B is 1:0.25.
the temperature of the heating and curing is 60 ℃, and the time of the heating and curing is 2 hours.
Example 2
The detailed description is the same as example 1; except that the weight ratio of the epoxy resin, reactive diluent and filler in example 2 was 1:0.17:0.16.
example 3
The detailed description is the same as example 1; in contrast, the flame retardant described in example 3 comprises aluminum hydroxide, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), the weight ratio of the aluminum hydroxide to DOPO being 1:0.4.
comparative example 1
The detailed description is the same as example 1; except that the flame retardant described in comparative example 1 includes aluminum hydroxide.
Comparative example 2
The detailed description is the same as example 1; in contrast, the flame retardant in comparative example 2 comprises aluminum hydroxide, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), the weight ratio of the aluminum hydroxide to the DOPO being 1:2.
comparative example 3
The detailed description is the same as example 1; except that the bisphenol a epoxy resin, bisphenol F epoxy resin, and alicyclic epoxy resin described in comparative example 3 were 1 in weight ratio: 1:1.
performance test method
The pouring sealants obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance test, and the test data are shown in Table 1.
1. Flame retardant rating: UL-94 (thickness: 1.5 mm)
2. Yellowing resistance: the electronic pouring sealant is prepared, and the completely cured product is placed in a condition with illumination at 180 ℃ for 3 days to see whether yellowing occurs.
3. Shore hardness: GB/T531-1999.
4. Breakdown voltage: GB/T7752, 500v/min.
Performance test data
TABLE 1
Claims (10)
1. The yellowing-resistant flame-retardant epoxy resin electronic pouring sealant is characterized by comprising the following components in parts by weight:
a component A and a component B, wherein the component A comprises: 80-130 parts of epoxy resin, 10-20 parts of reactive diluent, 10-20 parts of filler, 5-10 parts of flexibilizer and 5-15 parts of flame retardant; the component B comprises the following components: 50-80 parts of curing agent and 5-15 parts of accelerator.
2. The electronic potting adhesive for the yellowing-resistant flame-retardant epoxy resin, which is disclosed in claim 1, wherein the epoxy resin comprises bisphenol A epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin, and the weight ratio of the bisphenol A epoxy resin to the bisphenol F epoxy resin to the alicyclic epoxy resin is 1: (1-2):
(5-8)。
3. the electronic potting adhesive for the yellowing-resistant flame-retardant epoxy resin, which is disclosed in claim 2, is characterized in that the weight ratio of the epoxy resin to the reactive diluent to the filler is 1: (0.1-0.2): (0.1-0.2).
4. A yellowing-resistant flame-retardant epoxy resin electronic pouring sealant according to claim 1 or 3, wherein said filler comprises modified inorganic powder material with a mesh size of 800-2000 mesh.
5. The electronic potting adhesive for yellowing resistant flame retardant epoxy resin of claim 4, wherein the modified inorganic powder material is modified by a coupling agent.
6. The yellowing-resistant flame-retardant epoxy resin electronic pouring sealant according to claim 5, wherein the flame retardant comprises aluminum hydroxide and DOPO, and the weight ratio of the aluminum hydroxide to the DOPO is 1:
(0.2-0.5)。
7. the electronic potting adhesive for yellowing resistant and flame retardant epoxy resin of claim 6, wherein the curing agent comprises one of an aromatic amine curing agent, an anhydride curing agent, a polyamide curing agent and an aliphatic polyamine curing agent.
8. A method for preparing the yellowing-resistant flame-retardant epoxy resin electronic pouring sealant according to any one of claims 1 to 7, comprising the following steps:
s1, uniformly stirring epoxy resin, an active diluent, a filler, a toughening agent and a flame retardant to prepare a component A;
s2, uniformly mixing a curing agent and an accelerator to prepare a component B;
s3, mixing the component A and the component B, and heating and curing.
9. The preparation method of the yellowing-resistant flame-retardant epoxy resin electronic pouring sealant is characterized in that the weight ratio of the component A to the component B is 1: (0.1-0.3).
10. The method for preparing the yellowing-resistant flame-retardant epoxy resin electronic pouring sealant according to claim 9, wherein the temperature of the heating and curing is 50-75 ℃, and the time of the heating and curing is 1-3h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117025150A (en) * | 2023-07-24 | 2023-11-10 | 江苏耀鸿电子有限公司 | Heat-resistant flame-retardant epoxy resin glue solution for PCB and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117025150A (en) * | 2023-07-24 | 2023-11-10 | 江苏耀鸿电子有限公司 | Heat-resistant flame-retardant epoxy resin glue solution for PCB and preparation method thereof |
| CN117025150B (en) * | 2023-07-24 | 2024-01-02 | 江苏耀鸿电子有限公司 | Heat-resistant flame-retardant epoxy resin glue solution for PCB and preparation method thereof |
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