CN111218092A - Processing method of light-color yellowing-resistant epoxy resin composition for packaging - Google Patents
Processing method of light-color yellowing-resistant epoxy resin composition for packaging Download PDFInfo
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- CN111218092A CN111218092A CN201911374065.1A CN201911374065A CN111218092A CN 111218092 A CN111218092 A CN 111218092A CN 201911374065 A CN201911374065 A CN 201911374065A CN 111218092 A CN111218092 A CN 111218092A
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- epoxy resin
- mixing
- crushing
- antioxidant
- parts
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 49
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 49
- 238000004383 yellowing Methods 0.000 title claims abstract description 40
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- 238000003672 processing method Methods 0.000 title claims abstract description 17
- 238000004806 packaging method and process Methods 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000002156 mixing Methods 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims description 53
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 26
- 229920001568 phenolic resin Polymers 0.000 claims description 26
- 239000005011 phenolic resin Substances 0.000 claims description 26
- 239000000945 filler Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 14
- -1 phenolic aldehyde Chemical class 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 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 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007822 coupling agent Substances 0.000 claims description 12
- 239000003063 flame retardant Substances 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 11
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 9
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 9
- 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 claims description 8
- 230000002087 whitening effect Effects 0.000 claims description 8
- 239000011256 inorganic filler Substances 0.000 claims description 7
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 7
- 239000003607 modifier Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- PRWJPWSKLXYEPD-UHFFFAOYSA-N 4-[4,4-bis(5-tert-butyl-4-hydroxy-2-methylphenyl)butan-2-yl]-2-tert-butyl-5-methylphenol Chemical compound C=1C(C(C)(C)C)=C(O)C=C(C)C=1C(C)CC(C=1C(=CC(O)=C(C=1)C(C)(C)C)C)C1=CC(C(C)(C)C)=C(O)C=C1C PRWJPWSKLXYEPD-UHFFFAOYSA-N 0.000 claims description 6
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 claims description 6
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 claims description 6
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 235000010290 biphenyl Nutrition 0.000 claims description 5
- 239000004305 biphenyl Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- VETPHHXZEJAYOB-UHFFFAOYSA-N 1-n,4-n-dinaphthalen-2-ylbenzene-1,4-diamine Chemical compound C1=CC=CC2=CC(NC=3C=CC(NC=4C=C5C=CC=CC5=CC=4)=CC=3)=CC=C21 VETPHHXZEJAYOB-UHFFFAOYSA-N 0.000 claims description 4
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- 239000002250 absorbent Substances 0.000 claims description 4
- 230000002745 absorbent Effects 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001971 elastomer Polymers 0.000 claims description 4
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 4
- 150000001282 organosilanes Chemical class 0.000 claims description 4
- DXGLGDHPHMLXJC-UHFFFAOYSA-N oxybenzone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 DXGLGDHPHMLXJC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 4
- 239000001993 wax Substances 0.000 claims description 4
- ODJQKYXPKWQWNK-UHFFFAOYSA-L 3-(2-carboxylatoethylsulfanyl)propanoate Chemical compound [O-]C(=O)CCSCCC([O-])=O ODJQKYXPKWQWNK-UHFFFAOYSA-L 0.000 claims description 3
- AIXZBGVLNVRQSS-UHFFFAOYSA-N 5-tert-butyl-2-[5-(5-tert-butyl-1,3-benzoxazol-2-yl)thiophen-2-yl]-1,3-benzoxazole Chemical compound CC(C)(C)C1=CC=C2OC(C3=CC=C(S3)C=3OC4=CC=C(C=C4N=3)C(C)(C)C)=NC2=C1 AIXZBGVLNVRQSS-UHFFFAOYSA-N 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003508 Dilauryl thiodipropionate Substances 0.000 claims description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052794 bromium Inorganic materials 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 235000019304 dilauryl thiodipropionate Nutrition 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 claims description 2
- USLPZCOPYRKTGY-UHFFFAOYSA-N 2-(2-phenylethenyl)benzonitrile Chemical compound N#CC1=CC=CC=C1C=CC1=CC=CC=C1 USLPZCOPYRKTGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 125000002723 alicyclic group Chemical group 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- 239000012184 mineral wax Substances 0.000 claims description 2
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 claims description 2
- WGKLOLBTFWFKOD-UHFFFAOYSA-N tris(2-nonylphenyl) phosphite Chemical compound CCCCCCCCCC1=CC=CC=C1OP(OC=1C(=CC=CC=1)CCCCCCCCC)OC1=CC=CC=C1CCCCCCCCC WGKLOLBTFWFKOD-UHFFFAOYSA-N 0.000 claims description 2
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000012178 vegetable wax Substances 0.000 claims description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims 2
- 238000005507 spraying Methods 0.000 claims 2
- 150000008064 anhydrides Chemical class 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 238000000465 moulding Methods 0.000 abstract description 9
- 238000005476 soldering Methods 0.000 abstract description 5
- 229920006336 epoxy molding compound Polymers 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000007723 die pressing method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000011342 resin composition Substances 0.000 description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 1
- DYDWGWXTSKSNFD-UHFFFAOYSA-N 5-(2-phenylethenyl)-2-[4-(2-phenylethenyl)-2-sulfophenyl]benzenesulfonic acid Chemical compound C=1C=C(C=2C(=CC(C=CC=3C=CC=CC=3)=CC=2)S(O)(=O)=O)C(S(=O)(=O)O)=CC=1C=CC1=CC=CC=C1 DYDWGWXTSKSNFD-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08L63/04—Epoxynovolacs
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/02—Polyglycidyl ethers of bis-phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/04—Epoxynovolacs
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a processing method of a light-color yellowing-resistant epoxy resin composition, wherein a double-roller open mill, a single-screw extruder or a double-screw extruder is selected as processing equipment; the processing method comprises the steps of raw material pretreatment, mixing process, cooling, crushing and forming. The invention has the following technical effects: the epoxy resin composition processed by the method has the characteristics of light yellow or white color, and after molding, the epoxy resin composition is cured for 4 to 8 hours at 175 ℃ and does not turn yellow after reflow soldering treatment at 260 ℃.
Description
Technical Field
The invention relates to a processing method of a light-color yellowing-resistant epoxy resin composition for packaging. Belongs to the technical field of thermosetting plastics, and further belongs to the processing technology in the technical field of epoxy molding compounds.
Background
The epoxy molding compound is generally dark color such as black green, yellow and the like, and the colorant is used for covering the internal structure of the package and preventing light and rays from influencing the performance of the package. Certain environments require that the epoxy molding compound be light colored or white.
White epoxy molding compounds have several technical difficulties.
One is that there is no existing process equipment. As the molding compound is an unconventional product, under the processing equipment and process of a common molding compound, the material turns green or black after the white molding compound is processed. The reason is that the metal in the equipment enters the material with the process, which makes the material black and yellow after heating. The present invention overcomes this problem by using suitable equipment.
Secondly, due to the particularity of a formula system, the matching of all components needs a special processing method, and the invention is realized by controlling the granularity of raw material processing, the processing temperature and time, the pretreatment of raw materials and other processes.
In the prior art, a processing method for processing a black epoxy molding compound generally comprises the following steps: the two-roll mill processing method, the single-screw or double-screw extruder processing method, the used equipment is generally metal materials without plating ceramics. In the process flow, if the temperature is too high or the processing time is too long due to improper parameters, the white material can be yellowed. If the particle size is not proper, the material is not mixed uniformly. The processing equipment uses metal material, can make the metal get into the material during processing for the material discolours.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a processing method of a light-color yellowing-resistant epoxy resin composition for packaging.
Under the existing processing technology, metal in equipment can enter the resin composition in the processing process, so that the resin composition is blackened and easily yellowed.
The technical scheme of the invention is as follows:
a processing method of a light-color yellowing-resistant epoxy resin composition,
the light-color yellowing-resistant epoxy resin composition comprises the following components in parts by weight:
4-25 parts of epoxy resin A;
4-25 parts of a curing agent B;
0.01-3 parts of accelerator C;
15-89 parts of an inorganic filler D;
0-25 parts of flame retardant E;
0-5 parts of an anti-yellowing agent F;
0.05-3 parts of a release agent G;
0.01-3 parts of coupling agent H;
0-10 parts of whitening agent I;
0-3 parts of modifier and other additives J.
The epoxy resin can be one or more of phenolic aldehyde type epoxy resin, bisphenol A type structure epoxy resin, biphenyl type structure epoxy resin, naphthalene type structure epoxy resin, o-cresol type structure epoxy resin, DCPD type structure epoxy resin, polyfunctional group structure epoxy resin, alicyclic epoxy resin and the like.
The structural formula of each epoxy resin is as follows:
the curing agent can be one or more of linear phenolic resin, XY-lock type phenolic resin, bisphenol A type phenolic resin, DCPD type phenolic resin, biphenyl type phenolic resin or polyfunctional phenolic resin.
The structural formula of each curing agent is as follows:
the accelerator generally determines the resin crosslinking structure, reaction process and conditions, and the type of accelerator is as follows: the curing accelerator is one or more of organic phosphorus compounds, imidazole compounds, tertiary amine compounds and derivatives thereof.
The inorganic filler generally determines the mechanical properties of the material, such as strength, density, thermal conductivity and water absorption, and can be one or more of crystalline or fused angle or fused sphere silica powder, titanium dioxide powder, alumina powder and magnesia powder.
The flame retardant determines the flame retardant grade of the material, and a flame retardant without bromine and antimony elements is generally used in the halogen-free formula epoxy resin composition. The flame retardant is one or more of a bromine-containing flame retardant, antimony trioxide, aluminum hydroxide, magnesium hydroxide, zinc borate and an organic phosphorus compound.
The anti-yellowing agent comprises at least one antioxidant and at least one ultraviolet absorbent;
the antioxidant is selected from one or more of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1010), n-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (antioxidant 1076), tris [2, 4-di-tert-butylphenyl ] phosphite (antioxidant 168), 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane (antioxidant CA), didodecanediol thiodipropionate (antioxidant DLTDP), dilauryl thiodipropionate (antioxidant DLTP), N, N' -di- β -naphthyl p-phenylenediamine (antioxidant DNP), tris (nonylphenyl) phosphite (antioxidant TNP) and triphenyl phosphite (antioxidant TPP);
the ultraviolet absorbent is selected from one or more of 2- (2 ' -hydroxy-5 ' -methylphenyl) benzotriazole (UV-P), 2, 4-dihydroxybenzophenone (UV-O), 2-hydroxy-4-methoxybenzophenone (UV-9), 2-hydroxy-4-n-octoxybenzophenone (UV-531), and 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-phenyl) -5-chlorobenzotriazole (UVP-327).
The release agent is one or a combination of more of synthetic waxes such as mineral wax, vegetable wax, polyethylene or polyamide wax and the like.
The modifier is rubber, organosilane or a combination of one or more of the rubber and the organosilane.
The coupling agent, the coloring agent and the modifying agent can be used for treating the whole material and can also be used for treating the filler.
The whitening agent is ultra-white ultra-pure silicon dioxide, ultra-white ultra-pure aluminum oxide, 2, 5-bis (5-tert-butyl-2-benzoxazolyl) thiophene, 4' -distyrylbiphenyl-2, 2' -disulfonic acid, 1, 4' -bis [2- (o-cyanophenyl) vinyl ] benzene, 2' - (4,4' -distyryl-) bisbenzoxazole or one or more of the materials.
The processing equipment adopts a double-roller open mill, preferably a double-roller open mill with a metal surface plated with ceramic, and more preferably a double-roller open mill with a ceramic roller, so that metal in the equipment is prevented from entering materials through abrasion in the processing process, and yellowing caused by the metal is reduced.
The processing equipment can also adopt a single-screw or double-screw extruder, preferably a double-screw extruder, and more preferably a double-screw extruder with the screw block material of the extruder being metal surface plated with ceramic. Thereby avoiding the metal in the equipment from entering the material through abrasion in the processing process and reducing the yellowing factor of the material.
The processing method comprises the steps of raw material pretreatment, mixing process, cooling, crushing and forming;
the raw material pretreatment comprises the following steps:
1) crushing the epoxy resin: the temperature of the crushing environment is 5-15 ℃, the humidity is less than or equal to 10 percent, and the particle size after crushing is less than or equal to 10 meshes, preferably less than or equal to 60 meshes.
The improper temperature of the crushing environment can cause agglomeration and incapability of crushing; improper humidity can cause the resin to absorb moisture and change properties. The finer the crushing particle size is, the more beneficial the shortening of the processing time is, the blackening of the material caused by the abrasion of processing equipment is reduced, and thus the yellowing resistant effect of the material is improved. The temperature and humidity of the crushing environment and the granularity of the epoxy resin ensure excellent yellowing resistance.
2) Premixing of the filler: mixing the filler in a high-speed mixer (the rotating speed is more than or equal to 100rpm, preferably more than or equal to 500rpm) for more than 5min, preferably more than 10 min; the coupling agent is sprayed into the filler (the rotating speed is more than or equal to 100rpm, preferably more than or equal to 800rpm) and mixed for more than 10min, preferably more than 20 min.
The more uniform the filler is mixed, the more uniform the coupling agent is sprayed, the more favorable the processing time is shortened, and the yellowing resistance effect of the material is improved. The treatment process of the filler ensures the excellent anti-yellowing effect of the material.
3) Pretreatment of phenolic resin and accelerator: premixing the phenolic resin and the accelerant in a reaction kettle at the temperature of 100 ℃ and 200 ℃ for 10-60 min.
The phenolic resin and the accelerator are mixed in advance, so that the later-stage material mixing time can be shortened, and the yellowing resistance effect of the material is improved. The pretreatment of the phenolic resin and the accelerator ensures the excellent yellowing resistance of the materials.
4) Ball milling and crushing the phenolic resin and the additive, wherein the particle size after ball milling and crushing is less than or equal to 10 meshes, preferably less than or equal to 60 meshes.
5) High-speed mixing of all the raw materials after crushing: the raw materials are mixed in a high-speed mixer (at a speed of 100rpm or more, preferably 500rpm or more) for 10min or more, preferably 20min or more.
Compared with the mixing process, the material and equipment are less abraded during high-speed mixing. The mixing processing time can be shortened by improving the uniformity of the materials during high-speed mixing, so that the excellent yellowing resistance effect of the materials is ensured.
The mixing process comprises the following steps:
when the processing equipment adopts a double-roller open mill, the processing conditions are as follows: the roller temperature of the main roller is 30-100 ℃, and the roller temperature of the auxiliary roller is 50-120 ℃; preferably, the roller temperature of the main roller is 50-80 ℃, and the roller temperature of the auxiliary roller is 70-90 ℃; the mixing time is 3-25min, preferably 5-10 min.
When the processing equipment adopts a single-screw extruder or a double-screw extruder, the processing conditions are as follows: the mixing temperature is 70-150 ℃, preferably 90-130 ℃; the mixing time is 1-10min, preferably 2-5 min.
The cooling and crushing process comprises the following steps:
after the mixing procedure, the materials are pressed into sheets and cooled, and the cooling temperature is 0-10 ℃. Too high material of cooling temperature can be very soft, is unfavorable for follow-up smashing, and too low material moisture absorption can result in to the cooling temperature, and the material performance changes.
After cooling, the material is crushed into particles by a crusher, the particle size of the particles is less than or equal to 10 meshes, preferably less than or equal to 20 meshes. The temperature of the pulverizing environment is 0-15 deg.C, and the humidity is 0-55%. Improper particle size can lead to product appearance defects during subsequent forming processes and defects in product applications. Too high temperature of the crushing and forming environment can cause the material to be caked, and too low temperature can cause the material to absorb moisture easily, and the material performance is changed.
The forming process is as follows:
crushing the materials, and then molding, wherein the molding environment temperature is 0-20 ℃. The material of the mould used for mould pressing can be hard alloy, preferably hard alloy with ceramic sprayed on the surface. The friction between metal and materials is reduced to the maximum extent, and the blackening and yellowing resistance of the surface of the product are avoided.
Preferably, the first and second electrodes are formed of a metal,
the light-color yellowing-resistant epoxy resin composition comprises the following components in parts by weight:
4-7.4 parts of epoxy resin A;
4.5-14 parts of curing agent B;
0.05 part of accelerator C;
65-85 parts of inorganic filler D;
0-15 parts of flame retardant E;
5 parts of an anti-yellowing agent F;
0.2 part of release agent G;
0.4 part of coupling agent H;
0.3 part of whitening agent I;
0.15 part of modifier J.
Most preferably, the first and second substrates are,
the light-color yellowing-resistant epoxy resin composition comprises the following components in parts by weight:
4-7.4 parts of epoxy resin A;
9.9-14 parts of curing agent B;
0.05 part of accelerator C;
65-71 parts of inorganic filler D;
1.5-15 parts of a flame retardant E;
5 parts of an anti-yellowing agent F;
0.2 part of release agent G;
0.4 part of coupling agent H;
0.3 part of whitening agent I;
0.15 part of modifier J.
The invention has the following technical effects: the epoxy resin composition processed by the method has the characteristics of light yellow or white color, curing for 4-8 hours at 175 ℃ after molding, and no yellowing of the color after reflow soldering treatment at 260 ℃, and has unexpected technical effects.
Detailed Description
The invention is further illustrated, but is not intended to be limited, by the following specific examples;
the sources of materials used in the examples of the invention and comparative examples are as follows:
epoxy resin A: o-cresol type A1 (available from Yueyang petrochemical)
Curing agent B: novolac B1 (available from santa yunnanensis resin); biphenyl phenolic B2 (from Hunan Jiasheng)
Accelerator C: 2-methylimidazole (available from four nations);
inorganic filler D: crystalline silica D1, fused spherical silica D2 (both available from Feizu birry), alumina D3 (available from Tianjin ze xi), titanium dioxide (available from Australian Fei Lian);
and (3) a flame retardant E: brominated epoxy E1 (available from south asian resins); aluminum hydroxide E2 (Japanese light Metal)
The anti-yellowing agent F is prepared by mixing tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010, Basff brand), β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester (antioxidant 1076, Basff brand), tris [ 2.4-di-tert-butylphenyl ] phosphite (antioxidant 168, Basff brand), 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane (antioxidant CA, Wuhanxin Jiali biotechnology), didodecanediol thiodipropionate (antioxidant DLTDP, Tianjin optical giant limonite chemical industry), dilauryl thiodipropionate (antioxidant DLTP, Beijing Yizhongwei chemical industry), 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole (UV-P, Wuhan Hongyenyuanxin), 2-hydroxy-4-n-octyloxy benzophenone (UV-531, Bahan Kao) and anti-yellowing agent F according to the weight ratio of 1: 1: 1: 1.
And (3) release agent G: carnauba wax (a tree brand);
coupling agent H: KH560 (from jiang su morning light);
whitening agent I: the method comprises the following steps of selecting four compounds of ultra-white ultra-pure silicon dioxide (new Guangzhou Songliner material), ultra-white ultra-pure aluminum oxide (chemical industry of Fushan Xianglong), 2, 5-bis (5-tert-butyl-2-benzoxazolyl) thiophene (biological medicine of Jiangsu Aikang) and 4,4 '-distyrylbiphenyl-2, 2' -disulfonic acid (chemical industry of Beijing Williaceae) according to the proportion of 2: 2: 1: 1 weight ratio to prepare the whitening agent I.
Modifier J: CTBN (U.S. Tao's)
The application effect characterization method comprises the following steps:
the formula is processed into slices, and then post-curing (175 ℃, 4h) and three times of reflow soldering (260 ℃) treatment are carried out.
The reflectivity f1, f2 and f3 of 680nm, 560nm and 420nm are respectively tested by an ultraviolet-visible spectrophotometer.
The introduced yellowing index H indicates the degree of yellowing of the material, and H ═ f1-f3)/f2 × 100, the smaller the numerical value, the worse the yellowing, and the larger the numerical value (close to 100), the better the yellowing resistance.
Table 1: the epoxy resin compositions of examples 1 to 2 were formulated in the unit (g), and in each example, the total weight of the epoxy resin composition was 1000g
| Example 1 | Example 2 | |
| A1 | 74 | 40 |
| B1 | 140 | |
| B2 | 99 | |
| C | 0.5 | 0.5 |
| D1 | 500 | 210 |
| D2 | 440 | |
| D3 | 210 | |
| E1 | 15 | |
| E2 | 150 | |
| F | 50 | 50 |
| G | 2 | 2 |
| H | 4 | 4 |
| I | 3 | 3 |
| J | 1.5 | 1.5 |
Example 1
The kinds and amounts of the respective materials were weighed as in Table 1.
The processing method comprises the steps of raw material pretreatment, mixing process, cooling, crushing and forming;
the processing environment temperature is 5 ℃ and the humidity is 5%.
The raw material pretreatment comprises the following operations:
1) crushing the epoxy resin: crushing the epoxy resin to 60 meshes;
2) premixing of the filler: the filler is mixed in a high-speed mixer at 500rpm for 10min, and the coupling agent is sprayed in at 800rpm for 20 min.
3) Pretreating phenolic resin and an accelerator, and grinding by ball milling: premixing phenolic resin and an accelerator in a reaction kettle at 200 ℃ for 60min, cooling, and ball-milling to 60 meshes;
4) high-speed mixing of all the raw materials after crushing: high-speed mixing of all the raw materials after crushing: mixing the raw materials in a high-speed mixer at 500rpm for 20 min;
the mixing process comprises the following steps:
a double-roller open mill with ceramic rollers, wherein the roller temperature of a main roller is 100 ℃, and the roller temperature of an auxiliary roller is 120 ℃; the mixing time is 10 min;
the cooling and crushing process comprises the following steps:
pressing the materials into sheets after the mixing process and cooling the sheets to 10 ℃;
after cooling, the materials are crushed into 20-mesh particles by a crusher;
the forming process is as follows:
and (3) carrying out compression molding on the material particles, wherein the die used for die pressing is made of hard alloy with the surface sprayed with ceramic.
The product obtained by the process can realize light yellow or white color after being packaged. After molding, the mixture is cured for 4 to 8 hours at 175 ℃ and is subjected to reflow soldering treatment at 260 ℃, and the yellowing index is 56.
Example 2
The kinds and amounts of the respective materials were weighed as in Table 1.
The processing method comprises the steps of raw material pretreatment, mixing process, cooling, crushing and forming;
the processing environment temperature is 5 ℃ and the humidity is 5%.
The raw material pretreatment comprises the following operations:
1) crushing the epoxy resin: crushing the epoxy resin to 60 meshes;
2) premixing of the filler: the filler is mixed in a high-speed mixer at 500rpm for 10min, and the coupling agent is sprayed in at 800rpm for 20 min.
3) Pretreating phenolic resin and an accelerator, and grinding by ball milling: premixing phenolic resin and an accelerator in a reaction kettle at 200 ℃ for 60min, cooling, and ball-milling to 60 meshes;
4) high-speed mixing of all the raw materials after crushing: high-speed mixing of all the raw materials after crushing: mixing the raw materials in a high-speed mixer at 500rpm for 20 min;
the mixing process comprises the following steps:
processing with a double-screw extruder at 130 deg.C for 5 min;
the cooling and crushing process comprises the following steps:
pressing the materials into sheets after the mixing process and cooling the sheets to 10 ℃;
after cooling, the materials are crushed into 20-mesh particles by a crusher;
the forming process is as follows:
and (3) carrying out compression molding on the material particles, wherein the die used for die pressing is made of hard alloy with the surface sprayed with ceramic.
The product obtained by the process can realize light yellow or white color after being packaged. After molding, the mixture is cured for 4 to 8 hours at 175 ℃ and is subjected to reflow soldering treatment at 260 ℃, and the yellowing index is 60.
Comparative example 1
The same formulation as in example 1 was used to process epoxy molding compounds using conventional black epoxy molding compound processing techniques and equipment. The mark is that the equipment is not sprayed with ceramic, the process listed by the invention is not adopted, and the yellowing index is 20.
By comparison, the yellowing indexes of the two examples are 56 and 60, which are far greater than the yellowing index of 20 of the comparative example 1. Therefore, it can be demonstrated that the processing method of the present invention can effectively improve the yellowing resistance of the composition.
Claims (9)
1. A processing method of a light-color yellowing-resistant epoxy resin composition is characterized in that,
the light-color yellowing-resistant epoxy resin composition comprises the following components in parts by weight:
4-25 parts of epoxy resin A;
4-25 parts of a curing agent B;
0.01-3 parts of accelerator C;
15-89 parts of an inorganic filler D;
0-25 parts of flame retardant E;
0-5 parts of an anti-yellowing agent F;
0.05-3 parts of a release agent G;
0.01-3 parts of coupling agent H;
0-10 parts of whitening agent I;
0-3 parts of modifier J;
the epoxy resin is one or more of phenolic aldehyde type epoxy resin, bisphenol A type structure epoxy resin, biphenyl type structure epoxy resin, naphthalene type structure epoxy resin, o-cresol type structure epoxy resin, DCPD type structure epoxy resin, polyfunctional group structure epoxy resin, alicyclic epoxy resin and the like;
the curing agent is one or more of linear phenolic resin, XY-lock type phenolic resin, bisphenol A type phenolic resin, DCPD type phenolic resin, biphenyl type phenolic resin or polyfunctional phenolic resin, anhydride curing agent and alicyclic amine curing agent;
the accelerant is one or more of an organic phosphorus compound, an imidazole compound, a tertiary amine compound and derivatives thereof;
the inorganic filler is one or more of crystalline or fused angle or fused spherical silicon dioxide powder, titanium dioxide powder, alumina powder and magnesia powder;
the flame retardant is one or more of a bromine-containing flame retardant, antimony trioxide, aluminum hydroxide, magnesium hydroxide, zinc borate and an organic phosphorus compound;
the anti-yellowing agent comprises at least one antioxidant and at least one ultraviolet absorbent;
the antioxidant is selected from one or more of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1010), n-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (antioxidant 1076), tris [2, 4-di-tert-butylphenyl ] phosphite (antioxidant 168), 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane (antioxidant CA), didodecanediol thiodipropionate (antioxidant DLTDP), dilauryl thiodipropionate (antioxidant DLTP), N, N' -di- β -naphthyl p-phenylenediamine (antioxidant DNP), tris (nonylphenyl) phosphite (antioxidant TNP) and triphenyl phosphite (antioxidant TPP);
the ultraviolet absorbent is selected from one or more of 2- (2 ' -hydroxy-5 ' -methylphenyl) benzotriazole (UV-P), 2, 4-dihydroxybenzophenone (UV-O), 2-hydroxy-4-methoxybenzophenone (UV-9), 2-hydroxy-4-n-octoxybenzophenone (UV-531), and 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-phenyl) -5-chlorobenzotriazole (UVP-327);
the release agent is one or more of synthetic wax such as mineral wax, vegetable wax, polyethylene or polyamide wax;
the modifier is rubber, organosilane or a combination of one or more of the rubber and the organosilane;
the whitening agent is ultra-white ultra-pure silicon dioxide, ultra-white ultra-pure aluminum oxide, 2, 5-bis (5-tert-butyl-2-benzoxazolyl) thiophene, 4' -distyrylbiphenyl-2, 2' -disulfonic acid, 1, 4' -bis [2- (o-cyanophenyl) vinyl ] benzene, 2' - (4,4' -distyryl-) bisbenzoxazole, or one or a combination of more of the materials;
the processing equipment is a double-roller open mill, a single-screw or double-screw extruder;
the processing method comprises the steps of raw material pretreatment, mixing process, cooling, crushing and forming;
the raw material pretreatment comprises the following operations:
1) crushing the epoxy resin: the temperature of the crushing environment is 5-15 ℃, the humidity is less than or equal to 10 percent, and the granularity after crushing is less than or equal to 10 meshes;
2) premixing of the filler: the filler is mixed in a high-speed mixer for more than 5min at the rotating speed of more than or equal to 100 rpm; spraying the coupling agent into the filler, wherein the rotating speed is more than or equal to 100rpm, and mixing for more than 10 min;
3) pretreatment of phenolic resin and accelerator: premixing phenolic resin and an accelerant in a reaction kettle at the temperature of 100-200 ℃ for 10-60 min;
4) ball milling and crushing the phenolic resin and the additive, wherein the particle size of the crushed phenolic resin and the additive is less than or equal to 10 meshes;
5) high-speed mixing of all the raw materials after crushing: mixing the raw materials in a high-speed mixer at a rotating speed of more than or equal to 100rpm for more than 10 min;
the mixing process comprises the following steps:
when the processing equipment adopts a double-roller open mill, the processing conditions are as follows: the roller temperature of the main roller is 30-100 ℃, and the roller temperature of the auxiliary roller is 50-120 ℃; mixing for 3-25 min;
when the processing equipment adopts a single-screw extruder and a double-screw extruder, the processing conditions are as follows: the mixing temperature is 70-150 ℃; mixing for 1-10 min;
the cooling and crushing process comprises the following steps:
pressing the materials into sheets after the mixing procedure and cooling the sheets at the temperature of 0-10 ℃;
cooling the material, and pulverizing into granules with granularity less than 10 meshes by a pulverizer, wherein the pulverizing environment temperature is 0-15 ℃, and the humidity is 0-55%;
the forming process is as follows:
crushing the materials, and then performing compression molding at the ambient temperature of 0-20 ℃; the material of the mould used for mould pressing can be hard alloy.
2. The method of claim 1, wherein the pre-treatment of the feedstock comprises a size of less than or equal to 60 mesh after the epoxy resin is crushed.
3. The method according to claim 1, wherein the pre-mixing treatment process of the filler in the raw material pretreatment comprises the following steps: the filler is mixed in a high-speed mixer for more than 10min at the rotating speed of more than or equal to 500 rpm; and (3) spraying the coupling agent into the filler, wherein the rotating speed is more than or equal to 800rpm, and mixing for more than 20 min.
4. The method according to claim 1, wherein in the pretreatment of the raw materials, the phenolic resin and the additive are subjected to ball milling and crushing, and the particle size after ball milling and crushing is less than or equal to 60 meshes.
5. The method of claim 1, wherein in the pretreatment of the feedstock, the high speed mixing of all the feedstock after comminution: the raw materials are mixed for more than 20min in a high-speed mixer at a rotating speed of more than or equal to 500 rpm.
6. The method of claim 1, wherein the mixing process comprises:
when the processing equipment adopts a double-roller open mill, the processing conditions are as follows: the roller temperature of the main roller is 50-80 ℃, and the roller temperature of the auxiliary roller is 70-90 ℃; mixing for 5-10 min;
when the processing equipment adopts a single-screw extruder or a double-screw extruder, the processing conditions are as follows: the mixing temperature is 90-130 ℃; the mixing time is 2-5 min.
7. The method of claim 1, wherein said cooling pulverization comprises: after cooling, the material is crushed into particles with the particle size less than or equal to 20 meshes by a crusher.
8. The method of claim 1, wherein the processing equipment is a two-roll mill with a ceramic-coated metal surface.
9. The method of claim 1, wherein the processing equipment is a twin screw extruder having a ceramic-coated metal surface.
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| CN107033546A (en) * | 2017-04-28 | 2017-08-11 | 华南理工大学 | It is a kind of to be used to make epoxy molding plastic of light-reflecting components and preparation method thereof |
| CN107955335A (en) * | 2017-12-25 | 2018-04-24 | 科化新材料泰州有限公司 | A kind of composition epoxy resin preparation method prepared using mixer |
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| CN107033546A (en) * | 2017-04-28 | 2017-08-11 | 华南理工大学 | It is a kind of to be used to make epoxy molding plastic of light-reflecting components and preparation method thereof |
| CN107955335A (en) * | 2017-12-25 | 2018-04-24 | 科化新材料泰州有限公司 | A kind of composition epoxy resin preparation method prepared using mixer |
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