CN113930156A - Organic resin modified organic silicon solvent-free impregnating varnish and preparation method thereof - Google Patents
Organic resin modified organic silicon solvent-free impregnating varnish and preparation method thereof Download PDFInfo
- Publication number
- CN113930156A CN113930156A CN202111321941.1A CN202111321941A CN113930156A CN 113930156 A CN113930156 A CN 113930156A CN 202111321941 A CN202111321941 A CN 202111321941A CN 113930156 A CN113930156 A CN 113930156A
- Authority
- CN
- China
- Prior art keywords
- parts
- resin
- component
- organic resin
- organic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920005989 resin Polymers 0.000 title claims abstract description 142
- 239000011347 resin Substances 0.000 title claims abstract description 142
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 81
- 239000010703 silicon Substances 0.000 title claims abstract description 81
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000002966 varnish Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- 238000007599 discharging Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 12
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 12
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 239000003112 inhibitor Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 230000000536 complexating effect Effects 0.000 claims description 6
- 239000013256 coordination polymer Substances 0.000 claims description 6
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 claims description 6
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000006068 polycondensation reaction Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229920001225 polyester resin Polymers 0.000 claims description 5
- 239000004645 polyester resin Substances 0.000 claims description 5
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 238000007259 addition reaction Methods 0.000 claims description 3
- ZPOLOEWJWXZUSP-AATRIKPKSA-N bis(prop-2-enyl) (e)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C\C(=O)OCC=C ZPOLOEWJWXZUSP-AATRIKPKSA-N 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- JGWUKKFNKOUBPW-UHFFFAOYSA-N 2-ethenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[SiH]1O[SiH2]O[SiH2]O[SiH2]O1 JGWUKKFNKOUBPW-UHFFFAOYSA-N 0.000 claims description 2
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 2
- 239000004962 Polyamide-imide Substances 0.000 claims description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 125000000304 alkynyl group Chemical group 0.000 claims description 2
- ZPOLOEWJWXZUSP-WAYWQWQTSA-N bis(prop-2-enyl) (z)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C/C(=O)OCC=C ZPOLOEWJWXZUSP-WAYWQWQTSA-N 0.000 claims description 2
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229920006122 polyamide resin Polymers 0.000 claims description 2
- 229920002312 polyamide-imide Polymers 0.000 claims description 2
- 229920002530 polyetherether ketone Polymers 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 239000009719 polyimide resin Substances 0.000 claims description 2
- 229920001955 polyphenylene ether Polymers 0.000 claims description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical group [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 claims 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 claims 1
- 238000006459 hydrosilylation reaction Methods 0.000 abstract description 5
- 230000000977 initiatory effect Effects 0.000 abstract description 4
- 230000007246 mechanism Effects 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 2
- 229910004674 SiO0.5 Inorganic materials 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 10
- 239000003973 paint Substances 0.000 description 10
- 238000006266 etherification reaction Methods 0.000 description 9
- 230000006872 improvement Effects 0.000 description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 7
- 238000005886 esterification reaction Methods 0.000 description 6
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 6
- 230000032050 esterification Effects 0.000 description 5
- 230000001976 improved effect Effects 0.000 description 5
- -1 silicon hydrogen Chemical class 0.000 description 5
- 229920002050 silicone resin Polymers 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000001723 curing Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 238000013006 addition curing Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000004246 zinc acetate 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/445—Block-or graft-polymers containing polysiloxane sequences containing polyester sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
- C09D183/12—Block or graft copolymers containing polysiloxane sequences containing polyether sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides organic resin modified organic silicon solvent-free impregnating varnish and a preparation method thereof, belonging to the technical field of organic silicon resin. The organic resin modified organic silicon resin has a structural general formula of (RSiO)1.5)x(MeViSiO)m(MeHSiO)n(R2SiO)k(Me3SiO0.5)y(ii) a Wherein R can be methyl or phenyl, x is an integer of 10-100, y is an integer of 10-40, m is an integer of 10-40, n is an integer of 10-50, and K is an integer of 0-20. The organic resin modified organic silicon solvent-free impregnating varnish disclosed by the invention is an organic silicon insulating varnish product adopting a hydrosilylation curing mechanism in a platinum catalyst initiation system, does not contain any organic solvent, does not precipitate low molecular substances when the impregnating varnish is cured into a film, does not influence the electrical performance, is pollution-free, and belongs to an environment-friendly insulating impregnating resin product.
Description
Technical Field
The invention relates to the technical field of organic silicon resin, in particular to organic resin modified organic silicon solvent-free impregnating varnish and a preparation method thereof.
Background
The organic silicon resin is a common resin at present, is widely applied to the fields of impregnating varnish, paint, mica tape adhesive, modification of organic resin such as polyester and epoxy resin and the like, but has poor mechanical strength, poor adhesion to a base material and easy cracking, so that the organic silicon resin has many limitations in application. The organic resin is introduced into the organic silicon resin through chemical reaction, so that the brittleness of the organic silicon resin is effectively improved, the bonding performance of the organic silicon resin is improved, and the advantages of the organic resin are organically combined with the high heat resistance of the organic silicon.
At present, many organic resin (including polyester resin, epoxy resin, acrylic resin and the like) modified organic silicon resin related products exist, but the organic resin modified organic silicon resin related products are prepared by toluene, xylene or other solvents such as propylene glycol methyl ether acetate, ethanol and the like. The volatilization of the solvent in the using process can bring about the problems of environmental pollution and the like, and the solvent system is limited in some using occasions. The organic resin modified organic silicon solvent-free impregnating varnish product is obtained by adopting a solvent-free system and modifying organic silicon resin, and is cured in a hydrosilylation way.
The organic silicon solvent-free impregnating varnish product is a large application form of organic silicon resin, and has the inherent defects of the organic silicon resin in the application process, low mechanical strength, poor adhesion to a substrate and easy cracking. The patent aims to combine the advantages of organic resin with those of organic silicon resin, introduces organic resin into organic silicon resin, solves the bottleneck problem of low mechanical strength and poor adhesion force in the application process of the organic silicon solvent-free impregnating varnish product, and simultaneously solves the technical problem that organic resin modified organic silicon resin has solvent in the current world.
Disclosure of Invention
The invention aims to provide organic resin modified organic silicon solvent-free impregnating varnish and a preparation method thereof, which form an organic silicon insulating varnish product with a hydrosilylation curing mechanism with a platinum catalyst initiation system.
The technical scheme of the invention is realized as follows:
the invention provides organic resin modified organic silicon solvent-free impregnating varnish, wherein the structural general formula of the organic resin modified organic silicon resin is (RSiO)1.5)x (MeViSiO) m(MeHSiO)n (R2SiO)k (Me3SiO0 .5)y(ii) a Wherein R can be methyl or phenyl, x is an integer of 10-100, y is an integer of 10-40, m is an integer of 10-40, nIs an integer of 10 to 50, and K is an integer of 0 to 20.
The invention is further improved by being prepared from a component A, a component B and organic resin, wherein the component A is prepared from the following raw materials in parts by weight: 800 parts of phenyltrimethoxysilane, 400 parts of methylvinyldimethoxysilane, 200 parts of dimethyldiethoxysilane, 0-100 parts of diphenyldiethoxysilane, 400 parts of hexamethyldisiloxane, 500 parts of toluene, 500 parts of water and 2-5 parts of hydrolysis assistant; the component B is prepared from the following raw materials in parts by weight: 800 parts of phenyltrimethoxysilane, 10-50 parts of methyltrimethoxysilane, 500 parts of methylhydro diethoxysilane, 50-100 parts of dimethyldiethoxysilane, 400 parts of hexamethyldisiloxane, 1000 parts of toluene, 500 parts of water and 2-5 parts of hydrolysis assistant.
As a further improvement of the invention, the mass ratio of the component A to the component B to the organic resin is as follows: the component A comprises: the component B comprises: organic resin = (500-: (100-600): (5-50).
As a further improvement of the invention, the component A or the component B is prepared by the following steps:
(1) adding the toluene, water, hydrolysis assistant and other bed materials into a reaction kettle, starting stirring, and fully mixing;
(2) uniformly mixing other raw materials, and dropwise adding at normal temperature for 1-2 h;
(3) heating the material to 60-80 ℃, and hydrolyzing for 5-8h while keeping stirring;
(4) stopping stirring after the reaction is finished, standing for layering, and adding pure water for washing until the material is neutral;
(5) putting the materials into a reaction kettle, adding a formula amount of polycondensation balance auxiliary agent, heating to a reflux temperature, and concentrating and balancing for 2-4 h;
(6) standing for layering, and washing with water to neutrality;
(7) decompressing to remove toluene solvent, heating to 160-200 ℃, removing low-boiling-point substances under vacuum of below 300Pa, controlling the time to be 1-5h, sampling at certain time intervals during the period to measure the viscosity, and discharging when the material reaches the required viscosity to respectively obtain the resin of the component A or the resin of the component B.
As a further improvement of the invention, the resin of the component A achieves the viscosity of 1000-1500CP at 23 ℃; the component B resin reaches a viscosity of 600-1000 CP at 23 ℃.
As a further improvement of the invention, the hydrolysis auxiliary agent is selected from at least one of hydrochloric acid, sulfuric acid and ammonia water; the balance auxiliary agent is at least one of concentrated sulfuric acid, concentrated nitric acid, p-toluenesulfonic acid and strong acid cation resin.
In a further improvement of the present invention, the organic resin is at least one selected from the group consisting of a polyester resin, an epoxy resin, a polyamide resin, a polyurethane resin, a polyacrylic resin, a polyimide resin, a polyphenylene ether resin, a polyphenylene sulfide resin, a polyamideimide resin, and a polyether ether ketone resin.
The invention further provides a preparation method of the organic resin modified organic silicon solvent-free impregnating varnish, which comprises the steps of mixing organic resin and A, B component for polymerization reaction to obtain modified organic silicon oligomer, adding a platinum catalyst and an inhibitor for addition reaction and curing to obtain the organic resin modified organic silicon solvent-free impregnating varnish.
The reaction equation of the polymerization reaction of the organic resin and the A, B component is as follows, formula (1):
the reaction equation for initiating hydrosilylation reaction curing by a platinum catalyst is as follows, as shown in formula (2):
as a further improvement of the invention, the platinum catalyst is a platinum complex formed by complexing chloroplatinic acid, a Karster catalyst and at least one of nitrogen-containing, phosphorus-containing, sulfur-containing, vinyl compounds or alkynyl-containing groups.
As a further improvement of the invention, the inhibitor is selected from at least one of vinylcyclotetrasiloxane, hexamethyldisilazane, pyridine, pyrrole, triphenylphosphine and 1-ethynylcyclohexanol, 3, 5-dimethyl-3-hexyn-1-ol, 3-methyl-1-butyn-3-ol, diallyl maleate, diallyl fumarate.
The invention has the following beneficial effects: the organic resin modified organic silicon solvent-free impregnating varnish is prepared by the steps of carrying out prepolymerization reaction on organic resin and organic silicon resin in advance, carrying out polymerization reaction on carboxyl or hydroxyl in a molecular chain of the organic resin and silanol in the organic silicon resin to obtain a modified organic silicon oligomer, wherein the molecular chain of the oligomer contains silicon vinyl (Si-Vi) and silicon hydrogen (Si-H) groups, compounding a platinum catalyst and an inhibitor system to obtain an organic resin modified organic silicon impregnating varnish product cured by silicon hydrogen addition reaction initiated by the platinum catalyst, and finally curing the product in a silicon hydrogen addition mode. The introduction of the organic resin can effectively improve the brittleness of the organic resin, improve the bonding performance of the organic resin and organically combine the advantages of the organic resin with the high heat resistance of the organic silicon. The organic resin modified organic silicon solvent-free impregnating varnish and a platinum catalyst initiation system form an organic silicon insulating varnish product based on a hydrosilylation curing mechanism, the product does not contain any organic solvent, no low molecular substance is separated out when the impregnating varnish is cured into a film, the electrical performance is not influenced, no pollution is caused, and the organic resin modified organic silicon solvent-free impregnating varnish belongs to an environment-friendly insulating impregnating resin product.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The component A comprises the following raw materials in parts by weight: 600 parts of phenyltrimethoxysilane, 400 parts of methylvinyldimethoxysilane, 20 parts of dimethyldiethoxysilane, 50 parts of diphenyldiethoxysilane, 200 parts of hexamethyldisiloxane, 800 parts of toluene, 350 parts of water and 3.5 parts of 37% concentrated hydrochloric acid; the component B comprises the following raw materials in parts by weight: 400 parts of phenyltrimethoxysilane, 20 parts of methyltrimethoxysilane, 400 parts of methylhydro-diethoxysilane, 20 parts of dimethyldiethoxysilane, 200 parts of hexamethyldisiloxane, 600 parts of toluene, 200 parts of water and 2 parts of 37% concentrated hydrochloric acid.
The preparation method of the component A or the component B comprises the following steps:
(1) adding toluene, water and hydrochloric acid into a reaction kettle, starting stirring, and fully mixing;
(2) uniformly mixing other raw materials, and dropwise adding at normal temperature within 1 h;
(3) heating the material to 60 ℃, and hydrolyzing for 5 hours while keeping stirring;
(4) stopping stirring after the reaction is finished, standing for layering, and adding pure water for washing until the material is neutral;
(5) putting the materials into a reaction kettle, adding a formula amount of polycondensation balance auxiliary agent p-toluenesulfonic acid, heating to a reflux temperature, concentrating and balancing for 2 hours;
(6) standing for layering, and washing with water to neutrality;
(7) decompressing to remove toluene solvent, heating to 160 ℃, removing low-boiling-point substances under vacuum of below 300Pa, controlling the time to be 1h, sampling at certain time intervals during the period to measure the viscosity, and discharging when the materials reach the required viscosity to respectively obtain the component A or B resin. When the viscosity of the component A reaches 1100CP/23 ℃, discharging, and when the viscosity of the component B reaches 700 CP/23 ℃, discharging.
The preparation method of the organic resin modified organic silicon solvent-free impregnating varnish comprises the following steps: firstly synthesizing organic silicon resin, and then carrying out esterification or etherification reaction on carboxyl or hydroxyl in the organic resin and silanol in the organic silicon resin to obtain the modified resin. Wherein the silicone resin comprises A, B components. The method comprises the following specific steps:
s1, taking 100 parts of organic silicon component A resin and 10 parts of dimethylbenzene unsaturated polyester resin containing carboxylic acid groups, and esterifying at 180 ℃ under the action of zinc acetate. The silicon hydroxyl in the organic silicon resin and the carboxyl in the polyester resin are subjected to esterification reaction to obtain the polyester modified component A resin.
S2, taking the modified organic silicon A, B component resin, preparing paint according to the mass ratio of 1:0.9, adding a platinum complex formed by complexing a vinyl compound of a Kaster catalyst according to 0.01% of the amount of the paint base, adding an inhibitor 1-ethynyl cyclohexanol according to 0.5%, and uniformly stirring to obtain the organic resin modified organic silicon solvent-free impregnating varnish.
Example 2
Firstly synthesizing organic silicon resin, and then carrying out esterification or etherification reaction with carboxyl or hydroxyl in the organic resin and silanol in the organic silicon resin to obtain the modified resin. Wherein the silicone resin comprises A, B components.
The component A comprises the following raw materials in parts by weight: 750 parts of phenyltrimethoxysilane, 300 parts of methylvinyldimethoxysilane, 100 parts of dimethyldiethoxysilane, 0 part of diphenyldiethoxysilane, 250 parts of hexamethyldisiloxane, 900 parts of toluene, 450 parts of water and 4.5 parts of 37% concentrated hydrochloric acid; the component B comprises the following raw materials in parts by weight: 500 parts of phenyltrimethoxysilane, 30 parts of methyltrimethoxysilane, 450 parts of methylhydro-diethoxysilane, 100 parts of dimethyldiethoxysilane, 300 parts of hexamethyldisiloxane, 650 parts of toluene, 300 parts of water and 3 parts of 37% concentrated hydrochloric acid.
The preparation method of the component A or the component B comprises the following steps:
(1) adding toluene, water and hydrochloric acid in a formula amount into a reaction kettle, starting stirring, and fully mixing;
(2) uniformly mixing other raw materials, and dropwise adding at normal temperature for 2 h;
(3) heating the material to 80 ℃, and hydrolyzing for 8 hours while keeping stirring;
(4) stopping stirring after the reaction is finished, standing for layering, and adding pure water for washing until the material is neutral;
(5) putting the materials into a reaction kettle, adding a polycondensation balance auxiliary agent, namely strong acid cation resin, according to the formula amount, heating to a reflux temperature, and concentrating and balancing for 4 hours;
(6) standing for layering, and washing with water to neutrality;
(7) decompressing to remove toluene solvent, heating to 200 ℃, removing low-boiling-point substances under vacuum of below 300Pa, controlling the time to be 5h, sampling at certain time intervals during the period to measure the viscosity, and discharging when the materials reach the required viscosity to respectively obtain the component A or B resin. When the viscosity of the component A reaches 1500CP/23 ℃, discharging, and when the viscosity of the component B reaches 1000 CP/23 ℃, discharging.
The preparation method of the organic resin modified organic silicon solvent-free impregnating varnish comprises the following steps: firstly synthesizing organic silicon resin, and then carrying out esterification or etherification reaction on carboxyl or hydroxyl in the organic resin and silanol in the organic silicon resin to obtain the modified resin. Wherein the silicone resin comprises A, B components. The method comprises the following specific steps:
s1, under the action of concentrated sulfuric acid, 200g of organic silicon component A resin and 15g of E-44 epoxy resin containing hydroxyl are taken, the etherification temperature is 210 ℃, and the silicon hydroxyl in the organic silicon resin and the hydroxyl in the epoxy resin are subjected to etherification reaction to obtain epoxy resin modified component A resin.
S2, taking the modified organic silicon A, B component resin, preparing paint according to the mass ratio of 1:1.2, adding a platinum complex formed by complexing a vinyl compound of a Kaster catalyst according to 0.01% of the amount of the paint base, adding an inhibitor diallyl fumarate according to 0.1%, and uniformly stirring to obtain the organic resin modified organic silicon solvent-free impregnating varnish.
Example 3
Firstly synthesizing organic silicon resin, and then carrying out esterification or etherification reaction with carboxyl or hydroxyl in the organic resin and silanol in the organic silicon resin to obtain the modified resin. Wherein the silicone resin comprises A, B components.
The component A comprises the following raw materials in parts by weight: 800 parts of phenyltrimethoxysilane, 400 parts of methylvinyldimethoxysilane, 50 parts of dimethyldiethoxysilane, 50 parts of diphenyldiethoxysilane, 400 parts of hexamethyldisiloxane, 1000 parts of toluene, 500 parts of water and 5 parts of 25% ammonia water; the component B comprises the following raw materials in parts by weight: 800 parts of phenyltrimethoxysilane, 50 parts of methyltrimethoxysilane, 500 parts of methylhydro-diethoxysilane, 80 parts of dimethyldiethoxysilane, 300 parts of hexamethyldisiloxane, 900 parts of toluene, 450 parts of water and 5 parts of 25% ammonia water.
The preparation method of the component A or the component B comprises the following steps:
(1) adding toluene, water and ammonia water in a formula amount into a reaction kettle, starting stirring, and fully mixing;
(2) uniformly mixing other raw materials, and dropwise adding at normal temperature within 1.5 h;
(3) heating the material to 70 ℃, and hydrolyzing for 6.5 hours under stirring;
(4) stopping stirring after the reaction is finished, standing for layering, and adding pure water for washing until the material is neutral;
(5) putting the materials into a reaction kettle, adding a polycondensation balance auxiliary agent concentrated sulfuric acid with a formula amount, heating to a reflux temperature, and concentrating and balancing for 3 hours;
(6) standing for layering, and washing with water to neutrality;
(7) decompressing to remove toluene solvent, heating to 180 ℃, removing low-boiling-point substances under vacuum of below 300Pa, controlling the time to be 5h, sampling at certain time intervals during the period to measure the viscosity, and discharging when the materials reach the required viscosity to respectively obtain the component A or B resin. When the viscosity of the component A reaches 1300CP/23 ℃, discharging, and when the viscosity of the component B reaches 800 CP/23 ℃, discharging.
The preparation method of the organic resin modified organic silicon solvent-free impregnating varnish comprises the following steps: firstly synthesizing organic silicon resin, and then carrying out esterification or etherification reaction on carboxyl or hydroxyl in the organic resin and silanol in the organic silicon resin to obtain the modified resin. Wherein the silicone resin comprises A, B components. The method comprises the following specific steps:
s1, taking 150g of organic silicon component resin B and 20g of polyethylene glycol PEG-400 resin containing terminal hydroxyl, and carrying out etherification reaction on silicon hydroxyl in the organic silicon resin and hydroxyl in polyether resin at the etherification temperature of 200 ℃ under the action of tetrabutyl orthotitanate to obtain polyether resin modified component B resin.
S2, taking the modified organic silicon A, B component resin, preparing paint according to the mass ratio of 1:1, adding a platinic chloride acid catalyst vinyl compound according to 0.05% of the amount of the paint base, complexing to form a platinum complex, adding an inhibitor triphenylphosphine according to 0.1%, and uniformly stirring to obtain the organic resin modified organic silicon solvent-free impregnating varnish.
Comparative example 1
To compare the improved effect, the experimental formulation of example 1 was chosen for comparison, except that no organic resin modifying component was added to the paint formulation, and the rest was the same as in example 1.
The component A comprises the following raw materials in parts by weight: 600 parts of phenyltrimethoxysilane, 400 parts of methylvinyldimethoxysilane, 20 parts of dimethyldiethoxysilane, 50 parts of diphenyldiethoxysilane, 200 parts of hexamethyldisiloxane, 800 parts of toluene, 350 parts of water and 3.5 parts of 37% concentrated hydrochloric acid; the component B comprises the following raw materials in parts by weight: 400 parts of phenyltrimethoxysilane, 20 parts of methyltrimethoxysilane, 400 parts of methylhydro-diethoxysilane, 20 parts of dimethyldiethoxysilane, 200 parts of hexamethyldisiloxane, 600 parts of toluene, 200 parts of water and 2 parts of 37% concentrated hydrochloric acid.
The preparation method of the component A or the component B comprises the following steps:
(1) adding toluene, water and hydrochloric acid into a reaction kettle, starting stirring, and fully mixing;
(2) uniformly mixing other raw materials, and dropwise adding at normal temperature within 1 h;
(3) heating the material to 60 ℃, and hydrolyzing for 5 hours while keeping stirring;
(4) stopping stirring after the reaction is finished, standing for layering, and adding pure water for washing until the material is neutral;
(5) putting the materials into a reaction kettle, adding a formula amount of polycondensation balance auxiliary agent p-toluenesulfonic acid, heating to a reflux temperature, concentrating and balancing for 2 hours;
(6) standing for layering, and washing with water to neutrality;
(7) decompressing to remove toluene solvent, heating to 160 ℃, removing low-boiling-point substances under vacuum of below 300Pa, controlling the time to be 1h, sampling at certain time intervals during the period to measure the viscosity, and discharging when the materials reach the required viscosity to respectively obtain the component A or B resin. When the viscosity of the component A reaches 1100CP/23 ℃, discharging, and when the viscosity of the component B reaches 700 CP/23 ℃, discharging.
Preparing paint from organic silicon A, B component resin according to the mass ratio of 1:0.9, adding a platinum complex formed by complexing a vinyl compound of a Kaster catalyst according to 0.01% of the amount of the paint base, adding an inhibitor 1-ethynyl cyclohexanol according to 0.5%, and uniformly stirring to obtain the organic silicon solvent-free impregnating varnish.
Test example 1
The organic resin modified organic silicon solvent-free impregnating varnish prepared in the embodiment 1 and the comparative example 1 of the invention is subjected to performance test, the result is shown in the table 1, and the bonding force of the modified organic silicon resin is obviously improved from the table 1.
TABLE 1 comparison of conventional Properties before and after modification
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The organic resin modified organic silicon solvent-free impregnating varnish is characterized in that the structural general formula of the organic resin modified organic silicon resin is (RSiO)1.5)x (MeViSiO) m(MeHSiO)n (R2SiO)k (Me3SiO0 .5)y(ii) a Wherein R can be methyl or phenyl, x is an integer of 10-100, y is an integer of 10-40, m is an integer of 10-40, n is an integer of 10-50, and K is an integer of 0-20.
2. The organic resin modified organic silicon solvent-free impregnating varnish according to claim 1, which is characterized by being prepared from a component A, a component B and organic resin, wherein the component A is prepared from the following raw materials in parts by weight: 800 parts of phenyltrimethoxysilane, 400 parts of methylvinyldimethoxysilane, 200 parts of dimethyldiethoxysilane, 0-100 parts of diphenyldiethoxysilane, 400 parts of hexamethyldisiloxane, 500 parts of toluene, 500 parts of water and 2-5 parts of hydrolysis assistant; the component B is prepared from the following raw materials in parts by weight: 800 parts of phenyltrimethoxysilane, 10-50 parts of methyltrimethoxysilane, 500 parts of methylhydro diethoxysilane, 50-100 parts of dimethyldiethoxysilane, 400 parts of hexamethyldisiloxane, 1000 parts of toluene, 500 parts of water and 2-5 parts of hydrolysis assistant.
3. The organic resin modified silicone solvent-free impregnating varnish according to claim 2, wherein the mass ratio of the component A, the component B and the organic resin is as follows: the component A comprises: the component B comprises: organic resin = (500-: (100-600): (5-50).
4. The organic resin modified silicone solventless impregnating varnish according to claim 2, wherein the component A or the component B is prepared by the following steps:
adding the toluene, water, hydrolysis assistant and other bed materials into a reaction kettle, starting stirring, and fully mixing;
uniformly mixing other raw materials, and dropwise adding at normal temperature for 1-2 h;
heating the material to 60-80 ℃, and hydrolyzing for 5-8h while keeping stirring;
stopping stirring after the reaction is finished, standing for layering, and adding pure water for washing until the material is neutral;
putting the materials into a reaction kettle, adding a formula amount of polycondensation balance auxiliary agent, heating to a reflux temperature, and concentrating and balancing for 2-4 h;
standing for layering, and washing with water to neutrality;
decompressing to remove toluene solvent, heating to 160-200 ℃, removing low-boiling-point substances under vacuum of below 300Pa, controlling the time to be 1-5h, sampling at certain time intervals during the period to measure the viscosity, and discharging when the material reaches the required viscosity to respectively obtain the resin of the component A or the resin of the component B.
5. The organic resin modified silicone solvent-free impregnating varnish according to claim 4, wherein the A component resin achieves a viscosity of 1000-1500CP at 23 ℃; the component B resin reaches a viscosity of 600-1000 CP at 23 ℃.
6. The organic resin modified silicone solventless impregnating varnish according to claim 4, wherein the hydrolysis aid is at least one selected from the group consisting of hydrochloric acid, sulfuric acid, and ammonia; the balance auxiliary agent is at least one of concentrated sulfuric acid, concentrated nitric acid, p-toluenesulfonic acid and strong acid cation resin.
7. The organic resin-modified silicone solventless impregnating varnish according to claim 4, wherein the organic resin is at least one selected from the group consisting of polyester resins, epoxy resins, polyamide resins, polyurethane resins, polyacrylic resins, polyimide resins, polyphenylene ether resins, polyphenylene sulfide resins, polyamideimide resins, and polyether ether ketone resins.
8. A process for preparing the organic resin modified silicone solventless impregnating varnish according to any one of claims 1 to 7, wherein the organic resin is mixed with A, B component to undergo polymerization reaction to obtain modified silicone oligomer, and then platinum catalyst and inhibitor are added to undergo addition reaction to cure to obtain the organic resin modified silicone solventless impregnating varnish.
9. The production method according to claim 8, wherein the platinum catalyst is a platinum-gold complex formed by complexing chloroplatinic acid, a kast catalyst, and at least one of nitrogen-containing, phosphorus-containing, sulfur-containing, vinyl-containing compounds, or alkynyl-containing groups.
10. The method according to claim 8, wherein the inhibitor is at least one selected from the group consisting of vinylcyclotetrasiloxane, hexamethyldisilazane, pyridine, pyrrole, triphenylphosphine, and 1-ethynylcyclohexanol, 3, 5-dimethyl-3-hexyn-1-ol, 3-methyl-1-butyn-3-ol, diallyl maleate, and diallyl fumarate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111321941.1A CN113930156A (en) | 2021-11-09 | 2021-11-09 | Organic resin modified organic silicon solvent-free impregnating varnish and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111321941.1A CN113930156A (en) | 2021-11-09 | 2021-11-09 | Organic resin modified organic silicon solvent-free impregnating varnish and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113930156A true CN113930156A (en) | 2022-01-14 |
Family
ID=79286216
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111321941.1A Pending CN113930156A (en) | 2021-11-09 | 2021-11-09 | Organic resin modified organic silicon solvent-free impregnating varnish and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113930156A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4404348A (en) * | 1981-08-12 | 1983-09-13 | Rhone-Poulenc Specialites Chimiques | Solventless organosilicon coating/impregnating compositions |
| CN102504265A (en) * | 2011-11-03 | 2012-06-20 | 杭州吉华高分子材料有限公司 | Method for preparing polyester modified organic silicon resin and coating containing the resin |
| CN104448329A (en) * | 2014-12-05 | 2015-03-25 | 四川东材科技集团股份有限公司 | Preparation methods of phenolic epoxy-organic silicone resin and heat-resistant insulating impregnating varnish thereof |
| CN105295720A (en) * | 2015-11-03 | 2016-02-03 | 株洲时代新材料科技股份有限公司 | Preparation method for organic silicon impregnating varnish |
-
2021
- 2021-11-09 CN CN202111321941.1A patent/CN113930156A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4404348A (en) * | 1981-08-12 | 1983-09-13 | Rhone-Poulenc Specialites Chimiques | Solventless organosilicon coating/impregnating compositions |
| CN102504265A (en) * | 2011-11-03 | 2012-06-20 | 杭州吉华高分子材料有限公司 | Method for preparing polyester modified organic silicon resin and coating containing the resin |
| CN104448329A (en) * | 2014-12-05 | 2015-03-25 | 四川东材科技集团股份有限公司 | Preparation methods of phenolic epoxy-organic silicone resin and heat-resistant insulating impregnating varnish thereof |
| CN105295720A (en) * | 2015-11-03 | 2016-02-03 | 株洲时代新材料科技股份有限公司 | Preparation method for organic silicon impregnating varnish |
Non-Patent Citations (5)
| Title |
|---|
| 尤小姿等: "环氧改性硅树脂的制备与性能研究", 《绝缘材料》 * |
| 徐滨士等: "《表面工程新技术》", 31 January 2002, 国防工业出版社 * |
| 王雅丽等: "对苯二甲酸型聚酯改性的有机硅漆", 《工程塑料应用》 * |
| 甘肃油漆厂涂料工业研究所第三研究室: "有机硅树脂的研究", 《涂料工业》 * |
| 章基凯: "《有机硅材料》", 31 October 1999, 中国物资出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110591375B (en) | High-performance epoxy-silicone rubber modified material with interpenetrating network structure | |
| CN107779091B (en) | Organosiloxane compositions and coatings, articles, methods and uses | |
| CN109054734B (en) | Adhesive prepared based on amino-containing siloxane and preparation and use methods thereof | |
| CN106590501B (en) | Single-component epoxy modified organosilicon sealant and preparation method thereof | |
| CN110527300B (en) | High-strength epoxy-silicone rubber modified material with interpenetrating network structure | |
| CN114262550B (en) | Silane modified acrylic resin, synthesis method and primer for silicone rubber | |
| CN112679958A (en) | Silicon rubber and preparation method thereof, and piezoresistor and preparation method thereof | |
| CN113881377B (en) | Anhydride-curable organic silicon modified epoxy resin pouring sealant and preparation method thereof | |
| CN102492116A (en) | Epoxy resin and polyhedral silsesquioxane nano hybrid material and its preparation method | |
| CN112280044B (en) | Low-viscosity high-strength toughened silicone resin composition and preparation method thereof | |
| CN110564162B (en) | Epoxy resin-silicone rubber composite material with cross-linked extended interpenetrating network structure and preparation method thereof | |
| CN108329474B (en) | Organic silicon resin for single-component addition type organic silicon impregnating varnish and preparation method and application thereof | |
| CN114502610A (en) | Oxygen-curable silicone composition and cured product thereof | |
| CN113652193A (en) | High-strength flowing silica gel and preparation method and application thereof | |
| JPS5927952A (en) | Epoxy resin-modified silicone resin composition | |
| CN113930156A (en) | Organic resin modified organic silicon solvent-free impregnating varnish and preparation method thereof | |
| CN112646545A (en) | Self-adhesive liquid silicone rubber preparation capable of spraying and preparation method thereof | |
| CN115584204B (en) | Ultralow release force organic silicon UV coating | |
| US20200299462A1 (en) | Method for preparing ultraviolet (uv) curing polymethyl siloxane containing acrylate structure | |
| CN111499870A (en) | Boiling-resistant organic silicon pressure-sensitive adhesive tackifier and preparation method thereof | |
| Wei et al. | Cycloaliphatic epoxy-functionalized polydimethylsiloxanes for comprehensive modifications of epoxy thermosets | |
| CN110790936A (en) | Dual-curing organic silicon resin and preparation method thereof | |
| CN108219137B (en) | Addition type organic silicon resin and preparation method and application thereof | |
| CN111040168A (en) | Epoxy modified organic silicon resin and preparation method thereof | |
| JP3681582B2 (en) | Epoxy group-containing silicone resin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220114 |