CN104356894B - A kind of preparation method of high-temperature resistant silicone modified unsaturated polyester resin coating - Google Patents
A kind of preparation method of high-temperature resistant silicone modified unsaturated polyester resin coating Download PDFInfo
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- CN104356894B CN104356894B CN201410615096.2A CN201410615096A CN104356894B CN 104356894 B CN104356894 B CN 104356894B CN 201410615096 A CN201410615096 A CN 201410615096A CN 104356894 B CN104356894 B CN 104356894B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 21
- 239000011248 coating agent Substances 0.000 title claims abstract description 18
- 238000000576 coating method Methods 0.000 title claims abstract description 18
- 229920006337 unsaturated polyester resin Polymers 0.000 title claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920006305 unsaturated polyester Polymers 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 229920006334 epoxy coating Polymers 0.000 claims abstract description 15
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004576 sand Substances 0.000 claims abstract description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 12
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical class OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003822 epoxy resin Substances 0.000 claims abstract description 11
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 235000011037 adipic acid Nutrition 0.000 claims abstract description 7
- 239000001361 adipic acid Substances 0.000 claims abstract description 7
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003801 milling Methods 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 6
- 125000000524 functional group Chemical group 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- KMOUUZVZFBCRAM-UHFFFAOYSA-N 1,2,3,6-tetrahydrophthalic anhydride Chemical compound C1C=CCC2C(=O)OC(=O)C21 KMOUUZVZFBCRAM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000003085 diluting agent Substances 0.000 claims abstract description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 3
- UFDHBDMSHIXOKF-UHFFFAOYSA-N tetrahydrophthalic acid Natural products OC(=O)C1=C(C(O)=O)CCCC1 UFDHBDMSHIXOKF-UHFFFAOYSA-N 0.000 claims abstract description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000010445 mica Substances 0.000 claims description 10
- 229910052618 mica group Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000440 bentonite Substances 0.000 claims description 8
- 229910000278 bentonite Inorganic materials 0.000 claims description 8
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 7
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 150000003384 small molecules Chemical class 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- BPYFPNZHLXDIGA-UHFFFAOYSA-N diphenylsilicon Chemical compound C=1C=CC=CC=1[Si]C1=CC=CC=C1 BPYFPNZHLXDIGA-UHFFFAOYSA-N 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 229920000728 polyester Polymers 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 238000010790 dilution Methods 0.000 abstract description 4
- 239000012895 dilution Substances 0.000 abstract description 4
- -1 after agitated Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 3
- 239000002952 polymeric resin Substances 0.000 abstract description 2
- 229920003002 synthetic resin Polymers 0.000 abstract description 2
- 238000009396 hybridization Methods 0.000 abstract 1
- 229960004063 propylene glycol Drugs 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
-
- 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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- 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
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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Compositions Of Macromolecular Compounds (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating, comprises the following steps: (1), with the alkoxyorganosilicon of two functional groups and trifunctional for mixing raw material, through hydrolytic condensation, synthesizes organic-silicone prepolymer；(2) with 1,2 propylene glycol, 1,4 butanediols, adipic acid, THPA and maleic anhydride for Material synthesis unsaturated polyester (UP)；Add organosilicon performed polymer and epoxy resin E 51, proceed graft reaction, be eventually adding reactive diluent dilution, i.e. can get tri compound resin；(3) the inorganic mixed fillers mixed by a certain percentage is mixed with above-mentioned tri compound resin, after agitated, sand milling, prepare finely disseminated high-temperature resistant silicone unsaturated polyester resin epoxy coating.Preparation method of the present invention is simple, and prepared high-temperature resistant silicone unsaturated polyester resin epoxy coating is the high-performance organic inorganic hybridization composite of a kind of excellent combination property.
Description
Technical field
The present invention relates to the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating；Belong to the preparing technical field of high-performance organic-inorganic hybrid composite material.
Background technology
High-temperature resistant coating refers to paint film invariant color more than 300 DEG C, does not falls off, and remains to keep the coating of suitable physical mechanical performance, and it has broad application prospects at modern industry, military affairs, space industry.Unsaturated polyester resin production technology is easy, and raw material is easy to get, and can at room temperature solidify, normal pressure compacted under.Not only having the resistance to chemical corrosion of excellence after goods are cured, also have good mechanical property, proportion is the most relatively small.Epoxy resin be a class have good bonding, corrosion-resistant,
The thermosetting polymer synthetic material of the performances such as insulation, high intensity.These advantages allow unsaturated polyester resin and epoxy resin by the common concern of industry, have obtained applying more at industrial circle.But, the heat resistance of both resins is the most bad, is typically suitable only at 160 DEG C use, and goods weatherability is poor.Therefore, improve the high temperature resistant of goods by modes such as chemical modification and inorganic filler blending and weather resistance becomes the effective way improving resin property.Organic siliconresin also referred to as polysiloxanes is that a class is alternately linked the general designation forming the polymer that skeleton, different organic groups link again with silicon atom by silicon atom and oxygen atom.Both containing " organic group " in its molecular structure, and contained again " inorganic structure ", this special composition and molecular structure make it integrate Characteristics of Organic and inorganic matter function.One of advantage that organic siliconresin is the most prominent has the thermo oxidative stability of excellence exactly, after 250 DEG C are heated 24 hours, silicones weightlessness is only 2-8%, the most also has the advantage such as good weatherability properties and electrical insulating property, can be widely used for the field such as high-temperaure coating and insulating protection.But the adhesive property of organic siliconresin is poor, need to improve its adhesiveness by modification.
Summary of the invention
It is an object of the invention to, there is the problems such as weatherability difference for existing high-temperature resistant coating, the present invention provides the preparation method of a kind of high-temperature resistant silicone-unsaturated polyester resin-epoxy coating, the high-temperature resistant coating that the method is prepared not only has good high temperature resistant, weather resistance, also has good waterproof, anticorrosion and adhesive property.
The molecular structure of organic siliconresin is incorporated in the middle of unsaturated polyester (UP) and epoxy resin by the method for MOLECULE DESIGN by the present invention, prepare a kind of high temperature resistant and weatherability tri compound of good performance macromolecule resin, afterwards the inorganic high-temperature resistant fillers such as this modified resin and hollow glass micropearl, glass dust, mica powder, silicon powder are mixed, prepare and can be resistant to 500 DEG C of high temperature above by resistant to elevated temperatures organosilicon-unsaturated polyester resin-epoxy coating, thus widened macromolecule resin as the range of high-temperature resistant coating and application.
The technical scheme is that the preparation method of a kind of high-temperature resistant silicone-unsaturated polyester resin-epoxy coating of the present invention comprises the following steps:
(1) with the alkoxyorganosilicon of two functional groups and trifunctional for mixing raw material, through hydrolytic condensation, organic-silicone prepolymer is first synthesized.
(2) with 1,2-propylene glycol, 1,4-butanediol, adipic acid, THPA and maleic anhydride are Material synthesis unsaturated polyester (UP), organosilicon performed polymer and epoxy resin E-51 is added when the synthesis of unsaturated polyester resin is nearly completed, proceed the graft reaction between resin, it is eventually adding reactive diluent styrene to carry out with it being sufficiently mixed, diluting, i.e. can get tri compound resin.
(3) hollow glass micropearl mixed by a certain percentage, mica powder, Pulvis Talci, bentonite are mixed with above-mentioned tri compound resin, after homogenizer is sufficiently stirred for sand milling with sand mill, prepares finely disseminated high-temperature resistant silicone-unsaturated polyester resin-epoxy coating.
In the methods of the invention, the alkoxyorganosilicon of two functional groups and trifunctional is two or more in MTES, dimethoxydiphenylsilane, diphenyl silanediol, VTES and phenyltrimethoxysila,e.Preferably diphenyl silanediol, phenyltrimethoxysila,e, its mass ratio of MTES is: 1:(0.37-5.29): (1.65-6.34), be preferably in a proportion of: 1:2.3:4.12.
In the methods of the invention, selected epoxy resin is E-12, the one in E-20, E-21, E-44, E-51, preferably E-51；
In the methods of the invention, selected inorganic filler is more than three kinds in particle diameter hollow glass micropearl between 10-100 μm, glass dust, mica powder, silicon powder, montmorillonite, Pulvis Talci, preferably hollow glass micropearl, mica powder, Pulvis Talci, bentonite.Its mass ratio is 1:(0.1-0.5): (0.1-0.6): (0.05-0.40) preferred mass is than for 1:0.3:0.2:0.15.
In the methods of the invention, the ratio of tri compound resin and inorganic mixed fillers is 1:0.15-0.5, and preferred mass ratio is for 1:0.42.
The invention has the beneficial effects as follows, preparation method of the present invention is simple, and prepared high-temperature resistant silicone-unsaturated polyester resin-epoxy coating not only has good high temperature resistant, weather resistance, also has good waterproof, anticorrosion and adhesive property.It it is the high-performance organic-inorganic hybrid composite material of a kind of excellent combination property.
Detailed description of the invention
Embodiment 1:
(1) synthesis of organosilicon performed polymer
Accurately weigh 74.2 grams of dehydrated alcohol, 41.2 grams of MTESs, 10.0 grams and 23.0 grams phenyltrimethoxysila,e of diphenyl silanediol, be injected separately in the there-necked flask presetting stirring and condensing plant.Bath temperature being set to 50 DEG C, is under agitation slowly dropped into the deionized water 22.3 grams that appropriate PH is 4 in there-necked flask, dropping in 1.5 hours is complete, is warming up to 120 DEG C afterwards and continues reaction 1 hour.Finally decompression removes dehydrated alcohol, residual moisture and low molecular weight substance, i.e. can get organosilicon performed polymer.
(2) preparation of organosilicon-unsaturated polyester resin-epoxy resin
nullBy 7.5 gram 1,2-propylene glycol、11.6 gram 1,4-butanediol、5.7 g of adipic acid、20 grams of THPAs and 35 grams of maleic anhydrides put in there-necked flask，It is placed on digital display thermal-arrest magnetic stirring apparatus，Install condensation reflux unit additional，It is heated to 160 DEG C of back flow reaction 40min，Then heat to 200 DEG C，90 DEG C it are cooled to when system acid number reaches 15mgKOH/g，It is sequentially added into 20 grams of organosilicon performed polymers、10 grams of E-51 and 3.6 grams of zinc Isoocatanoates，Again it is warmed up to 120 DEG C of reaction 1h，It is cooled to the water in 100 DEG C of evacuation removing systems and other small molecule by-product afterwards，It is eventually adding 50 grams dissolved with 0.036 gram of hydroquinone、The styrene of 0.15 gram of benzoyl peroxide is sufficiently mixed with it、Dilution，I.e. can get tri compound resin.
(3) preparation of high-temperature resistant silicone-unsaturated polyester resin-epoxy coating
Accurately weigh hollow glass micropearl 25 grams, mica powder 7.5 grams, Pulvis Talci 5.0 grams, bentonite 3.8 grams, put into mix and blend 30 minutes in homogenizer, put into 98.3 grams of tri compound resins afterwards and be sufficiently mixed；Then the compound after above-mentioned stirring is injected in sand mill and carry out abundant sand milling 1.5 hours, i.e. can get high-temperature resistant silicone-unsaturated polyester resin-epoxy coating.
Embodiment 2:
(1) synthesis of organosilicon performed polymer
Accurately weigh 45 grams of dehydrated alcohol, 20.0 grams of MTESs, diphenyl silanediol 10.0 grams and, 15.0 grams of phenyltrimethoxysila,e, be injected separately in the there-necked flask presetting stirring and condensing plant.Bath temperature being set to 50 DEG C, is under agitation slowly dropped into the deionized water 13.5 grams that appropriate PH is 4 in there-necked flask, dropping in 1.5 hours is complete, is warming up to 120 DEG C afterwards and continues reaction 1 hour.Finally decompression removes dehydrated alcohol, residual moisture and low molecular weight substance, i.e. can get organosilicon performed polymer.
(2) preparation of organosilicon-unsaturated polyester resin-epoxy resin
nullBy 7.5 gram 1,2-propylene glycol、11.6 gram 1,4-butanediol、5.7 g of adipic acid、20 grams of THPAs and 35 grams of maleic anhydrides put in there-necked flask，It is placed on digital display thermal-arrest magnetic stirring apparatus，Install condensation reflux unit additional，It is heated to 160 DEG C of back flow reaction 40min，Then heat to 200 DEG C，90 DEG C it are cooled to when system acid number reaches 15mgKOH/g，It is sequentially added into 20 grams of organosilicon performed polymers、10 grams of E-51 and 3.6 grams of zinc Isoocatanoates，Again it is warmed up to 120 DEG C of reaction 1h，It is cooled to the water in 100 DEG C of evacuation removing systems and other small molecule by-product afterwards，It is eventually adding 55 grams dissolved with 0.04 gram of hydroquinone、The styrene of 0.17 gram of benzoyl peroxide is sufficiently mixed with it、Dilution，I.e. can get tri compound resin.
(3) preparation of high-temperature resistant silicone-unsaturated polyester resin-epoxy coating
Accurately weigh hollow glass micropearl 10 grams, mica powder 2.0 grams, Pulvis Talci 3.0 grams, bentonite 1.5 grams, put into mix and blend 30 minutes in homogenizer, put into 55 grams of tri compound resins afterwards and be sufficiently mixed；Then the compound after above-mentioned stirring is injected in sand mill and carry out abundant sand milling 1.5 hours, i.e. can get high-temperature resistant silicone-unsaturated polyester resin-epoxy coating.
Embodiment 3:
(1) synthesis of organosilicon performed polymer
Accurately weigh 55 grams of dehydrated alcohol, 25.0 grams of MTESs, 10.0 grams and 30.0 grams phenyltrimethoxysila,e of diphenyl silanediol, be injected separately in the there-necked flask presetting stirring and condensing plant.Bath temperature being set to 50 DEG C, is under agitation slowly dropped into the deionized water 19.5 grams that appropriate PH is 4 in there-necked flask, dropping in 1.5 hours is complete, is warming up to 120 DEG C afterwards and continues reaction 1 hour.Finally decompression removes dehydrated alcohol, residual moisture and low molecular weight substance, i.e. can get organosilicon performed polymer.
(2) preparation of organosilicon-unsaturated polyester resin-epoxy resin
nullBy 7.5 gram 1,2-propylene glycol、11.6 gram 1,4-butanediol、5.7 g of adipic acid、20 grams of THPAs and 35 grams of maleic anhydrides put in there-necked flask，It is placed on digital display thermal-arrest magnetic stirring apparatus，Install condensation reflux unit additional，It is heated to 160 DEG C of back flow reaction 40min，Then heat to 200 DEG C，90 DEG C it are cooled to when system acid number reaches 15mgKOH/g，It is sequentially added into 15 grams of organosilicon performed polymers、15 grams of E-51 and 3.6 grams of zinc Isoocatanoates，Again it is warmed up to 120 DEG C of reaction 1h，It is cooled to the water in 100 DEG C of evacuation removing systems and other small molecule by-product afterwards，It is eventually adding 45 grams dissolved with 0.03 gram of hydroquinone、The styrene of 0.14 gram of benzoyl peroxide is sufficiently mixed with it、Dilution，I.e. can get tri compound resin.
(3) preparation of high-temperature resistant silicone-unsaturated polyester resin-epoxy coating
Accurately weigh hollow glass micropearl 10 grams, mica powder 4.0 grams, Pulvis Talci 5.0 grams, bentonite 3.0 grams, put into mix and blend 30 minutes in homogenizer, put into 62.9 grams of tri compound resins afterwards and be sufficiently mixed；Then the compound after above-mentioned stirring is injected in sand mill and carry out abundant sand milling 1.5 hours, i.e. can get high-temperature resistant silicone-unsaturated polyester resin-epoxy coating.
Claims (8)
1. the preparation method of a high-temperature resistant silicone modified unsaturated polyester resin coating, it is characterised in that
Said method comprising the steps of:
(1) with the alkoxyorganosilicon of two functional groups and trifunctional for mixing raw material, through hydrolytic condensation, first
First synthesize organic-silicone prepolymer；
(2) it is former with 1,2-propylene glycol, 1,4-butanediol, adipic acid, THPA and maleic anhydride
Material synthesis unsaturated polyester (UP)；Organic siliconresin pre-polymerization is added when the synthesis of unsaturated polyester resin is nearly completed
Body and epoxy resin, proceed the graft reaction between resin, be eventually adding reactive diluent styrene with
It carries out being sufficiently mixed, diluting, and i.e. can get tri compound resin；
(3) hollow glass micropearl mixed by a certain percentage, mica powder, Pulvis Talci, bentonite are constituted
Inorganic mixed fillers mix with above-mentioned tri compound resin, fully stir with sand mill through homogenizer
Mix, after sand milling, prepare finely disseminated high-temperature resistant silicone-unsaturated polyester resin-epoxy coating.
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that in the step (1) of described method, the most accurately weigh 74.2 grams anhydrous
Ethanol, 41.2 grams of MTESs, 10.0 grams and 23.0 grams phenyl trimethoxies of diphenyl silanediol
Base silane, is injected separately in the there-necked flask presetting stirring and condensing plant；Bath temperature is set to 50 DEG C,
In there-necked flask, under agitation it is slowly dropped into the deionized water 22.3 grams that appropriate PH is 4, within 1.5 hours, drips
Finish, be warming up to 120 DEG C afterwards and continue reaction 1 hour；Finally decompression removes dehydrated alcohol, residual moisture and low
Middle Molecular Substance, i.e. can get organic-silicone prepolymer.
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that in described method step (2), by 7.5 grams of 1,2-PDs, 11.6 grams
BDO, 5.7 g of adipic acid, 20 grams of THPAs and 35 grams of maleic anhydrides put in there-necked flask,
It is placed on digital display thermal-arrest magnetic stirring apparatus, installs condensation reflux unit additional, be heated to 160 DEG C of back flow reaction 40min,
Then heat to 200 DEG C, be cooled to 90 DEG C when system acid number reaches 15mgKOH/g, be sequentially added into 20 grams
Organic-silicone prepolymer, 10 grams of E-51 and 3.6 grams of zinc Isoocatanoates, be warmed up to 120 DEG C of reaction 1h again,
It is cooled to the water in 100 DEG C of evacuation removing systems and other small molecule by-product afterwards, is eventually adding 50 grams
Carry out with it being sufficiently mixed dissolved with the styrene of 0.036 gram of hydroquinone, 0.15 gram of benzoyl peroxide, dilute
Release, i.e. can get tri compound resin.
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that in described method step (3), accurately weigh hollow glass micropearl 25 grams,
Mica powder 7.5 grams, Pulvis Talci 5.0 grams, bentonite 3.8 grams, put into mix and blend 30 in homogenizer
Minute, put into 98.3 grams of tri compound resins afterwards and be sufficiently mixed；Then by after above-mentioned stirring
Compound inject in sand mill and carry out abundant sand milling 1.5 hours, i.e. can get high-temperature resistant silicone-unsaturation
Polyester resin-epoxy coating.
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that the alkoxyorganosilicon of described two functional groups and trifunctional is diphenyl silicon two
Alcohol, phenyltrimethoxysila,e, MTES, its mass ratio is: 1:(0.37-5.29):
(1.65-6.34)。
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that described epoxy resin is E-12, in E-20, E-21, E-44, E-51
Kind.
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that selected inorganic mixed fillers is hollow between 10-100 μm of particle diameter
Glass microballoon, mica powder, Pulvis Talci, bentonite；Its mass ratio is 1:(0.1-0.5): (0.1-0.6):
(0.05-0.40)。
The system of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating the most according to claim 1
Preparation Method, it is characterised in that described tri compound resin is 1 with the mass ratio of inorganic mixed fillers:
(0.15-0.5)。
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| CN107254050A (en) * | 2017-06-16 | 2017-10-17 | 江苏三木化工股份有限公司 | Solid polyester modified silicone resin for Heat Resistant Powder Coatings and preparation method thereof |
| CN107603202A (en) * | 2017-09-30 | 2018-01-19 | 南京晟强橡塑有限公司 | A kind of rubber pocket former polyurethane rubber bolster |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070385A (en) * | 2007-06-20 | 2007-11-14 | 胡孟进 | Process for preparing high wear-resistant, high-luster, high-hardness and high-temperature resisting orgnaic silicon resin |
| CN102268219A (en) * | 2011-08-23 | 2011-12-07 | 江西省科学院应用化学研究所 | Preparation method of solvent-free type organosilicon high-temperature-resistant paint |
| CN103436094A (en) * | 2013-08-27 | 2013-12-11 | 华南理工大学 | Thermosetting high temperature resisting printing ink for touch screen as well as preparation method of printing ink |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090056610A (en) * | 2007-11-30 | 2009-06-03 | (재)경기대진테크노파크 | A waterproof thermal insulation coating resin composition |
-
2014
- 2014-11-05 CN CN201410615096.2A patent/CN104356894B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070385A (en) * | 2007-06-20 | 2007-11-14 | 胡孟进 | Process for preparing high wear-resistant, high-luster, high-hardness and high-temperature resisting orgnaic silicon resin |
| CN102268219A (en) * | 2011-08-23 | 2011-12-07 | 江西省科学院应用化学研究所 | Preparation method of solvent-free type organosilicon high-temperature-resistant paint |
| CN103436094A (en) * | 2013-08-27 | 2013-12-11 | 华南理工大学 | Thermosetting high temperature resisting printing ink for touch screen as well as preparation method of printing ink |
Non-Patent Citations (4)
| Title |
|---|
| 新型无溶剂有机硅耐高温树脂的制备及性能研究;董晓娜等;《广东化工》;20100331;第37卷(第3期);89-91 * |
| 有机硅改性不饱和聚酯树脂的制备及应用研究;张建华等;《绝缘材料》;20070131;第40卷(第1期);11-13 * |
| 有机硅改性不饱和聚酯的制备与应用研究;张建华;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20071215;全文 * |
| 有机硅改性酚醛环氧树脂耐高温胶粘剂的研制;王丁等;《中国胶粘剂》;20070331;第16卷(第3期);23-27 * |
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