CN104356894A - Preparation method of high-temperature-resistant organic silicon modified unsaturated polyester resin coating - Google Patents
Preparation method of high-temperature-resistant organic silicon modified unsaturated polyester resin coating Download PDFInfo
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- CN104356894A CN104356894A CN201410615096.2A CN201410615096A CN104356894A CN 104356894 A CN104356894 A CN 104356894A CN 201410615096 A CN201410615096 A CN 201410615096A CN 104356894 A CN104356894 A CN 104356894A
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- unsaturated polyester
- polyester resin
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- temperature resistant
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000011248 coating agent Substances 0.000 title claims abstract description 20
- 238000000576 coating method Methods 0.000 title claims abstract description 20
- 229920006337 unsaturated polyester resin Polymers 0.000 title claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 title abstract 5
- 239000010703 silicon Substances 0.000 title abstract 5
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 25
- 229920006305 unsaturated polyester Polymers 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims abstract description 10
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 8
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 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
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 235000011037 adipic acid Nutrition 0.000 claims abstract description 5
- 239000001361 adipic acid Substances 0.000 claims abstract description 5
- 239000000945 filler Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 3
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000011521 glass Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 229920001296 polysiloxane Polymers 0.000 claims description 13
- 239000004576 sand Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000010445 mica Substances 0.000 claims description 11
- 229910052618 mica group Inorganic materials 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 11
- 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 10
- 239000000203 mixture Substances 0.000 claims description 10
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 8
- 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 8
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 229960004063 propylene glycol Drugs 0.000 claims description 5
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 4
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 150000001298 alcohols Chemical class 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
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 125000000524 functional group Chemical group 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
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000012764 mineral filler Substances 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 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 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000002952 polymeric resin Substances 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 3
- 239000011206 ternary composite Substances 0.000 abstract 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 239000003085 diluting agent Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 235000013772 propylene glycol Nutrition 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 229920002050 silicone resin Polymers 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- -1 polysiloxane Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 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
-
- 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
-
- 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
-
- 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
-
- 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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a preparation method of a high-temperature-resistant organic silicon modified unsaturated polyester resin coating. The preparation method comprises the following steps: (1) performing hydrolytic condensation on two-functional group and three-functional group alkoxy organic silicon as mixing raw materials to synthesize an organic silicon resin prepolymer; (2) synthesizing unsaturated polyester from raw materials including 1,2-propanediol, 1,4-butanediol, adipic acid, tetrahydrophthalic anhydride and cis-butenedioic anhydride, adding the organic silicon resin prepolymer and epoxy resin E-51 for continuous grafting reaction, and finally adding an active diluent for diluting to obtain ternary composite resin; (3) mixing inorganic mixing fillers mixed according to a certain ratio with the ternary composite resin, stirring, and sanding to prepare the high-temperature-resistant organic silicon-unsaturated polyester resin-epoxy resin coating with good dispersion property. The preparation method is simple; the prepared high-temperature-resistant organic silicon-unsaturated polyester resin-epoxy resin coating is a high-performance organic-inorganic hybrid composite material with excellent comprehensive performance.
Description
technical field
The present invention relates to a kind of preparation method 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 nondiscoloration more than 300 DEG C, does not come off, and still can keep the coating of suitable physical mechanical property, and it has broad application prospects at modern industry, military affairs, space industry.Unsaturated polyester resin production technique is easy, and raw material is easy to get, and can at room temperature solidify, normal pressure compacted under.Goods not only have excellent resistance to chemical corrosion after solidification, and also have good mechanical property, proportion is also relatively little.Epoxy resin is the thermosetting polymer synthetic materials that a class has the performances such as good bonding, corrosion-resistant, insulation, high strength.These advantages allow unsaturated polyester resin and epoxy resin be subject to the common concern of industry, obtain apply more at industrial circle.But the resistance toheat of these two kinds of resins is all bad, use at being generally suitable only for 160 DEG C, and goods weathering resistance is poor.Therefore, the high temperature resistant of goods is improved by modes such as chemical modification and mineral filler blending and weather resistance becomes the effective way improving resin property.Silicone resin also claims polysiloxane to be that a class alternately links by Siliciumatom and Sauerstoffatom the general designation forming the polymkeric substance that skeleton, different organic groups link with Siliciumatom again.Both containing " organic group " in its molecular structure, again containing " inorganic structure ", this special composition and molecular structure make it integrate Characteristics of Organic and inorganics function.One of advantage that silicone resin is the most outstanding is exactly have excellent thermo-oxidative stability, 250 DEG C of heating are after 24 hours, silicone resin weightlessness is only 2-8%, also has the advantage such as good weatherability properties and electrical insulating property simultaneously, can be widely used in the field such as high-temperaure coating and insulating protection.But the adhesive property of silicone resin is poor, need to improve its adhesivity by modification.
summary of the invention
The object of the invention is, there is the problems such as weathering resistance difference for existing high-temperature resistant coating, the invention provides a kind of preparation method of high-temperature resistant silicone-unsaturated polyester resin-epoxypaint, 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 silicone resin is incorporated in the middle of unsaturated polyester and epoxy resin by the method for molecular designing by the present invention, prepare a kind of high temperature resistant tri compound macromolecule resin of good performance with weathering resistance, afterwards this modified resin is mixed with inorganic high-temperature resistant fillers such as hollow glass micropearl, glass powder, mica powder, silicon powders, obtained can resistant to elevated temperatures organosilicon-unsaturated polyester resin-epoxypaint can resistance to more than 500 DEG C high temperature, thus widened macromolecule resin as the use range of high-temperature resistant coating and Application Areas.
Technical scheme of the present invention is, the preparation method of a kind of high-temperature resistant silicone-unsaturated polyester resin-epoxypaint 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, first synthesize organic-silicone prepolymer.
(2) with 1,2-propylene glycol, 1,4-butyleneglycol, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE are Material synthesis unsaturated polyester, organosilicon performed polymer and epoxy resin E-51 is added close to when completing in the synthesis of unsaturated polyester resin, proceed the graft reaction between resin, finally add reactive thinner vinylbenzene fully to mix with it, dilute, tri compound resin can be obtained.
(3) hollow glass micropearl mixed by a certain percentage, mica powder, talcum powder, wilkinite are mixed with above-mentioned tri compound resin, obtained finely disseminated high-temperature resistant silicone-unsaturated polyester resin-epoxypaint after homogenizer and sand mill fully stir sand milling.
In the methods of the invention, the alkoxyorganosilicon of two functional groups and trifunctional is two or more in Union carbide A-162, dimethoxydiphenylsilane, Diphenylsilanediol, vinyltriethoxysilane and phenyltrimethoxysila,e.Preferably Diphenylsilanediol, phenyltrimethoxysila,e, its mass ratio of Union carbide A-162 are: 1:(0.37-5.29): (1.65-6.34), preferred proportion is: 1:2.3:4.12.
In the methods of the invention, selected epoxy resin is the one in E-12, E-20, E-21, E-44, E-51, is preferably E-51;
In the methods of the invention, selected mineral filler is more than three kinds in the hollow glass micropearl of particle diameter between 10-100 μm, glass powder, mica powder, silicon powder, polynite, talcum powder, is preferably hollow glass micropearl, mica powder, talcum powder, wilkinite.Its mass ratio is 1:(0.1-0.5): (0.1-0.6): (0.05-0.40) preferred mass is than being 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 is than being 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-epoxypaint not only has good high temperature resistant, weather resistance, also has good waterproof, anticorrosion and adhesive property.It is a kind of high-performance organic-inorganic hybrid composite material of excellent combination property.
Embodiment
Embodiment 1:
(1) synthesis of organosilicon performed polymer
Accurately take 74.2 grams of dehydrated alcohols, 41.2 grams of Union carbide A-162s, Diphenylsilanediol 10.0 grams and 23.0 grams of phenyltrimethoxysila,e, inject the there-necked flask presetting stirring and condensing equipment respectively.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly the appropriate PH of instillation is the deionized water 22.3 grams of 4, within 1.5 hours, dropwises, and is warming up to 120 DEG C afterwards and continues reaction 1 hour.Finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain organosilicon performed polymer.
(2) preparation of organosilicon-unsaturated polyester resin-epoxy resin
By 7.5 gram 1, 2-propylene glycol, 11.6 gram 1, 4-butyleneglycol, 5.7 g of adipic acid, 20 grams of tetrahydrophthalic anhydride and 35 grams of MALEIC ANHYDRIDE drop in there-necked flask, be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 160 DEG C of back flow reaction 40min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add 20 grams of organosilicon performed polymers successively, 10 grams of E-51 and 3.6 gram of isocaprylic acid zinc, again be warmed up to 120 DEG C of reaction 1h, be cooled to 100 DEG C afterwards and vacuumize water in removing system and other small molecule by-product, finally add 50 grams and be dissolved with 0.036 gram of Resorcinol, the vinylbenzene of 0.15 gram of benzoyl peroxide fully mixes with it, dilution, tri compound resin can be obtained.
(3) preparation of high-temperature resistant silicone-unsaturated polyester resin-epoxypaint
Accurately take hollow glass micropearl 25 grams, mica powder 7.5 grams, talcum powder 5.0 grams, wilkinite 3.8 grams, mix and blend 30 minutes in input homogenizer, drop into 98.3 grams of tri compound resins afterwards and be uniformly mixed fully; Then the compound after above-mentioned stirring is injected sand mill and carry out abundant sand milling 1.5 hours, high-temperature resistant silicone-unsaturated polyester resin-epoxypaint can be obtained.
Embodiment 2:
(1) synthesis of organosilicon performed polymer
Accurately take 45 grams of dehydrated alcohols, 20.0 grams of Union carbide A-162s, Diphenylsilanediol 10.0 grams and, 15.0 grams of phenyltrimethoxysila,e, inject the there-necked flask presetting stirring and condensing equipment respectively.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly the appropriate PH of instillation is the deionized water 13.5 grams of 4, within 1.5 hours, dropwises, and is warming up to 120 DEG C afterwards and continues reaction 1 hour.Finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain organosilicon performed polymer.
(2) preparation of organosilicon-unsaturated polyester resin-epoxy resin
By 7.5 gram 1, 2-propylene glycol, 11.6 gram 1, 4-butyleneglycol, 5.7 g of adipic acid, 20 grams of tetrahydrophthalic anhydride and 35 grams of MALEIC ANHYDRIDE drop in there-necked flask, be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 160 DEG C of back flow reaction 40min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add 20 grams of organosilicon performed polymers successively, 10 grams of E-51 and 3.6 gram of isocaprylic acid zinc, again be warmed up to 120 DEG C of reaction 1h, be cooled to 100 DEG C afterwards and vacuumize water in removing system and other small molecule by-product, finally add 55 grams and be dissolved with 0.04 gram of Resorcinol, the vinylbenzene of 0.17 gram of benzoyl peroxide fully mixes with it, dilution, tri compound resin can be obtained.
(3) preparation of high-temperature resistant silicone-unsaturated polyester resin-epoxypaint
Accurately take hollow glass micropearl 10 grams, mica powder 2.0 grams, talcum powder 3.0 grams, wilkinite 1.5 grams, mix and blend 30 minutes in input homogenizer, drop into 55 grams of tri compound resins afterwards and be uniformly mixed fully; Then the compound after above-mentioned stirring is injected sand mill and carry out abundant sand milling 1.5 hours, high-temperature resistant silicone-unsaturated polyester resin-epoxypaint can be obtained.
Embodiment 3:
(1) synthesis of organosilicon performed polymer
Accurately take 55 grams of dehydrated alcohols, 25.0 grams of Union carbide A-162s, Diphenylsilanediol 10.0 grams and 30.0 grams of phenyltrimethoxysila,e, inject the there-necked flask presetting stirring and condensing equipment respectively.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly the appropriate PH of instillation is the deionized water 19.5 grams of 4, within 1.5 hours, dropwises, and is warming up to 120 DEG C afterwards and continues reaction 1 hour.Finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain organosilicon performed polymer.
(2) preparation of organosilicon-unsaturated polyester resin-epoxy resin
By 7.5 gram 1, 2-propylene glycol, 11.6 gram 1, 4-butyleneglycol, 5.7 g of adipic acid, 20 grams of tetrahydrophthalic anhydride and 35 grams of MALEIC ANHYDRIDE drop in there-necked flask, be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 160 DEG C of back flow reaction 40min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add 15 grams of organosilicon performed polymers successively, 15 grams of E-51 and 3.6 gram of isocaprylic acid zinc, again be warmed up to 120 DEG C of reaction 1h, be cooled to 100 DEG C afterwards and vacuumize water in removing system and other small molecule by-product, finally add 45 grams and be dissolved with 0.03 gram of Resorcinol, the vinylbenzene of 0.14 gram of benzoyl peroxide fully mixes with it, dilution, tri compound resin can be obtained.
(3) preparation of high-temperature resistant silicone-unsaturated polyester resin-epoxypaint
Accurately take hollow glass micropearl 10 grams, mica powder 4.0 grams, talcum powder 5.0 grams, wilkinite 3.0 grams, mix and blend 30 minutes in input homogenizer, drop into 62.9 grams of tri compound resins afterwards and be uniformly mixed fully; Then the compound after above-mentioned stirring is injected sand mill and carry out abundant sand milling 1.5 hours, high-temperature resistant silicone-unsaturated polyester resin-epoxypaint can be obtained.
Claims (8)
1. a preparation method for high-temperature resistant silicone modified unsaturated polyester resin coating, is characterized 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 synthesize organic-silicone prepolymer;
(2) with 1,2-PD, BDO, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE for Material synthesis unsaturated polyester; Add organosilicon performed polymer and epoxy resin E-51 in the synthesis of unsaturated polyester resin close to when completing, proceed the graft reaction between resin, finally add reactive thinner vinylbenzene and fully mix with it, dilute, tri compound resin can be obtained;
(3) the inorganic mixed fillers hollow glass micropearl mixed by a certain percentage, mica powder, talcum powder, wilkinite are mixed with above-mentioned tri compound resin, fully stir through homogenizer and sand mill, after sand milling, obtained finely disseminated high-temperature resistant silicone-unsaturated polyester resin-epoxypaint.
2. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, it is characterized in that, in the step (1) of described method, first accurately take 74.2 grams of dehydrated alcohols, 41.2 grams of Union carbide A-162s, Diphenylsilanediol 10.0 grams and 23.0 grams of phenyltrimethoxysila,e, inject the there-necked flask presetting stirring and condensing equipment respectively; Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly the appropriate PH of instillation is the deionized water 22.3 grams of 4, within 1.5 hours, dropwises, and is warming up to 120 DEG C afterwards and continues reaction 1 hour; Finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain organosilicon performed polymer.
3. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, it is characterized in that, in described method steps (2), by 7.5 gram 1, 2-propylene glycol, 11.6 gram 1, 4-butyleneglycol, 5.7 g of adipic acid, 20 grams of tetrahydrophthalic anhydride and 35 grams of MALEIC ANHYDRIDE drop in there-necked flask, be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 160 DEG C of back flow reaction 40min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add 20 grams of organosilicon performed polymers successively, 10 grams of E-51 and 3.6 gram of isocaprylic acid zinc, again be warmed up to 120 DEG C of reaction 1h, be cooled to 100 DEG C afterwards and vacuumize water in removing system and other small molecule by-product, finally add 50 grams and be dissolved with 0.036 gram of Resorcinol, the vinylbenzene of 0.15 gram of benzoyl peroxide fully mixes with it, dilution, tri compound resin can be obtained.
4. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, it is characterized in that, in described method steps (3), accurately take hollow glass micropearl 25 grams, mica powder 7.5 grams, talcum powder 5.0 grams, wilkinite 3.8 grams, mix and blend 30 minutes in input homogenizer, drops into 98.3 grams of tri compound resins afterwards and is uniformly mixed fully; Then the compound after above-mentioned stirring is injected sand mill and carry out abundant sand milling 1.5 hours, high-temperature resistant silicone-unsaturated polyester resin-epoxypaint can be obtained.
5. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, it is characterized in that, the alkoxyorganosilicon of described two functional groups and trifunctional is two or more in Union carbide A-162, dimethoxydiphenylsilane, Diphenylsilanediol, vinyltriethoxysilane and phenyltrimethoxysila,e; Be preferably Diphenylsilanediol, phenyltrimethoxysila,e, Union carbide A-162, its mass ratio is: 1:(0.37-5.29): (1.65-6.34), preferred mass ratio is: 1:2.3:4.12.
6. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, it is characterized in that, described epoxy resin is the one in E-12, E-20, E-21, E-44, E-51, is preferably E-51.
7. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, it is characterized in that, selected mineral filler is more than three kinds in the hollow glass micropearl of particle diameter between 10-100 μm, glass powder, mica powder, silicon powder, polynite, talcum powder, is preferably hollow glass micropearl, mica powder, talcum powder, wilkinite; Its mass ratio is 1:(0.1-0.5): (0.1-0.6): (0.05-0.40) preferred mass is than being 1:0.3:0.2:0.15.
8. the preparation method of a kind of high-temperature resistant silicone modified unsaturated polyester resin coating according to claim 1, is characterized in that, the mass ratio of described tri compound resin and inorganic mixed fillers is 1:(0.15-0.5), preferred mass is than being 1:0.42.
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| CN105778386A (en) * | 2016-03-10 | 2016-07-20 | 江西省科学院应用化学研究所 | Preparation method for organic silicone modified unsaturated polyester ternary nano-composite material |
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| CN106750232A (en) * | 2016-12-12 | 2017-05-31 | 衡阳山泰化工有限公司 | A kind of improved polyester resin and preparation method thereof |
| 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 |
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Effective date of registration: 20170814 Address after: 336002 Jiangxi Yuanzhou Yichun Medicine Park Bin Jiang special mechanical and electrical industry base Patentee after: JIANGXI PROVINCE HANGYU NEW MATERIAL Co.,Ltd. Address before: 330096 Nanchang East Road, Jiangxi, No. 7777 Patentee before: Institute of Applied Chemistry, Jiangxi Academy of Sciences |
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Application publication date: 20150218 Assignee: Jiangxi Hangyu Electronic Material Co.,Ltd. Assignor: JIANGXI PROVINCE HANGYU NEW MATERIAL Co.,Ltd. Contract record no.: X2023980052595 Denomination of invention: Preparation method of high-temperature resistant organosilicon modified unsaturated polyester resin coating Granted publication date: 20160817 License type: Common License Record date: 20231215 |