CN106634409A - Organosilicone modified epoxy resin high-temperature-resistant anti-corrosion coating and preparation method thereof - Google Patents
Organosilicone modified epoxy resin high-temperature-resistant anti-corrosion coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an organosilicone modified epoxy resin high-temperature-resistant anti-corrosion coating and a preparation method thereof. The organosilicone modified epoxy resin high-temperature-resistant anti-corrosion coating is characterized by being prepared from epoxy resin E-20, methyltriethoxysilane, dibutyltin dilaurate, a polyamide curing agent, boric acid, butyl titanate, nano SiO2, azodiisobutyronitrile, butyl methacrylate, a nano antimony tin oxide, nano TiO2, KH-570, polyvinyl alcohol, kaolin, Sb2O3, ammonium polyphosphate, hollow glass microspheres, talcum powder and the like as raw materials. Titanium-boron-containing organosilicone resin is synthesized, ATO powder and nano TiO2 are modified by using KH-570, and material slurry which is stable and good in dispersion can be prepared; as Sb2O/kaolin composite flame-retardant micro powder is prepared by using a ball milling method and is used together with the ammonium polyphosphate, a synergistic effect can be achieved, and a relatively good flame-retardancy effect can be achieved, that is, the organosilicone modified epoxy resin high-temperature-resistant anti-corrosion coating can be prepared.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint,
And its preparation technology.
Background technology
Organic siliconresin is widely used in fire-resistant anticorrosion paint, high-temperature-resistant insulating paint, fire resistant heat-insulating flame-retardant and applies
Material etc., but when there are problems that poor adhesive force, temperature are higher paint film mechanical strength so as to application be restricted.With one
The inorganic material for having excellent temperature tolerance and insulating properties a bit is modified to organic resin and adulterates, be in recent years one new grind
Study carefully direction.There is high temperature resistant due to being widely used in corrosion resistant coating field with many excellent performances in epoxy resin
The shortcomings of poor, poor toughness of property, crisp matter, with Organosiliconpolymermodified modified epoxy resin to improve epoxy coating toughness,
Heat resistance, corrosion resistance have great importance.
Pang jade is rather in its master thesis《Modifying epoxy resin by organosilicon coating preparation and performance study》In one text, with
Methltriethoxysilone, dimethyldiethoxysilane, phenyl triethoxysilane are raw material, catalyst HCl's
Under effect, after hydrolysis-condensation reaction, organosilicon polymer is formed；Using organosilicon polymer as modifying agent, to asphalt mixtures modified by epoxy resin
Fat E-20 is modified, and using modified resin as matrix, adds various color stuffings, auxiliary agent and curing agent to be prepared into high temperature resistant
Anticorrosive paint.But it is not enough to there is high-temperature resistant anti-corrosive performance.
The present invention with MTES as silicon source, butyl titanate as titanium source, boric acid as boron source, HCl as catalyst,
Dimethylbenzene is solvent, and dibutyl tin laurate is catalyst, and Jing hydrolysis-condensations have been synthesized titaniferous-boron organic siliconresin；
The modified ATO powders of KH-570, nano-TiO2, with polyvinyl alcohol as dispersant, stable well dispersed slip is made, use modified
Epoxy resin is prepared for transparent heat insulating dope as film forming matter；Sb is prepared for ball-milling method2O3/ kaolin composite flame-proof micro mist,
Sb2O3Belong to additive flame retardant, based on stibium trioxide powder, kaolin is attached to stibium trioxide powder surface, fully with stibium trioxide powder occur physics,
Chemical action, is used in combination with APP, produces cooperative effect, and flame retardant effect is more preferably；Receiving after modification of graft process
Rice SiO2Particle has extraordinary dispersiveness and storage stability after grinding, dispersed with stirring, in organic siliconresin；I.e.
Obtain a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint.
The content of the invention
The invention mainly solves the technical problem of provide a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint and
Its preparation technology, the coating high temperature resistant made according to the technique, antiseptic property are good.
The technical problem to be solved is realized using following technical scheme：
Epoxy resin E-20 20-33, MTES 10-22, dibutyl tin laurate 1-3, polyamide curing agent
1-2, boric acid 3-5, butyl titanate 3-6, Nano-meter SiO_223-5, the 1-2 of silane coupling A -174, azodiisobutyronitrile 1-3, methyl
Butyl acrylate 1-3, nanometer antimony oxide tin 2-4, nano-TiO24-6, KH-570 1-2, polyvinyl alcohol 1-2, kaolin 2-5,
Sb2O3 1-4, APP 1-3, hollow glass micropearl 1-3, talcum powder 1-2, dimethylbenzene, distilled water, HCl, absolute ethyl alcohol, ammonia
Water, appropriate toluene.
A kind of preparation method of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint, it is characterised in that according to the following steps
Carry out：
A. by MTES, boric acid, absolute ethyl alcohol mixing, the butyl titanate of xylene soluble is added, stirring is equal
It is even, 50-70 DEG C, plus the mixed liquor of distilled water and HCl are warming up to, tune pH is 3-4, and insulation reaction 1-2h filters, filtrate is existed
120-140 DEG C vacuumizes, and obtains the liquid of clear viscous, as titaniferous-boron organic siliconresin；
B. dimethylbenzene is added in epoxy resin E-20, in 60-80 DEG C of heating water bath and is stirred, filtered after dissolving completely, added
Resulting material, dibutyl tin laurate are mixed in a, are stirred, oil bath heating 2-4h at 130-150 DEG C；
C. dried Nano-meter SiO_2 is taken2In being placed in toluene, after ultrasonic disperse, silane coupling A -174 is added dropwise and reacts, suction filtration,
It is scattered in toluene after washing, drying, in N2Under protection, 60-80 DEG C is warming up to, azodiisobutyronitrile, methacrylic acid is added dropwise
Butyl ester reacts, suction filtration, and drying obtains the Nano-meter SiO_2 of surface grafting polymerization process2；
D. under room temperature, to nanometer antimony oxide tin, nano-TiO2Middle addition water, adds KH-570, polyvinyl alcohol under magnetic agitation,
PH to 7-9 is adjusted with ammoniacal liquor, adds resulting material in c, ultrasonic disperse 1-2h that slurry is obtained；
E. 1-2h, and Sb are calcined in kaolin grinding washing after 700-900 DEG C2O3Mixing, is placed in water ultrasonic disperse and makes
Slurries, after ball milling 3-5h baking oven is put into, and in 110-130 DEG C of drying 2-4h, obtains composite micro-powder, and it is mixed with APP
It is even, it is stand-by；
F. by b, d, e and other leftover materials mixing, 10-30min is ground, adds polyamide curing agent, stirred, heated up
To 95-115 DEG C, solidify 1-2h, obtain final product a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint.
The reaction mechanism of the present invention is as follows：
（1）With MTES as silicon source, butyl titanate as titanium source, boric acid as boron source, HCl as catalyst, dimethylbenzene
For solvent, dibutyl tin laurate is catalyst, and Jing hydrolysis-condensations have been synthesized titaniferous-boron organic siliconresin；Boron element
Doping, the heat resistance of resin can be significantly improved, be conducive to the raising of decay resistance；The organosilicon tree of synthesized Doped with Titanium
The heat endurance of fat is optimal.
（2）After modification, Nano-meter SiO_22The surface physicochemical property of particle there occurs obvious change, hydroxyl
Quantity is significantly reduced, organic polymer layers in particle surface success glycerol polymerization；Nanometer after modification of graft process
SiO2Particle has extraordinary dispersiveness and storage stability after grinding, dispersed with stirring, in organic siliconresin.
（3）Nanometer antimony oxide tin（ATO）In being usually used in transparent heat insulating dope, with very high ultraviolet infrared shielding effect,
And there is good transmitance in visible region, the present invention is by the modified ATO powders of Silane coupling reagent KH-570, nano-TiO2,
It is aided with the dispersion of polyethylene of dispersing agent alcohol again, after high speed dispersion and ultrasonic wave dispersion, makes stable and well dispersed material
Slurry, with modified epoxy as film forming matter, is prepared for transparent heat insulating dope.
（4）Sb is prepared for ball-milling method2O3/ kaolin composite flame-proof micro mist, Sb2O3Belong to additive flame retardant, with stibium trioxide
Based on powder, kaolin is attached to stibium trioxide powder surface, fully physics, chemical action occurs with stibium trioxide powder；
It is used in combination with APP, produces cooperative effect, flame retardant effect is more preferably.
（5）There are many holes inside hollow glass micropearl, thermal conductivity factor, density are all very low, and applying can show in coating
The heat-insulation and heat-preservation effect of the increase coating of work；It is talcum powder surface lubrication, anti-stick, the mechanical force of coating, case hardness can be improved with
And being coated with property, main component is aqueous magnesium silicate, it is adaptable to high-temperature resistant coating.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint, is obtained by the raw material of following weight parts (g)：
Epoxy resin E-20 23, MTES 22, dibutyl tin laurate 3, polyamide curing agent 2, boric acid 5,
Butyl titanate 6, Nano-meter SiO_225, silane coupling A -174 1, azodiisobutyronitrile 3, butyl methacrylate 3 is nano oxidized
Antimony tin 4, nano-TiO26, KH-570 1, polyvinyl alcohol 1, kaolin 5, Sb2O3 4, APP 3, hollow glass micropearl 3 is sliding
Stone flour 2, dimethylbenzene, distilled water, HCl, absolute ethyl alcohol, ammoniacal liquor, appropriate toluene.
A kind of preparation method of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint, it is characterised in that according to the following steps
Carry out：
A. by MTES, boric acid, absolute ethyl alcohol mixing, the butyl titanate of xylene soluble is added, stirring is equal
It is even, 60-70 DEG C, plus the mixed liquor of distilled water and HCl are warming up to, tune pH is 3-4, and insulation reaction 2h is filtered, by filtrate in 130-
140 DEG C vacuumize, and obtain the liquid of clear viscous, as titaniferous-boron organic siliconresin；
B. dimethylbenzene is added in epoxy resin E-20, in 70-80 DEG C of heating water bath and is stirred, filtered after dissolving completely, added
Resulting material, dibutyl tin laurate are mixed in a, are stirred, oil bath heating 2h at 140-150 DEG C；
C. dried Nano-meter SiO_2 is taken2In being placed in toluene, after ultrasonic disperse, silane coupling A -174 is added dropwise and reacts, suction filtration,
It is scattered in toluene after washing, drying, in N2Under protection, 70-80 DEG C is warming up to, azodiisobutyronitrile, methacrylic acid is added dropwise
Butyl ester reacts, suction filtration, and drying obtains the Nano-meter SiO_2 of surface grafting polymerization process2；
D. under room temperature, to nanometer antimony oxide tin, nano-TiO2Middle addition water, adds KH-570, polyvinyl alcohol under magnetic agitation,
PH to 7-8 is adjusted with ammoniacal liquor, adds resulting material in c, ultrasonic disperse 2h that slurry is obtained；
E. 1h, and Sb are calcined in kaolin grinding washing after 800-900 DEG C2O3Mixing, is placed in water ultrasonic disperse and makes slurry
Liquid, after ball milling 3h baking oven is put into, and in 120-130 DEG C of drying 2h, obtains composite micro-powder, and it is well mixed with APP, stand-by；
F. by b, d, e and other leftover materials mixing, 30min is ground, adds polyamide curing agent, stirred, be warming up to
105-115 DEG C, solidify 2h, obtain final product a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint.
A kind of performance test results of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint prepared by above-described embodiment are such as
Shown in lower：
Based on ordinary carbon steel, with sand papering, then carry out sassafras with absolute ethyl alcohol and acetone and wipe, obtained by its surface coating
Coating, is put into baking oven, is solidified, and coating performance test shows：
Resistance to impact >=64kg.cm-1, the boiling water resistance 8h of coating, resistance to water (25 DEG C) 34d, acid resistance (10%HCl) 6d,
Alkali resistance (10%NaOH) 4d, 535 DEG C of heat resistance, solvent resistant acetone 3d, salt spray resistance 34d, coating is intact, cold-hot alternately 52
Individual circulation.
Claims (2)
1. a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint, it is characterised in that be obtained by the raw material of following weight parts：
Epoxy resin E-20 20-33, MTES 10-22, dibutyl tin laurate 1-3, polyamide curing agent
1-2, boric acid 3-5, butyl titanate 3-6, Nano-meter SiO_223-5, the 1-2 of silane coupling A -174, azodiisobutyronitrile 1-3, methyl
Butyl acrylate 1-3, nanometer antimony oxide tin 2-4, nano-TiO24-6, KH-570 1-2, polyvinyl alcohol 1-2, kaolin 2-5,
Sb2O3 1-4, APP 1-3, hollow glass micropearl 1-3, talcum powder 1-2, dimethylbenzene, distilled water, HCl, absolute ethyl alcohol, ammonia
Water, appropriate toluene.
2. the preparation method of a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint according to claim 1, it is special
Levy and be, carry out according to the following steps：
A. by MTES, boric acid, absolute ethyl alcohol mixing, the butyl titanate of xylene soluble is added, stirring is equal
It is even, 50-70 DEG C, plus the mixed liquor of distilled water and HCl are warming up to, tune pH is 3-4, and insulation reaction 1-2h filters, filtrate is existed
120-140 DEG C vacuumizes, and obtains the liquid of clear viscous, as titaniferous-boron organic siliconresin；
B. dimethylbenzene is added in epoxy resin E-20, in 60-80 DEG C of heating water bath and is stirred, filtered after dissolving completely, added
Resulting material, dibutyl tin laurate are mixed in a, are stirred, oil bath heating 2-4h at 130-150 DEG C；
C. dried Nano-meter SiO_2 is taken2In being placed in toluene, after ultrasonic disperse, silane coupling A -174 is added dropwise and reacts, suction filtration, wash
Wash, dry after be scattered in toluene, in N2Under protection, 60-80 DEG C is warming up to, azodiisobutyronitrile, methacrylic acid fourth is added dropwise
Ester reacts, suction filtration, and drying obtains the Nano-meter SiO_2 of surface grafting polymerization process2；
D. under room temperature, to nanometer antimony oxide tin, nano-TiO2Middle addition water, adds KH-570, polyvinyl alcohol under magnetic agitation, use
Ammoniacal liquor adjusts pH to 7-9, adds resulting material in c, ultrasonic disperse 1-2h that slurry is obtained；
E. 1-2h, and Sb are calcined in kaolin grinding washing after 700-900 DEG C2O3Mixing, is placed in water ultrasonic disperse and makes
Slurries, after ball milling 3-5h baking oven is put into, and in 110-130 DEG C of drying 2-4h, obtains composite micro-powder, and it is mixed with APP
It is even, it is stand-by；
F. by b, d, e and other leftover materials mixing, 10-30min is ground, adds polyamide curing agent, stirred, heated up
To 95-115 DEG C, solidify 1-2h, obtain final product a kind of modifying epoxy resin by organosilicon fire-resistant anticorrosion paint.
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Cited By (9)
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| CN107201159A (en) * | 2017-06-17 | 2017-09-26 | 合肥市晨雷思建筑材料科技有限公司 | A kind of cracking resistance, anti-dropout coating and preparation method |
| CN112194981A (en) * | 2020-09-18 | 2021-01-08 | 东来涂料技术（上海）股份有限公司 | Low-temperature reaction type high-temperature-resistant coating and preparation method thereof |
| WO2021050463A1 (en) * | 2019-09-09 | 2021-03-18 | Dow Silicones Corporation | Method of preparing alkoxy-functional organosilicon compounds |
| CN112592615A (en) * | 2021-01-18 | 2021-04-02 | 张晓峰 | Organic silicon modified epoxy resin anticorrosive paint |
| CN113480845A (en) * | 2021-07-16 | 2021-10-08 | 江西省铭新科技有限公司 | Regenerated PA plastic particle prepared from waste cloth and method thereof |
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| CN118047931A (en) * | 2024-02-18 | 2024-05-17 | 广东依斯特新材料有限公司 | Hydrophobic wear-resistant modified acrylic resin and synthesis process thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107201159A (en) * | 2017-06-17 | 2017-09-26 | 合肥市晨雷思建筑材料科技有限公司 | A kind of cracking resistance, anti-dropout coating and preparation method |
| WO2021050463A1 (en) * | 2019-09-09 | 2021-03-18 | Dow Silicones Corporation | Method of preparing alkoxy-functional organosilicon compounds |
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