CN104673063A - High-temperature-resistant, anti-corrosion and thermal-insulation coating and preparation technology thereof - Google Patents
High-temperature-resistant, anti-corrosion and thermal-insulation coating and preparation technology thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature-resistant, anti-corrosion and thermal-insulation coating which comprises components in parts by weight as follows: 45-60 parts of film-forming resin, 20-30 parts of a pigment and filler, 15-30 parts of an aid and 25-30 parts of a solvent. The invention further designs a preparation technology of the high-temperature-resistant, anti-corrosion and thermal-insulation coating. The technology comprises steps as follows: firstly, mixing the film-forming resin with the pigment and the filler, sequentially adding an antifoaming agent, a leveling agent, a coupling agent, a crosslinking agent and a curing agent, and evenly stirring the mixture at the normal temperature to obtain the high-temperature-resistant, anti-corrosion and thermal-insulation coating. The coating has the advantages of environment-friendliness, low cost, high hardness, long service life, good heat resistance, good flexibility, good high-temperature resistance and the like.
Description
Technical field
The invention belongs to coating preparation field, be specifically related to a kind of high-temperature resistant anti-corrosive thermal insulating coating and preparation technology thereof.
Background technology
Along with the development of China's modern industry, particularly in industries such as metallurgy, petrochemical industry, the energy, novel material and military projects, the application of high temperature service and auxiliary facility gets more and more, but the oxygen generation oxidizing reaction of metallic substance in hot environment easily and in air, produce corrosion phenomena, thus make metallic substance lose intensity gradually and cause structural disappearance, become the hidden danger of various accident.Therefore, high temperature service surface generally all needs application fire-resistant anticorrosion paint to protect, and to prevent metallic substance oxidation corrosion, extends the work-ing life of high temperature service.
Easily there is thermal destruction and carbonization under the high temperature conditions in common coating; soil layer is destroyed; can not play a protective role to base material; and high-temperature resistant coating can keep not embrittlement under the high temperature conditions, do not peel off with base material, do not keep certain physics and chemistry and mechanical property while bubbling, make object can at high temperature from the impact of the undesirable condition such as chemical corrosion, oxidation corrosion.
At present, high-temperature resistant coating mainly can be divided into refractory inorganic paint and the large class of organic high temperature-resistant coating two, refractory inorganic paint forms primarily of inorganic component, high temperature resistant inorganic coating owing to having environmental protection, the advantage such as cost is low, hardness is high, the life-span is long, heat resistanceheat resistant excellent performance, and receive the concern of people; Organic high temperature-resistant coating mainly contains several classes such as organic coating, modified epoxy resin paint, phenolic resin paint, polyurethane coating, wherein silicone resin because of in the component of its uniqueness and molecule containing silicon-carbon bonds structure, make silicone resin well merge organism and inorganics characteristic, be widely used in paint field.
The coating protection majority of high temperature service adopts silicone based high-temperature resistant coating, and use temperature, within the scope of 400-600 DEG C, selects pure organosilicon coating; When use temperature is below 400 DEG C, select research of silicone modified coating.Pure silicone resin has thermostability, scale resistance, weathering resistance, lower temperature resistance are good, and surface energy is low, dielectric strength advantages of higher, but generally needs hot setting, brings inconvenience to large-area construction, and its antiseptic power, poor adhesive force.Organic-silicon-modified resin is development in recent years, can reduce the internal stress of high-temperature coatings, and can increase again the snappiness of high-temperature coatings, the performance such as high temperature resistant, the two has the complementary feature of learning from other's strong points to offset one's weaknesses.
Summary of the invention
Technical problem to be solved by this invention is, for the shortcoming that above prior art exists, a kind of high-temperature resistant anti-corrosive thermal insulating coating and preparation technology thereof are proposed, this coating environmental protection, cost is low, hardness is high, the life-span is long, heat resistanceheat resistant performance is good, good, the high temperature resistant advantage such as good of snappiness, and preparation technology is simple.
The technical scheme that the present invention solves above technical problem is:
A kind of high-temperature resistant anti-corrosive thermal insulating coating, this high-temperature resistant anti-corrosive thermal insulating coating comprises following component by weight:
Film-forming resin: 45-60 part
Color stuffing: 20-30 part
Auxiliary agent: 15-30 part
Solvent: 25-30 part
Wherein, film-forming resin is the mixture of modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin, wherein, film-forming resin by modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin in mass ratio 3:2:4 mix;
Color stuffing is the mixture of composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, wherein color stuffing by composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder in mass ratio 3:2:1:1:1-4:1:1:1:1 mix, expanded vermiculite size is 200-220 order; Glass powder is one or more in lead glass powder, vanadium glass powder, boron glass powder or phosphoric acid glass powder;
Auxiliary agent comprises following component by weight: defoamer: 2-5 part, flow agent: 2-4 part, solidifying agent: 4-8 part, coupling agent: 4-8, glue crosslinking agent: 3-5;
Wherein, defoamer is polysiloxane defoamer, flow agent is the one in cellaburate or polypropylene vinegar ester, solidifying agent is one or more in quadrol, diethylenetriamine, triethylene tetramine, diamino-diphenyl MSM, isophorone diamine or polyamide 6 50, coupling agent is one or more in γ aminopropyltriethoxy silane, γ-Mercaptopropyltriethoxysilane or γ-glycidyl ether Trimethoxy silane, and linking agent is tetra-n-butyl titanate;
Solvent is the mixture that propyl carbinol, ethanol and Virahol mix in any proportion.
The further technical scheme of the present invention is:
In aforementioned high-temperature resistant anti-corrosive thermal insulating coating, the preparation method of modifying epoxy resin by organosilicon is as follows:
Epoxy resin 6101 is dissolved in ethyl acetate solution, add in the there-necked flask that whipping appts, reflux exchanger and thermometer are housed, first pass into water of condensation, and be warming up to 85-90 DEG C gradually, then Union carbide A-162, deionized water and catalyzer is added successively, high-speed stirring, insulation reaction 3-5h, stirring velocity is 600-800r/min.
In aforementioned high-temperature resistant anti-corrosive thermal insulating coating, catalyzer is the one in stannous octoate or dibutyl tin dilaurate.
In aforementioned high-temperature resistant anti-corrosive thermal insulating coating, method of preparing methyl phenyl polysiloxane is as follows:
A. get methyltrimethoxy silane and diphenyldimethoxysilane, add in the glass reaction still with reflux, add the acetone of methyltrimethoxy silane and dimethoxydiphenylsilane total mass 0.2 times;
B. be 70-80 DEG C in temperature, rotating speed is in glass reaction still, add deionized water under 550-600r/min, and the amount of deionized water is the summation of methoxyl group mole number in methyltrimethoxy silane and dimethoxydiphenylsilane;
C., after dropwising, continue to stir, reflux 4-5h, add organic solvent, regulate its solid content to be 70%-75%, then add isocaprylic acid zinc, the add-on of isocaprylic acid zinc is the zinc metal/solid resin mass ratio in isocaprylic acid zinc is 1.5%, after continuing to stir, cooling to leuco base phenyl polysiloxane;
Wherein, the amount adding methyltrimethoxy silane and diphenyldimethoxysilane is methyltrimethoxy silane and diphenyldimethoxysilane mol ratio 2:1-3:1.
In aforementioned high-temperature resistant anti-corrosive thermal insulating coating, the preparation method of organic-silicon-modified unsaturated polyester resin is as follows:
A. get dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane and inject the there-necked flask presetting stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly instill deionized water, 1-1.5h dropwises, and is warming up to 110 DEG C afterwards and continues reaction 1h, finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain the organosilicon performed polymer of pale yellow transparent;
The mass ratio wherein adding dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane is 10:7:2:1.5;
B. by 1, 2-propylene glycol, 1, 4-butyleneglycol, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE drop in there-necked flask, then be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 160-165 DEG C of back flow reaction 40-50min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer and isocaprylic acid zinc, again be warming up to 120 DEG C of reaction 1h, organosilicon performed polymer and unsaturated polyester is made to carry out condensation reaction, the water in removing system and other small molecule by-product is vacuumized after reaction terminates, add in the most backward system containing Resorcinol, benzoyl peroxide and cinnamic mixed diluent, organic-silicon-modified unsaturated polyester resin can be obtained after abundant mixing,
Wherein the mass ratio of 1,2-PD, BDO, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE is 10:5:8:6:3, and Resorcinol, benzoyl peroxide and cinnamic mass ratio are 15:1:100.
The present invention also designs a kind of preparation technology of high-temperature resistant anti-corrosive thermal insulating coating, and this high-temperature resistant anti-corrosive thermal insulating coating preparation technology concrete steps are as follows:
(1) modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified insatiable hunger, vibrin and mixed solvent are added in dispersion cylinder, control the temperature of dispersion cylinder at 45-50 DEG C, high-speed stirring is even, and stirring velocity is 500-600r/min, and churning time is 30-40min;
(2) in step (1), add composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, high-speed stirring 30min again, stirring velocity is 700-800 r/min, controls the temperature of dispersion cylinder at 80-85 DEG C;
(3) in step (2), add defoamer, flow agent, coupling agent, linking agent and solidifying agent successively again, stir at normal temperatures and namely obtain the heat insulation painting of high-temperature resistant anti-corrosive.
The invention has the beneficial effects as follows:
(1) modifying epoxy resin by organosilicon prepared in the present invention has the excellent properties of organosilicon material and epoxy resin concurrently, not only can reduce the internal stress of epoxy resin with modifying epoxy resin by organosilicon but also can increase the performance such as high thermal resistance, toughness.
(2) the aminomethyl phenyl resin prepared in the present invention has good thermotolerance, be suitable as the base-material of high-temperature resistant coating, methyl phenyl silicone resin contains a resinoid of methyl silica structure unit and phenyl silica structure unit simultaneously in addition, due to the introducing of phenyl, effectively raise it in thermo-elasticity, to the performance in the agglutinating value(of coal) of various base material and the consistency of the material such as organic resin and pigment etc.
(3) molecular structure of silicone resin is made successfully to be incorporated on the molecular chain of unsaturated polyester resin in the present invention, make unsaturated polyester resin its initial decomposition temperature after organic-silicon-modified rise to 340 DEG C from 295 DEG C, resistance toheat is significantly improved.
(4) in the present invention, glass powder with low melting point is joined in coating the effect playing " two-step film forming ", because the heat resisting temperature scope of most of silicone resin is between 200-450 DEG C, therefore the temperature tolerance only leaning on silicone resin is very limited, adds glass micro mist and the temperature tolerance scope of silicone resin coating can be made to be expanded.
(5) the composite iron-titanium powder powder added in the present invention can react in the iron atom of steel surface, generate water-fast tertiary iron phosphate complex salt, and firmly at steel surface, play passivation and delay decorations effect, and completely cut off water, oxygen, chlorion etc., play Chemical Preservation effect.
(6) crystal whisker of hexa potassium titanate used in the present invention, wherein potassium ion occupies in the middle of tunnel, has higher stability, thus makes crystal whisker of hexa potassium titanate have chemical stability, insulativity, reflected infrared, excellent antiseptic property etc.
(7) sepiolite added in the present invention is a kind of natural rich magnesium types layered silicate, in needle-like micropore with dead slot structure, has dispel high surface area and strong absorption property, in pin pencil, and internal porous, thermal conductivity is lower, is a kind of excellent thermal insulation material; Expanded vermiculite in the present invention is a kind of iron, magnesium silicate stratiform fragment of complexity, and be wherein full of countless tiny space, thermal conductivity is low, is a kind of excellent thermal insulation material.
(8) by technical scheme of the present invention, the work-ing life of coating can be increased, this coating can not bubble, chap, whiten and the problem such as delamination, this coating also has very strong anticorrosive and salt fog resistance performance, firmly can be adsorbed on metallic surface, thus have good anti-rust and corrosionproperties, and the anticorrosion time is long; This coating application is convenient, easy handling, the advantages such as short construction period.
Embodiment
embodiment 1
The present embodiment provides a kind of high-temperature resistant anti-corrosive thermal insulating coating, and this high-temperature resistant anti-corrosive thermal insulating coating comprises following component by weight:
Modifying epoxy resin by organosilicon: 15 parts, methyl phenyl silicone resin: 10 parts, organic-silicon-modified unsaturated polyester resin: 20 parts,
Composite iron-titanium powder: 9 parts, crystal whisker of hexa potassium titanate: 6 parts, sepiolite: 3 parts, size is 200-220 object expanded vermiculite: 3 parts, lead glass powder: 3 parts, polysiloxane defoamer: 2 parts, cellaburate: 4 parts, quadrol: 8 parts, γ aminopropyltriethoxy silane: 6 parts, tetra-n-butyl titanate: 4 parts, the mixture of propyl carbinol, ethanol and Virahol: 25 parts;
The preparation method of modifying epoxy resin by organosilicon is as follows:
Epoxy resin 6101 is dissolved in ethyl acetate solution, add in the there-necked flask that whipping appts, reflux exchanger and thermometer are housed, first pass into water of condensation, and be warming up to 85 DEG C gradually, then Union carbide A-162, deionized water and stannous octoate is added successively, high-speed stirring, insulation reaction 4h, stirring velocity is 600r/min.
Method of preparing methyl phenyl polysiloxane is as follows:
A. get methyltrimethoxy silane and diphenyldimethoxysilane, add in the glass reaction still with reflux, add the acetone of methyltrimethoxy silane and dimethoxydiphenylsilane total mass 0.2 times;
B. be 70 DEG C in temperature, rotating speed is in glass reaction still, add deionized water under 580r/min, and the amount of deionized water is the summation of methoxyl group mole number in methyltrimethoxy silane and dimethoxydiphenylsilane;
C., after dropwising, continue to stir, reflux 4h, add organic solvent, regulate its solid content to be 75%, then add isocaprylic acid zinc, the add-on of isocaprylic acid zinc is the zinc metal/solid resin mass ratio in isocaprylic acid zinc is 1.5%, after continuing to stir, cooling to leuco base phenyl polysiloxane;
Wherein, the amount adding methyltrimethoxy silane and diphenyldimethoxysilane is methyltrimethoxy silane and diphenyldimethoxysilane mol ratio 2:1-3:1.
The preparation method of organic-silicon-modified unsaturated polyester resin is as follows:
A. get dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane and inject the there-necked flask presetting stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly instill deionized water, 1.2h dropwises, and is warming up to 110 DEG C afterwards and continues reaction 1h, finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain the organosilicon performed polymer of pale yellow transparent;
The mass ratio wherein adding dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane is 10:7:2:1.5;
B. by 1, 2-propylene glycol, 1, 4-butyleneglycol, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE drop in there-necked flask, then 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 45min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer and isocaprylic acid zinc, again be warming up to 120 DEG C of reaction 1h, organosilicon performed polymer and unsaturated polyester is made to carry out condensation reaction, the water in removing system and other small molecule by-product is vacuumized after reaction terminates, add in the most backward system containing Resorcinol, benzoyl peroxide and cinnamic mixed diluent, organic-silicon-modified unsaturated polyester resin can be obtained after abundant mixing,
Wherein, the mass ratio of 1,2-PD, BDO, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE is 10:5:8:6:3, and Resorcinol, benzoyl peroxide and cinnamic mass ratio are 15:1:100.
The preparation technology of above-mentioned high-temperature resistant anti-corrosive thermal insulating coating, this high-temperature resistant anti-corrosive thermal insulating coating preparation technology concrete steps are as follows:
(1) mixed solvent of modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified insatiable hunger, vibrin is added in dispersion cylinder, control the temperature of dispersion cylinder at 4 DEG C, high-speed stirring is even, and stirring velocity is 550r/min, and churning time is 30min;
(2) in step (1), add composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, high-speed stirring 30min again, stirring velocity is 750 r/min, controls the temperature of dispersion cylinder at 80 DEG C;
(3) in step (2), add polysiloxane defoamer, flow agent cellaburate, coupling agent γ aminopropyltriethoxy silane, linking agent tetra-n-butyl titanate and curing agent ethylene diamine successively again, stir at normal temperatures and namely obtain the heat insulation painting of high-temperature resistant anti-corrosive.
embodiment 2
The present embodiment provides a kind of high-temperature resistant anti-corrosive thermal insulating coating, and this high-temperature resistant anti-corrosive thermal insulating coating comprises following component by weight:
Modifying epoxy resin by organosilicon: 15 parts, methyl phenyl silicone resin: 10 parts, organic-silicon-modified unsaturated polyester resin: 20 parts, composite iron-titanium powder: 12 parts, crystal whisker of hexa potassium titanate: 3 parts, sepiolite: 3 parts, size is 200-220 object expanded vermiculite: 3 parts, lead glass powder: 3 parts, polysiloxane defoamer: 5 parts, polypropylene vinegar ester: 3 parts, diamino-diphenyl MSM: 8 parts, γ-glycidyl ether Trimethoxy silane: 5 parts, tetra-n-butyl titanate: 5 parts, the mixture that propyl carbinol, ethanol and Virahol mix in any proportion: 30 parts;
The preparation method of modifying epoxy resin by organosilicon is as follows:
Epoxy resin 6101 is dissolved in ethyl acetate solution, add in the there-necked flask that whipping appts, reflux exchanger and thermometer are housed, first pass into water of condensation, and be warming up to 90 DEG C gradually, then Union carbide A-162, deionized water and dibutyl tin dilaurate is added successively, high-speed stirring, insulation reaction 5h, stirring velocity is 800r/min.
Method of preparing methyl phenyl polysiloxane is as follows:
A. get methyltrimethoxy silane and diphenyldimethoxysilane, add in the glass reaction still with reflux, add the acetone of methyltrimethoxy silane and dimethoxydiphenylsilane total mass 0.2 times;
B. be 80 DEG C in temperature, rotating speed is in glass reaction still, add deionized water under 600r/min, and the amount of deionized water is the summation of methoxyl group mole number in methyltrimethoxy silane and dimethoxydiphenylsilane;
C., after dropwising, continue to stir, reflux 5h, add organic solvent, regulate its solid content to be 70%, then add isocaprylic acid zinc, the add-on of isocaprylic acid zinc is the zinc metal/solid resin mass ratio in isocaprylic acid zinc is 1.5%, after continuing to stir, cooling to leuco base phenyl polysiloxane;
Wherein, the amount adding methyltrimethoxy silane and diphenyldimethoxysilane is methyltrimethoxy silane and diphenyldimethoxysilane mol ratio 2:1-3:1.
The preparation method of organic-silicon-modified unsaturated polyester resin is as follows:
A. get dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane and inject the there-necked flask presetting stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly instill deionized water, 1.5h dropwises, and is warming up to 110 DEG C afterwards and continues reaction 1h, finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain the organosilicon performed polymer of pale yellow transparent;
The mass ratio wherein adding dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane is 10:7:2:1.5;
B. by 1, 2-propylene glycol, 1, 4-butyleneglycol, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE drop in there-necked flask, then be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 165 DEG C of back flow reaction 50min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer and isocaprylic acid zinc, again be warming up to 120 DEG C of reaction 1h, organosilicon performed polymer and unsaturated polyester is made to carry out condensation reaction, the water in removing system and other small molecule by-product is vacuumized after reaction terminates, add in the most backward system containing Resorcinol, benzoyl peroxide and cinnamic mixed diluent, organic-silicon-modified unsaturated polyester resin can be obtained after abundant mixing,
Wherein, the mass ratio of 1,2-PD, BDO, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE is 10:5:8:6:3, and Resorcinol, benzoyl peroxide and cinnamic mass ratio are 15:1:100.
The preparation technology of above-mentioned high-temperature resistant anti-corrosive thermal insulating coating, this high-temperature resistant anti-corrosive thermal insulating coating preparation technology concrete steps are as follows:
(1) modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified insatiable hunger, vibrin and mixed solvent are added in dispersion cylinder, control the temperature of dispersion cylinder at 50 DEG C, high-speed stirring is even, and stirring velocity is 600r/min, and churning time is 40min;
(2) in step (1), add composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, high-speed stirring 30min again, stirring velocity is 700 r/min, controls the temperature of dispersion cylinder at 85 DEG C;
(3) in step (2), add defoamer, flow agent polypropylene vinegar ester, coupling agent γ-glycidyl ether Trimethoxy silane, linking agent tetra-n-butyl titanate and solidifying agent diamino-diphenyl MSM successively again, stir at normal temperatures and namely obtain the heat insulation painting of high-temperature resistant anti-corrosive.
embodiment 3
The present embodiment provides a kind of high-temperature resistant anti-corrosive thermal insulating coating, and this high-temperature resistant anti-corrosive thermal insulating coating comprises following component by weight:
Modifying epoxy resin by organosilicon: 18 parts, methyl phenyl silicone resin: 12 parts, organic-silicon-modified unsaturated polyester resin: 24 parts, composite iron-titanium powder: 9 parts, crystal whisker of hexa potassium titanate: 6 parts, sepiolite: 3 parts, size is 200-220 object expanded vermiculite: 3 parts, lead glass powder: 3 parts, polysiloxane defoamer: 4 parts, cellaburate: 2 parts, isophorone diamine: 4 parts, γ-Mercaptopropyltriethoxysilane: 4 parts, tetra-n-butyl titanate: 3 parts, the mixture that propyl carbinol, ethanol and Virahol mix in any proportion: 27 parts;
The preparation method of modifying epoxy resin by organosilicon is as follows:
Epoxy resin 6101 is dissolved in ethyl acetate solution, add in the there-necked flask that whipping appts, reflux exchanger and thermometer are housed, first pass into water of condensation, and be warming up to 88 DEG C gradually, then the sub-tin of Union carbide A-162, deionized water and octoate catalyst is added successively, high-speed stirring, insulation reaction 3h, stirring velocity is 700r/min.
Method of preparing methyl phenyl polysiloxane is as follows:
A. get methyltrimethoxy silane and diphenyldimethoxysilane, add in the glass reaction still with reflux, add the acetone of methyltrimethoxy silane and dimethoxydiphenylsilane total mass 0.2 times;
B. be 75 DEG C in temperature, rotating speed is in glass reaction still, add deionized water under 550r/min, and the amount of deionized water is the summation of methoxyl group mole number in methyltrimethoxy silane and dimethoxydiphenylsilane;
C., after dropwising, continue to stir, reflux 4h, add organic solvent, regulate its solid content to be 72%, then add isocaprylic acid zinc, the add-on of isocaprylic acid zinc is the zinc metal/solid resin mass ratio in isocaprylic acid zinc is 1.5%, after continuing to stir, cooling to leuco base phenyl polysiloxane;
Wherein, the amount adding methyltrimethoxy silane and diphenyldimethoxysilane is methyltrimethoxy silane and diphenyldimethoxysilane mol ratio 2:1-3:1.
The preparation method of organic-silicon-modified unsaturated polyester resin is as follows:
A. get dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane and inject the there-necked flask presetting stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly instill deionized water, 1h dropwises, and is warming up to 110 DEG C afterwards and continues reaction 1h, finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain the organosilicon performed polymer of pale yellow transparent;
The mass ratio wherein adding dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane is 10:7:2:1.5;
B. by 1, 2-propylene glycol, 1, 4-butyleneglycol, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE drop in there-necked flask, then be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 162 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 a certain amount of organosilicon performed polymer and isocaprylic acid zinc, again be warming up to 120 DEG C of reaction 1h, organosilicon performed polymer and unsaturated polyester is made to carry out condensation reaction, the water in removing system and other small molecule by-product is vacuumized after reaction terminates, add in the most backward system containing Resorcinol, benzoyl peroxide and cinnamic mixed diluent, organic-silicon-modified unsaturated polyester resin can be obtained after abundant mixing,
Wherein, the mass ratio of 1,2-PD, BDO, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE is 10:5:8:6:3, and Resorcinol, benzoyl peroxide and cinnamic mass ratio are 15:1:100.
The preparation technology of above-mentioned high-temperature resistant anti-corrosive thermal insulating coating, this high-temperature resistant anti-corrosive thermal insulating coating preparation technology concrete steps are as follows:
(1) modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified insatiable hunger, vibrin and mixed solvent are added in dispersion cylinder, control the temperature of dispersion cylinder at 48 DEG C, high-speed stirring is even, and stirring velocity is 500r/min, and churning time is 35min;
(2) in step (1), add composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, high-speed stirring 30min again, stirring velocity is 800 r/min, controls the temperature of dispersion cylinder at 82 DEG C;
(3) in step (2), adding defoamer successively is again polysiloxane defoamer, flow agent cellaburate, coupling agent γ-Mercaptopropyltriethoxysilane, linking agent tetra-n-butyl titanate and solidifying agent isophorone diamine, stirs at normal temperatures and namely obtains the heat insulation painting of high-temperature resistant anti-corrosive.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (6)
1. a high-temperature resistant anti-corrosive thermal insulating coating, is characterized in that: this high-temperature resistant anti-corrosive thermal insulating coating comprises following component by weight:
Film-forming resin: 45-60 part
Color stuffing: 20-30 part
Auxiliary agent: 15-30 part
Solvent: 25-30 part
Wherein, described film-forming resin is the mixture of modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin, wherein, film-forming resin by modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin in mass ratio 3:2:4 mix;
Described color stuffing is the mixture of composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, wherein color stuffing by composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder in mass ratio 3:2:1:1:1-4:1:1:1:1 mix, described expanded vermiculite size is 200-220 order; Described glass powder is one or more in lead glass powder, vanadium glass powder, boron glass powder or phosphoric acid glass powder;
Described auxiliary agent comprises following component by weight: defoamer: 2-5 part, flow agent: 2-4 part, solidifying agent: 4-8 part, coupling agent: 4-8, glue crosslinking agent: 3-5;
Wherein, described defoamer is polysiloxane defoamer, described flow agent is the one in cellaburate or polypropylene vinegar ester, described solidifying agent is one or more in quadrol, diethylenetriamine, triethylene tetramine, diamino-diphenyl MSM, isophorone diamine or polyamide 6 50, described coupling agent is one or more in γ aminopropyltriethoxy silane, γ-Mercaptopropyltriethoxysilane or γ-glycidyl ether Trimethoxy silane, and described linking agent is tetra-n-butyl titanate;
Described solvent is the mixture that propyl carbinol, ethanol and Virahol mix in any proportion.
2. high-temperature resistant anti-corrosive thermal insulating coating according to claim 1, is characterized in that: the preparation method of described modifying epoxy resin by organosilicon is as follows:
Epoxy resin 6101 is dissolved in ethyl acetate solution, add in the there-necked flask that whipping appts, reflux exchanger and thermometer are housed, first pass into water of condensation, and be warming up to 85-90 DEG C gradually, then Union carbide A-162, deionized water and catalyzer is added successively, high-speed stirring, insulation reaction 3-5h, stirring velocity is 600-800r/min.
3. high-temperature resistant anti-corrosive thermal insulating coating according to claim 2, is characterized in that, described catalyzer is the one in stannous octoate or dibutyl tin dilaurate.
4. high-temperature resistant anti-corrosive thermal insulating coating according to claim 1, is characterized in that: described method of preparing methyl phenyl polysiloxane is as follows:
A. get methyltrimethoxy silane and diphenyldimethoxysilane, add in the glass reaction still with reflux, add the acetone of methyltrimethoxy silane and dimethoxydiphenylsilane total mass 0.2 times;
B. be 70-80 DEG C in temperature, rotating speed is in glass reaction still, add deionized water under 550-600r/min, and the amount of deionized water is the summation of methoxyl group mole number in methyltrimethoxy silane and dimethoxydiphenylsilane;
C., after dropwising, continue to stir, reflux 4-5h, add organic solvent, regulate its solid content to be 70%-75%, then add isocaprylic acid zinc, the add-on of isocaprylic acid zinc is the zinc metal/solid resin mass ratio in isocaprylic acid zinc is 1.5%, after continuing to stir, cooling to leuco base phenyl polysiloxane;
Wherein, the described amount adding methyltrimethoxy silane and diphenyldimethoxysilane is methyltrimethoxy silane and diphenyldimethoxysilane mol ratio 2:1-3:1.
5. high-temperature resistant anti-corrosive thermal insulating coating according to claim 1, is characterized in that: the preparation method of described organic-silicon-modified unsaturated polyester resin is as follows:
A. get dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane and inject the there-necked flask presetting stirring and condenser apparatus;
Bath temperature is set to 50 DEG C, under agitation in there-necked flask, slowly instill deionized water, 1-1.5h dropwises, and is warming up to 110 DEG C afterwards and continues reaction 1h, finally decompression removing dehydrated alcohol, residual moisture and low molecular weight substance, can obtain the organosilicon performed polymer of pale yellow transparent;
The wherein said mass ratio adding dehydrated alcohol, Union carbide A-162, Diphenylsilanediol and vinyltriethoxysilane is 10:7:2:1.5;
B. by 1, 2-propylene glycol, 1, 4-butyleneglycol, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE drop in there-necked flask, then be placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, be heated to 160-165 DEG C of back flow reaction 40-50min, then 200 DEG C are warming up to, 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer and isocaprylic acid zinc, again be warming up to 120 DEG C of reaction 1h, organosilicon performed polymer and unsaturated polyester is made to carry out condensation reaction, the water in removing system and other small molecule by-product is vacuumized after reaction terminates, add in the most backward system containing Resorcinol, benzoyl peroxide and cinnamic mixed diluent, organic-silicon-modified unsaturated polyester resin can be obtained after abundant mixing,
The mass ratio of wherein said 1,2-PD, BDO, hexanodioic acid, tetrahydrophthalic anhydride and MALEIC ANHYDRIDE is 10:5:8:6:3, and described Resorcinol, benzoyl peroxide and cinnamic mass ratio are 15:1:100.
6. the preparation technology of high-temperature resistant anti-corrosive thermal insulating coating as claimed in claim 1, it is characterized in that, this high-temperature resistant anti-corrosive thermal insulating coating preparation technology concrete steps are as follows:
(1) modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified insatiable hunger, vibrin and mixed solvent are added in dispersion cylinder, control the temperature of dispersion cylinder at 45-50 DEG C, high-speed stirring is even, and stirring velocity is 500-600r/min, and churning time is 30-40min;
(2) in step (1), add composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass powder, high-speed stirring 30min again, stirring velocity is 700-800 r/min, controls the temperature of dispersion cylinder at 80-85 DEG C;
(3) in step (2), add defoamer, flow agent, coupling agent, linking agent and solidifying agent successively again, stir at normal temperatures and namely obtain the heat insulation painting of high-temperature resistant anti-corrosive.
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