CN104673063B - 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, and in particular to a kind of high-temperature resistant anti-corrosive insulating moulding coating and its preparation technology.
Background technology
With continuing to develop for China's modern industry, particularly in industries such as metallurgy, petrochemical industry, the energy, new material and military projects,
The application of high-temperature service and auxiliary facility is more and more, but metal material easily occurs in hot environment with the oxygen in air
Oxidation reaction, produces corrosion phenomena, so that metal material gradually loses intensity and causes structural missing, as various accidents
Hidden danger.Therefore, high-temperature service surface is typically necessary application fire-resistant anticorrosion paint and is protected, to prevent metal material oxygen
Change corrosion, extend the service life of high-temperature service.
Common coating is susceptible to thermal degradation and carbonization under the high temperature conditions so that soil layer is destroyed, it is impossible to base
Material plays a protective role, and high-temperature resistant coating can keep not embrittlement under the high temperature conditions, not with base material peel off, bubbling is not same
When keep certain physics and chemistry and mechanical performance so that object can be bad from chemical attack, oxidation corrosion etc. at high temperature
The influence of situation.
At present, high-temperature resistant coating can be divided mainly into refractory inorganic paint and the major class of organic high temperature-resistant coating two, inorganic resistance to
High-temperature coatings are mainly made up of inorganic component, and high temperature resistant inorganic coating is due to environmental protection, low cost, hardness high, long lifespan, anti-
The advantages of hot property is excellent, and paid close attention to by people；Organic high temperature-resistant coating mainly has organic coating, modified epoxy to apply
Several classes such as material, phenolic resin coating, polyurethane coating, wherein organic siliconresin in its unique component and molecule because containing silicon-carbon
Bond structure so that organic siliconresin has merged organic matter and inorganic matter characteristic well, is obtained extensively in paint field
Application.
The coating protection of high-temperature service is most to use organic silicon high-temperature resistant coating, and temperature in use is in 400-600 DEG C of scope
It is interior, from pure organosilicon coating；When temperature in use is below 400 DEG C, from research of silicone modified coating.Pure organic siliconresin has
Heat endurance, oxidative resistance, weatherability, lower temperature resistance are good, and surface can be low, the advantages of dielectric strength is high, but generally require height
Temperature solidification, brings inconvenience to large-area construction, and its antiseptic power, poor adhesive force.Organic-silicon-modified resin is to send out in recent years
What exhibition was got up, the internal stress of high-temperature coatings can be reduced, the performances such as pliability, the high temperature resistant of high-temperature coatings can be increased again, the two
With the complementary feature learnt from other's strong points to offset one's weaknesses.
The content of the invention
The technical problems to be solved by the invention are, for the shortcoming that above prior art is present, propose a kind of high temperature resistant
Anticorrosive heat insulating coating and its preparation technology, the coating environmental protection, low cost, hardness high, long lifespan, heat resistanceheat resistant performance are good, pliability is good,
The advantages of high temperature resistant is good, and preparation process is simple.
The present invention solve above technical problem technical scheme be：
A kind of high-temperature resistant anti-corrosive insulating moulding coating, the high-temperature resistant anti-corrosive insulating moulding coating includes following components by weight：
Wherein, film-forming resin is that modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturation are poly-
The mixture of ester resin, wherein, film-forming resin by modifying epoxy resin by organosilicon, methyl phenyl silicone resin and it is organic-silicon-modified not
Saturated 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 dust, wherein
Color stuffing is by composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust in mass ratio 3：2：1：1：1 mixing
Form, expanded vermiculite size is 200-220 mesh；Glass dust is in lead glass powder, vanadium glass dust, boron glass powder or phosphoric acid glass powder
One or more；
Auxiliary agent includes following components by weight：Defoamer：2-5 parts, levelling agent：2-4 parts, curing agent：It is 4-8 parts, even
Connection agent：4-8, crosslinking agent：3-5；
Wherein, defoamer is polysiloxane-based defoamer, and levelling agent is the one kind in cellaburate or polyacrylate,
Curing agent is ethylenediamine, diethylenetriamine, triethylene tetramine, diamino-diphenyl MSM, IPD or polyamide 6 50
In one or more, coupling agent be γ aminopropyltriethoxy silane, γ-Mercaptopropyltriethoxysilane or γ-contracting
One or more in water glycerine ether trimethoxy silane, crosslinking agent is tetra-n-butyl titanate；
Solvent is the mixture that n-butanol, ethanol and isopropanol mix in any proportion.
Further technical scheme is the present invention：
In foregoing high-temperature resistant anti-corrosive insulating moulding coating, the preparation method of modifying epoxy resin by organosilicon is as follows：
Epoxy resin 6101 is dissolved in ethyl acetate solution, is added and agitating device, reflux condenser and temperature is housed
In the there-necked flask of meter, be first passed through condensed water, and be gradually heating to 85-90 DEG C, then sequentially add MTES,
Deionized water and catalyst, high-speed stirred, insulation reaction 3-5h, mixing speed is 600-800r/min.
In foregoing high-temperature resistant anti-corrosive insulating moulding coating, catalyst is the one kind in stannous octoate or dibutyl tin dilaurate.
In foregoing high-temperature resistant anti-corrosive insulating moulding coating, method of preparing methyl phenyl polysiloxane is as follows：
A. MTMS and diphenyldimethoxysilane are taken, the glass reaction kettle with reflux is added
In, add the acetone of 0.2 times of MTMS and dimethoxydiphenylsilane gross mass；
B. temperature be 70-80 DEG C, rotating speed be 550-600r/min under to deionized water is added in glass reaction kettle, go from
The amount of sub- water is the summation of the middle methoxyl group molal quantity of both MTMS and dimethoxydiphenylsilane；
C. after completion of dropping, continue to stir, flow back 4-5h, add organic solvent, adjust its solid content for 70%-75%, so
After add zinc Isoocatanoate, the addition of zinc Isoocatanoate is 1.5% for the zinc metal/hard resin mass ratio in zinc Isoocatanoate, is continued
After stirring, cooling obtains leuco base phenyl polysiloxane；
Wherein, the amount for adding MTMS and diphenyldimethoxysilane is MTMS and two
Benzene dimethoxysilane mol ratio 2：1-3：1.
In foregoing high-temperature resistant anti-corrosive insulating moulding coating, the preparation method of organic-silicon-modified unsaturated polyester resin is as follows：
A. the injection of absolute ethyl alcohol, MTES, diphenyl silanediol and VTES is taken pre-
It is equipped with the there-necked flask of stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation to slowly being dripped in there-necked flask
Enter deionized water, 1-1.5h completion of dropping is warming up to 110 DEG C and continues to react 1h afterwards, and absolute ethyl alcohol, residual is finally removed under reduced pressure
Moisture and low molecular weight substance, you can obtain the organosilicon performed polymer of pale yellow transparent；
Wherein add absolute ethyl alcohol, MTES, diphenyl silanediol and VTES
Mass ratio is 10：7：2：1.5；
B. 1,2-PD, BDO, adipic acid, THPA and maleic anhydride are put into there-necked flask
In, it is subsequently placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, it is heated to 160-165 DEG C of back flow reaction 40-
50min, then heats to 200 DEG C, and 90 DEG C are cooled to when system acid number reaches 15mgKOH/g, adds a certain amount of organosilicon pre-
Aggressiveness and zinc Isoocatanoate, are warming up to 120 DEG C of reaction 1h again, organosilicon performed polymer is carried out condensation reaction with unsaturated polyester (UP),
Water and other small molecule by-products that reaction is vacuumized in removing system after terminating, add in most backward system and contain to benzene two
The mixed diluent of phenol, benzoyl peroxide and styrene, organic-silicon-modified unsaturated polyester (UP) is can obtain after being sufficiently mixed
Resin；
Wherein the mass ratio of 1,2-PD, BDO, adipic acid, THPA and maleic anhydride is 10：
5：8：6：3, the mass ratio of hydroquinones, benzoyl peroxide and styrene is 15：1：100.
The present invention also designs a kind of preparation technology of high-temperature resistant anti-corrosive insulating moulding coating, prepared by the high-temperature resistant anti-corrosive insulating moulding coating
Technique is comprised the following steps that：
（1）By the mixed of modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin
Bonding solvent is added in dispersion cylinder, controls the temperature of dispersion cylinder at 45-50 DEG C, and high-speed stirred is uniform, and mixing speed is 500-600r/
Min, mixing time is 30-40min；
（2）Again to step（1）Middle addition composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust,
High-speed stirred 30min, mixing speed is 700-800r/min, controls the temperature of dispersion cylinder at 80-85 DEG C；
（3）Again to step（2）In sequentially add defoamer, levelling agent, coupling agent, crosslinking agent and curing agent, at normal temperatures
Stirs the high-temperature resistant anti-corrosive insulating moulding coating that obtain.
The beneficial effects of the invention are as follows：
（1）The modifying epoxy resin by organosilicon prepared in the present invention has the superiority of organosilicon material and epoxy resin concurrently
Can, the internal stress of epoxy resin can be not only reduced with modifying epoxy resin by organosilicon but also the performances such as heat-resisting quantity, toughness can have been increased.
（2）The aminomethyl phenyl resin prepared in the present invention has good heat resistance, is suitable as the base of high-temperature resistant coating
Material, the methyl phenyl silicone resin resinoid containing methyl silica structure unit and phenyl silica structure unit simultaneously in addition, by
In the introducing of phenyl, it is effectively raised in thermoelasticity, to materials such as the cohesivenesses and organic resin and pigment of various base materials
The aspect such as compatibility performance.
(3) molecular structure of organic siliconresin is made successfully to be incorporated into the strand of unsaturated polyester resin in the present invention
On, unsaturated polyester resin is risen to 340 DEG C, heat resistance from 295 DEG C through organic-silicon-modified its initial decomposition temperature afterwards
It is significantly improved.
（4）Glass powder with low melting point is added in the present invention plays a part of " two-step film forming " in coating, due to most of
The heat resisting temperature scope of organic siliconresin is between 200-450 DEG C, therefore only the temperature tolerance by organic siliconresin is extremely limited
, add glass micro mist to cause that the temperature tolerance scope of silicone resin coating is expanded.
（5）The composite iron-titanium powder powder added in the present invention can react in the iron atom of steel surface, generate insoluble
In the phosphoric acid iron complex salt of water, and firmly in steel surface, the slow decorations effect of passivation is played, and completely cut off water, oxygen, chlorion etc., risen
To chemical preservation effect.
（6）The crystal whisker of hexa potassium titanate used in the present invention, wherein potassium ion are occupied in the middle of tunnel, with stability higher,
So that crystal whisker of hexa potassium titanate has chemical stability, insulating properties, reflection infrared ray, excellent antiseptic property etc..
（7）The sepiolite added in the present invention is a kind of natural rich magnesium types phyllosilicate, in needle-like micropore and dead slot knot
Structure, with high surface and the strong absorption property of dispelling, in pin pencil, internal porous, thermal conductivity factor is relatively low, is a kind of excellent thermal insulation
Material；Expanded vermiculite in the present invention is a kind of complicated iron, magnesium silicate stratiform fragment, is filled with countless tiny skies
Gap, thermal conductivity factor is low, is a kind of excellent heat-insulating material.
（8）By technical scheme, by increasing capacitance it is possible to increase the service life of coating, the coating will not occur foaming, tortoise
Split, whiten and the problems such as delamination, the coating also has very strong anticorrosive and resistance to saltfog energy, can firmly adsorb in metal watch
Face, so that there are good anti-rust and corrosionproperties, and the anti-corrosion time is long；The coating application is convenient, it is easy to operate, short construction period
The advantages of.
Specific embodiment
Embodiment 1
The present embodiment provides a kind of high-temperature resistant anti-corrosive insulating moulding coating, and the high-temperature resistant anti-corrosive insulating moulding coating is by weight
Including following components：
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 the expanded vermiculite of 200-220 mesh：
3 parts, lead glass powder：3 parts, polysiloxane-based defoamer：2 parts, cellaburate：4 parts, ethylenediamine：8 parts, gamma-amino propyl group three
Ethoxysilane：6 parts, tetra-n-butyl titanate：4 parts, the mixture of n-butanol, ethanol and isopropanol：25 parts；
The preparation method of modifying epoxy resin by organosilicon is as follows：
Epoxy resin 6101 is dissolved in ethyl acetate solution, is added and agitating device, reflux condenser and temperature is housed
In the there-necked flask of meter, condensed water is first passed through, and is gradually heating to 85 DEG C, then sequentially added MTES, go
Ionized water and stannous octoate, high-speed stirred, insulation reaction 4h, mixing speed is 600r/min.
Method of preparing methyl phenyl polysiloxane is as follows：
A. MTMS and diphenyldimethoxysilane are taken, the glass reaction kettle with reflux is added
In, add the acetone of 0.2 times of MTMS and dimethoxydiphenylsilane gross mass；
B. be 70 DEG C in temperature, rotating speed be under 580r/min to adding deionized water in glass reaction kettle, deionized water
It is the summation of the middle methoxyl group molal quantity of both MTMS and dimethoxydiphenylsilane to measure；
C. after completion of dropping, continue to stir, flow back 4h, add organic solvent, it is 75% to adjust its solid content, is subsequently adding
Zinc Isoocatanoate, the addition of zinc Isoocatanoate is 1.5% for the zinc metal/hard resin mass ratio in zinc Isoocatanoate, continues to stir
Afterwards, cooling obtains leuco base phenyl polysiloxane；
Wherein, the amount for adding MTMS and diphenyldimethoxysilane is MTMS and two
Benzene dimethoxysilane mol ratio 2：1-3：1.
The preparation method of organic-silicon-modified unsaturated polyester resin is as follows：
A. the injection of absolute ethyl alcohol, MTES, diphenyl silanediol and VTES is taken pre-
It is equipped with the there-necked flask of stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation to slowly being dripped in there-necked flask
Enter deionized water, 1.2h completion of dropping is warming up to 110 DEG C and continues to react 1h afterwards, and absolute ethyl alcohol, residual water is finally removed under reduced pressure
Divide and low molecular weight substance, you can obtain the organosilicon performed polymer of pale yellow transparent；
Wherein add absolute ethyl alcohol, MTES, diphenyl silanediol and VTES
Mass ratio is 10：7：2：1.5；
B. 1,2-PD, BDO, adipic acid, THPA and maleic anhydride are put into there-necked flask
In, it is subsequently placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, 160 DEG C of back flow reaction 45min are heated to, so
After be warming up to 200 DEG C, be cooled to 90 DEG C when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer with it is different
Zinc octoate, is warming up to 120 DEG C of reaction 1h again, organosilicon performed polymer is carried out condensation reaction with unsaturated polyester (UP), and reaction terminates
The water and other small molecule by-products in removing system are vacuumized afterwards, are added in most backward system and are contained hydroquinones, peroxidating
The mixed diluent of benzoyl and styrene, organic-silicon-modified unsaturated polyester resin is can obtain after being sufficiently mixed；
Wherein, the mass ratio of 1,2-PD, BDO, adipic acid, THPA and maleic anhydride is 10：
5：8：6：3, the mass ratio of hydroquinones, benzoyl peroxide and styrene is 15：1：100.
The preparation technology of above-mentioned high-temperature resistant anti-corrosive insulating moulding coating, the high-temperature resistant anti-corrosive insulating moulding coating preparation technology specific steps
It is as follows：
（1）By the mixed of modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin
Bonding solvent is added in dispersion cylinder, controls the temperature of dispersion cylinder at 4 DEG C, and high-speed stirred is uniform, and mixing speed is 550r/min, stirring
Time is 30min；
（2）Again to step（1）Middle addition composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust,
High-speed stirred 30min, mixing speed is 750r/min, controls the temperature of dispersion cylinder at 80 DEG C；
（3）Again to step（2）In sequentially add polysiloxane-based defoamer, levelling agent cellaburate, coupling agent γ-ammonia
Base propyl-triethoxysilicane, crosslinking agent tetra-n-butyl titanate and curing agent ethylene diamine, stirring at normal temperatures, it is resistance to obtain
High-temperature anticorrosion insulating moulding coating.
Embodiment 2
The present embodiment provides a kind of high-temperature resistant anti-corrosive insulating moulding coating, and the high-temperature resistant anti-corrosive insulating moulding coating is by weight
Including following components：
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 the expanded vermiculite of 200-220 mesh：3
Part, lead glass powder：3 parts, polysiloxane-based defoamer：5 parts, polyacrylate：3 parts, diamino-diphenyl MSM：8 parts, γ-
Glycidyl ether trimethoxy silane：5 parts, tetra-n-butyl titanate：5 parts, n-butanol, ethanol and isopropanol are mixed in any proportion
The mixture of conjunction：30 parts；
The preparation method of modifying epoxy resin by organosilicon is as follows：
Epoxy resin 6101 is dissolved in ethyl acetate solution, is added and agitating device, reflux condenser and temperature is housed
In the there-necked flask of meter, condensed water is first passed through, and is gradually heating to 90 DEG C, then sequentially added MTES, go
Ionized water and dibutyl tin dilaurate, high-speed stirred, insulation reaction 5h, mixing speed is 800r/min.
Method of preparing methyl phenyl polysiloxane is as follows：
A. MTMS and diphenyldimethoxysilane are taken, the glass reaction kettle with reflux is added
In, add the acetone of 0.2 times of MTMS and dimethoxydiphenylsilane gross mass；
B. be 80 DEG C in temperature, rotating speed be under 600r/min to adding deionized water in glass reaction kettle, deionized water
It is the summation of the middle methoxyl group molal quantity of both MTMS and dimethoxydiphenylsilane to measure；
C. after completion of dropping, continue to stir, flow back 5h, add organic solvent, it is 70% to adjust its solid content, is subsequently adding
Zinc Isoocatanoate, the addition of zinc Isoocatanoate is 1.5% for the zinc metal/hard resin mass ratio in zinc Isoocatanoate, continues to stir
Afterwards, cooling obtains leuco base phenyl polysiloxane；
Wherein, the amount for adding MTMS and diphenyldimethoxysilane is MTMS and two
Benzene dimethoxysilane mol ratio 2：1-3：1.
The preparation method of organic-silicon-modified unsaturated polyester resin is as follows：
A. the injection of absolute ethyl alcohol, MTES, diphenyl silanediol and VTES is taken pre-
It is equipped with the there-necked flask of stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation to slowly being dripped in there-necked flask
Enter deionized water, 1.5h completion of dropping is warming up to 110 DEG C and continues to react 1h afterwards, and absolute ethyl alcohol, residual water is finally removed under reduced pressure
Divide and low molecular weight substance, you can obtain the organosilicon performed polymer of pale yellow transparent；
Wherein add absolute ethyl alcohol, MTES, diphenyl silanediol and VTES
Mass ratio is 10：7：2：1.5；
B. 1,2-PD, BDO, adipic acid, THPA and maleic anhydride are put into there-necked flask
In, it is subsequently placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, 165 DEG C of back flow reaction 50min are heated to, so
After be warming up to 200 DEG C, be cooled to 90 DEG C when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer with it is different
Zinc octoate, is warming up to 120 DEG C of reaction 1h again, organosilicon performed polymer is carried out condensation reaction with unsaturated polyester (UP), and reaction terminates
The water and other small molecule by-products in removing system are vacuumized afterwards, are added in most backward system and are contained hydroquinones, peroxidating
The mixed diluent of benzoyl and styrene, organic-silicon-modified unsaturated polyester resin is can obtain after being sufficiently mixed；
Wherein, the mass ratio of 1,2-PD, BDO, adipic acid, THPA and maleic anhydride is 10：
5：8：6：3, the mass ratio of hydroquinones, benzoyl peroxide and styrene is 15：1：100.
The preparation technology of above-mentioned high-temperature resistant anti-corrosive insulating moulding coating, the high-temperature resistant anti-corrosive insulating moulding coating preparation technology specific steps
It is as follows：
（1）By modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin and mixed
Bonding solvent is added in dispersion cylinder, controls the temperature of dispersion cylinder at 50 DEG C, and high-speed stirred is uniform, and mixing speed is 600r/min, is stirred
The time is mixed for 40min；
（2）Again to step（1）Middle addition composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust,
High-speed stirred 30min, mixing speed is 700r/min, controls the temperature of dispersion cylinder at 85 DEG C；
（3）Again to step（2）In sequentially add defoamer, levelling agent polyacrylate, coupling agent γ-glycidyl ether
Trimethoxy silane, crosslinking agent tetra-n-butyl titanate and curing agent diamino-diphenyl MSM, stir obtain final product at normal temperatures
To high-temperature resistant anti-corrosive insulating moulding coating.
Embodiment 3
The present embodiment provides a kind of high-temperature resistant anti-corrosive insulating moulding coating, and the high-temperature resistant anti-corrosive insulating moulding coating is by weight
Including following components：
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 the expanded vermiculite of 200-220 mesh：3
Part, lead glass powder：3 parts, polysiloxane-based defoamer：4 parts, cellaburate：2 parts, IPD：4 parts, γ-sulfydryl
Propyl-triethoxysilicane：4 parts, tetra-n-butyl titanate：3 parts, the mixing that n-butanol, ethanol and isopropanol mix in any proportion
Thing：27 parts；
The preparation method of modifying epoxy resin by organosilicon is as follows：
Epoxy resin 6101 is dissolved in ethyl acetate solution, is added and agitating device, reflux condenser and temperature is housed
In the there-necked flask of meter, condensed water is first passed through, and is gradually heating to 88 DEG C, then sequentially added MTES, go
Ionized water and octoate catalyst stannous, high-speed stirred, insulation reaction 3h, mixing speed is 700r/min.
Method of preparing methyl phenyl polysiloxane is as follows：
A. MTMS and diphenyldimethoxysilane are taken, the glass reaction kettle with reflux is added
In, add the acetone of 0.2 times of MTMS and dimethoxydiphenylsilane gross mass；
B. be 75 DEG C in temperature, rotating speed be under 550r/min to adding deionized water in glass reaction kettle, deionized water
It is the summation of the middle methoxyl group molal quantity of both MTMS and dimethoxydiphenylsilane to measure；
C. after completion of dropping, continue to stir, flow back 4h, add organic solvent, it is 72% to adjust its solid content, is subsequently adding
Zinc Isoocatanoate, the addition of zinc Isoocatanoate is 1.5% for the zinc metal/hard resin mass ratio in zinc Isoocatanoate, continues to stir
Afterwards, cooling obtains leuco base phenyl polysiloxane；
Wherein, the amount for adding MTMS and diphenyldimethoxysilane is MTMS and two
Benzene dimethoxysilane mol ratio 2：1-3：1.
The preparation method of organic-silicon-modified unsaturated polyester resin is as follows：
A. the injection of absolute ethyl alcohol, MTES, diphenyl silanediol and VTES is taken pre-
It is equipped with the there-necked flask of stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation to slowly being dripped in there-necked flask
Enter deionized water, 1h completion of dropping is warming up to 110 DEG C and continues to react 1h afterwards, and absolute ethyl alcohol, residual moisture is finally removed under reduced pressure
And low molecular weight substance, you can obtain the organosilicon performed polymer of pale yellow transparent；
Wherein add absolute ethyl alcohol, MTES, diphenyl silanediol and VTES
Mass ratio is 10：7：2：1.5；
B. 1,2-PD, BDO, adipic acid, THPA and maleic anhydride are put into there-necked flask
In, it is subsequently placed on digital display thermal-arrest magnetic stirring apparatus, install condensation reflux unit additional, 162 DEG C of back flow reaction 40min are heated to, so
After be warming up to 200 DEG C, be cooled to 90 DEG C when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer with it is different
Zinc octoate, is warming up to 120 DEG C of reaction 1h again, organosilicon performed polymer is carried out condensation reaction with unsaturated polyester (UP), and reaction terminates
The water and other small molecule by-products in removing system are vacuumized afterwards, are added in most backward system and are contained hydroquinones, peroxidating
The mixed diluent of benzoyl and styrene, organic-silicon-modified unsaturated polyester resin is can obtain after being sufficiently mixed；
Wherein, the mass ratio of 1,2-PD, BDO, adipic acid, THPA and maleic anhydride is 10：
5：8：6：3, the mass ratio of hydroquinones, benzoyl peroxide and styrene is 15：1：100.
The preparation technology of above-mentioned high-temperature resistant anti-corrosive insulating moulding coating, the high-temperature resistant anti-corrosive insulating moulding coating preparation technology specific steps
It is as follows：
（1）By modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin and mixed
Bonding solvent is added in dispersion cylinder, controls the temperature of dispersion cylinder at 48 DEG C, and high-speed stirred is uniform, and mixing speed is 500r/min, is stirred
The time is mixed for 35min；
（2）Again to step（1）Middle addition composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust,
High-speed stirred 30min, mixing speed is 800r/min, controls the temperature of dispersion cylinder at 82 DEG C；
（3）Again to step（2）In sequentially add defoamer for polysiloxane-based defoamer, levelling agent cellaburate, idol
Connection agent γ-Mercaptopropyltriethoxysilane, crosslinking agent tetra-n-butyl titanate and curing agent IPD, stirs at normal temperatures
Mix and uniformly obtain high-temperature resistant anti-corrosive insulating moulding coating.
In addition to the implementation, the present invention can also have other embodiment.All use equivalents or equivalent transformation shape
Into technical scheme, all fall within the protection domain of application claims.
Claims (6)
1. a kind of high-temperature resistant anti-corrosive insulating moulding coating, it is characterised in that：The high-temperature resistant anti-corrosive insulating moulding coating by weight include with
Lower component：
Wherein, described film-forming resin is modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturation
The mixture of polyester resin, wherein, film-forming resin is 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 dust, its
Middle color stuffing is by composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust in mass ratio 3：2：1：1：1 mixes
Conjunction is formed, and described expanded vermiculite size is 200-220 mesh；Described glass dust is lead glass powder, vanadium glass dust, boron glass powder
Or one or more in phosphoric acid glass powder；
Described auxiliary agent includes following components by weight：Defoamer：2-5 parts, levelling agent：2-4 parts, curing agent：4-8 parts,
Coupling agent：4-8, crosslinking agent：3-5；
Wherein, described defoamer is polysiloxane-based defoamer, and described levelling agent is cellaburate or polyacrylate
In one kind, described curing agent is ethylenediamine, diethylenetriamine, triethylene tetramine, diamino-diphenyl MSM, isophorone
One or more in diamines or polyamide 6 50, described coupling agent is γ aminopropyltriethoxy silane, γ-sulfydryl third
One or more in ethyl triethoxy silicane alkane or γ-glycidyl ether trimethoxy silane, described crosslinking agent is metatitanic acid
Four N-butyls；
Described solvent is the mixture that n-butanol, ethanol and isopropanol mix in any proportion.
2. high-temperature resistant anti-corrosive insulating moulding coating according to claim 1, it is characterised in that：Described silicon-modified epoxy tree
The preparation method of fat is as follows：
Epoxy resin 6101 is dissolved in ethyl acetate solution, is added equipped with agitating device, reflux condenser and thermometer
In there-necked flask, be first passed through condensed water, and be gradually heating to 85-90 DEG C, then sequentially add MTES, go from
Sub- water and catalyst, high-speed stirred, insulation reaction 3-5h, mixing speed is 600-800r/min.
3. high-temperature resistant anti-corrosive insulating moulding coating according to claim 2, it is characterised in that described catalyst is stannous octoate
Or the one kind in dibutyl tin dilaurate.
4. high-temperature resistant anti-corrosive insulating moulding coating according to claim 1, it is characterised in that：Described methyl phenyl silicone resin system
Preparation Method is as follows：
A. MTMS and diphenyldimethoxysilane are taken, in glass reaction kettle of the addition with reflux, plus
Enter the acetone of 0.2 times of MTMS and dimethoxydiphenylsilane gross mass；
B. it is 70-80 DEG C in temperature, rotating speed is to adding deionized water, deionized water in glass reaction kettle under 550-600r/min
Amount for the middle methoxyl group molal quantity of both MTMS and dimethoxydiphenylsilane summation；
C. after completion of dropping, continue to stir, flow back 4-5h, add organic solvent, adjust its solid content for 70%-75%, then
Zinc Isoocatanoate is added, the addition of zinc Isoocatanoate is 1.5% for the zinc metal/hard resin mass ratio in zinc Isoocatanoate, is continued
After stirring, cooling obtains leuco base phenyl polysiloxane；
Wherein, the described amount for adding MTMS and diphenyldimethoxysilane for MTMS with
Diphenyldimethoxysilane mol ratio 2：1-3：1.
5. high-temperature resistant anti-corrosive insulating moulding coating according to claim 1, it is characterised in that：Described organic-silicon-modified unsaturation
The preparation method of polyester resin is as follows：
A. the injection of absolute ethyl alcohol, MTES, diphenyl silanediol and VTES is taken to preset
In the there-necked flask of stirring and condenser apparatus.Bath temperature is set to 50 DEG C, under agitation to being slowly dropped into there-necked flask
Ionized water, 1-1.5h completion of dropping is warming up to 110 DEG C and continues to react 1h afterwards, and absolute ethyl alcohol, residual moisture is finally removed under reduced pressure
And low molecular weight substance, you can obtain the organosilicon performed polymer of pale yellow transparent；
Wherein described addition absolute ethyl alcohol, MTES, diphenyl silanediol and VTES
Mass ratio be 10：7：2：1.5；
B. by 1,2-PD, BDO, adipic acid, THPA and maleic anhydride put into there-necked flask in, so
After 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 heat to 200 DEG C, be cooled to 90 DEG C when system acid number reaches 15mgKOH/g, add a certain amount of organosilicon performed polymer with
Zinc Isoocatanoate, is warming up to 120 DEG C of reaction 1h again, organosilicon performed polymer is carried out condensation reaction, reaction knot with unsaturated polyester (UP)
The water and other small molecule by-products in removing system are vacuumized after beam, is added in most backward system and is contained hydroquinones, peroxide
Change the mixed diluent of benzoyl and styrene, organic-silicon-modified unsaturated polyester resin is can obtain after being sufficiently mixed；
The mass ratio of wherein described 1,2-PD, BDO, adipic acid, THPA and maleic anhydride is
10：5：8：6：3, the mass ratio of described hydroquinones, benzoyl peroxide and styrene is 15：1：100.
6. the preparation technology of high-temperature resistant anti-corrosive insulating moulding coating as claimed in claim 1, it is characterised in that the high-temperature resistant anti-corrosive every
Hot Paint preparation technology is comprised the following steps that：
(1) it is the mixing of modifying epoxy resin by organosilicon, methyl phenyl silicone resin and organic-silicon-modified unsaturated polyester resin is molten
Agent is added in dispersion cylinder, controls the temperature of dispersion cylinder at 45-50 DEG C, and high-speed stirred is uniform, and mixing speed is 500-600r/min,
Mixing time is 30-40min；
(2) again to composite iron-titanium powder, crystal whisker of hexa potassium titanate, sepiolite, expanded vermiculite and glass dust is added in step (1), at a high speed
Stirring 30min, mixing speed is 700-800r/min, controls the temperature of dispersion cylinder at 80-85 DEG C；
(3) stirred at normal temperatures to defoamer, levelling agent, coupling agent, crosslinking agent and curing agent is sequentially added in step (2) again
It is uniform to obtain high-temperature resistant anti-corrosive insulating moulding coating.
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| CN104673063A (en) | 2015-06-03 |
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