CN101787244B - Antifouling flash insulator coating and preparation method thereof - Google Patents
Antifouling flash insulator coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of antifouling flash insulator coating which is prepared by mixing fluorine-containing polysiloxane component A, linear hydroxyl-terminated polysiloxane component B, organic and inorganic silicon dioxide taken as reinforcing material component C, functional powder material component D, cross-linking agent E, catalyst component F and tackifier component G. The method prepares the single-component moisture curing antifouling flash insulator coating which is removed alcohol and oxime by adding fluorine-containing silicon material into the hydroxyl-terminated linear silicone and the reinforcing material, and has good electrical performance and aging resistance, better antifouling flash capability and excellent hydrophobicity and hydrophobicity migration performance.
Description
Technical field
The present invention relates to coating technology, specifically condensation cured antifouling flash insulator coating of a kind of fluorine silicon rubber and preparation method thereof.
Background technology
The organosilicon antifouling flash insulator is the faster insulating material of a class novel electric power electric information, the particularly insulator of porcelain class or category of glass of present development, and its anti-fouling flashover performance, hydrophobic nature, migration of hydrophobicity all can reach existing service requirements.The metallic cable that exposes out of doors, because climate change, the erosion of dust storm precipitation and the destruction of birds, its the normal power transmission and transformation work that made surface corrosion or burn-in effects, particularly in diastrous weather, be more prone to produce all kinds of accidents and affect people's electricity consumption or produce structure deteriorate, need to adopt more high-grade composite insulating material solve and avoid above-mentioned unfavorable situation.
The sub-coating of many organic silicon insulations that occurs in the market all is the silicon rubber that adopts common single-component moisture-curable, through brushing on porcelain class or the category of glass insulator and on the cable electric transmission pole tower after the dilution.Because its electric property and anti-pollution, anti ageing property produce not easily efflorescence, pollution flashover etc. and cause power outage.
Chinese patent application CN1545104A discloses the application of self cure add-on type fluosilicic rubber on insulator, but can not obtain target product by its disclosed method, do not belong to the trifluoropropyl siloxane class coating of single-component moisture-curable yet, be unsuitable in the insulator surface coating.
Because the variation of weather and electricity consumption grade promote, power industry needs electric property and anti-pollution flashover ability insulator stronger, better ageing resistance to satisfy the use needs.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of antifouling flash insulator coating, the coating that obtains has good electric property, extremely low surface energy, hydrophobic nature and migration of hydrophobicity are better than pure silicon rubber-like coating, can obviously improve the serviceability of composite insulator.
The present invention also aims to provide a kind of a kind of antifouling flash insulator coating of described method preparation.
The preparation method of a kind of antifouling flash insulator coating of the present invention is that supporting material component C, functional powder material component D, linking agent E, catalyst component F, tackifier component G, mixed preparing form by fluorine-containing polysiloxane component A, linear hydroxyl-terminated polysiloxane B component, organic and inorganic silicon dioxide.
Component A is fluorine-containing silicone resin or silicone oil, and contains hydroxyl or alkoxy-functional, and fluorine content accounts for the 0.3%---10% quality among the component A.
The parts by weight consumption of each component is as follows:
Component A:5--15
B component: 20--50
Component C:10---50
Component D:0---30
Component E:2---8
Component F:0.1---1
Component G:1---5
Each composition weight umber summation is 100.
Component A is selected from fluorine silicon resene polysiloxane A1 or fluorine-containing linear polysiloxane component A2, and its structure is as follows:
Hydroxyl MDT fluorine silicon resene polysiloxane component A1
Wherein, R1 is that methyl or phenyl R2 is fluorocarbon based; M=0.3-0.4, D=0.3-0.35, T1=0.2-0.3, T2=0.1-0.2, X=0.05-0.1
Fluorine-containing linear polysiloxane component component A2
Wherein, R1 is methyl or hydroxyl, and R2 is methyl or fluoroalkyl; R3 is the alkoxyl group of methyl or ethylidene, and M is methyl;
Component B is selected from the linear hydroxyl-terminated polysiloxane of following structure:
R is methyl or phenyl, and M is methyl;
Component C is selected from organic White Carbon black of the MQ silicone resin that contains methyl or hydroxyl, or specific surface area is 150-380 square metre hydrophobic type gas phase White Carbon black;
Component D is AL
2O
3, AL (OH)
3, Fe
2O
3, ZnO, TiO
2, in the carbon black one or more, particle diameter is the 0.05-10 micron;
Component E is selected from alkoxyl group or the oximido one type of silane of trifunctional or four-functional group; Comprise methyltrimethoxy silane, Union carbide A-162, vinyltrimethoxy silane, tetramethoxy-silicane, four Diacetylmonoxime base silanes, methyl tributanoximo silane or vinyl tributyl ketoximyl silane;
Component F is selected from the organic tin catalyzer, tin laurate class or stannous octoate;
Component G is selected from silane coupling agent or its hydrolyzate.In aminopropyl trimethoxysilane, glycidoxy-propyltrimethoxy silane, methyl allyl acyloxypropyl trimethoxysilane, anilinomethyl trimethoxy silane, the aminoethyl aminopropyl triethoxysilane.Select one or more mixtures.
Component A1 is the silicone resin that obtains by after hydrocarbon compoud containing fluorine base silane and other silane hydrolysis reaction, cleaning, the filtration; A2 be by after fluorine-containing cyclosiloxane and the ring-opening polymerization of methyl cyclosiloxane with methyl or hydroxy-end capped, or made by line style fluorosilicone and the vinyl alkoxy silane addition reaction that side group closes hydrogen;
The B component is made by the ring-opening polymerization of methyl or phenyl cyclosiloxane.Viscosity is at the full methyl of 500---80000cps or contain the linear hydroxyl-terminated silicone oil of phenyl;
Component C is that the hydrophobic specific surface area of surface-treated with silane is 150-380M
2The gas phase White Carbon black; Or the MQ silicone resin of hydroxyl or methyl blocking, wherein M: Q is 0.6-1.5: 1;
Component D is the hydrophobic burning powder of surface-treated with silane;
Component E is the silane of three-functionality-degree or four functionality;
Component F is the catalyzer that contains organic tin compound;
Component G is by the product after the chlorine-containing silane esterification, uses behind use or the mixed hydrolysis separately.
With component A, B, C, D, E, F, the G proceed step by step is anhydrous fully mix, remove low molecule after, get final product to get product of the present invention evenly mixing below 60 ℃.
During use, can use after suitably adding ethers or the volatile solvent cut of alkanes with active according to the viscosity of construction requirement joint product, also can not add solvent and directly use.
The present invention compared with prior art has following advantage:
1, because the present invention adopts fluorine-containing polysiloxane A raw material, the product electric property that obtains is better than existing pure silicon rubber-type insulation compound
2, product of the present invention can reach higher hydrophobic angle, and mean value can reach more than 110 °, and its migration of hydrophobicity is better than pure silicon coating, and anti-pollution flashover is stronger.
3, the present invention can prepare the coating of high strength, low-viscosity solvent-free type, gets final product direct spraying without solvent cut during use, environmental protection and energy saving.
4, by adjusting the ratio of phenyl, phenyl content namely can make fluorine-containing V0 level coating more than 16%, and dielectric loss angle tangent can reach below 2 ‰.
5, can make coating ageing-resistant and the anti-pollution flashover type insulator that the UV resistant irradiation is stronger, significantly promote the antifouling property of coating, and anti-highly basic degree.Erosion to acid rain, grey haze, high dust, seawater and birds droppings has obvious resistivity.
Embodiment
Synthetic each component
Component A is synthetic
1.A1 fluorine silicon resin polysiloxane is synthetic
In flask, add aminomethyl phenyl dimethoxy silane 36.4 grams, ten trifluoro octyl group Trimethoxy silanes, 280.8 grams, methyl trimethoxy oxygen base silicon burns 81.6 grams, 3,5-dimethylphenyl chlorosilane 34.1 grams. and toluene 310g mixed, and splashed into water 72 grams through 1 hour, dropwised.Stir after 30 minutes, temperature rising reflux 1 hour adds toluene 300 grams, layering after water 250 grams stir.Remove the sour water layer, organic layer neutralizes with NaHCO3, then with filtering after the anhydrous slufuric acid drying.
Under normal pressure, distill out alcohol and solvent, get the toluene of 50% solid content and the mixture of fluorine silicon resin.Water white transparency, HO-(hydroxyl) content is about 1.73%.Be transparent semi-fluid behind the desolventizing, viscosity 4.5-5 ten thousand centipoises.
Synthesizing of A2 flucride siloxane line style body
In flask, rear adding nitrogen (N2) dries, add hexamethyl cyclotrisiloxane 222 grams, methyl nine fluorine hexyl cyclotrisiloxane 241 grams,. hexamethyldisiloxane 20.5 grams, stirred rear adding trifluoromethayl sulfonic acid 0.6 gram g 30 minutes, stir after 30 minutes, slowly be warmed up to 75 ℃ of reactions 7 hours.Be cooled to again about 40 ℃, pass into the NH3 neutralization.Stirred cold filtration 1 hour.To cross the filtered product decompression and heat up, and under 170 ℃/2mmHg, deviate to hang down and boil and unreacted reactant, get the fluorine-containing alkyl polydimethylsiloxane of line style, yield about 78%.Appearance colorless is transparent, about viscosity 350cps.
Synthesizing of B component
Two ends are the silica-based alkane line style of the polyphenylmethyl base body of HO-(hydroxyl) end-blocking
In flask, add methyl D4 and methyl phenyl ring siloxane D3-D5, (phenyl calculates according to content requirement) mixture, the rear adding KOH aqueous solution (being calculated as 5% with KOH) dries, stirring is warmed up to 130 °～140 ℃, about ring-opening reaction 1 hour, and then 160 ℃ of beginnings, slowly splashing into pure water, amount of water is 1～1.5% of cyclosiloxane total amount.Minimum temperature is about 130 ℃, and the time of splashing into is 4 hours.Then add the acetic acid neutralization, filter, make with extra care to get the terminal hydroxy group polyphenylmethyl baseline type siloxanes of water white viscosity between 3250～5000CPS.About yield 84%.
Component G's is synthetic
R aminopropyl triethoxysilane and anilinomethyl triethoxysilane equimolar amount are added (1: 1), then add pure water 1mol.After 3.5 hours, decompression namely gets light yellow transparent liquid after taking off low molecule at 80 ℃ of left and right sides stirring reactions
Join glue example one:
Be that the polydimethylsiloxane B of terminal hydroxy group of 20g 500cps and 20g 1200cps and hydroxyl MQ silicone resin C (the MQ ratio is 0.8: 1) 25g and specific surface area are 380M with viscosity
2Gas phase White Carbon black C:15g in kneader, dehydration is mixed into the basestocks that viscosity is 5000 centipoises, and this basestocks 80g adds the mixture 15g of A1:30g and A2:15g premixing glue, methyl tributanoximo silane E:12g, dibutyl tin laurate F:0.8g, tackifier G:1.2g.Above component mixes between 40-60 ℃ in temperature under wet condition and namely gets product, viscosity 2700cps, and directly brushing is on the surface of clean porcelain insulator.
Test after solidifying, bonding is cohesive failure, dielectric loss angle tangent tg δ 0.9%, dielectric strength E:22kV/mm, volume specific resistance 1.2*10
14Ω m, electric index is a little more than the pure silicon ketone antifouling flash insulator coating of fluorine-containing composition not; Average contact angle is greater than 115 °, shearing resistance 2.3Mpa, tearing toughness 6.2kN/m, elongation at break 150%.Composite insulator is because of fifty percent of the surface contamination compound inslation subclass that caused creeping discharge phenomenon is the pure silicon ketone when filthy.Use that migration of hydrophobicity shows after 15 days, obviously be better than not fluorine-containing silicone composite insulator.
Join glue example two:
With terminal hydroxy group polydimethyl phenylbenzene polysiloxane B, contain phenyl 22% viscosity 3250cps40g and hydrophobic type 380M
2White Carbon black C:16g dewaters in kneader and is mixed to 9000cps, and then the basis of formation material adds 20 gram A1,10 gram A2 and nano level Tio
2D:10g premix dehydrating mixt.10 gram methyl three ethoxy silane E and 2 restrain aminoethyl aminopropyl triethoxysilane G vacuum to be mixed after 3-5 minute, added 0.8 gram dibutyl tin laurate F and mixed 30 minutes between 40-55 ℃ under vacuum, and behind stable viscosity, the taking-up product also packages.Can dilute this product with trichloromethane again, get viscosity to easy spraying shape, spary on clean porcelain insulator, test performance again after it solidifies.
Surface drying 12 minutes, test after solidifying can reach the fire-retardant rank of V0, and bonding is cohesive failure, dielectric loss angle tangent tg δ 0.4%, dielectric strength E:24kV/mm, volume specific resistance 1.1*10
15Ω m, electric index is higher than the not pure silicon ketone antifouling flash insulator coating of fluorine-containing composition; Average contact angle (118 °), shearing resistance 3.8Mpa, tearing toughness 8.1kN/m, elongation at break 180%.Composite insulator is because of sixty percent of the surface contamination compound inslation subclass that caused creeping discharge phenomenon is the pure silicon ketone when filthy.Use after 15 days the migration of hydrophobicity sex expression obvious, be better than not fluorine-containing silicone composite insulator.
Join glue example three:
Terminal hydroxy group must be gathered dimethyl silyl siloxanes B:2000cps get 40g, with 300M
2Hydrophobic silica white C:6g, in kneader, make the base-material of 2210cps left and right sides viscosity; Then adding C hydroxyl MQ resin (M/Q is 0.7: 1) 30g mixes jointly; The A1 resin that adds again 10g, the A2 of 26g, E methyl trimethoxy oxosilane 18g, acetic acid 2g heat up below 100 ℃ 60 ℃ of-70 ℃ of stirring reactions 3 hours, and low-boiling-point substance is taken off in decompression, gets final product without extractum to 110 ℃/20mmHg.Under N2 (nitrogen) must protect, cool to 35-45 ℃, add again G epoxypropoxy triethoxyl silane 3g; Behind the F dibutyl tin dilaurate 0.7g, namely get product under wet condition, mixing.
Product water white transparency of the present invention, viscosity 850cps.Can be painted on various naked cables surface.Test after solidifying, bonding is cohesive failure, dielectric loss angle tangent tg δ 0.5%, dielectric strength E:25kV/mm, volume specific resistance 3.4*10
14Ω m, electric index is apparently higher than the pure silicon ketone antifouling flash insulator coating of fluorine-containing composition not; 121 ° of average contact angles, shearing resistance 1.8Mpa, tearing toughness 5.8kN/m, elongation at break 190%.Composite insulator is because of fifty percent of the surface contamination compound inslation subclass that caused creeping discharge phenomenon is the pure silicon ketone when filthy.Use that migration of hydrophobicity shows after 14 days, obviously be better than not fluorine-containing silicone composite insulator.
Claims (6)
1. the preparation method of an antifouling flash insulator coating is characterized in that by fluorine-containing polysiloxane component A, linear hydroxyl-terminated polysiloxane B component, organic or inorganic silicon-dioxide being that supporting material component C, functional powder material component D, linking agent E, catalyst component F, tackifier component G mixed preparing form; The parts by weight consumption of each component is as follows:
Component A:5--15
B component: 20--50
Component C:10---50
Component D:0---30
Component E:2---8
Component F:0.1---1
Component G:1---5
Each composition weight umber summation is 100;
Described component A is fluorine-containing silicone resin or silicone oil, and contains hydroxyl or alkoxy-functional, and fluorine content accounts for the 0.3%---10% quality among the component A; Component A is selected from fluorine silicon resene polysiloxane A1 or fluorine-containing linear polysiloxane component A2, and its structure is as follows:
Hydroxyl MDT fluorine silicon resene polysiloxane component A1,
Wherein, R1 is that methyl or phenyl R2 is fluorocarbon based;
M＝0.3-0.4，D＝0.3-0.35，T1＝0.2-0.3，T2＝0.1-0.2，X＝0.05-0.15
Fluorine-containing linear polysiloxane component A2
Wherein, R1 is methyl or hydroxyl, and R2 is methyl or fluoroalkyl; R3 is the alkoxyl group of methyl or ethylidene, and M is methyl; Component B is selected from the linear hydroxyl-terminated polysiloxane of following structure:
R is that methyl or phenyl M is methyl;
Component C is selected from the MQ silicone resin that contains methyl or hydroxyl, or specific surface area is 150-380 square metre hydrophobic type gas phase White Carbon black; Component D selects AL
2O
3, AL (OH)
3, Fe
2O
3, ZnO, TiO
2, in the carbon black one or more, its particle diameter is at the 0.05-10 micron; Component E is selected from alkoxyl group or the oximido one type of silane of trifunctional or four-functional group; Component F is selected from the organic tin catalyzer; Component G is selected from silane coupling agent or its hydrolyzate.
2. method according to claim 1 is characterized in that:
Component E is selected from methyltrimethoxy silane, Union carbide A-162, vinyltrimethoxy silane, tetramethoxy-silicane, four Diacetylmonoxime base silanes, methyl tributanoximo silane or vinyl tributyl ketoximyl silane; Component F is selected from tin laurate class or stannous octoate; Component G is selected from aminopropyl trimethoxysilane, glycidoxy-propyltrimethoxy silane, methyl allyl acyloxypropyl trimethoxysilane, anilinomethyl trimethoxy silane, the aminoethyl aminopropyl triethoxysilane; Select one or more mixtures.
3. method according to claim 2 is characterized in that:
Component A1 is the silicone resin that obtains by after hydrocarbon compoud containing fluorine base silane and other silane hydrolysis reaction, cleaning, the filtration; A2 be by after fluorine-containing cyclosiloxane and the ring-opening polymerization of methyl cyclosiloxane with methyl or hydroxy-end capped, or made by line style fluorosilicone and the vinyl alkoxy silane addition reaction that side group closes hydrogen; The B component is to be made by the ring-opening polymerization of methyl or phenyl cyclosiloxane; That viscosity is at the full methyl of 500---80000cps or contain the linear hydroxyl-terminated silicone oil of phenyl;
Component C is that the hydrophobic specific surface area of surface-treated with silane is 150-380M
2The gas phase White Carbon black; Or the MQ silicone resin of hydroxyl or methyl blocking, wherein M: Q is 0.6-1.5: 1;
Component G is by the product after the chlorine-containing silane esterification, uses behind use or the mixed hydrolysis separately.
4. method according to claim 3, it is characterized in that component A, B, C, D, E, F, the G proceed step by step is anhydrous fully mix, remove low molecule after, get final product to get product of the present invention evenly mixing below 60 ℃.
5. the antifouling flash insulator coating for preparing of the described method of one of claim 1-4.
6. the using method of antifouling flash insulator coating claimed in claim 5 is characterized in that adding the rear use of volatile ethers or alkane solvents dilution, perhaps directly uses.
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