CN104557133A - Anti-corrosion and anti-icing polysiloxane material for concrete and preparation method of anti-corrosion and anti-icing polysiloxane material - Google Patents

Anti-corrosion and anti-icing polysiloxane material for concrete and preparation method of anti-corrosion and anti-icing polysiloxane material Download PDF

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CN104557133A
CN104557133A CN201410680572.9A CN201410680572A CN104557133A CN 104557133 A CN104557133 A CN 104557133A CN 201410680572 A CN201410680572 A CN 201410680572A CN 104557133 A CN104557133 A CN 104557133A
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icing
siloxanes
concrete
blocking
silsesquioxane
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CN104557133B (en
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王洪松
李磊
王伟
王瑞
蒋永菁
田倩
刘加平
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Sobute New Materials Co Ltd
Nanjing Bote Building Materials Co Ltd
Bote Building Materials Tianjin Co Ltd
Panzhihua Bote Building Materials Co Ltd
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Sobute New Materials Co Ltd
Nanjing Bote Building Materials Co Ltd
Bote Building Materials Tianjin Co Ltd
Panzhihua Bote Building Materials Co Ltd
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Abstract

The invention provides an anti-corrosion and anti-icing polysiloxane material for concrete. The anti-corrosion and anti-icing polysiloxane material comprises the following components in parts by weight: 20-70 parts of amino-modified polyether polysiloxane, 10-30 parts of crosslinked polyethylene or hexenyl siloxane, 10-20 parts of poly(methylphenylsilsesquioxane), 5-10 parts of poly(propylmethylsilsesquioxane) and 5-10 parts of alkoxy silane. The invention also provides a preparation method of the anti-corrosion and anti-icing polysiloxane material for concrete. The polysiloxane material can be used for effectively reducing the surface energy of the concrete and improving the surface hydrophobicity as well as anti-corrosion and anti-icing performances of the concrete, has excellent anti-corrosion and anti-icing capacities and can be applied to the protection of the concrete under the water work, maritime work and low-temperature climates.

Description

A kind of Concrete Anti corrodes anti-icing silicone materials and preparation method thereof
Technical field
The invention belongs to concrete protection technical field, particularly a kind of Concrete Anti corrodes anti-icing silicone materials and preparation method thereof, can be used for the anti-icing protection of concrete protection against corrosion, improves concrete service life.
Background technology
As everyone knows, concrete must be faced with the erosion of external environment under arms in process, and especially along with China's infrastructure construction is carried out, concrete Service Environment is more and more harsher.Such as, the deteriorated air (SO continued 2, CO 2), the high humidity of coastland and inorganic salt, west area saline and alkaline condition etc., all greatly accelerate concrete deteriorated process, had a strong impact on concrete service life.How to extend concrete structure service life under severe conditions, become the pressing issues that engineering faces.
Concrete deterioration always inside expansion from surface, chloride erosion, Acid rain damages, freeze-thaw cycle, freezing erosion are the major causes causing concrete structure durability to decline, and finally jeopardize the safety of engineering structure.Therefore, under corrosion and freeze-thaw damage environment, only by improving quality and the thickness of concrete protective layer material, cannot ensure that concrete structure safety in design life is on active service, one or more anti-deteriorated enhancements must be taked.
Concrete Anti corrosion technology has obtained concern and the research of a large amount of industry personnel, and some measures also achieve good effect.Reinforcing steel bar corrosion inhibitor, concrete galvanic protection, stainless steel rebar, reinforcing steel bar surface coating, anti-corrosion reinforcing bar etc.; practice shows; concrete surface coating protection method is the method for economical and efficient the most; but there is more deficiency with the conventional surface protective coating that epoxy coat, polyurethane coating are representative; the problems such as poor durability, anti-corrosion capability are limited, so more and more urgent to the requirement of more high performance concrete protective coating.
Concrete Anti icing technology has caused the extensive concern of global scientific research personnel, and the multiple country of some ice damages has set up particular study mechanism, carries out a large amount of scientific researches to icing principle.The ice control solution that anti-icing technology mainly contains Four types is anti-icing, mechanical deicing, and heat energy is anti-icing and coating is anti-icing.The anti-icing principle of solution utilizes anti-freeze fluid to mix with the water collected by stromal surface, because the freezing point of mixed solution reduces greatly, makes that water is unlikely to freeze from the teeth outwards.So-called mechanical deicing, is exactly mechanically that ice is broken, then blows down by air-flow, or utilizes centrifugal force, vibrates ice is removed.Heat energy is anti-icing is exactly utilize various energy heats object, makes article surface temperature more than 0 DEG C, with E to object that is anti-icing or deicing.And ice-covering-proof coating realizes anti-ice object mainly through material surface property and microfacies pattern, this kind of material require has anti-freeze property and ice-phobic concurrently, alleviates even elimination ice and snow gather from sticking power two aspect extending freezing time and reduction ice.From principle, coating is anti-icing is a kind of very desirable anti-icing method, because it belongs to active protection, energy consumption is little, environmental friendliness and applied widely.But existing coating antiicing coating still exists problems such as hydrophobic performance is not good, poor durability.
The low surface energy coatings composition that patent CN103492486A discloses a kind of moisture curable composition and prepares thus, have employed the polymkeric substance based on Silante terminated urethane; But said composition moisture-curable poor controllability, the compatible stability of urethane and polysiloxane is poor, and the phase separation in solidification process is wayward, causes hydrophobic performance unstable.
Patent CN102757708A discloses a kind of Anti-ice paint and preparation method thereof, and the polyacrylic acid grafted PDMS multipolymer containing POSS realizes Anti-ice-and-snow ability, and it has good consistency and sticking power; But its contact angle is less, only have about 105 °, hydrophobic performance is limited.
Patent CN101792631A discloses a kind of high hydrophobic static-electricity conducting anti-icing coating and preparation method thereof, fluorocarbon resin, conducting powder, silicoorganic compound are adopted to prepare a kind of low surface energy antiicing coating with static conductive character, mainly utilize the low surface energy of fluorinated acrylic resin to realize anti-icing effect, protect for wire surface; But, but its resistance to low temperature and low temperature flexibility poor, and the poor durability of fluorinated acrylic resin, can not meet the requirement of concrete digital preservation.
Summary of the invention
Goal of the invention: in order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of Concrete Anti to corrode anti-icing silicone materials and preparation method thereof.
Technical scheme: a kind of Concrete Anti provided by the invention corrodes anti-icing silicone materials, comprise the component of following weight part: amino modified polyether polysiloxane 20-70 part, cross-linking polyethylene or vinyl siloxanes 10-30 part, polyphenylmethyl base silsesquioxane 10-20 part, poly-hydroxypropyl methyl silsesquioxane 5-10 part, organoalkoxysilane 5-10 part.
As preferably, the weight-average molecular weight of described amino modified polyether polysiloxane is 40000-60000; Described amino modified polyether polysiloxane adopts following methods to obtain: silicon oil of low hydrogen content, α-thiazolinyl epoxy compounds and α-alkenyl polyether generation hydrosilylation addition reaction, obtained polyethers-epoxy silicon oil intermediate; Polyethers-epoxy silicon oil intermediate organic amine open loop, obtains amino modified polyether polysiloxane.The polyether-type organopolysiloxane utilizing polyamine or diamine ring-opening to improve performance to obtain has many side-chain amino group structure, and molecular structure flexibility is better, and second-order transition temperature is low, has better softness.
As preferred further, described silicon oil of low hydrogen content is the containing hydrogen silicone oil of reactive hydrogen content below 0.15%; Organic amine comprises quadrol, N, N-dimethylated propyl diethylenetriamine, piperazine and N-aminoethyl piperazine at interior polyamine or diamine.
Preferred as another kind, described crosslinked polyethylene radical siloxane or hexenyl siloxanes are that ethenyl blocking siloxanes or hexenyl endcapped siloxanes react obtained cross linking polysiloxane by platinum metals complex catalysis, described ethenyl blocking siloxanes or hexenyl endcapped siloxanes comprise the dimethyl siloxane of dimethyl ethenyl end-blocking, the dimethyl siloxane of dimetylhexene base end-blocking, the methyl vinyl silicone of dimethyl ethenyl end-blocking, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of vinyl-dimethyl base siloxy end-blocking, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of vinyl dimethylsilyl bis end-blocking, the polydimethylsiloxanepolymer polymer of vinyl-dimethyl oxygen base siloxy end-blocking, the polydimethylsiloxanepolymer polymer of hexenyl dimethylsilyl bis end-blocking, the polymerization degree of described ethenyl blocking siloxanes or hexenyl endcapped siloxanes is 10-100.Crosslinked polyethylene radical siloxane obtains cross-linking type polysiloxane by the crosslinked of end-vinyl, and molecular structure is finer and close, shows excellent physical strength and thermostability.
Preferred as another kind, described polyphenylmethyl base silsesquioxane is obtained by phenyl triethoxysilane, Union carbide A-162 hydrolytic condensation.
Preferred as another kind, described poly-hydroxypropyl methyl silsesquioxane is obtained by Union carbide A-162, propyl-triethoxysilicane hydrolytic condensation.
Described polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane have Si-O-Si main chain and Si-O dipole compensation, form microporous structure, relative conventional silicone structure has better thermotolerance, acid resistance and lower surface energy and hydrophobicity; Thus the Tc of water can be reduced, extend the crystallization time of water, and the sticking power of ice and concrete substrates can be reduced.
Preferred as another kind, described organoalkoxysilane comprises Union carbide A-162, butyl trimethoxy silane, butyl triethoxyl silane, octyl group Trimethoxy silane, octyltri-ethoxysilane, isooctyltrimethoxysi,ane, dodecyltrimethoxysilane, dodecyl triethoxysilane.Described oxyalkylsiloxane has small molecule structure, and easy diffusion in concrete, and to be had more than needed hydroxyl reaction with concrete, improves the perviousness of material at concrete surface, sticking power.
Present invention also offers the preparation method that above-mentioned Concrete Anti corrodes anti-icing silicone materials, comprise the following steps:
(1) preparation of amino modified polyether polysiloxane: silicon oil of low hydrogen content, α-thiazolinyl epoxy compounds and α-alkenyl polyether generation hydrosilylation addition reaction, obtained polyethers-epoxy silicon oil intermediate; Polyethers-epoxy silicon oil intermediate organic amine open loop, obtains amino modified polyether polysiloxane;
(2) preparation of crosslinked polyethylene radical siloxane or hexenyl siloxanes: ethenyl blocking siloxanes or hexenyl endcapped siloxanes react under the complex catalysis of platinum metals, to obtain final product;
(3) polyphenylmethyl base silsesquioxane: phenyl triethoxysilane, Union carbide A-162 hydrolysis-condensation reaction, product and amine react, and obtain polyphenylmethyl base silsesquioxane;
(4) preparation of poly-hydroxypropyl methyl silsesquioxane: Union carbide A-162, propyl-triethoxysilicane hydrolysis-condensation reaction, product and amine react, and obtain poly-hydroxypropyl methyl silsesquioxane;
(5) preparation of silicone materials: amino modified polyether polysiloxane, cross-linking polyethylene or vinyl siloxanes, polyphenylmethyl base silsesquioxane, poly-hydroxypropyl methyl silsesquioxane, organoalkoxysilane mixing, temperature reaction, to obtain final product.
Beneficial effect: silicone materials provided by the invention effectively can reduce concrete surface energy, improves concrete surface hydrophobicity, improve the performance that concrete puts corrosive ice, there is the excellent ice-covering-proof ability of protection against corrosion, can be applicable to concrete protection under water conservancy project, extra large work and microthermal climate.
Specifically, relative to traditional defense material, this material has uniqueness in the ice-covering-proof Application Areas of protection against corrosion and acts on significantly:
The main chain of this silicone materials be Si-O-Si not easily by UV-light and ozone decomposed, have better thermostability, radioresistance and weather-proof ability than other macromolecular materials; Functional amino modified and crosslinked group and microporous structure give the flexibility of material excellence, physical strength and more low surface energy.When polysiloxane chain containing larger space steric group and hydrophobic grouping, very high contact angle and very low contact angle hysteresis (roll angle) being shown to water, is conducive to concrete automatically cleaning, ice-covering-proof, protection against corrosion.
Concrete original surface has vesicular structure and hydrophilic high surface energy interface, and former hydrophilic interface can be made after adopting polysiloxane process to become hydrophobic interfaces, reduces surface energy, thus the erosion of salt ion in anti-sealing and water.This material realizes the ice-covering-proof object of protection against corrosion with specific physical chemical property and microfacies pattern, when with not containing component disclosed by the invention analogous material composition compared with time, material feed composition of the present invention can demonstrate the protection against corrosion anti-icing performance of increase.
Embodiment
In order to understand the present invention better, below in conjunction with embodiment, content of the present invention is further described, but content of the present invention is not limited to the scope of embodiment statement.
The containing hydrogen silicone oil that following examples use is the containing hydrogen silicone oil of reactive hydrogen content below 0.15%.
Embodiment 1
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 75g containing hydrogen silicone oil, 3g glycidyl allyl ether, 220g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into quadrol and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 8: 2) mixed solvent washing impurity-removing, obtain viscous liquid, to obtain final product.
2) preparation of crosslinking vinyl siloxanes: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, at 25 DEG C, add the polydimethylsiloxane-Polymethyl methacrylate multipolymer of 400g vinyl-dimethyl base siloxy end-blocking successively, 15g divinyl tetramethyl disiloxane, 5g vinyltrimethoxy silane add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.2g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 180ml, propyl-triethoxysilicane 20ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 140ml, propyl-triethoxysilicane 60ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 2
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 85g containing hydrogen silicone oil, 3.5g glycidyl allyl ether, 240g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into quadrol and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 9: 1) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of 230g vinyl-dimethyl base siloxy end-blocking is added successively at 25 DEG C, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of 270g vinyl dimethylsilyl bis end-blocking, 20g divinyl tetramethyl disiloxane, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.4g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 180ml, propyl-triethoxysilicane 25ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 140ml, propyl-triethoxysilicane 65ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 3
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 100g containing hydrogen silicone oil, 4g glycidyl allyl ether, 225g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into quadrol and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform, (weight ratio is 9: 1 mixed solvent washing impurity-removings, obtains viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, divinyl tetramethyl disiloxane is added successively at 25 DEG C, tetramethyl-tetravinyl cyclosiloxane, vinyltrimethoxy silane, vinyltriethoxysilane, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of vinyl-dimethyl base siloxy end-blocking, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of vinyl dimethylsilyl bis end-blocking, the polydimethylsiloxanepolymer polymer of vinyl-dimethyl oxygen base siloxy end-blocking or the polydimethylsiloxanepolymer polymer of hexenyl dimethylsilyl bis end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 0.3%, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 180ml, propyl-triethoxysilicane 20ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 140ml, propyl-triethoxysilicane 60ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 4
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 75g containing hydrogen silicone oil, 2g glycidyl allyl ether, 195g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into piperazine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 8: 2) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, 40g tetramethyl-tetravinyl cyclosiloxane is added successively at 25 DEG C, 30g vinyltrimethoxy silane, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of 310g vinyl-dimethyl base siloxy end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.8g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 170ml, propyl-triethoxysilicane 30ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 110ml, propyl-triethoxysilicane 90ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 5
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 70g containing hydrogen silicone oil, 3g glycidyl allyl ether, 200g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into N, N-dimethylated propyl diethylenetriamine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 9: 1) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of 260g vinyl dimethylsilyl bis end-blocking is added successively at 25 DEG C, the polydimethylsiloxanepolymer polymer of 100g vinyl-dimethyl oxygen base siloxy end-blocking, 13g vinyltriethoxysilane, 7g divinyl tetramethyl disiloxane, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.5g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 160ml, propyl-triethoxysilicane 10ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 160ml, propyl-triethoxysilicane 50ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 80.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 6
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 85g containing hydrogen silicone oil, 2.5g glycidyl allyl ether, 210g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into N, N-dimethylated propyl diethylenetriamine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 8: 2) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, 10g divinyl tetramethyl disiloxane is added successively at 25 DEG C, 10g vinyltriethoxysilane, the polydimethylsiloxanepolymer polymer of 100g vinyl-dimethyl oxygen base siloxy end-blocking, the polydimethylsiloxanepolymer polymer of 150g hexenyl dimethylsilyl bis end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.05g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 170ml, propyl-triethoxysilicane 15ml, 0.0.lmol/L hydrochloric acid 25mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 110ml, propyl-triethoxysilicane 160ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 15mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 7
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 65g containing hydrogen silicone oil, 5g glycidyl allyl ether, 175g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into piperazine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 9: 1) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, 16g divinyl tetramethyl disiloxane is added successively at 25 DEG C, 4g tetramethyl-tetravinyl cyclosiloxane, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of 165g vinyl-dimethyl base siloxy end-blocking, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of 225g vinyl dimethylsilyl bis end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 150ml, propyl-triethoxysilicane 20ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 150ml, propyl-triethoxysilicane 50ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 15mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 8
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 90g containing hydrogen silicone oil, 2g glycidyl allyl ether, 180g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into piperazine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 8: 2) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, 10g tetramethyl-tetravinyl cyclosiloxane is added successively at 25 DEG C, 20g vinyltrimethoxy silane, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of 350g vinyl-dimethyl base siloxy end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.8g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 180ml, propyl-triethoxysilicane 20ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 140ml, propyl-triethoxysilicane 60ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 9
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 80g containing hydrogen silicone oil, 3g glycidyl allyl ether, 125g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into N-aminoethyl piperazine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 9: 1) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, 10g divinyl tetramethyl disiloxane is added successively at 25 DEG C, 5g tetramethyl-tetravinyl cyclosiloxane, 10g vinyltriethoxysilane, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of 150g vinyl-dimethyl base siloxy end-blocking, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of 150g vinyl dimethylsilyl bis end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.5g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 180ml, propyl-triethoxysilicane 20ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 140ml, propyl-triethoxysilicane 60ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 4.0mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Embodiment 10
1) amino modified polyether polysiloxane preparation: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add 75g containing hydrogen silicone oil, 4g glycidyl allyl ether, 160g allyl polyethenoxy polyethenoxy ether successively, logical N2 stirs 10min, be warming up to 90 DEG C, be added dropwise to platinum catalyst reaction 4h, obtain polyethers-epoxy silicon oil intermediate; Then the ratio being 1.05: 1.00 with amine and polyethers-epoxy silicon oil intermediate epoxy group(ing) mol ratio drops into N-aminoethyl piperazine and continues to react 4h, and decompression, except after low-boiling-point substance, is down to room temperature; With hexanaphthene/chloroform (weight ratio is 9: 1) mixed solvent washing impurity-removing, obtain viscous liquid.
2) preparation of crosslinking vinyl siloxanes: have agitator at device, reflux condensing tube, in the 1000mL three-necked bottle of thermometer, 25g divinyl tetramethyl disiloxane is added successively at 25 DEG C, 5g tetramethyl-tetravinyl cyclosiloxane, 5g vinyltrimethoxy silane, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of 240g vinyl-dimethyl base siloxy end-blocking, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of 165g vinyl dimethylsilyl bis end-blocking, add platinum catalyst and be warming up to 80 DEG C, stirring reaction 1-2h, add reaction terminating stablizer 1-ethynyl-1-hexalin 1.7g, be down to room temperature and obtain viscous liquid.
3) preparation of polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 170ml, propyl-triethoxysilicane 30ml, 0.0.lmol/L hydrochloric acid 10mL, at 50 DEG C, react 30min, then be warmed up to 70 DEG C of reaction 2h; Then, at 80 DEG C, gained hydrolysate is reacted 3h with triethylamine in mibk, with hydrochloric acid neutralization, obtain phenyl methyl silsesquioxane copolymer.Have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, add Union carbide A-162 165ml, propyl-triethoxysilicane 55ml, 0.0.lmol/L hydrochloric acid 20mL, Virahol 100.0mL60 DEG C of lower magnetic force stirring reaction adds 28% ammoniacal liquor 8mL after l hour, heat up 80 DEG C and continue reaction 1 hour, with hydrochloric acid neutralization, obtain methyl-propyl silsesquioxane copolymer.
4) Concrete Anti corrodes the preparation of ice-covering-proof material: have in the 1000mL three-necked bottle of agitator, reflux condensing tube, thermometer at device, amino modified polyether polysiloxane, crosslinking vinyl siloxanes, polyphenylmethyl base silsesquioxane and poly-hydroxypropyl methyl silsesquioxane, oxyalkylsiloxane is added successively at 25 DEG C, be warming up to 60 DEG C of mechanical stirring and after 2 hours, cool rear discharging, obtain Concrete Anti and corrode ice-covering-proof material.
Concrete Anti obtained for embodiment 1 to 10 is corroded ice-covering-proof material and carry out contrast experiment at the standard concrete test test specimen of 100mm × 100mm × 100mm, the protection against corrosion anti-icing performance of evaluating material, result is as shown in table 1.Concrete sample is dry cleansing process after 28d maintenance, and all test specimens carry out under same experimental conditions.
Resistance to acids and bases, frost resistance, concrete carbonization degree, the chloride permeability degree of depth, material cohesion, freezing sticking power require to measure according to building industry industry product standard JG/T335-2011 " concrete structure protection film-forming type coating "; Contact angle test adopts the DSA25 optical contact angle instrument test of Kruss company,
The material antiseptic erosion anti-icing performance that table 1 embodiment 1 to 10 is obtained

Claims (8)

1. a Concrete Anti corrodes anti-icing silicone materials, it is characterized in that: the component comprising following weight part: amino modified polyether polysiloxane 20-70 part, cross-linking polyethylene or vinyl siloxanes 10-30 part, polyphenylmethyl base silsesquioxane 10-20 part, poly-hydroxypropyl methyl silsesquioxane 5-10 part, organoalkoxysilane 5-10 part.
2. a kind of Concrete Anti according to claim 1 corrodes anti-icing silicone materials, it is characterized in that: the weight-average molecular weight of described amino modified polyether polysiloxane is 40000-60000; Described amino modified polyether polysiloxane adopts following methods to obtain: silicon oil of low hydrogen content, α-thiazolinyl epoxy compounds and α-alkenyl polyether generation hydrosilylation addition reaction, obtained polyethers-epoxy silicon oil intermediate; Polyethers-epoxy silicon oil intermediate organic amine open loop, obtains amino modified polyether polysiloxane.
3. a kind of Concrete Anti according to claim 2 corrodes anti-icing silicone materials, it is characterized in that: described silicon oil of low hydrogen content is the containing hydrogen silicone oil of reactive hydrogen content below 0.15%; Organic amine comprises quadrol, N, N-dimethylated propyl diethylenetriamine, piperazine and N-aminoethyl piperazine at interior polyamine or diamine.
4. a kind of Concrete Anti according to claim 1 corrodes anti-icing silicone materials, it is characterized in that: described crosslinked polyethylene radical siloxane or hexenyl siloxanes are that ethenyl blocking siloxanes or hexenyl endcapped siloxanes react obtained cross linking polysiloxane under the complex catalysis of platinum metals, described ethenyl blocking siloxanes or hexenyl endcapped siloxanes comprise the dimethyl siloxane of dimethyl ethenyl end-blocking, the dimethyl siloxane of dimethyhexenes base end-blocking, the methyl vinyl silicone of dimethyl ethenyl end-blocking, polydimethylsiloxane-Polymethyl methacrylate the multipolymer of vinyl-dimethyl base siloxy end-blocking, polydimethylsiloxanes-poly-methylhexenylsiloxane the multipolymer of vinyl dimethylsilyl bis end-blocking, the polydimethylsiloxanepolymer polymer of vinyl-dimethyl oxygen base siloxy end-blocking, the polydimethylsiloxanepolymer polymer of hexenyl dimethylsilyl bis end-blocking, the polymerization degree of described ethenyl blocking siloxanes or hexenyl endcapped siloxanes is 10-100.
5. a kind of Concrete Anti according to claim 1 corrodes anti-icing silicone materials, it is characterized in that: described polyphenylmethyl base silsesquioxane is obtained by phenyl triethoxysilane, Union carbide A-162 hydrolytic condensation.
6. a kind of Concrete Anti according to claim 1 corrodes anti-icing silicone materials, it is characterized in that: described poly-hydroxypropyl methyl silsesquioxane is obtained by Union carbide A-162, propyl-triethoxysilicane hydrolytic condensation.
7. a kind of Concrete Anti according to claim 1 corrodes anti-icing silicone materials, it is characterized in that: described organoalkoxysilane comprises Union carbide A-162, butyl trimethoxy silane, butyl triethoxyl silane, octyl group Trimethoxy silane, octyltri-ethoxysilane, isooctyltrimethoxysi,ane, dodecyltrimethoxysilane, dodecyl triethoxysilane.
8. the Concrete Anti described in any one of claim 1-7 corrodes the preparation method of anti-icing silicone materials, it is characterized in that: comprise the following steps:
(1) preparation of amino modified polyether polysiloxane: silicon oil of low hydrogen content, α-thiazolinyl epoxy compounds and α-alkenyl polyether generation hydrosilylation addition reaction, obtained polyethers-epoxy silicon oil intermediate; Polyethers-epoxy silicon oil intermediate organic amine open loop, obtains amino modified polyether polysiloxane;
(2) preparation of crosslinked polyethylene radical siloxane or hexenyl siloxanes: ethenyl blocking siloxanes or hexenyl endcapped siloxanes react under the complex catalysis of platinum metals, to obtain final product;
(3) polyphenylmethyl base silsesquioxane: phenyl triethoxysilane, Union carbide A-162 hydrolysis-condensation reaction, product and amine react, and obtain polyphenylmethyl base silsesquioxane;
(4) preparation of poly-hydroxypropyl methyl silsesquioxane: Union carbide A-162, propyl-triethoxysilicane hydrolysis-condensation reaction, product and amine react, and obtain poly-hydroxypropyl methyl silsesquioxane;
(5) preparation of silicone materials: amino modified polyether polysiloxane, cross-linking polyethylene or vinyl siloxanes, polyphenylmethyl base silsesquioxane, poly-hydroxypropyl methyl silsesquioxane, organoalkoxysilane mixing, temperature reaction, to obtain final product.
CN201410680572.9A 2014-11-24 2014-11-24 A kind of antiseptic concrete loses anti-icing silicone materials and preparation method thereof Active CN104557133B (en)

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