CN102432336B - Preparation for organic/inorganic composite corrosion-resisting protective film coating layer for concrete and application thereof - Google Patents
Preparation for organic/inorganic composite corrosion-resisting protective film coating layer for concrete and application thereof Download PDFInfo
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- CN102432336B CN102432336B CN 201110287760 CN201110287760A CN102432336B CN 102432336 B CN102432336 B CN 102432336B CN 201110287760 CN201110287760 CN 201110287760 CN 201110287760 A CN201110287760 A CN 201110287760A CN 102432336 B CN102432336 B CN 102432336B
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- 239000004567 concrete Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000009501 film coating Methods 0.000 title claims abstract description 21
- 239000007888 film coating Substances 0.000 title claims abstract description 19
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- 239000010410 layer Substances 0.000 title abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 8
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 abstract description 6
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- 238000012360 testing method Methods 0.000 description 11
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
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- 238000011010 flushing procedure Methods 0.000 description 5
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- 230000004888 barrier function Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method for an organic/inorganic composite corrosion-resisting protective film coating layer. The method is as follows: blending ethyl orthosilicate, deionized water and ethanol based on a mole ratio of 1: (3-4): (3-5) at room temperature, and adding an organic modifier HTPDMS (hydroxybutyl-terminated polydimethylsiloxane) under the action of catalyst dibutyltin dilaurate. The invention also discloses a neutral organic/inorganic composite corrosion-resisting thin film coating layer and a method for corrosion-resisting coating processing on concrete with the coating layer. The invention prepares the organic/inorganic composite corrosion-resisting thin film coating layer material by the sol-gel technology, wherein the prepared material has advantages of simple preparation method, economy, practicability, low production cost and so on. The production and construction are safe. The prepared material can be widely used for protecting the concrete.
Description
Technical field
The present invention relates to the impregnating material field, relate in particular to a kind of preparation method who utilizes the neutral organic/inorganic composite concrete etching resistant film coating of sol-gel technique preparation, and utilize this coating that skeleton construction is carried out preserving method.
Background technology
Along with the day by day variation of concrete environment for use, the increasingly sharpening of environmental pollution, concrete structure is also become increasingly conspicuous by the erosion of environment.
Well-known corrosive medium all be unable to do without this medium of water to the corrosive nature of concrete material or reinforcing bar, such as carboniogenesis, salt corrosion, chloride ion corrosion.The destruction that cause because of entering of water concrete inside is divided into four-stage substantially.Fs: moisture penetration; Subordinate phase: because the infiltration of water, the reactive silicon dioxide that contains in the concrete reacts with alkali, generates water glass, volumetric expansion; Calcium hydroxide and water, carbon dioxide reaction generate calcium carbonate, make concrete pH value reduce steel bar corrosion; Phase III: follow the carrying out of basic material reaction, the concrete expansion volume increases, and produces the crack; Quadravalence section: can cause behind the cracking that corrosive deposit more easily invades, promote corrosion and the volume of reinforcing bar further to expand strength decreased.
Famous American concrete Mei Ta professor (P.K.Mehta) once had following discussion: " in the long run/term, concrete penetrability or water permeability are unique features directly related with weather resistance." (" the osmosis type coating surface is processed and concrete durability "/Zhao Tiejun writes).A host of facts prove, have prevented entering of water, and the disease of concrete structure comprises that steel bar corrosion, alkali-aggregate reaction and freeze-thaw cycle destruction not can occur.Therefore, except the design and construction requirement of the anti-drain structure of structure and material density, the various additional anticorrosive measure with water-proof function often becomes requisite barrier in the total corrosion protection system.
Concrete is kept apart with corrosive medium on every side, be coated with and carry out coating the method that is a kind of economy, easily goes on the surface of concrete structure, its main purpose is to improve hydrophobic nature and the enhancing concrete corrosion resistant ability of concrete surface.
At present, traditional corrosion protection coating has Resins, epoxy, the coating such as vinyl coating, bituminous composition, chlorinated rubber.
Although above several coating waterproof, preservative effect can reach and prevent steel reinforced concrete erosion, all exist defective, as poor adhesive force, easily aging, the life-span is short, alkali resistance is poor.These sealing membranes have sealed concrete capillary channel simultaneously, and the meeting of shedding of inside concrete steam is so that this closing membrane breaks, and greatly shorten work-ing life.
Though the research in the compound film of organic-inorganic field launches, but the quantity of research, go deep into degree and net result all with to compare gap abroad larger, especially in the application of antiseptic concrete, major part has still adopted introducing polymer substance (additive, complex compound etc.) or directly added nano particle carries out modification, preparation process is also complicated, wayward.
Summary of the invention
The purpose of this invention is to provide a kind of osmosis type strong adhesion, good toughness, water white transparency concrete organic/inorganic composite anticorrosive film coating.
A kind of preparation method of organic/inorganic composite anticorrosive film coating may further comprise the steps:
At room temperature, with tetraethoxy (TEOS) and deionized water, ethanol according to 1: (3～4): the mol ratio of (3～5) prepares, stir, the catalyzer dibutyl tin laurate that adds 0.5-2%wt, stir, mixing speed preferably is controlled at 300r/min, churning time 1.5-2.5h, then the organic modifiers hydroxyl-terminated injecting two methyl siloxane (PDMS-OH) that adds with respect to TEOS quality 10-20% stirs 2-4h to transparent and stable colloidal sol, namely makes organic/inorganic composite anticorrosive film coating of the present invention.Described transparent and stable dissolved adhesiveness is 4-6mPas.
The content of hydroxyl is at 8%wt in the described hydroxyl-terminated injecting two methyl siloxane (PDMS-OH).
Tetraethoxy (TEOS) is selected with the proportioning of deionized water, ethanol, water and amount of alcohol increase can affect later stage gel cracking, mainly be because the cracking that the volatilization of solvent causes, amount affects again the preparation of complex sol very little, therefore the mol ratio of tetraethoxy (TEOS) and deionized water, ethanol is defined as 1 among the preparation method of the present invention: (3～4): (3～5).
The present invention is directed to SiO
2The problem that exists in the base compound thin film study of organic-inorganic and the application at room temperature in conjunction with the collosol and gel technology of preparing, is carried out neutral SiO
2The development work of the compound etching resistant film of base organic-inorganic.Tetraethoxy, as a kind of organosilicon small molecules, its perviousness, ageing resistance are all relatively good, and its hydrolysate have hydroxyl can with the concrete surface hydroxyl reaction, play effect bonding, that reinforce.The molecule of two, three or four tetraethoxys can be grouped to dimer, tripolymer or the tetramer simultaneously.That is to say, include the inorganic structure of silica skeleton in the polymer, can produce enhancing, consolidation effect.Yet research finds that simple tetraethoxysilance material fragility is larger, after the reinforcing easily cracked, peel off, do not reach desirable reinforced effects, therefore the present invention improves its fragility by the adding organic modifiers.
The present invention selects organosilicon material-end to contain the polydimethylsiloxane (PDMS-OH) of hydroxyl as organic modifiers.Compare other organic materialss, organosilicon material is that skeleton is that Si-O key, side chain are-CH
3Group, end contain the macromolecular material of half organic half inorganic structure of hydroxyl, it is with the characteristic of organic polymer, can stand for a long time concrete high alkalinity environment (pH=12.5-13.5), terminal hydroxy group and colloidal sol fast setting under its high-alkali effect have good chemerosiveness resistent in addition simultaneously.Thereby PDMS-OH has many unique distinctions in performance.Polydimethylsiloxane (PDMS) is spirane structure, and siloxane bond outside the methyl face, is shielding siloxane bond towards screw shaft, and in this structure, the bond angle of siloxane bond rotates in easily occuring near 150 ℃.In addition, methyl also can rotate freely around siloxane bond, PDMS/SiO
2Molecule easily produces the conformation conversion, eliminates the stress that produces in the gel conversion process, suppresses embrittlement.The inorganic silicon network that forms by tetraethoxy (TEOS) hydrolysis (Si-OH) with organic PDMS-OH properties-correcting agent dehydrating condensation, form a kind of surface with the Si-O-Si network structure of hydrophobic grouping:
Further improve the corrosion resistance nature of film on cast concrete base, toughness, mechanical property etc.Simultaneously, the matrix material molecular weight of preparation is little, and viscosity is little, can be penetrated into inside concrete, forms the osmosis type film, has avoided the defective of film-forming type film, be not easy to discharge such as the gas of inside concrete, and easy cracking, work-ing life is short etc.
Because concrete is high alkalinity, so require its coating to possess alkali-proof feature, consider that acidic sol reduces concrete surface pH value, weather resistance reduces, the alkalescence collosol and gel time is too short, be unfavorable for construction, the present invention adopts the organic/inorganic complex sol of preparation neutrality under the effect of catalyzer (dibutyl tin laurate) to apply.Under neutrallty condition, under the effect of dibutyltin dilaurate catalyst, accelerated the hydroxyl of TEOS hydrolysis formation and the hydroxyl dehydrating condensation speed among the PDMS-OH, impel the formation of Si-O-Si structure in the complex sol.The catalyzer of other preparation organic-inorganic composite sol is acid or alkali, for example HCl, ammoniacal liquor.
A kind of organic/inorganic composite anticorrosive film coating that utilizes above-mentioned preparation method to make carries out anticorrosion coating to concrete method: before the concrete processing of concrete its structure is checked, whether whether clear and definite concrete surface play ash, peel off, have leakless, leak etc., in case of necessity with wire brush concrete surface, the water blast gun flushing concrete surface of polishing, the insecure mortar of concrete surface, the illusive dirt settling of dust and unfavorable pollutent of filming are thoroughly removed totally seasoning after the flushing; Apply organic/inorganic compounding etching resistant film coating at concrete surface, coated weight is at 300-600g/m
2, depth of penetration 3-8mm, after applying under 20 ± 3 ℃, relative air humidity 40%-60% one week of maintenance.
In preparation method's of the present invention reaction process, owing to introducing the effect of chemical bond between inorganic phase and organic phase, prepared hybrid material nothing on macroscopic view is separated, thereby shows the character of transparent and homogeneous.
The present invention has following characteristics:
1. the neutral organic-inorganic composite sol of sol-gel technique preparation has excellent perviousness, has small molecule structure, the cement of percdation concrete capillary hole wall and aquation reacts and forms the polysiloxane inierpeneirating network structure, by chemical bonding firmly, give the long-term hydrophobic nature of microtexture of concrete surface, and the maintenance ventilating function, greatly reduce the intrusion of water and harmful chlorion etc.
2.Si-O-Si structure strengthens the hardness of film, concrete is played the effect of reinforcing
3. alkali resistance is strong, and it is high alkalinity environment (pH=12.5-13.5) that the present invention can tolerate concrete for a long time.
4. the resistance to chemical attack ability is strong.Have very high chemical stability and erosion resistance because this Si-O-Si is the coating of skeleton, and can effectively stop the corrosive medium such as water, oxygen, villaumite and reinforcing bar to connect
5. water white transparency shape colloidal sol tint retention is good, does not change the concrete primary colors.
6. final product is nontoxic, and the good feature of environmental protection and weather resistance are arranged.
With respect to present existing other organic/inorganic composite materials; the present invention utilizes the compound etching resistant film coated material of organic-inorganic of sol-gel technique preparation to have that the preparation method is simple, economical and practical, low cost and other advantages, and production and construction can be widely used in concrete protective safely.
Embodiment
Embodiment 1
1. neutral complex sol preparation: under the room temperature, TEOS and deionized water, ethanol are prepared by 1: 3: 3 mol ratio, and even with magnetic stirrer, the dibutyl tin laurate that adds 1%wt, magnetic agitation 1.5h, then the PDMS-OH magnetic that adds 15%wt stirs 2h and causes transparent and stable colloidal sol, and viscosity is 4-6mpas.
2. coating adopts the mode of brushing, the C35 concrete that adopts places concrete first standard chamber maintenance 28 days, removes nuisance and the pollutents such as the dust that is unfavorable on the test specimen surface filming, greasy dirt before brushing, seasoning after the flushing, making concrete surface is the dried shape of face.Concrete each face is brushed three times, and coated weight is at 300g/m
2, be at least 6h each pitch time.Then concrete sample is delivered to curing room and carried out normal curing 7 days, curing temperature is (20 ± 3) ℃, relative air humidity 40%-60%.
Embodiment 2
1. neutral complex sol preparation: under the room temperature, TEOS and deionized water, ethanol are prepared by 1: 3: 3 mol ratio, and even with magnetic stirrer, the dibutyl tin laurate that adds 1%wt, magnetic agitation 1.5h, then the PDMS-OH magnetic that adds 15%wt stirs 2h and causes transparent and stable colloidal sol, and viscosity is 4-6mpas.
2. coating adopts the mode of brushing, the C35 concrete that adopts places concrete first standard chamber maintenance 28 days, removes nuisance and the pollutents such as the dust that is unfavorable on the test specimen surface filming, greasy dirt before brushing, seasoning after the flushing, making concrete surface is the dried shape of face.Concrete each face is brushed three times, and coated weight is at 450g/m
2, be at least 6h each pitch time.Then concrete sample is delivered to curing room and carried out normal curing 7 days, curing temperature is (20 ± 3) ℃, relative air humidity 40%-60%.
Embodiment 3
1. neutral complex sol preparation: under the room temperature, TEOS and deionized water, ethanol are prepared by 1: 3: 3 mol ratio, and even with magnetic stirrer, the dibutyl tin laurate that adds 1%wt, magnetic agitation 1.5h, then the PDMS-OH magnetic that adds 15%wt stirs 2h and causes transparent and stable colloidal sol, and viscosity is 4-6mpas.
2. coating adopts the mode of brushing, the C35 concrete that adopts places concrete first standard chamber maintenance 28 days, removes nuisance and the pollutents such as the dust that is unfavorable on the test specimen surface filming, greasy dirt before brushing, seasoning after the flushing, making concrete surface is the dried shape of face.Concrete each face is brushed three times, and coated weight is at 600g/m
2, be at least 6h each pitch time.Then concrete sample is delivered to curing room and carried out normal curing 7 days, curing temperature is (20 ± 3) ℃, relative air humidity 40%-60%.
Salt-fog test
Be the impact of the neutral complex sol coating of research the present invention on concrete corrosion resistance nature; we adopt, and chlorion is to concrete effect under the salt-spray cabinet simulated marine atmosphere environment, and the neutral compound coating under the announcement controllable environment is to the provide protection of agent on crack resistance of concrete chloride permeability.The parameters such as temperature, humidity, drying temperature and cyclic wetting and drying test can be controlled in comprehensive salt spray corrosion test chamber, we adopt concentration is that 5% neutral NaCl watery solution is as salt fog source solution, temperature 35 degree, humidity 70%, salt-fog test (15d was carried out in the standard configuration concrete pouring in 28 days, 30d), after corrosion finishes.Take out test block, the working pressure trier is in axial direction rived test block, is coated with AgNO3 solution at the concrete splitting surface spraying, and chloride permeability part (AgCl) precipitation that obviously bleaches is measured the chloride permeability degree of depth in the concrete.Contrast finds that the concrete chloride ion depth of penetration that scribbles neutral composite anticorrosive film coating reduces 5-10mm, and therefore neutral composite anticorrosive film coating of the present invention has improved concrete resistance to corrosion significantly as can be known.
The moisture content test
Carry out the water-intake rate test by JTJ 275-2000 " ocean engineering concrete structural anticorrosion technical specifications " standard, processed concrete through the present invention and have good water-repellancy, water-intake rate drops to 4-5% by contrast concrete 8.5% respectively.The hydrophobic performance of neutral composite anticorrosive film coating improves along with the increase of PDMS content.
Claims (5)
1. the preparation method of an organic/inorganic composite concrete etching resistant film coating is characterized in that may further comprise the steps:
At room temperature, tetraethoxy and deionized water, ethanol are prepared by the mol ratio of 1:3 ~ 4:3 ~ 5, stir, the catalyzer dibutyl tin laurate that adds 0.5-2wt%, stir 1.5-2.5h, then the hydroxyl-terminated injecting two methyl siloxane that adds with respect to tetraethoxy quality 10-20% stirs 2-4h to transparent and stable colloidal sol, and described dissolved adhesiveness is 2-10mPas, namely makes organic/inorganic composite concrete etching resistant film coating; The content of hydroxyl is 5 ~ 8wt% in the described hydroxyl-terminated injecting two methyl siloxane.
2. the preparation method of organic/inorganic composite concrete etching resistant film coating as claimed in claim 1, it is characterized in that: described dissolved adhesiveness is 4-6mPas.
3. the preparation method of organic/inorganic composite concrete etching resistant film coating as claimed in claim 1, it is characterized in that: the stirring velocity behind the described adding catalyzer is 300r/min.
A utilization arbitrary such as claim 1 ~ 3 as described in the organic/inorganic composite concrete etching resistant film coating that makes of preparation method.
5. method of utilizing organic/inorganic composite concrete etching resistant film coating as claimed in claim 4 concrete to be carried out anticorrosion coating: pending concrete surface is removed clean, seasoning, apply organic/inorganic composite concrete etching resistant film coating at concrete surface, coated weight is at 300-600g/m
2, depth of penetration 3-8mm applies afterwards one week of maintenance under 20 ± 3 ℃ of room temperatures, relative air humidity 40%-60%.
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| CN 201110287760 CN102432336B (en) | 2011-09-26 | 2011-09-26 | Preparation for organic/inorganic composite corrosion-resisting protective film coating layer for concrete and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110287760 CN102432336B (en) | 2011-09-26 | 2011-09-26 | Preparation for organic/inorganic composite corrosion-resisting protective film coating layer for concrete and application thereof |
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| CN102432336A CN102432336A (en) | 2012-05-02 |
| CN102432336B true CN102432336B (en) | 2013-02-20 |
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| CN105712740A (en) * | 2016-02-01 | 2016-06-29 | 济南大学 | Nano core-shell structure organic-inorganic compound concrete protective agent and preparation method and application thereof |
| CN110191931A (en) * | 2017-01-30 | 2019-08-30 | 陶氏东丽株式会社 | Smears for concrete structure |
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| CN108587495B (en) * | 2018-03-02 | 2020-10-27 | 南宁珀源能源材料有限公司 | Method for improving performance of anaerobic adhesive by treating bonding surface with silane coupling agent |
| CN108410218A (en) * | 2018-03-16 | 2018-08-17 | 华南理工大学 | A kind of coupling agent modified organo-mineral complexing concrete protection coating and its preparation method and application |
| CN109374480B (en) * | 2018-12-12 | 2021-06-11 | 江苏科技大学 | Method for evaluating concrete surface coating to prolong durability life of concrete structure |
| CN111333394A (en) * | 2020-02-13 | 2020-06-26 | 卢加贵 | Hydrophobic foam concrete and preparation method thereof |
| CN112159251A (en) * | 2020-09-29 | 2021-01-01 | 国网福建省电力有限公司经济技术研究院 | Concrete reinforcing liquid and preparation method thereof |
| CN113185259B (en) * | 2021-03-09 | 2022-08-23 | 四川大学 | Integrally hydrophobic fireproof magnesium oxychloride thermal insulation foam material and preparation method thereof |
| CN113354347A (en) * | 2021-07-15 | 2021-09-07 | 贵州大学 | Composite waterproof agent for building material and preparation method thereof |
| CN114790119B (en) * | 2022-04-01 | 2023-03-17 | 哈尔滨工程大学 | Low-water-absorption organic/inorganic composite silicon-based coating on concrete surface and preparation method thereof |
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| CN101688316A (en) * | 2008-05-23 | 2010-03-31 | 塔塔钢铁有限公司 | Anti-corrosive hybrid sol-gel film on metallic substrates and method of producing the same |
| CN101892001A (en) * | 2010-07-15 | 2010-11-24 | 江苏科技大学 | Anticorrosive paint based on modified acrylic resin and preparation method thereof |
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| CN101688316A (en) * | 2008-05-23 | 2010-03-31 | 塔塔钢铁有限公司 | Anti-corrosive hybrid sol-gel film on metallic substrates and method of producing the same |
| CN101892001A (en) * | 2010-07-15 | 2010-11-24 | 江苏科技大学 | Anticorrosive paint based on modified acrylic resin and preparation method thereof |
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