CN106277911A - A kind of preparation method of silane emulsion waterproof agent for building - Google Patents
A kind of preparation method of silane emulsion waterproof agent for building Download PDFInfo
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- CN106277911A CN106277911A CN201610570985.0A CN201610570985A CN106277911A CN 106277911 A CN106277911 A CN 106277911A CN 201610570985 A CN201610570985 A CN 201610570985A CN 106277911 A CN106277911 A CN 106277911A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/65—Water proofers or repellants
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
- Paints Or Removers (AREA)
Abstract
The preparation method of a kind of silane emulsion waterproof agent for building, relates to the preparation method of a kind of waterproof agent for building.The present invention is to solve that existing emulsion silane preparation techniques process complexity, apparatus expensive, product have toxic, environment exists pollution, poor stability, the problem of easily layering.Preparation method: one, raw material weighs, adds solvent and emulsifying agent, adds catalyst and thickening agent after dissolving, adding emulsion acrylic resin after emulsifying, carry out high speed emulsifying, the pH adjusting system is 7～9, add stabilizer after high speed emulsifying and sterilize, continuing emulsifying, i.e. complete.Present invention process process safety is easy, it is not necessary to expensive device, and operating process is simple, environmentally safe, overcomes liquid silane and other emulsion silane poor stabilities, the easily problem of layering.The present invention is applicable to the preparation of liquid waterproof agent for building.
Description
Technical field
The present invention relates to the preparation method of a kind of silane emulsion waterproof agent for building
Background technology
Concrete is the most most widely used construction material, but a lot of concrete causes due to corrosion losing efficacy, in corruption
During erosion, water plays the concrete material of critically important effect, particularly coastal area, and moisture content invades inside xoncrete structure,
It is made to be caused because corroding losing efficacy.Traditional one-tenth model concrete surfacecti proteon coating blocks up at concrete surface by covering
Plug concrete pore, reaches the purpose stoping outside moisture to be invaded, and when its shortcoming is internal moisture discharge, can destroy surface and be coated with
Layer, causes coating failure, and it cannot be guaranteed that the breathability that has of concrete material itself.
Silane is a kind of Thief zone type waterproof material, can be sprayed on concrete surface, can improve the waterproof, anti-of concrete
Dirty, dust-proof, anticorrosion, weathering resistance and endurance quality.Because silane has the lowest surface tension, so its extended capability is very
By force, when being coated on the concrete substrate surface of porous, silane can penetrate into formation thin film on the wall of micropore, is leaked by hydrophobic group
At material surface, reach waterproof purpose, and the cross-linked network that silane has, after making dipping, the most do not destroy concrete table
The breathability in face, internal aqueous vapor can be to external diffusion.Its protective mechanism is that silane is coated in concrete surface, by concrete
The capillary suction effect of micropore, it is easy to penetrate in capillary porosity.Penetrate into the silane in capillary gap, at moisture and water
It is hydrolyzed into silanol under effect, with the hydroxyl generation condensation reaction in silicate, forms one layer at concrete surface pore inwall
The repellency netted siloxanes hydrophobic membranous layer of even compact, stops outside moisture and the entrance of harmful substance, in scolding water effect.
Silane waterproof material is divided into emulsion and mastic two class, and mastic is higher due to solid content, and denseness is relatively big, so easily making
Standby and to store the time longer, but its range of application is less；And emulsion flow degeneration is good, range of application is relatively big, but silane emulsion
Stability be always a difficult problem.In aqueous architectural coating, because of avoid employing various solvents to dilute organo-silicon compound,
Thus avoid the restricting condition for use of the aspects such as the toxicity of solvent, volatility and inflammability, make the application of moist surface become
Easily.But silane emulsion preparation still suffers from many difficulties, and such as alkoxy silane has strong hydrolyzable, decomposes simultaneously
The most easily causing condensation reaction, in water, stable existence is extremely difficult, thus while the water solublity of alkylalkoxy silane and moisture
A prose style free from parallelism is preferable, prepares moisture-stable and can play again the organo-silicon compound of waterproof action and remain a difficult problem, waterproof organic
In the preparation of silicon compound and storage, the pH value of emulsion, the selection of comonomer, additive, emulsifying agent and emulsification method are to breast
Stablizing of liquid is particularly significant.
Summary of the invention
The present invention is to solve existing emulsion silane preparation techniques process complexity, apparatus expensive, product have toxic,
Environment is existed pollution, poor stability, the problem of easily layering, it is proposed that the preparation side of a kind of silane emulsion waterproof agent for building
Method.
Silane emulsion waterproof agent for building of the present invention and preparation method thereof sequentially includes the following steps:
One, raw material weighs
In mass ratio for 40:(3～10): 0.2:2:10:5:1:1 weigh silane. thickening agent, catalyst, emulsifying agent, molten
Agent, emulsion acrylic resin, antibacterial and stabilizer；Described silane is propyl-triethoxysilicane, n-octyl triethoxysilicane
Alkane or the copolymer that both obtain in any proportion；Described thickening agent is amido silicon oil 301 or amido silicon oil 802；Described catalysis
Agent is triethylamine；Described emulsifying agent is that 18-amine. polyoxyethylene ether and different tridecanol polyoxyethylene ether mix for 1:1 in mass ratio
The mixture obtained；Described solvent is deionized water；Described antibacterial is ROCIMA 623；Described stabilizer is Polyethylene Glycol
6000；
Two, the preparation of polymer base material
In reactor, add solvent and emulsifying agent, be heated to 60～80 DEG C and be completely dissolved to emulsifying agent, be subsequently adding and urge
Agent and thickening agent, stir under mulser rotating speed is 3000rpm and add silane in three batches, is subsequently adding acrylic resin breast
Liquid, at 60～80 DEG C, reaction obtains reactant in 8～10 hours, reactant finally carries out in mulser high speed emulsifying and obtains
White emulsion；The step of described high speed emulsifying is: be 2000～4000rpm emulsified 0.5～2 hour at mulser rotating speed；Institute
Stating reactor is four-hole bottle；
Three, prepared by emulsion water-proof agent
Adding appropriate phosphoric acid in the white emulsion that step 2 obtains to the pH of system is 7～9, is subsequently placed in breast at a high speed
In change machine at rotating speed 3000rpm emulsified 0.5～1 hour, add stabilizer and antibacterial, continue under rotating speed 3000rpm
Emulsifying 0.5～1 hour, i.e. complete；If wherein occurring foaming can add defoamer in emulsion process.
The present invention possesses following beneficial effect
1, present invention process process safety is easy, it is not necessary to expensive device, and operating process is simple；
2, the emulsion water-proof agent that prepared by the inventive method is with water as solvent, harmless to humans, environmentally safe；
3, the emulsion water-proof agent hydrophobic effect that prepared by the inventive method is high；
4, the emulsion water-proof agent that prepared by the inventive method overcomes liquid silane and other emulsion silane poor stabilities, easily
The problem of layering, by selecting the emulsifying agent similar to silane monomer polarity to be wrapped up by the silicone hydroxyl after hydrolysis, evenly spreads to
In aqueous solvent, the silicone hydroxyl of the carbon-carbon double bond in acrylic acid and generation simultaneously interacts can form stabilising system, addition
Amido silicon oil can increase the denseness of system and guarantee system stability, the co-stabilizer Polyethylene Glycol being simultaneously introduced, and increases organic
Mutually with inorganic phase interface, these combined factors are got up so that product stability significantly improves, therefore can be kept more than four months
There is not aqueous phase and organic facies layering, color even free from admixture, without floating oil, and standing sedimentation does not occur；
5, the emulsion water-proof agent that prepared by the inventive method can keep the gas of material own compared to traditional concrete paint
The breathability of pore structure, is really to have " respiratory " waterproof coating material；
6, the emulsion water-proof agent that prepared by the inventive method be better than in water resistance and permeance property liquid silane monomer and
Conventional waterproof coating；
7, the emulsion water-proof agent that prepared by the inventive method is the most reasonable, and cost performance is high；
8, the emulsion water-proof agent that prepared by the inventive method is compared to creme silicane product, and mobility is excellent, and practice of construction is more
Add conveniently, and after introducing amido silicon oil copolymerization, waterproof effect gets a promotion.
Accompanying drawing explanation
Fig. 1 is that the contact angle of emulsion water-proof agent of embodiment 1 preparation and chloride ion reduction rate are with different silane and solvent
The quality of deionized water is than change curve, wherein, and the contact angle of the 1 emulsion water-proof agent prepared for n-octytriethoxysilane
Curve, the contact angle curve of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane, 3 is n-octytriethoxysilane system
The length of penetration curve of standby emulsion water-proof agent, the length of penetration of the 4 emulsion water-proof agent prepared for propyl-triethoxysilicane is bent
Line；
Fig. 2 is that the contact angle of emulsion water-proof agent of the emulsion water-proof agent of embodiment 2 preparation and chloride ion reduction rate are with difference
The quality of silane and solvent deionized water than change curve, the 1 emulsion water-proof agent prepared for n-octytriethoxysilane
Contact angle curve, the contact angle curve of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane, 3 is n-octyl three ethoxy
The chloride ion reduction rate curve of emulsion water-proof agent prepared by base silane, 4 is the emulsion water-proof prepared for propyl-triethoxysilicane
The chloride ion reduction rate curve of agent；
Fig. 3 is that the contact angle of emulsion water-proof agent of embodiment 3 preparation and length of penetration are with different propyl-triethoxysilicanes
Alkane and n-octytriethoxysilane quality are than change curve, and 1 is the length of penetration curve of emulsion water-proof agent, 2 emulsion water-proofs
The contact angle curve of agent；
Fig. 4 is that the contact angle of emulsion water-proof agent of embodiment 3 preparation and chloride ion reduction rate are with different propyl group three ethoxies
Base silane and n-octytriethoxysilane quality are than change curve, and 1 is the chloride ion reduction rate curve of emulsion water-proof agent, and 2
Contact angle curve for emulsion water-proof agent；
Fig. 5 is the contact angle mass change with different amido silicon oils 301 of the emulsion water-proof agent of embodiment 4 and 5 preparation
Curve chart, the contact angle of the 1 emulsion water-proof agent prepared for n-octytriethoxysilane is with the quality of different amido silicon oils 301
Change curve；The contact angle of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane is with the quality of different amido silicon oils 301
Change curve；
Fig. 6 is that the length of penetration of the emulsion water-proof agent of embodiment 4 and 5 preparation becomes with the quality of different amido silicon oils 301
Changing curve chart, the length of penetration of the 1 emulsion water-proof agent prepared for n-octytriethoxysilane is with different amido silicon oils 301
Mass-change curve；The length of penetration of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane is with different amido silicon oils 301
Mass-change curve；
Fig. 7 is the chloride ion reduction rate matter with different amido silicon oils 301 of the emulsion water-proof agent of embodiment 4 and 5 preparation
Amount change curve, the chloride ion reduction rate of the 1 emulsion water-proof agent prepared for n-octytriethoxysilane is with different amino
The mass-change curve of silicone oil 301；The chloride ion reduction rate of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane alkane is not with
The mass-change curve of same amido silicon oil 301；
Fig. 8 is the emulsion water-proof agent actual waterproof effect figure of embodiment 1 preparation.
Detailed description of the invention
Technical solution of the present invention is not limited to act detailed description of the invention set forth below, also includes between each detailed description of the invention
Arbitrarily reasonable combination.
Detailed description of the invention one: the preparation method of present embodiment silane emulsion waterproof agent for building sequentially includes the following steps:
One, raw material weighs
In mass ratio for 40:(3～10): 0.2:2:10:5:1:1 weigh silane. thickening agent, catalyst, emulsifying agent, molten
Agent, emulsion acrylic resin, antibacterial and stabilizer；
Two, the preparation of polymer base material
In reactor, add solvent and emulsifying agent, be heated to 60～80 DEG C and be completely dissolved to emulsifying agent, be subsequently adding and urge
Agent and thickening agent, stir under mulser rotating speed is 3000rpm and add silane in three batches, is subsequently adding acrylic resin breast
Liquid, at 60～80 DEG C, reaction obtains reactant in 8～10 hours, reactant finally carries out in mulser high speed emulsifying and obtains
White emulsion；Described reactor is four-hole bottle；
Three, prepared by emulsion water-proof agent
Adding appropriate phosphoric acid in the white emulsion that step 2 obtains to the pH of system is 7～9, is subsequently placed in breast at a high speed
In change machine at rotating speed 3000rpm emulsified 0.5～1 hour, add stabilizer and antibacterial, continue under rotating speed 3000rpm
Emulsifying 0.5～1 hour, i.e. complete.
1, this detailed description of the invention technical process is safe and simple, it is not necessary to expensive device, and operating process is simple；
2, the emulsion water-proof agent that prepared by this detailed description of the invention method is with water as solvent, harmless to humans, environmentally safe；
3, the emulsion water-proof agent hydrophobic effect that prepared by this detailed description of the invention method is high；
4, the emulsion water-proof agent that prepared by this detailed description of the invention method overcomes liquid silane and other emulsion silane is stable
Property poor, the easily problem of layering, by select the emulsifying agent similar to silane monomer polarity by the silicone hydroxyl parcel after hydrolysis, all
Even being distributed in aqueous solvent, the silicone hydroxyl of the carbon-carbon double bond in acrylic acid and generation simultaneously interacts can form liptinite
System, the amido silicon oil of addition can increase the denseness of system and guarantee system stability, the co-stabilizer Polyethylene Glycol being simultaneously introduced,
Increasing organic facies and inorganic phase interface, these combined factors are got up so that product stability significantly improves, can be kept four months
Below there is not aqueous phase and organic facies layering, color even free from admixture, without floating oil, and standing sedimentation does not occur；
5, the emulsion water-proof agent that prepared by this detailed description of the invention method can keep material compared to traditional concrete paint
The breathability of the air hole structure of material own, is really to have " respiratory " waterproof coating material；
6, the emulsion water-proof agent that prepared by this detailed description of the invention method is better than liquid silicon in water resistance and permeance property
Alkane monomer and conventional waterproof coating；
7, the emulsion water-proof agent that prepared by this detailed description of the invention method is the most reasonable, and cost performance is high；
8, the emulsion water-proof agent that prepared by this detailed description of the invention method is compared to creme silicane product, and mobility is excellent, real
Border construction is convenient, and after introducing amido silicon oil copolymerization, waterproof effect gets a promotion.
Detailed description of the invention two: present embodiment is unlike detailed description of the invention one: silane described in step one is third
Ethyl triethoxy silicane alkane, n-octytriethoxysilane or the copolymer that both obtain in any proportion.Other steps and parameter
Identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is unlike detailed description of the invention one or two: thickening described in step one
Agent is amido silicon oil 301 or amido silicon oil 802.Other steps are identical with detailed description of the invention one or two with parameter.
Detailed description of the invention four: present embodiment is unlike one of detailed description of the invention one to three: described in step one
Catalyst is triethylamine.Other steps are identical with one of detailed description of the invention one to three with parameter.
Detailed description of the invention five: present embodiment is unlike one of detailed description of the invention one to four: described in step one
The mixture that emulsifying agent is 18-amine. polyoxyethylene ether and different tridecanol polyoxyethylene ether is mixed to get for 1:1 in mass ratio；Step
Solvent described in rapid one is deionized water.Other steps are identical with one of detailed description of the invention one to four with parameter.
Detailed description of the invention six: present embodiment is unlike one of detailed description of the invention one to five: described in step one
Antibacterial is ROCIMA 623.Other steps are identical with one of detailed description of the invention one to five with parameter.
Detailed description of the invention seven: present embodiment is unlike one of detailed description of the invention one to six: described in step one
Stabilizer is polyethylene glycol 6000.Other steps are identical with one of detailed description of the invention one to six with parameter.
Detailed description of the invention eight: present embodiment is unlike one of detailed description of the invention one to seven: described in step 2
The step of high speed emulsifying is: be 2000～4000rpm emulsified 0.5～2 hour at mulser rotating speed.Other steps and parameter with
One of detailed description of the invention one to seven is identical.
Embodiment 1
The present embodiment silane emulsion waterproof agent for building and preparation method thereof sequentially includes the following steps:
One, raw material weighs
In mass ratio for 40:3:0.2:2:10:5:1:1 weigh silane. thickening agent, catalyst, emulsifying agent, solvent, propylene
Acid resin emulsion, antibacterial and stabilizer；Described silane is n-octytriethoxysilane；Described thickening agent is amido silicon oil
301；Described catalyst is triethylamine；Described emulsifying agent is that 18-amine. polyoxyethylene ether and different tridecanol polyoxyethylene ether are by quality
Than the mixture being mixed to get for 1:1；Described solvent is deionized water；Described antibacterial is ROCIMA623；Described stabilizer is
Polyethylene glycol 6000；
Two, the preparation of polymer base material
In reactor, add solvent and emulsifying agent, be heated to 70 DEG C and be completely dissolved to emulsifying agent, be subsequently adding catalyst
And thickening agent, stir under mulser rotating speed is 3000rpm and add silane in three batches, being subsequently adding emulsion acrylic resin,
At 70 DEG C, reaction obtains reactant in 9 hours, reactant finally carries out in mulser high speed emulsifying and obtains white emulsion；Institute
The step stating high speed emulsifying is: be 3000rpm emulsified 1 hour at mulser rotating speed；Described reactor is four-hole bottle；
Three, prepared by emulsion water-proof agent
Adding appropriate phosphoric acid in the white emulsion that step 2 obtains to the pH of system is neutrality, is subsequently placed at a high speed breast
In change machine at rotating speed 3000rpm emulsified 1 hour, add stabilizer and antibacterial, continue at rotating speed 3000rpm emulsified 1
Hour, i.e. complete；If wherein occurring foaming can add defoamer in emulsion process.
1, the present embodiment technical process is safe and simple, it is not necessary to expensive device, and operating process is simple；
2, the emulsion water-proof agent that prepared by the present embodiment method is with water as solvent, harmless to humans, environmentally safe；
3, the emulsion water-proof agent hydrophobic effect that prepared by the present embodiment method is high, and can long-time stable exist；
4, the emulsion water-proof agent that prepared by the present embodiment method overcomes liquid silane and other emulsion silane poor stabilities, holds
The easily problem of layering, by selecting the emulsifying agent similar to silane monomer polarity to be wrapped up by the silicone hydroxyl after hydrolysis, dispersed
In aqueous solvent, the silicone hydroxyl of the carbon-carbon double bond in acrylic acid and generation simultaneously interacts can form stabilising system, adds
Amido silicon oil can increase the denseness of system and guarantee system stability, the co-stabilizer Polyethylene Glycol being simultaneously introduced, increase has
Machine phase and inorganic phase interface, these combined factors are got up so that product stability significantly improves, and can keep more than four months not
There is aqueous phase and organic facies layering, color even free from admixture, without floating oil, and standing sedimentation does not occur；
5, the emulsion water-proof agent that prepared by the present embodiment method can keep material itself compared to traditional concrete paint
The breathability of air hole structure, is really to have " respiratory " waterproof coating material；
6, the emulsion water-proof agent that prepared by the present embodiment method is better than liquid silane monomer in water resistance and permeance property
With conventional waterproof coating；
7, the emulsion water-proof agent that prepared by the present embodiment method is the most reasonable, and cost performance is high；
8, the emulsion water-proof agent that prepared by the present embodiment method is compared to creme silicane product, and mobility is excellent, practice of construction
Convenient, and after introducing amido silicon oil copolymerization, waterproof effect gets a promotion, and contact angle is 90 °, and chloride ion reduction rate is
90%, length of penetration is 1mm.
Embodiment 2
The present embodiment is respectively adopted propyl-triethoxysilicane and n-octytriethoxysilane prepares emulsion water-proof agent, its
The mass ratio of middle propyl-triethoxysilicane and solvent deionized water be respectively as follows: 0.1:1,0.4:1,0.5:1,1:1,1.5:1,
1.75:1,2:1,2.25:1,2.5:1,3:1,3.5:1,3.75:1,4:1,4.25:1,4.5:1 and 5:1；N-octyl triethoxy
The mass ratio of silane and solvent deionized water be respectively as follows: 0.1:1,0.4:1,0.5:1,1:1,1.5:1,1.75:1,2:1,2.25:
1,2.5:1,3:1,3.5:1,3.75:1,4:1,4.25:1,4.5:1 and 5:1；Other steps and parameter are same as in Example 1；
The contact angle of emulsion water-proof agent, length of penetration and chloride ion reduction rate prepared by test the present embodiment are with different silicon
The quality of alkane and solvent deionized water is than change curve, and test result is as depicted in figs. 1 and 2；In Fig. 1,1 is n-octyl three second
The contact angle curve of emulsion water-proof agent prepared by TMOS, connecing of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane
Feeler curve, the length of penetration curve of the 3 emulsion water-proof agent prepared for n-octytriethoxysilane, 4 is propyl triethoxy
The length of penetration curve of emulsion water-proof agent prepared by silane；In Fig. 2,1 emulsion water-proof prepared for n-octytriethoxysilane
The contact angle curve of agent, the contact angle curve of the 2 emulsion water-proof agent prepared for propyl-triethoxysilicane, 3 is n-octyl three second
The chloride ion reduction rate curve of emulsion water-proof agent prepared by TMOS, 4 is that the emulsion prepared for propyl-triethoxysilicane is prevented
The chloride ion reduction rate curve of water preparation；
From Fig. 1 and 2 it can be seen that octyltri-ethoxysilane is made more effective than propyl-triethoxysilicane, and with
The rising of silane contents, contact angle, length of penetration, chloride ion content reduction rate all gradually rise, and just have decline to become after 4:1
Gesture, so selecting silane and the mass ratio most preferably 4:1 of solvent；
Embodiment 3
Silane described in the present embodiment is that propyl-triethoxysilicane and n-octytriethoxysilane are by the most in mass ratio
It is respectively the copolymer that 0.1:1,0.25:1,0.36:1,0.5:1,0.6:1,0.75:1,0.88:1 and 1:1 are mixed to get；Other
Step and parameter are same as in Example 1；
The contact angle of emulsion water-proof agent, length of penetration and chloride ion reduction rate prepared by test the present embodiment are with different third
Ethyl triethoxy silicane alkane and n-octytriethoxysilane quality are than change curve, and test result is as shown in Figure 3 and Figure 4；Fig. 3
In, the length of penetration curve of the 1 emulsion water-proof agent prepared for the present embodiment, connecing of the 2 emulsion water-proof agent prepared for the present embodiment
Feeler curve；In Fig. 4, the chloride ion reduction rate curve of the 1 emulsion water-proof agent prepared for the present embodiment, 2 prepare for the present embodiment
The contact angle curve of emulsion water-proof agent；From Fig. 3 and 4 it can be seen that along with system mix propyl-triethoxysilicane contain
Amount gradually rises, and contact angle, length of penetration, chloride ion reduction rate are all gradually weakening, so octyl group triethoxysilicane compares propyl group
Triethoxysilane is effective；
Embodiment 4
Silane described in the present embodiment is n-octytriethoxysilane；Described thickening agent is amido silicon oil 301；Amido silicon oil
The quality of 301 is respectively 1g, 2.5g, 5g, 7.5g, 10g, 15g, 20g, 25g and 30g, other steps and parameter and embodiment 1 phase
With；
The contact angle of emulsion water-proof agent, length of penetration and chloride ion reduction rate prepared by test the present embodiment are with different ammonia
The mass-change curve figure of base silicone oil 301, test result is as shown in Fig. 5～Fig. 7；Wherein, in Fig. 5,1 is n-octyl triethoxy
The contact angle of emulsion water-proof agent prepared by silane is with the mass-change curve of different amido silicon oils 301；In Fig. 6,1 is n-octyl
The length of penetration of emulsion water-proof agent prepared by triethoxysilane is with the mass-change curve of different amido silicon oils 301；Fig. 7
In, the chloride ion reduction rate of the 1 emulsion water-proof agent prepared for n-octytriethoxysilane is with the matter of different amido silicon oils 301
Amount change curve；
Embodiment 5
Silane described in the present embodiment is propyl-triethoxysilicane；Described thickening agent is amido silicon oil 301；Amido silicon oil
The quality of 301 is respectively 1g, 2.5g, 5g, 7.5g, 10g, 15g, 20g, 25g and 30g, other steps and parameter and embodiment 4 phase
With；
The contact angle of emulsion water-proof agent, length of penetration and chloride ion reduction rate prepared by test the present embodiment are with different ammonia
The mass-change curve figure of base silicone oil 301, test result is as shown in Fig. 5～Fig. 7；Wherein, in Fig. 5,2 is propyl-triethoxysilicane
The contact angle of emulsion water-proof agent prepared by alkane is with the mass-change curve of different amido silicon oils 301；In Fig. 6,2 is propyl group three second
The length of penetration of emulsion water-proof agent prepared by TMOS is with the mass-change curve of different amido silicon oils 301；In Fig. 7,2 are
The chloride ion reduction rate of emulsion water-proof agent prepared by propyl-triethoxysilicane alkane is with the mass change of different amido silicon oils 301
Curve；
Understand increasing along with the amido silicon oil content system from embodiment 4 and 5, the contact angle of emulsion, length of penetration,
Chloride ion reduction rate is all reducing, and comprehensive product stability considers, selecting addition is that 5g is optimal.
Wherein, the mensuration of contact angle, the mensuration of length of penetration and the test of chloride ion reduction rate described in embodiment 2～5
Method is:
Prepare before test:
Concrete sample makes and processes the normal concrete making test desirable strength grade C30 by country's working standard
OPC test specimen, specification 100mm × 100mm × 100mm, (curing temperature (20 ± 3) DEG C, relative air humidity is not less than standard conditions
90%) after maintenance 28d, removing surface of test piece and be unfavorable for the foreign material such as the dust of silane-coating, greasy dirt, tap water dries in the air after rinsing well
It is dry,
Ensure that surface of test piece is surface dry condition during the coating of silane emulsion waterproof agent for building, the side of brushing continuously during coating, should be used
Formula, it is ensured that be coated with the saturated overflow in surface.During horizontal plane brushing, brush and moisten or to mirror-like to surface of test piece, make to be coated with surface
Keeping moisture state a few minutes, coated weight uses 400g/m2, i.e. each face consumption is (100mm × 100mm) 4g；
One, the mensuration of contact angle
Use profile image analytical method, be specially and drop is dripped in solid sample surface, obtained with camera by microlens
Obtain the outline drawing picture of drop, then use image procossing and calculating to be calculated by the contact angle of the drop in image.Calculate contact
The method at angle is typically based on a specific mathematical model such as drop can be considered a part for ball or cone, then by measuring spy
Fixed parameter such as wide/height or calculates contact angle values by direct matching.Young-Laplace equation describes a closing
The inside and outside pressure differential at interface and the curvature at interface and the relation of interfacial tension, can be used to describe an axisymmetric drop exactly
Appearance profile, thus calculate its contact angle；
Two, the mensuration of length of penetration
Taking test specimen and carry out silane emulsion waterproof agent for building coating, each face consumption is (100mm × 100mm) 4g, is dried
After maintenance (curing temperature is (20 ± 3) DEG C, relative air humidity (60 ± 5) %) 14d, through oven for drying 24h of 50 DEG C, in temperature
Degree is (20 ± 3) DEG C, is cooled to room temperature under relative air humidity (60 ± 5) %, takes out test specimen, by concrete after dry maintenance 1d
Riving, spray water riving on surface, the degree of depth measuring the region not absorbing water is length of penetration.Put down with the arithmetic of three test specimens
Average, as measured value, is accurate to 0.1mm.
Three, the mensuration of chloride ion absorbtivity reduction rate
To one side silane coating emulsion waterproof agent for building (100mm × 100mm) 4g, get a test block simultaneously and be not coated by silicon
Alkane emulsion waterproof agent for building does blank, repeats operations described below.In addition to original surface and its opposite, its lap non-solvent epoxy
Coating coating seals.After being dried maintenance 14d (curing temperature is (20 ± 3) DEG C, relative air humidity (60 ± 5) %), all exist
After drying 48h at 50 DEG C, it is (20 ± 3) DEG C in temperature, under relative air humidity (60 ± 5) %, is cooled to room temperature.By sample original surface
Towards being placed down in suitable container, implantation temperature is the NaCl solution of the 5mol/L of (20 ± 3) DEG C, and liquid level exceeds test specimen bottom surface
Sample after 10mm, 24h, at 40 DEG C, dry 24h.Cutting surface of test piece 2mm, on the basis of new face, face is ground to the degree of depth for taking at 10mm
Powder.The chloride content of gained powder sample is analyzed by existing industry standard concrete acid soluble chlorides determination.In the degree of depth it is
At 11～20mm and 21～30mm, repeat said procedure.Using the arithmetic mean of instantaneous value of three groups of test specimens as measured value.
Computing formula is as follows:
The reducing effect (%) of △ C chloride absorbtivity in formula；
C0The chloride average content of blank group, for the meansigma methods of three degree of depth chloride absorbtivitys of each sample；
The chloride average content of C silane emulsion waterproof agent for building, for three degree of depth chloride absorbtivitys of each sample
Meansigma methods.
Claims (9)
1. the preparation method of a silane emulsion waterproof agent for building, it is characterised in that this preparation method sequentially includes the following steps:
One, raw material weighs
In mass ratio for 40:(3～10): 0.2:2:10:5:1:1 weigh silane. thickening agent, catalyst, emulsifying agent, solvent, third
Olefin(e) acid resin emulsion, antibacterial and stabilizer；
Two, the preparation of polymer base material
In reactor, add solvent and emulsifying agent, be heated to 60～80 DEG C and be completely dissolved to emulsifying agent, be subsequently adding catalyst
And thickening agent, stir under mulser rotating speed is 3000rpm and add silane in three batches, being subsequently adding emulsion acrylic resin,
At 60～80 DEG C, reaction obtains reactant in 8～10 hours, reactant finally carries out in mulser high speed emulsifying and obtains white
Color emulsion；Described reactor is four-hole bottle；
Three, prepared by emulsion water-proof agent
Adding appropriate phosphoric acid in the white emulsion that step 2 obtains to the pH of system is 7～9, is subsequently placed in high-speed emulsifying machine
In at rotating speed 3000rpm emulsified 0.5～1 hour, add stabilizer and antibacterial, continue emulsified at rotating speed 3000rpm
0.5～1 hour, i.e. complete.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
Described silane is propyl-triethoxysilicane, n-octytriethoxysilane or copolymer that both obtain in any proportion.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
Described thickening agent is amido silicon oil 301 or amido silicon oil 802.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
Described catalyst is triethylamine.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
The mixing that described emulsifying agent is 18-amine. polyoxyethylene ether and different tridecanol polyoxyethylene ether is mixed to get for 1:1 in mass ratio
Thing.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
Described solvent is deionized water.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
Described antibacterial is ROCIMA 623.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step one
Described stabilizer is polyethylene glycol 6000.
The preparation method of a kind of concrete silane emulsion waterproofing agent the most according to claim 1, it is characterised in that: step 2
The step of described high speed emulsifying is: be 2000～4000rpm emulsified 0.5～2 hour at mulser rotating speed.
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| CN107022080A (en) * | 2017-04-28 | 2017-08-08 | 青岛理工大学 | A kind of preparation method of novel silicon alkanes plural gel waterproof material |
| CN108786650A (en) * | 2018-05-10 | 2018-11-13 | 浙江科峰新材料有限公司 | A kind of emulsifier combination and its production technology |
| CN112552761A (en) * | 2020-12-18 | 2021-03-26 | 杨华 | Concrete salt-resistant protective agent |
| CN113529417A (en) * | 2021-07-19 | 2021-10-22 | 中交上海三航科学研究院有限公司 | Water-based organic silicon permeation type anti-corrosion impregnant and preparation method thereof |
| CN114051492A (en) * | 2019-08-06 | 2022-02-15 | 第一点有限公司 | Plaster treatment compound |
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