CN102351999A - Method for preparing nanoparticle water reducing agent - Google Patents
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- CN102351999A CN102351999A CN2011101996938A CN201110199693A CN102351999A CN 102351999 A CN102351999 A CN 102351999A CN 2011101996938 A CN2011101996938 A CN 2011101996938A CN 201110199693 A CN201110199693 A CN 201110199693A CN 102351999 A CN102351999 A CN 102351999A
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Abstract
The invention discloses a method for preparing a nanoparticle water reducing agent, which belongs to the technical field of the preparation of building material admixtures. The water reducing agent at a certain doping amount can achieve the dispersing and water reduction effects at the early stage of cement paste; meanwhile, the water reducing agent has the functions of room-temperature film formation and emulsion modification, so the comprehensive performance of cement concrete such as late-stage waterproofness, compactness, chloride ion permeation resistance, mechanical properties, durability and the like can be greatly improved. The nanoparticle water reducing agent can be widely applied to the fields of railways, bridges, tunnels, dams, offshore engineering, remedial works and the like.
Description
Technical field
The invention belongs to the additive for building material preparing technical field, be specifically related to a kind of preparation method of nanoparticle subtype water reducer.
Background technology
Concrete is the maximum material of construction of present consumption; Concrete admixture is the 6th component except cement, sand, stone, water, mineral admixture in the concrete; It is playing the part of very important role in the application of high performance concrete; In the concrete technology development process, the invention of high efficiency water reducing agent and application are acknowledged as the leap of technology for the third time in concrete technology field after Steel Concrete and prestressed reinforced concrete technology.High efficiency water reducing agent is as a kind in the admixture, and consumption is maximum therein, and its incorporation is not more than 5% of cement quality, mainly plays 3 different effects: concrete cast property is improved in (1).(2) under given working conditions, reduce water cement ratio, improve intensity and weather resistance on the coagulation.(3) guaranteeing to reduce the consumption of water and cement under the constant situation of concrete depositing performance and intensity, reduce the factor that drying shrinkage, hydration heat of cement etc. cause the concrete initial imperfection.Concrete development be unable to do without chemical admixture, and like the realization of new technologies such as pump concrete, sprayed concrete, self-leveling concrete, non-dispersible underwater concrete, high efficiency water reducing agent has played keying action.In addition along with world energy sources and conservation of resources require growing; A large amount of blast-furnace slags, flyash etc. are as cement composite material; High efficiency water reducing agent makes microfine mineral admixture be applied to high-performance concrete becomes possibility; Make resource be able to comprehensive utilization and also greatly improved concrete performance, produced huge economic benefit and social benefit thereupon.Water reducer has become indispensable component in the current cement concrete construction.
From the property development process of water reducer, the development of water reducer can be divided into four-stage: (1) is the exploitation and the application of the ordinary water-reducing agent of representative with sulfonated lignin; (2) be the high efficiency water reducing agent of representative with beta-naphthalenesulfonic-acid salt formaldehyde condensation products (PNS) and sulfonated melamine compound condenses (PMS); (3) the high efficiency water reducing agent that PNS and PMS are carried out modification with slump hold facility; (4) have high diminishing ability and the new and effective water reducer of degree of mobilization hold facility, typical in polycarboxylate high-efficiency water reducing agent (PC).Wherein, it is the most extensive that polycarboxylic acids dehydragent is used, and synthesis technique mainly comprises with the methoxy poly (ethylene glycol) being that starting ester is combined to the synthetic water reducer technology of the big monomer two-step approach of ester class and is the synthetic water reducer technology of the direct single stage method of raw material with the unsaturated ethers.Since in the suitability for industrialized production, the one-step synthesis process less energy consumption, simple to operate, therefore more be subjected to producer and investigator's favor.So this patent also adopts single stage method synthetic.
It is electrostatic repulsion and sterically hindered effect that water reducer improves the mobile main mechanism of action of cement concrete.The former is meant that the side group that water reducer has a negative charge can be adsorbed onto cement particle surface, forms electric double layer, produces electrostatic repulsion between the adjacent cement granules, and flucculation structure is destroyed, and discharges intergranular parcel water, thereby increases the flowability of system; The latter is meant the segment of grafting certain-length polyoxy alkyl oxide in the water reducer; Wetting ability is extremely strong; Thereby can adsorb a certain amount of water molecules and form stable solvation moisture film, this layer moisture film can reduce intergranular sliding resistance, thereby the mobile of system further improved.
Yet the effect of water reducer only is embodied in early stage to the improvement of cement concrete flowing property, and is little atomic to the improvement of other later stage performances of cement concrete such as mechanical property, weather resistance.
On the other hand, as the polymer emulsion of another kind admixture commonly used, it is to the effect that all increases significantly of concrete over-all properties.Adopt polymer emulsion or re-dispersible glue powder that mortar and concrete are carried out modification, can give mortar and concrete many superior performances.A large amount of research and practices show that polymkeric substance adds cement-based mortar and concrete system, present two aspects of its acting body: to the improvement of new sand cutting slurry performance, such as improving the early stage cohesive force of mortar, improving serviceability and operable time etc.; To the improvement of back mortar performance of condensing, as improve mechanical property, improve folding strength and ultimate deformation; Increase snappiness, improve mortar bonding intensity, reduce volumetric shrinkage; Reduce porosity, improve impervious water tolerance etc., finally reach the function that prolongs mortar or concrete system work-ing life.
Polymer-modified cement mortar has been compared following tangible advantage with other sand-cement slurry with concrete modifying measure (as adding fiber cement concrete) with concrete: sand-cement slurry and mechanical properties of concrete improve; Especially folding strength is improved; Though ultimate compression strength decreases, toughness is improved; Mortar and concrete rigidity reduce, and deformability increases, and is favourable to many engineerings; Mortar and concrete pore rate decrease, and the microfracture development suppresses to some extent; Mortar and concrete weather resistance and corrosion resistance improve to some extent; Be specially adapted to damaged sand-cement slurry and concrete repairing work; Adapt to existing sand-cement slurry and concrete process for making fully.
Polymkeric substance generally includes following viewpoint to the also ununified to some extent final conclusion of cement concrete modifying mechanism:
(1) polymers to alter the structural form of cement stone, hydrated cementitious product and pore structure.
(2) polymkeric substance has influenced the aquation and the setting and harden process of cement.
(3) polymkeric substance has improved the bonding of cement and aggregate interfacial transition zone, has reduced tiny crack in the system, improves mechanical performance of concrete.
(4) polymkeric substance has certain water-reduction, and concrete w/c decreases, and improves its serviceability.
(5) polymkeric substance has covered concrete microstructure hole, and porosity reduces, and density increases, thereby improves concrete impermeability, improves concrete durability.
Owing to receive the influence of type of polymer and volume, concrete modifying function mechanism possibly be one of above-mentioned, also might be the synergy of above-mentioned several modified effects.Emulsion itself has certain water-reduction, has report to point out that when the emulsion volume reached 12%, concrete can add water reducer can obtain good water-reducing property.
In sum; If the function of water reducer and emulsion can be combined; Develop a kind of nanoparticle subtype water reducer; Give the function of its emulsion; Can improve the cement concrete flowing property preferably; Final room temperature film-forming, and then reach raising, improve the purpose of the over-all properties of cement concrete is with a wide range of applications and is worth.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nanoparticle subtype water reducer.
A kind of preparation method of nanoparticle subtype water reducer, carry out according to following steps:
A, with emulsifiers dissolve in deionized water, be warming up to 40～90 ℃, obtain clarifying emulsifier solution;
B, acrylic monomer, vinylbenzene, esters monomer, methacrylic disulfonate acid and chain-transfer agent mixed after; In emulsifier solution, drip; Add 1～30g initiator simultaneously; Polymerization 1～5 hour; After the end; Sustained reaction 1～12 hour, the cooling cooling is regulated stoste pH value to alkalescence with NaOH behind the elimination residue;
Perhaps,
A ' adds 5～500g deionized water in advance in reaction kettle, be warming up to 40-90 ℃;
B ' at the uniform velocity splashes into reaction kettle after acrylic monomer, vinylbenzene, esters monomer, methacrylic disulfonate acid and chain-transfer agent are mixed; Dropping time 1～5h; Drip 2～100g initiator; Initiator drips time 1～8h; Finish back insulation 0.5～12h; The cooling cooling is regulated stoste pH value to alkalescence with NaOH behind the elimination residue.
Emulsifying agent that step a adds and deionized water ratio are (20～100g): (50～700ml).
The mass ratio of acrylic monomer that step b adds, vinylbenzene, esters monomer and methacrylic disulfonate acid is (1～50) g: (50～800) g: (5～600g): (1～50) g; The mass ratio of acrylic monomer that step b ' adds, vinylbenzene, esters monomer and methacrylic disulfonate acid is (1～50) g: (50～800) g: (5～600g): (1～50) g.
Said emulsifying agent is selected from a kind of in alkyl-sulphate, fatty alcohol polyoxyethylene ether sulfate, aliphatic alcohol sulfate, lauryl diglycollic amide, dodecanamide propyl trimethyl-glycine, fatty alcohol-polyoxyethylene ether, fatty alcohol-polyoxyethylene ether succinate sodium sulfonate, dodecanamide propyl amine oxide, linear alkylbenzene sulfonate, polyoxyethylene sorbitan monolaurate, the Natvosol and more than one.
Said acrylic monomer is selected from one or more in vinylformic acid, methacrylic acid, vinylformic acid ammonium salt, vinylformic acid monovalent metal salt, vinylformic acid divalent metal salt, methacrylic acid ammonium salt, methacrylic acid monovalent metal salt, the methacrylic acid divalent metal salt.
Said esters monomer is selected from one or more in butoxy end-blocking polyoxyethylene glycol allyl ethers, methoxy-terminated polyoxyethylene glycol allyl ethers, butoxy end-blocking polyoxyethylene glycol methallyl ethers, propoxy-end-blocking polyoxyethylene glycol allyl ethers, butoxy end-blocking polyoxyethylene glycol 3-butene-1-alcohol ether, the oxyethyl group end-blocking polyoxyethylene glycol polypropylene glycol allyl ethers.
Said chain-transfer agent is selected from one or more in thioglycerol, mercaptoethanol, Thiovanic acid, 2-Thiovanic acid, 3-Thiovanic acid, thiohydracrylic acid, mercaptosuccinic acid, Thiovanic acid monooctyl ester, 2-Thiovanic acid monooctyl ester, the 3-sulfydryl ethyl sulfonic acid, and add-on is 0～100g.
Said initiator is one or more in dibenzoyl peroxide, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, Diisopropyl azodicarboxylate, V-50 initiator, the dilauroyl peroxide.
Beneficial effect of the present invention: 1, the prepared nanoparticle subtype water reducer of the present invention can improve the cement concrete flowing property preferably, improves diminishing dissemination in early stage.2, mix cement concrete after, significantly improve impervious and anti-ion permeability of sand-cement slurry and concrete later stage, improve its weather resistance.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1
20g propyl group sodium sulfate is dissolved in the 250ml deionized water, is warming up to 60 ℃, obtain clarifying emulsifier solution.After 30g vinylformic acid, 200g vinylbenzene, 100g butoxy end-blocking polyoxyethylene glycol allyl ethers, the mixing of 2g methacrylic disulfonate acid; In emulsifier solution, drip; Add the 20g dibenzoyl peroxide simultaneously; Polyase 13 hour; After the end, sustained reaction 5 hours, cooling cooling; Regulate stoste pH value to alkalescence with NaOH behind the elimination residue, get nanoparticle property water reducer.
Test nanoparticle subtype water reducer size is 180nm, and dispersion index is 0.134.
Embodiment 2
25g sodium alkyl sulfate and 25g polyoxyethylenated alcohol sodium sulfate are dissolved in the 50ml deionized water, are warming up to 80 ℃, obtain clarifying emulsifier solution.After 10g methacrylic acid, 50g vinylbenzene, 20g methoxy-terminated polyoxyethylene glycol allyl ethers, the mixing of 30g methacrylic disulfonate acid; In emulsifier solution, drip; Add the 40g Potassium Persulphate simultaneously; Polymerization 2 hours; After the end, sustained reaction 7 hours, cooling cooling; Regulate stoste pH value to alkalescence with NaOH behind the elimination residue, get nanoparticle property water reducer.
Test nanoparticle subtype water reducer size is 80nm, and dispersion index is 0.04.
Embodiment 3
90g dodecanamide propyl trimethyl-glycine is dissolved in the 600ml deionized water, is warming up to 55 ℃, obtain clarifying emulsifier solution.After 2g ammonium acrylate sodium, 600g vinylbenzene, 300g butoxy end-blocking polyoxyethylene glycol methallyl ethers, 300g propoxy-end-blocking polyoxyethylene glycol allyl ethers, 50g methacrylic acid sulfonic acid, the mixing of 0.05g 3-sulfydryl ethyl sulfonic acid; In emulsifier solution, drip; Add the 80g Diisopropyl azodicarboxylate simultaneously; Polymerization 4 hours; After the end, sustained reaction 12 hours, cooling cooling; Regulate stoste pH value to alkalescence with NaOH behind the elimination residue, get nanoparticle subtype water reducer.
Test nanoparticle subtype water reducer size is 210nm, and dispersion index is 0.092.
Embodiment 4
In reaction kettle, add the 500g deionized water in advance.Be warming up to 80 ℃.10g methacrylic acid, 50g vinylbenzene, 40g butoxy end-blocking polyoxyethylene glycol 3-butene-1-alcohol ether, 30g methacrylic disulfonate acid are at the uniform velocity splashed into reaction kettle after mixing; Dropping time 3h; Dropwise 5 0gV-50 initiator; Initiator drips time 5h; Finish back insulation 3h; Lower the temperature and cool off, regulate stoste pH value to alkalescence with NaOH behind the elimination residue, get nanoparticle property water reducer.
Test nanoparticle subtype water reducer size is 253nm, and dispersion index is 0.078.
Embodiment 5
In reaction kettle, add the 50g deionized water in advance.Be warming up to 90 ℃.7g ammonium acrylate sodium, 200g vinylbenzene, 60g oxyethyl group end-blocking polyoxyethylene glycol polypropylene glycol allyl ethers, 20g methacrylic disulfonate acid are at the uniform velocity splashed into reaction kettle after mixing; Dropping time 4h; Drip dilauroyl peroxide 100g; Initiator drips time 6h; Finish back insulation 0.5h; Lower the temperature and cool off, regulate stoste pH value to alkalescence with NaOH behind the elimination residue, get nanoparticle property water reducer.
Test nanoparticle subtype water reducer size is 276nm, and dispersion index is 0.178.
Embodiment 6
In reaction kettle, add the 100g deionized water in advance.Be warming up to 50 ℃.40g vinylformic acid, 800g vinylbenzene, 500g butoxy end-blocking polyoxyethylene glycol allyl ethers, 20g methacrylic disulfonate acid, 10g mercaptosuccinic acid are at the uniform velocity splashed into reaction kettle after mixing; Dropping time 2h; Drip initiator ammonium persulfate 10g; Initiator drips time 4h; Finish back insulation 10h; Lower the temperature and cool off, regulate stoste pH value to alkalescence with NaOH behind the elimination residue, get nanoparticle property water reducer.
Test nanoparticle subtype water reducer size is 321nm, and dispersion index is 0.12.
The resulting product performance test result of embodiment 1-6 is following:
(1) flowing property test: GB/T8077-2000 " mixing earth admixture homogeneity testing method ".Adopt clean slurry degree of mobilization, reference cement.
Experimental result shows that nanoparticle subtype water reducer diminishing is excellent, under cement concrete workability and cement consumption permanence condition, can reduce the mixing water amount, and dispersion, water-reduction are provided.And mobile through the time loss change not quite, water-reduction preferably can both be provided in 2 hours, the flowing property test all is better than the commercial like product.
1) permeability resistance test: ASTM C1202 direct current measurement method
Experimental result shows that nanoparticle subtype water reducer can improve cement concrete impermeability, resistance of chloride ion penetration greatly.The commercial like product does not almost have modified effect to the cement concrete impermeability, and nanoparticle subtype water reducer effect is obvious.
Claims (8)
1. the preparation method of a nanoparticle subtype water reducer is characterized in that, carries out according to following steps:
A, with emulsifiers dissolve in deionized water, be warming up to 40～90 ℃, obtain clarifying emulsifier solution;
B, acrylic monomer, vinylbenzene, esters monomer, methacrylic disulfonate acid and chain-transfer agent mixed after; In emulsifier solution, drip; Add 1～30g initiator simultaneously; Polymerization 1～5 hour; After the end; Sustained reaction 1～12 hour, the cooling cooling is regulated stoste pH value to alkalescence with NaOH behind the elimination residue;
Perhaps,
A ' adds 5～500g deionized water in advance in reaction kettle, be warming up to 40-90 ℃;
B ' at the uniform velocity splashes into reaction kettle after acrylic monomer, vinylbenzene, esters monomer, methacrylic disulfonate acid and chain-transfer agent are mixed; Dropping time 1～5h; Drip 2～100g initiator; Initiator drips time 1～8h; Finish back insulation 0.5～12h; The cooling cooling is regulated stoste pH value to alkalescence with NaOH behind the elimination residue.
2. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1, it is characterized in that emulsifying agent that step a adds and deionized water ratio are (20～100g): (50～700ml).
3. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1; It is characterized in that the mass ratio of acrylic monomer that step b adds, vinylbenzene, esters monomer and methacrylic disulfonate acid is (1～50) g: (50～800) g: (5～600g): (1～50) g; The mass ratio of acrylic monomer that step b ' adds, vinylbenzene, esters monomer and methacrylic disulfonate acid is (1～50) g: (50～800) g: (5～600g): (1～50) g.
4. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1; It is characterized in that said emulsifying agent is selected from a kind of in alkyl-sulphate, fatty alcohol polyoxyethylene ether sulfate, aliphatic alcohol sulfate, lauryl diglycollic amide, dodecanamide propyl trimethyl-glycine, fatty alcohol-polyoxyethylene ether, fatty alcohol-polyoxyethylene ether succinate sodium sulfonate, dodecanamide propyl amine oxide, linear alkylbenzene sulfonate, polyoxyethylene sorbitan monolaurate, the Natvosol and more than one.
5. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1; It is characterized in that said acrylic monomer is selected from one or more in vinylformic acid, methacrylic acid, vinylformic acid ammonium salt, vinylformic acid monovalent metal salt, vinylformic acid divalent metal salt, methacrylic acid ammonium salt, methacrylic acid monovalent metal salt, the methacrylic acid divalent metal salt.
6. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1; It is characterized in that said esters monomer is selected from one or more in butoxy end-blocking polyoxyethylene glycol allyl ethers, methoxy-terminated polyoxyethylene glycol allyl ethers, butoxy end-blocking polyoxyethylene glycol methallyl ethers, propoxy-end-blocking polyoxyethylene glycol allyl ethers, butoxy end-blocking polyoxyethylene glycol 3-butene-1-alcohol ether, the oxyethyl group end-blocking polyoxyethylene glycol polypropylene glycol allyl ethers.
7. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1; It is characterized in that; Said chain-transfer agent is selected from one or more in thioglycerol, mercaptoethanol, Thiovanic acid, 2-Thiovanic acid, 3-Thiovanic acid, thiohydracrylic acid, mercaptosuccinic acid, Thiovanic acid monooctyl ester, 2-Thiovanic acid monooctyl ester, the 3-sulfydryl ethyl sulfonic acid, and add-on is 0～100g.
8. according to the preparation method of the said a kind of nanoparticle subtype water reducer of claim 1; It is characterized in that; Said initiator is a dibenzoyl peroxide, Potassium Persulphate, one or more in Sodium Persulfate, ammonium persulphate, Diisopropyl azodicarboxylate, V-50 initiator, the dilauroyl peroxide.
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Application publication date: 20120215 |