CN102849978A - Sustained-release polycarboxylic high-performance water reducing agent and preparation method thereof - Google Patents
Sustained-release polycarboxylic high-performance water reducing agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a sustained-release polycarboxylic high-performance water reducing agent and a preparation method thereof. The water reducing agent comprises: 0.13mol of monomer methyl alkenyl polyoxyethelene or allyl polyoxyethylene ether or polyoxypropylene ether, 0.32mol of monomer acrylic acid or methacrylic acid, 0.01mol of monomer sodium methallyl sulfonate, 0.12mol of monomer acrylamide or 2-acrylamide-methylpropanesulfonic acid, and 0.05mol of monomer ethyl acetate or styrene. Deionized water is adopted as a reaction medium, and the materials are subjected to a reaction with an initiating agent and a chain transfer agent for 4-6h with a maintained temperature of 58-62 DEG C. Copolymerization is carried out, such that a polymer with a molecular weight of 50000-120000 is obtained; the temperature is reduced to below 40 DEG C, and an alkali solution is added for regulating the pH of the system to 6-8, such that the water reducing agent is obtained. The sustained-release polycarboxylic high-performance water reducing agent provided by the invention has high water reduction rate. When an equivalent solid dosage is 0.2%, a water reduction rate can reach 35%. A slump performance is good. Concrete slump and extension degree have no loss in 3h. The water reducing agent is widely adaptable with concrete raw materials.
Description
Technical field
The present invention relates to a kind of cement water reducing agent and preparation method thereof, be specifically related to a kind of slow-release type polycarboxylate high-performance water reducing agent and preparation method thereof.
Background technology
Water reducer refers under concrete workability and cement consumption permanence condition, can reduce the mixing water amount, improve concrete strength; Or under workability and intensity permanence condition, save the admixture of cement consumption.
Continuous progress along with Building technology, large span, high level, high-rise building emerge in an endless stream, correspondingly, to the material of construction of consumption maximum---concrete has proposed requirements at the higher level, require concrete to satisfy the various performances such as high-strength, good workability, high-durability.For this reason, in the situation that water-binder ratio constantly reduces, still require concrete flowability to satisfy the requirement of pumping construction.This just requires water reducer except having higher water-reducing effect, can also effectively control concrete slump-loss, solves better the problems such as concrete bleed, slow setting, bleeding.And traditional high efficiency water reducing agent (such as naphthalenesulfonate, melamine sulfonate, sulfamate etc.) is difficult to satisfy well these requirements at the higher level.
Poly carboxylic acid series water reducer is the novel water reducer that grew up in recent years.Have advantages of a lot of uniquenesses: from better consistency is arranged between the different cement relatively; Even when low-dosage, poly carboxylic acid series water reducer also can make concrete have high workability; And when low water-cement ratio, have low viscosity and good slump retention; The molecular structure degree of freedom is quite large, and the synthetic controllable parameter of admixture is many, and the potentiality of high performance are large, can carry out Molecular Structure Design to it, produce the admixture of " ideal ", solve better the problems such as diminishing, bleed, slow setting, bleeding.
In the prior art, on the one hand, along with the large-scale popularization of domestic polycarboxylate water-reducer is used, lot production producer emerges successively, overwhelming majority existence in these producers lacks qualified technical personnel, the scientific research insufficient investment, after in case production technique is determined, its polycarboxylate water-reducer product becomes standardized product substantially, meet water reducer can not meet the demands the time, usually adopt compounded technology to solve problem, can not adjust from the microcosmic angle of water reducer molecular structure, also just can't tackle the problem at its root.On the other hand; China still is in the large-scale basis Facilities Construction and urbanization process is carried forward vigorously the stage; the concrete raw materials is day by day complicated; adaptability problem between other starting material of water reducer and concrete seems particularly outstanding, often shows as that the water reducer water-reducing rate is inadequate, concrete slump loss is too fast, concrete mix segregation bleeding etc.
For this reason, in the urgent need to developing a kind of slow-release type polycarboxylate high-performance water reducing agent, to improve the water reducer performance, improve the adaptability between water reducer and other starting material of concrete, improve concrete slump retention.
Based on this, following several improving technology to polycarboxylate high performance water-reducing agent has appearred in the prior art:
Chinese patent CN201010119879.3 has introduced the gather materials control slow release polycarboxylate water reducing agent of silt content impact of a kind of inhibition, it is characterized in that the weight ratio of component is: poly carboxylic acid series water reducer 75-95 part, retardant 2-5 part, sustained release dosage 5-25 part.Microvoid structure is many because natural zeolite powder has, specific surface area is large, surface adsorption is strong, can be with natural zeolite powder as sustained release dosage.The present invention utilizes natural zeolite powder to make sustained release dosage, and after poly carboxylic acid series water reducer, retardant mixed, the natural zeolite powder particle surface can adsorb a large amount of poly carboxylic acid series water reducers and a small amount of retardant; Be incorporated in the concrete with gelling material, gather materials and after water stirs, the strong natural zeolite powder of clay meeting preferentially adsorbed surface adsorption, avoid polycarboxylate water-reducer by the clay excessive adsorption, thereby guaranteed poly carboxylic acid series water reducer in cement granules absorption and the performance dissemination.This kind method is only utilized the principle of preferentially adsorbed zeolite powder and can not be reached the purpose of controlling concrete slump loss from Molecular Structure Design.
Chinese patent CN200810045737.X has introduced a kind of sustained-release water reducing agent of cement concrete, it is characterized in that: by layered double hydroxide, and the cement concrete that is scattered in this layered double hydroxide forms with water reducer; Layered double-metal hydroxide is stratiform MgAl double-metal hydroxide or stratiform CaAl double-metal hydroxide, and described water reducer is naphthalene water reducer or poly carboxylic acid series water reducer; The preparation method of sustained-release water reducing agent comprises the steps such as preparation layered double hydroxide, preparation bimetallic oxide, preparation sustained-release water reducing agent.The present invention joins the product of roasting bimetallic oxide of layered double hydroxide in the solution that contains water reducer, and water reducer enters interlayer in the process that the stratiform structural remodeling occurs, and makes Powdered water reducer; During use, the admixture of water reducer with sustained release performance enters in the concrete, slowly discharges, and can effectively reduce concrete slump loss; Powdered sustained-release water reducing agent also can obviously reduce transportation cost.The method needs first preparation through the layered double hydroxide of roasting, complex process, and equipment investment is many, and the factor that affects quality product increases, and is unfavorable for suitability for industrialized production.
Chinese patent CN201010033828.9 has introduced a kind of preparation method of slow-release type polycarboxylate water reducer.This water reducer is that Soxylat A 25-7 or the large monomer of ester, (methyl) vinylformic acid, unsaturated sulfonic acid or its salt monomer a, monoolefin carboxylic acid derivative b, diolefin carboxylic acid derivative c and the water that will contain unsaturated double-bond join in the reactor, under the effect of initiator persulphate, 60～85 ℃ of lower reactions 1.0～6.0 hours; Then cool to 40～55 ℃, be neutralized to pH=6～8 with basic solution and make.The present invention introduces the poly carboxylic acid main chain with monoolefin carboxylic acid derivative b, diolefin carboxylic acid derivative c, makes the polycarboxylate water-reducer that makes have slow release effect to concrete flowability.Loss and the evaporation of the concrete moisture that causes under long-time transportation and the comparatively high temps have effectively been prevented.But when this kind sustained-release water reducing agent used under the summer high temperature condition, concrete slump loss was very fast, still can't satisfy the engineering construction requirement.
Chinese patent CN201110318536.4 has introduced a kind of high collapse protection type polycarboxylate water-reducer with slowly releasing effect and preparation method thereof.It is characterized in that: it can be by 5～30mol% monomer A, 30～60mol% monomers B, 20～55mol% monomer C is at initiator, 60～80 ℃ of insulation reaction 1～3h under chain-transfer agent and the stopper effect, it is 30000～100000 polymkeric substance that copolymerization obtains molecular weight, then adding the alkali neutralization forms, monomer A+B+C=100mol%, described monomer C is calculated in molar ratio as 1:20～13:20 and is formed by guarantor's auxiliary agent 1 and guarantor auxiliary agent 2 that collapses that collapses, monomer A is that polymerization degree n is 20～60 prenol Soxylat A 25-7, allyl polyglycol ether, 1-methyl-2-propenyl polyglycol ether or allyl group polypropylene glycol ether, monomers B are vinylformic acid or methacrylic acid.Its function of slump protection is excellent, and the slump is not lost substantially in the 3h.But this water reducer water-reducing rate is on the low side (when the solid volume of folding was 0.2%, water-reducing rate was lower than 30%), and the adaptability between the starting material such as cement, sandstone is not ideal enough.
Chinese patent CN201210056013.1 has introduced a kind of multi-branched polycarboxylic water reducer with function of slump protection and preparation method thereof.The invention discloses a kind of multi-branched polycarboxylic water reducer with function of slump protection, this polycarboxylate water-reducer is to carry out aqueous solution polymerization by following monomer under the effect of polymerization starter to form: monomer A accounts for 3～10% of total reactant weight; Monomers B accounts for 80～90% of total reactant weight; Monomer C accounts for 3～6% of reactant total reactant weight; Monomer D accounts for 0.5～2% of total reactant total amount; The deionized water of above-mentioned four kinds of monomer reactant gross weights 100～200% in addition again.The technical solution used in the present invention not only itself has the effect of collapsing of protecting preferably, mixes use with the polycarboxylate water-reducer of other classifications, can improve the function of slump protection of other products.But this water reducer water-reducing rate is on the low side (when the solid volume of folding was 0.2%, water-reducing rate was lower than 30%), and the diminishing function does not have slowly releasing effect, can't satisfy the engineering that the concrete slump retaining performance is had higher requirements.
Summary of the invention
Main purpose of the present invention provides a kind of slow-release type polycarboxylate high-performance water reducing agent and preparation method thereof, and this water reducer water-reducing property is excellent, and can slow down concrete slump loss.
For achieving the above object, the technical solution adopted in the present invention is: the technical solution adopted in the present invention is as follows:
A kind of slow-release type polycarboxylate high-performance water reducing agent is characterized in that: comprising:
0.13mol monomer A,
0.32mol monomers B,
0.01mol monomer C,
0.12mol monomer D,
0.05mol monomer E,
Take deionized water as reaction medium, with initiator, chain-transfer agent, insulation reaction 4～6h under 60 ± 2 ℃ of conditions, it is 50000～120000 polymkeric substance that copolymerization obtains molecular weight, then cools to below 40 ℃, adds liquid caustic soda regulation system pH value and both must 6～8;
The total consumption of described deionized water is 1.5 times of monomer total mass; Described initiator amount is 0.3～3% of reaction total monomer weight by weight, and the consumption of chain-transfer agent is 0.02～0.5% of reaction total monomer weight by weight;
Described monomer A is that the polymerization degree is 30～60 methyl thiazolinyl polyoxyethylene or allyl polyethenoxy ether or polyethenoxy ether;
Described monomers B is acrylic or methacrylic acid;
Described monomer C is methylpropene sodium sulfonate;
Described monomer D is acrylamide or 2-acrylamido-methyl propane sulfonic acid;
Described monomer E is ethyl acetate or vinylbenzene;
Described initiator is one or more mixing in Sodium Persulfate, Potassium Persulphate, the hydrogen peroxide;
Described chain-transfer agent is one or more mixing in Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid, mercaptoethanol, the sodium bisulfite;
Described liquid caustic soda is the aqueous solution of sodium hydroxide, potassium hydroxide, quadrol or trolamine.Namely commonly used any one or composite liquid caustic soda can.Be more preferably, described liquid caustic soda is that concentration is 40% sodium hydroxide solution, and raw material is easy to get, and is with low cost and result of use good.
The consumption of monomer is the optimum feed stock ratio that participates in reaction in the technique scheme, but the variation that those skilled in the art can instruction according to the present invention be equal to.For example: be equal to because the parameter that the error of industrial production itself causes changes with technical scheme of the present invention; Perhaps increase the consumption of other monomers for the utilization ratio that improves some monomer, and then carry out raw material and separate, but because must comprise the consumption that the present invention proposes, therefore also be equal to technical scheme of the present invention.
The preparation method of slow-release type polycarboxylate high-performance water reducing agent of the present invention may further comprise the steps:
A, partial monosomy B, monomer C, monomer D, monomer E are dissolved in the deionized water, stir, get the minor comonomer solution for later use;
B, chain-transfer agent is dissolved in the deionized water, stirs, get the chain-transfer agent solution for later use;
C, monomer A and deionized water are dropped into heating for dissolving in the reaction vessel, after monomer A is dissolved fully, the monomers B and the initiator that add surplus continue to stir and heat up, and treat that temperature rises to 60 ± 2 ℃, the beginning synchronous uniform velocity drips minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1～3h, and reaction is cooled to below 40 ℃ after finishing, add between liquid caustic soda regulation system pH value to 6～8, both.General finished product concentration is about 40%.
The amount of the amount of the monomers B that further, adds among the described step a and monomer C or monomer D or monomer E is suitable; Be more preferably suitable with the amount of monomer D.Its purpose mainly is to guarantee have monomers B acrylic or methacrylic acid also just to be arranged as main chain in the whole reaction process, causes new polyreaction, impels to react completely.
Further, the deionized water consumption among described step a, the b is to dissolve material fully as degree.Main like this is the dissolving of being convenient to follow-up monomer A and most of monomers B, saves the production time, enhances productivity.
Beneficial effect of the present invention: slow-release type polycarboxylate high-performance water reducing agent provided by the invention is to use the macromolecular structure principle of design, in aqueous medium, take acrylic or methacrylic acid as main chain, take the large monomer of unsaturated modified polyether as side chain, introduce novel unsaturated minor comonomer, optimize monomer ratio and reaction conditions, obtain having target molecular structure, the slow-release type polycarboxylate high-performance water reducing agent of functional group, molecular weight distribution.This water reducer water-reducing rate is high, and when the solid volume of folding was 0.2%, water-reducing rate can reach 35%; Function of slump protection is excellent, free of losses in concrete slump and the divergence 3h.And and has widely adaptability between concrete raw material.
Embodiment
For those skilled in the art are known and clear and definite technical scheme of the present invention more, the spy provides following preferred embodiment, but technological thought of the present invention is not limited to following examples.
Embodiment one
Be 30～60 methyl thiazolinyl polyoxyethylene 0.13mol monomer A is the polymerization degree;
0.32mol monomers B is vinylformic acid;
0.01mol monomer C is methylpropene sodium sulfonate;
0.12mol monomer D is acrylamide;
0.05mol monomer E is ethyl acetate;
Initiator is that sodium sulfate, Potassium Persulphate are by the mixture of 1:1;
Chain-transfer agent is Thiovanic acid;
Preparation process:
A, with monomer C, monomer D, monomer E, be dissolved in the deionized water with the monomers B of monomer D equimolar amount, stir, get the minor comonomer solution for later use;
B, chain-transfer agent is dissolved in the deionized water, stirs, get the chain-transfer agent solution for later use; The consumption of chain-transfer agent is 0.05% of reaction total monomer weight by weight;
C, monomer A and deionized water are dropped into heating for dissolving in the reaction vessel, after monomer A is dissolved fully, the monomers B and the initiator that add surplus, described initiator amount is 0.5% of reaction total monomer weight by weight, continue to stir and heat up, treat that temperature rises to 60 ± 2 ℃, the beginning synchronous uniform velocity drips minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 2h, and reaction is cooled to below 40 ℃ after finishing, add concentration and be between 40% sodium hydroxide solution regulation system pH value to 6～8, discharging, obtaining molecular weight is 80000～100000, the product of solid content 40%.
The total consumption of deionized water is 1.5 times of monomer total mass in three steps.
Embodiment two
0.13mol monomer A is the polymerization degree is 30～60 allyl polyethenoxy ether;
0.32mol monomers B is methacrylic acid;
0.01mol monomer C is methylpropene sodium sulfonate;
0.12mol monomer D is 2-acrylamido-methyl propane sulfonic acid;
0.05mol monomer E is vinylbenzene;
Initiator is hydrogen peroxide;
Chain-transfer agent is the mixture that Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid mix by 1:1:1;
Preparation process:
A, with monomer C, monomer D, monomer E, be dissolved in the deionized water with the monomers B of monomer D equimolar amount, stir, get the minor comonomer solution for later use;
B, chain-transfer agent is dissolved in the deionized water, stirs, get the chain-transfer agent solution for later use; The consumption of chain-transfer agent is 0.2% of reaction total monomer weight by weight;
C, monomer A and deionized water are dropped into heating for dissolving in the reaction vessel, after monomer A is dissolved fully, the monomers B and the initiator that add surplus, described initiator amount is 1% of reaction total monomer weight by weight, continue to stir and heat up, treat that temperature rises to 60 ± 2 ℃, the beginning synchronous uniform velocity drips minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1.5h, and reaction is cooled to below 40 ℃ after finishing, add concentration and be between 40% sodium hydroxide solution regulation system pH value to 6～8, discharging, obtaining molecular weight is 60000～100000, the product of solid content 40%.
The total consumption of deionized water is 1.5 times of monomer total mass in three steps.
Embodiment three
0.13mol monomer A is the polymerization degree is 30～60 polyethenoxy ether;
0.32mol monomers B is vinylformic acid;
0.01mol monomer C is methylpropene sodium sulfonate;
0.12mol monomer D is acrylamide;
0.05mol monomer E is ethyl acetate;
Initiator is that sodium sulfate, hydrogen peroxide are by the mixture of 2:1;
Chain-transfer agent is sodium bisulfite;
Preparation process:
A, with monomer C, monomer D, monomer E, be dissolved in the deionized water with the monomers B of monomer D equimolar amount, stir, get the minor comonomer solution for later use;
B, chain-transfer agent is dissolved in the deionized water, stirs, get the chain-transfer agent solution for later use; The consumption of chain-transfer agent is 0.4% of reaction total monomer weight by weight;
C, monomer A and deionized water are dropped into heating for dissolving in the reaction vessel, after monomer A is dissolved fully, the monomers B and the initiator that add surplus, described initiator amount is 2% of reaction total monomer weight by weight, continue to stir and heat up, treat that temperature rises to 60 ± 2 ℃, the beginning synchronous uniform velocity drips minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 3h, and reaction is cooled to below 40 ℃ after finishing, add concentration and be between 40% sodium hydroxide solution regulation system pH value to 6～8, discharging, obtaining molecular weight is 60000～80000, the product of solid content 41%.
The total consumption of deionized water is 1.5 times of monomer total mass in three steps.
Wherein the product of embodiment 1 (solid content: 40%) to carry out the test situation of performance comparison as follows with currently available products:
The currently available products source: the JJPC-C type polycarboxylate high performance water-reducing agent mother liquor that the strong outstanding Science and Technology Ltd. in Chongqing produces (solid content: 40%), with sample 1 expression.
1, water-reducing rate simultaneous test
(GB8076-2008) test by " concrete admixture ".
Concrete match ratio is the water-reducing rate result when:
2, function of slump protection test
Concrete mix:
Concrete work performance experimental result:
As seen, product of the present invention has the water-reducing rate higher than currently available products, and when the solid volume of folding was 0.2%, water-reducing rate surpassed 35%; Have more excellent function of slump protection: under the prerequisite of composite other retardant not, when the solid volume of folding is 0.2%, the interior free of losses of concrete slump and divergence 3h.
Claims (7)
1. slow-release type polycarboxylate high-performance water reducing agent is characterized in that: comprising:
0.13mol monomer A,
0.32mol monomers B,
0.01mol monomer C,
0.12mol monomer D,
0.05mol monomer E,
Take deionized water as reaction medium, with initiator, chain-transfer agent, insulation reaction 4～6h under 60 ± 2 ℃ of conditions, it is 50000～120000 polymkeric substance that copolymerization obtains molecular weight, then cools to below 40 ℃, adds liquid caustic soda regulation system pH value and both must 6～8;
The total consumption of described deionized water is 1.5 times of monomer total mass; Described initiator amount is 0.3～3% of reaction total monomer weight by weight, and the consumption of chain-transfer agent is 0.02～0.5% of reaction total monomer weight by weight;
Described monomer A is that the polymerization degree is 30～60 methyl thiazolinyl polyoxyethylene or allyl polyethenoxy ether or polyethenoxy ether;
Described monomers B is acrylic or methacrylic acid;
Described monomer C is methylpropene sodium sulfonate;
Described monomer D is acrylamide or 2-acrylamido-methyl propane sulfonic acid;
Described monomer E is ethyl acetate or vinylbenzene;
Described initiator is one or more mixing in Sodium Persulfate, Potassium Persulphate, the hydrogen peroxide;
Described chain-transfer agent is one or more mixing in Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid, mercaptoethanol, the sodium bisulfite.
2. a kind of slow-release type polycarboxylate high-performance water reducing agent according to claim 1, it is characterized in that: described liquid caustic soda is the aqueous solution of sodium hydroxide, potassium hydroxide, quadrol or trolamine.
3. a kind of slow-release type polycarboxylate high-performance water reducing agent according to claim 2, it is characterized in that: described liquid caustic soda is that concentration is 40% sodium hydroxide solution.
4. the preparation method of slow-release type polycarboxylate high-performance water reducing agent according to claim 1 may further comprise the steps:
A, partial monosomy B, monomer C, monomer D, monomer E are dissolved in the deionized water, stir, get the minor comonomer solution for later use;
B, chain-transfer agent is dissolved in the deionized water, stirs, get the chain-transfer agent solution for later use;
C, monomer A and deionized water are dropped into heating for dissolving in the reaction vessel, after monomer A is dissolved fully, the monomers B and the initiator that add surplus continue to stir and heat up, and treat that temperature rises to 60 ± 2 ℃, the beginning synchronous uniform velocity drips minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1～3h, and reaction is cooled to below 40 ℃ after finishing, add between liquid caustic soda regulation system pH value to 6～8, both.
5. the preparation method of slow-release type polycarboxylate high-performance water reducing agent according to claim 4, it is characterized in that: the amount of the amount of the monomers B that adds among the described step a and monomer C or monomer D or monomer E is suitable.
6. the preparation method of slow-release type polycarboxylate high-performance water reducing agent according to claim 4, it is characterized in that: the amount of the amount of the monomers B that adds among the described step a and monomer D is suitable.
7. the preparation method of slow-release type polycarboxylate high-performance water reducing agent according to claim 4, it is characterized in that: the deionized water consumption among described step a, the b is to dissolve material fully as degree.
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