CN102849978B - Sustained-release polycarboxylic high-performance water reducing agent and preparation method thereof - Google Patents
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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 polycarboxylate-typehigh-performance high-performance water reducer and preparation method thereof.
Background technology
Water reducer refers under concrete workability and cement consumption permanence condition, can reduce mixing water amount, improve concrete strength; Or under workability and intensity permanence condition, save the admixture of cement consumption.
Along with the continuous progress of Building technology, large span, high level, high-rise building emerge in an endless stream, correspondingly, the material of construction maximum to consumption---concrete proposes requirements at the higher level, requires that concrete meets the various performances such as high-strength, excellent workability, high-durability.For this reason, when water-binder ratio constantly reduces, still require that concrete mobility meets the requirement of pumping construction.This just requires water reducer except having higher water-reducing effect, can also effectively control concrete slump-loss, solve the problems such as concrete bleed, slow setting, bleeding better.And traditional high efficiency water reducing agent (as naphthalenesulfonate, melamine sulfonate, sulfamate etc.) is difficult to meet these requirements at the higher level well.
Poly carboxylic acid series water reducer is the novel water reducer grown up in recent years.There is a lot of unique advantages: from have relatively better consistency between different cement; Even if when low-dosage, poly carboxylic acid series water reducer also can make concrete have high workability; And there is when low water-cement ratio low viscosity and good slump retention performance; Molecular structure degree of freedom is quite large, and the upper controllable parameter of admixture synthesis is many, and the potentiality of high performance are large, can carry out Molecular Structure Design, produce the admixture of " ideal ", solve the problems such as diminishing, bleed, slow setting, bleeding better to it.
In prior art, on the one hand, along with the large-scale popularization of domestic polycarboxylate water-reducer is applied, lot production producer emerges successively, overwhelming majority existence in these producers lacks qualified technical personnel, science research input is not enough, once after production technique determines, its polycarboxylate water-reducer product becomes standardized product substantially, meet water reducer when can not meet the demands, usual employing compounded technology solves problem, can not adjust, also just cannot tackle the problem at its root from the microcosmic angle of water reducer molecular structure.On the other hand; China is still in large-scale basis Facilities Construction and urbanization process carries forward vigorously the stage; concrete raw materials is day by day complicated; adaptability problem between water reducer and other starting material of concrete seems particularly outstanding, often shows as that 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 polycarboxylate-typehigh-performance high-performance water reducer, improving water reducer performance, improving the adaptability between water reducer and other starting material of concrete, improving concrete slump retention performance.
Based on this, in prior art, there is following several improving technology to polycarboxylate high performance water-reducing agent:
Chinese patent CN201010119879.3 describe a kind of suppression gather materials silt content impact control slow release polycarboxylate water reducing agent, 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.Because natural zeolite powder has, microvoid structure is many, specific surface area large, surface adsorption is strong, natural zeolite powder can be used as sustained release dosage.The present invention utilizes natural zeolite powder to make sustained release dosage, and after mixing with poly carboxylic acid series water reducer, retardant, natural zeolite powder particle surface can adsorb a large amount of poly carboxylic acid series water reducers and a small amount of retardant; To be incorporated in concrete with gelling material, to gather materials and after water stirs, the natural zeolite powder that clay meeting Preferential adsorption surface adsorption is strong, avoid polycarboxylate water-reducer by clay excessive adsorption, thus ensure that poly carboxylic acid series water reducer adsorbs and plays dissemination on cement granules.This kind of method only utilizes the principle of Preferential adsorption zeolite powder and can not reach from Molecular Structure Design the object controlling concrete slump loss.
Chinese patent CN200810045737.X describes a kind of sustained-release water reducing agent of cement concrete, it is characterized in that: by layered double hydroxide, and the cement concrete water reducer be scattered in this layered double hydroxide forms; 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 and prepares layered double hydroxide, prepares bimetallic oxide, prepares the steps such as sustained-release water reducing agent.The product of roasting bimetallic oxide of layered double hydroxide joins in the solution containing water reducer by the present invention, and in the process that stratiform structural remodeling occurs, water reducer enters interlayer, obtained Powdered water reducer; During use, a water reducer admixture with sustained release performance enters in concrete, and slow releasing, effectively can reduce concrete slump loss; Powdered sustained-release water reducing agent also obviously can reduce transportation cost.The method needs first to prepare the layered double hydroxide through roasting, complex process, and equipment investment is many, and the factor affecting quality product increases, and is unfavorable for suitability for industrialized production.
Chinese patent CN201010033828.9 describes a kind of preparation method of slow-release type polycarboxylate water reducer.This water reducer joins in reactor by the Soxylat A 25-7 containing unsaturated double-bond or ester polymeric monomer, (methyl) vinylformic acid, unsaturated sulfonic acid or its salt monomer a, monoolefin carboxylic acid derivative b, diolefin carboxylic acid derivative c and water, under the effect of initiator persulphate, react 1.0 ~ 6.0 hours at 60 ~ 85 DEG C; Then cool to 40 ~ 55 DEG C, be neutralized to pH=6 ~ 8 with basic solution and obtain.Monoolefin carboxylic acid derivative b, diolefin carboxylic acid derivative c are introduced poly carboxylic acid main chain by the present invention, make the polycarboxylate water-reducer obtained have slow release effect to concrete mobility.The loss of the concrete moisture caused under effectively prevent long-time transport and comparatively high temps and evaporation.But when this kind of sustained-release water reducing agent uses under summer high temperature condition, concrete slump loss is very fast, still cannot meet engineering construction requirement.
Chinese patent CN201110318536.4 describes 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 by 5 ~ 30mol% monomer A, 30 ~ 60mol% monomers B, 20 ~ 55mol% monomer C is at initiator, 60 ~ 80 DEG C of insulation reaction 1 ~ 3h under chain-transfer agent and stopper effect, copolymerization obtains the polymkeric substance that molecular weight is 30000 ~ 100000, then add alkali neutralization to form, monomer A+B+C=100mol%, described monomer C is calculated in molar ratio as 1:20 ~ 13:20 is formed by guarantor's auxiliary agent 1 and guarantor auxiliary agent 2 that collapses that collapses, monomer A to be polymerization degree n be 20 ~ 60 isopentenol polyoxyethylene ether, allyl polyglycol ether, 1-methyl-2-propenyl polyglycol ether or allyl group polypropylene glycol ether, monomers B is vinylformic acid or methacrylic acid.Its function of slump protection is excellent, and in 3h, the slump is not lost substantially.But this water reducer water-reducing rate is on the low side (when the solid volume of folding is 0.2%, water-reducing rate is lower than 30%), and adaptability between the starting material such as cement, sandstone is not ideal enough.
Chinese patent CN201210056013.1 describes 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 under the effect of polymerization starter, carries out aqueous solution polymerization by following monomer 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 protects the effect of collapsing preferably, used in combination 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 is 0.2%, water-reducing rate is lower than 30%), and diminishing function does not have slowly releasing effect, cannot meet the engineering had higher requirements to concrete slump retaining performance.
Summary of the invention
Main purpose of the present invention is to provide a kind of Slow release polycarboxylate-typehigh-performance high-performance water reducer 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 polycarboxylate-typehigh-performance high-performance water reducer, 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 DEG C of conditions, copolymerization obtains the polymkeric substance that molecular weight is 50000 ~ 120000, then cools to less than 40 DEG C, adds liquid caustic soda regulation system pH value and has both obtained 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 to be the polymerization degree be 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 propanesulfonic acid;
Described monomer E is ethyl acetate or vinylbenzene;
Described initiator is one or more mixing in Sodium Persulfate, Potassium Persulphate, hydrogen peroxide;
Described chain-transfer agent is one or more mixing in Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid, mercaptoethanol, sodium bisulfite;
Described liquid caustic soda is the aqueous solution of sodium hydroxide, potassium hydroxide, quadrol or trolamine.Namely conventional any one or composite liquid caustic soda can.Be more preferably, described liquid caustic soda to be concentration be 40% sodium hydroxide solution, raw material is easy to get, with low cost and result of use good.
In technique scheme, the consumption of monomer is the optimum feed stock ratio participating in reaction, but those skilled in the art can carry out according to instruction of the present invention the change that is equal to.Such as: because the Parameters variation that the error of industrial production itself causes is equal to technical scheme of the present invention; Or in order to the utilization ratio improving some monomer increases the consumption of other monomers, and then carry out raw material separation, but because the consumption of the present invention's proposition must be comprised, therefore be also equal to technical scheme of the present invention.
The preparation method of Slow release polycarboxylate-typehigh-performance high-performance water reducer of the present invention, comprises the following steps:
A, partial monosomy B, monomer C, monomer D, monomer E are dissolved in deionized water, stir, obtain minor comonomer solution for later use;
B, chain-transfer agent is dissolved in deionized water, stirs, obtain chain-transfer agent solution for later use;
C, monomer A and deionized water are dropped into heating for dissolving in reaction vessel, after monomer A is dissolved completely, add monomers B and the initiator of surplus, continue to stir and heat up, treat that temperature rises to 60 ± 2 DEG C, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1 ~ 3h, is cooled to less than 40 DEG C after reaction terminates, add between liquid caustic soda regulation system pH value to 6 ~ 8, both.General finished product concentration is about 40%.
Further, the amount of the monomers B added in described step a is suitable with the amount of monomer C or monomer D or monomer E; Be more preferably suitable with the amount of monomer D.Its object mainly ensures have monomers B also just to have acrylic or methacrylic acid as main chain in whole reaction process, causes new polyreaction, impels and react completely.
Further, the deionized water consumption in described step a, b is to dissolve material completely for degree.So mainly be convenient to the dissolving of follow-up monomer A and most of monomers B, save the production time, enhance productivity.
Beneficial effect of the present invention: Slow release polycarboxylate-typehigh-performance high-performance water reducer provided by the invention uses macromolecular structure principle of design, in aqueous medium, with acrylic or methacrylic acid for main chain, with unsaturated modified polyether polymeric monomer for side chain, introduce novel unsaturated minor comonomer, optimize monomer ratio and reaction conditions, obtain the Slow release polycarboxylate-typehigh-performance high-performance water reducer with target molecular structure, functional group, molecular weight distribution.This water reducer water-reducing rate is high, and when the solid volume of folding is 0.2%, water-reducing rate can reach 35%; Function of slump protection is excellent, free of losses in concrete slump and divergence 3h.And and there is between concrete raw material adaptability widely.
Embodiment
For making those skilled in the art clearly and technical scheme clearly of the present invention, spy provides preferred embodiment below, but technological thought of the present invention is not limited to following examples.
Embodiment one
0.13mol monomer A to be the polymerization degree be 30 ~ 60 methyl thiazolinyl polyoxyethylene;
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, by monomer C, monomer D, monomer E, be dissolved in deionized water with the monomers B of monomer D equimolar amount, stir, obtain minor comonomer solution for later use;
B, chain-transfer agent is dissolved in deionized water, stirs, obtain 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 reaction vessel, after monomer A is dissolved completely, add monomers B and the initiator of 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 DEG C, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, then insulation reaction 2h is continued, less than 40 DEG C are cooled to after reaction terminates, adding concentration is between sodium hydroxide solution regulation system pH value to 6 ~ 8 of 40%, discharging, obtaining molecular weight is 80000 ~ 100000, the product of solid content 40%.
In three steps, the total consumption of deionized water is 1.5 times of monomer total mass.
Embodiment two
0.13mol monomer A to be the polymerization degree be 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 propanesulfonic acid;
0.05mol monomer E is vinylbenzene;
Initiator is hydrogen peroxide;
The mixture that chain-transfer agent is Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid mix by 1:1:1;
Preparation process:
A, by monomer C, monomer D, monomer E, be dissolved in deionized water with the monomers B of monomer D equimolar amount, stir, obtain minor comonomer solution for later use;
B, chain-transfer agent is dissolved in deionized water, stirs, obtain 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 reaction vessel, after monomer A is dissolved completely, add monomers B and the initiator of 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 DEG C, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, then insulation reaction 1.5h is continued, less than 40 DEG C are cooled to after reaction terminates, adding concentration is between sodium hydroxide solution regulation system pH value to 6 ~ 8 of 40%, discharging, obtaining molecular weight is 60000 ~ 100000, the product of solid content 40%.
In three steps, the total consumption of deionized water is 1.5 times of monomer total mass.
Embodiment three
0.13mol monomer A to be the polymerization degree be 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, by monomer C, monomer D, monomer E, be dissolved in deionized water with the monomers B of monomer D equimolar amount, stir, obtain minor comonomer solution for later use;
B, chain-transfer agent is dissolved in deionized water, stirs, obtain 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 reaction vessel, after monomer A is dissolved completely, add monomers B and the initiator of 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 DEG C, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, then insulation reaction 3h is continued, less than 40 DEG C are cooled to after reaction terminates, adding concentration is between sodium hydroxide solution regulation system pH value to 6 ~ 8 of 40%, discharging, obtaining molecular weight is 60000 ~ 80000, the product of solid content 41%.
In three steps, the total consumption of deionized water is 1.5 times of monomer total mass.
Wherein embodiment 1 product (solid content: 40%) carry out the test situation of performance comparison with currently available products as follows:
Currently available products is originated: (solid content: 40%) represents with sample 1 the JJPC-C type polycarboxylate high performance water-reducing agent mother liquor that Chongqing Jian Jie Science and Technology Ltd. produces.
1, water-reducing rate simultaneous test
Test by " concrete admixture " (GB8076-2008).
Concrete match ratio is water-reducing rate result when:
2, function of slump protection test
Concrete mix:
Concrete work performance experimental result:
Visible, product of the present invention has the water-reducing rate higher than currently available products, and when the solid volume of folding is 0.2%, water-reducing rate is more than 35%; There is more excellent function of slump protection: under the prerequisite of other retardant not composite, when the solid volume of folding is 0.2%, free of losses in concrete slump and divergence 3h.
Claims (5)
1. a Slow release polycarboxylate-typehigh-performance high-performance water reducer, is characterized in that: by:
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 DEG C of conditions, copolymerization obtains the polymkeric substance that molecular weight is 50000 ~ 120000, then cools to less than 40 DEG C, adds liquid caustic soda regulation system pH value 6 ~ 8 and get final product;
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 to be the polymerization degree be 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 propanesulfonic acid;
Described monomer E is ethyl acetate or vinylbenzene;
Described initiator is one or more mixing in Sodium Persulfate, Potassium Persulphate, hydrogen peroxide;
Described chain-transfer agent is one or more mixing in Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid, mercaptoethanol, sodium bisulfite;
Concrete preparation process:
A, partial monosomy B, monomer C, monomer D, monomer E are dissolved in deionized water, stir, obtain minor comonomer solution for later use;
B, chain-transfer agent is dissolved in deionized water, stirs, obtain chain-transfer agent solution for later use;
C, monomer A and deionized water are dropped into heating for dissolving in reaction vessel, after monomer A is dissolved completely, add monomers B and the initiator of surplus, continue to stir and heat up, treat that temperature rises to 60 ± 2 DEG C, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1 ~ 3h, is cooled to less than 40 DEG C after reaction terminates, add between liquid caustic soda regulation system pH value to 6 ~ 8, both.
2. a kind of Slow release polycarboxylate-typehigh-performance high-performance water reducer according to claim 1, is characterized in that: described liquid caustic soda is the aqueous solution of sodium hydroxide, potassium hydroxide, quadrol or trolamine.
3. Slow release polycarboxylate-typehigh-performance high-performance water reducer according to claim 1, is characterized in that: the amount of the monomers B added in described step a is suitable with the amount of monomer C or monomer D or monomer E.
4. Slow release polycarboxylate-typehigh-performance high-performance water reducer according to claim 1, is characterized in that: the amount of the monomers B added in described step a is suitable with the amount of monomer D.
5. Slow release polycarboxylate-typehigh-performance high-performance water reducer according to claim 1, is characterized in that: the deionized water consumption in described step a, b is to dissolve material completely for degree.
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| CN102849978A (en) | 2013-01-02 |
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