CN102765899B - Low air leading reducing type polycarboxylic acid concrete water reducer and preparation method thereof - Google Patents
Low air leading reducing type polycarboxylic acid concrete water reducer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low air leading reducing type polycarboxylic acid concrete water reducer and a preparation method thereof. The water reducer is formed by a single body A and a single body B in copolymerization according to the molar ratio of 1:3-3.5. The single body A is modified polyether TPEG, and the single body B is one or several of crylic acid, methyl acrylate, acrylamide, methacrylic acid, methyl methacrylate and methacrylamide. The preparation method includes first adding H2O2 into modified polyether TPEG water solution under the temperature of 50-55 DEG C, stirring the mixture for 10-15min, simultaneously dropping mixed water solution of ascorbic acid and a chain transfer agent and single body B solution respectively and continuously conducting reaction for 0.5-1.0 hour in heat insulation mode after dropping is finished to obtain the polycarboxylic acid water reducer after pH value adjustment. The water reducer has higher water reducing rate, has low air content and a certain reducing function if used for concrete and is the multifunctional high-efficiency water reducer integrating water reducing, reducing and low air leading.
Description
Technical field
The invention belongs to polycarboxylic acid concrete water reducer field, specifically, relate to a kind of low bleed shrinkage type polycarboxylic acid concrete water reducer and preparation method thereof.
Background technology
The cracking that concrete causes because of contraction can cause concrete intensity and weather resistance to be had a greatly reduced quality, thereby further shortens concrete work-ing life.The concrete especially shrinkage cracking problem of high performance concrete has caused the great attention of engineering circles, though polycarboxylate water-reducer has reduced concrete contraction to a certain extent, but still be difficult to meet the demand of engineering, the high air content of polycarboxylate water-reducer has also had a strong impact on concrete intensity simultaneously, and the air content that therefore reduces concrete contraction and reduction polycarboxylate water-reducer is current urgent problem.
At present, people mainly control by following several measures or reduce concrete early-age shrinkage cracking: (1) is coordinated recently and reduced and shrink by complex optimum; (2) mix economization agent, fiber or swelling agent and improve the plastic shrinkage of concrete plastic shrinkage resistance to cleavage or compensating concrete; (3) thus by sprayed surface curing agent or early moist curing reduce concrete surface water evaporates speed reduce plastic shrinkage.The synthetic economization agent of current domestic research mainly contains: the NA-SP series concrete economization agent taking polyol as main component; Alkyl polyoxyethylene ether is the JM-SRA series concrete economization agent that reduces composition; The effective constituent of Metallurgical Research Institute, Department of Architecture development is polyethers and the organic JSJ type of aliphatic category economization agent; And the ZZD-A type economization agent of the institute of civil engineering of Zhejiang University development, its main component is methyl ether based polyalcohol and ethylene glycol based polymer.Though the use of these economization agents has reduced concrete contraction to a certain extent, engineering cost increases greatly, and synthesis technique complexity.
For the high problem of polycarboxylate water-reducer air content, mainly by adding a certain amount of defoamer to solve as siloxane polymer, though defoamer can significantly reduce the air content of polycarboxylate water-reducer, but exist the problem of consistency difficulty, along with the prolongation of storage period, composite defoamer in polycarboxylate water-reducer can be separated out with the form of oil droplet, though introduce froth breaking group and do not exist the problem of consistency in polycarboxylate water-reducer building-up process, but expensive, and froth breaking ability declines compared with composite.
Summary of the invention
The object of the invention is to provide a kind of and integrates diminishing, reduces, the polycarboxylic acid concrete water reducer of low bleed.
The present invention also provides the preparation method of above-mentioned low bleed shrinkage type polycarboxylic acid concrete water reducer.
The low bleed shrinkage type of one of the present invention polycarboxylic acid concrete water reducer, is formed by 1:3 ~ 3.5 copolymerization in molar ratio of monomer A, monomers B, wherein:
Monomer A is modified polyether TPEG;
Monomers B is the mixture of any one or a few arbitrary proportion in vinylformic acid, methyl acrylate, acrylamide, methacrylic acid, methyl methacrylate, Methacrylamide.
Wherein,
Described modified polyether TPEG molecular-weight average is 2400.
Also be added with " H
2o
2-xitix " oxidation-reduction initiator, wherein, H
2o
2consumption is 0.35 ~ 0.45% of monomer total mass, and xitix is 0.10 ~ 0.16% of monomer total mass.
Also be added with chain-transfer agent, described chain-transfer agent is the mixture of one or both arbitrary proportions in sodium allyl sulfonate, methallylsulfonic acid sodium, Thiovanic acid, thiohydracrylic acid, and its consumption is 0.17 ~ 0.22% of monomer total mass.
Preparation method comprises step:
1) modified polyether TPEG is added to the water to stirring and dissolving, heats up and remain on 50 ~ 55 DEG C;
2) in the solution obtaining to step 1), add initiator H
2o
2, stir 10 ~ 15min;
3) to step 2) drip respectively xitix, chain-transfer agent mixed aqueous solution and the monomers B aqueous solution in the solution that obtains simultaneously;
4) dropwise and under said temperature, be incubated polymerase 10 .5 ~ 1.0h, be then cooled to 25 ~ 30 DEG C;
5) with alkaline solution regulator solution pH value to 6.0 ~ 8.0, obtain polycarboxylate water-reducer.
Wherein:
Described step 1) strength of solution is 65 ~ 70%.
In described step 3), initiator, chain-transfer agent mixed aqueous solution time for adding are 2.5 ~ 3.0h.
In described step 3), monomers B aqueous solution time for adding is 2.0 ~ 2.5h.
In described step 4), after polyreaction, mending and adding water to solid content is 38 ~ 42%.
Described alkaline solution is 47% sodium hydroxide solution.
The using method of polycarboxylic acid concrete water reducer prepared by the present invention is: in clean slurry, this water reducer volume is cement quality 0.35% ~ 0.40%, and in concrete, this water reducer incorporation is 0.6% ~ 1.0% of gelling material weight.
The present invention is by the relation between low bleed shrinkage type polycarboxylate water-reducer molecular structure and its application performance, ensureing that under the serviceability condition that low bleed shrinkage type polycarboxylate water-reducer is good, the raw molecule structure of selection contains can reduce or reduce the air content of polycarboxylate water-reducer and the large monomer of capillary group.Under the effect of initiator, in the aqueous solution, carry out polyreaction.It is high except having water-reducing rate, and protect plasticity is good, and flowing degree of net paste of cement is large, through time flowing degree of net paste of cement loss little outside, also have advantages of that air content and surface tension are low, concrete works is had to larger benefit.Low bleed, low surface tension polycarboxylate water-reducer can effectively increase concrete intensity and reduce shrinkage cracking, be a kind ofly integrate diminishing, reduce, the multi-functional polycarboxylate water-reducer of low gas content amount, have water-reducing rate high, adapt to strong, intensity advantages of higher.
Embodiment
For a better understanding of the present invention, illustrate content of the present invention, but protection scope of the present invention is not limited to this below in conjunction with embodiment, the following stated umber is weight part.
Embodiment 1
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 87 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 50 DEG C, add 0.93 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and acrylic acid solution, wherein, consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.35 part, the Thiovanic acid of 0.45 part and 65 parts, time for adding is 2.5h; Vinylformic acid 0.28mol(20 part), time for adding is 2.0h.Dropwise at 50 DEG C and continue insulation reaction 1.0h, then add 167 parts of water, be cooled to 30 DEG C, add 47% sodium hydroxide solution adjusting pH value to 7.0.
Embodiment 2
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 87 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 55 DEG C, add 0.80 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and methacrylic acid, wherein: the consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.35 part, the thiohydracrylic acid of 0.40 part and 65 parts, time for adding is 2.5h; Methacrylic acid 0.297mol(25.6 part), time for adding is 2.0h.Dropwise at 55 DEG C and continue insulation reaction 1.0h, then add 177 parts of water, be cooled to 30 DEG C, add 47% sodium hydroxide solution adjusting pH value to 6.5.
Embodiment 3
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 110 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 52 DEG C, add 0.79 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and monomers B solution, wherein: the consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.23 part, the Thiovanic acid of 0.41 part and 65 parts, time for adding is 3.0h; Consisting of of monomers B solution: 0.24mol(17 part) acrylamide (5.7 parts of acrylamide solns that massfraction is 50%) of vinylformic acid and 0.04mol, time for adding is 2.5h.Dropwise at 52 DEG C and continue insulation reaction 1.0h, then add 145 parts of water, be cooled to 25 DEG C, add 47% sodium hydroxide solution adjusting pH value to 7.5.
Embodiment 4
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 87 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 54 DEG C, add 0.93 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and vinylformic acid, wherein: the consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.35 part, the methylpropene sodium sulfonate of 0.45 part and 65 parts, time for adding is 3.0h; Vinylformic acid 0.28mol(20 part), time for adding is 2.5h.Dropwise at 54 DEG C and continue insulation reaction 1.0h, then add 167 parts of water, be cooled to 30 DEG C, add 47% sodium hydroxide solution adjusting pH value to 7.0.
Water reducer prepared by above four embodiment is labeled as respectively #1, #2, #3, #4 in order, below the performance of four kinds of water reducers is analyzed.
One, only starch simultaneous test:
Select mountain aluminium cement PO-42.5 600g, water 174g, the concentration of water reducer is that 40%, 5 kind of water reducer volume is 2.1g, experimental result is in table 1:
Under table 1 different condition, make low bleed shrinkage type polycarboxylate water-reducer and only starch degree of mobilization contrast
Two, the capillary relation of water reducer surface tension and synthon:
For further studying synthetic large monomer to the capillary impact of water reducer, experiment is by water reducer pure water synthetic different material and saturated Ca (OH)
2surface tension in solution compares, and the results are shown in Table 2.
Table 2 surface tension experiment table
The saturated Ca (OH) of same concentrations
2in solution, in the existing polycarboxylate water-reducer of our company, the PCA-2 surface tension of ester class is lower than the PCA-1 of ethers, the surface tension of synthetic low bleed shrinkage type polycarboxylate water-reducer 1#, 2#, 3#, 4# is all lower than the existing PCA-1 of company and PCA-2, reduced rate reaches as high as 35.93%, and therefore the surface tension of synthon is larger on the capillary impact of water reducer.
Three, concrete reducing experiment:
Concrete shrinkage and intensity concrete shrinkage sample dimensions are 100mm × 100mm × 515mm, according to the test of " Standard for test methods of longterm performance and durability of ordinary concrete " (GBJ500 82-2009) regulation; Concrete strength sample dimensions is 100mm × 100mm × 100mm, tests according to " normal concrete Mechanics Performance Testing test method " (GB/T 50081-2002).Concrete mix is m (cement): m (coarse aggregate): m (fine aggregate)=1: 3.18: 2.27, cement is PO 42.5 cement of Cement Co., Ltd of Shandong Aluminum Co., Ltd. group, the consumption of water specifies according to GB, adjusting and making the slump is 210 ± 10mm, and experimental result is in table 3.
The concrete shrinkage experiment table of table 3 low bleed shrinkage type polycarboxylate water-reducer and polycarboxylate water-reducer
Table 3 is presented under identical condition, and the slump of low bleed shrinkage type water reducer and divergence are all large than the existing PCA-1 of company, PCA-2, shows that its water-reducing rate will be higher than the two; 1#, 2#, 3#, 4# have reached respectively 33.8%, 38.9%, 35.8% and 36.3% than the decrement of PCA-1, because PCA-1 itself also has reducing function, so the decrement of synthetic low bleed shrinkage type polycarboxylate water-reducer will be far below this numerical value.Concrete reducing experimental result and capillary experimental result are also substantially identical.
Embodiment 5
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 87 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 50 DEG C, add 0.9 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and acrylic acid solution, wherein, consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.28 part, the Thiovanic acid of 0.2 part, 0.26 part of sodium allyl sulfonate and 65 parts, time for adding is 2.5h; Methyl methacrylate 0.255mol(25.5 part), time for adding is 2.0h.Dropwise at 50 DEG C and continue insulation reaction 1.0h, then add 167 parts of water, be cooled to 30 DEG C, add 47% sodium hydroxide solution adjusting pH value to 7.0.
Embodiment 6
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 110 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 52 DEG C, add 0.90 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and monomers B solution, wherein: the consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.28 part, the thiohydracrylic acid of 0.1 part, 0.36 part of methallylsulfonic acid sodium and 65 parts, time for adding is 3.0h; Consisting of of monomers B solution: 0.13mol(11.2 part) methyl acrylate and 0.14mol(14 part) methyl methacrylate, time for adding is 2.5h.Dropwise at 52 DEG C and continue insulation reaction 1.0h, then add 145 parts of water, be cooled to 25 DEG C, add 47% sodium hydroxide solution adjusting pH value to 7.5.
Embodiment 7
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 87 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 55 DEG C, add 0.98 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and monomers B solution, wherein: the consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.25 part, the sodium allyl sulfonate of 0.48 part and 65 parts, time for adding is 2.5h; Consisting of of monomers B solution: 0.08mol(6.9 part) methyl acrylate and 0.18mol(15.5 part) methacrylic acid, time for adding is 2.0h.Dropwise at 55 DEG C and continue insulation reaction 1.0h, then add 177 parts of water, be cooled to 30 DEG C, add 47% sodium hydroxide solution adjusting pH value to 6.5.
Embodiment 8
Take 0.085mol molecular-weight average and be 205 parts by mass of 2400 modified polyether TPEG(), 87 parts of water, in four-hole bottle, are opened and are stirred, and are heated to 54 DEG C, add 0.87 part of H
2o
2mixing solutions with 12 parts of water, stirring reaction 10min, start to drip xitix, chain-transfer agent mixed aqueous solution and monomers B solution, wherein: the consisting of of xitix, chain-transfer agent mixed aqueous solution: the water of the xitix of 0.31 part, 0.3 part of Thiovanic acid, 0.2 part of thiohydracrylic acid and 65 parts, time for adding is 3.0h; Consisting of of monomers B solution: 0.1mol(7.2 part) vinylformic acid, 0.1mol(8.6 part) methyl acrylate, 0.09mol Methacrylamide (15.3 parts of methacryloyl amine aqueous solutions that massfraction is 50%), time for adding is 2.5h.Dropwise at 54 DEG C and continue insulation reaction 1.0h, then add 167 parts of water, be cooled to 30 DEG C, add 47% sodium hydroxide solution adjusting pH value to 7.0.
Claims (1)
1. a preparation method for low bleed shrinkage type polycarboxylic acid concrete water reducer, is characterized in that, is formed, wherein: monomer A is modified polyether TPEG by monomer A and monomers B 1:3～3.5 copolymerization in molar ratio; Monomers B is the mixture of any one or a few arbitrary proportion in vinylformic acid, methyl acrylate, acrylamide, methacrylic acid, methyl methacrylate, Methacrylamide; Modified polyether TPEG molecular-weight average is 2400;
Also be added with initiator: H
2o
2ascorbic Acid Oxidation reduction initiator, wherein, H
2o
2consumption is 0.35～0.45% of monomer total mass, and xitix is 0.10～0.16% of monomer total mass;
Also be added with chain-transfer agent: chain-transfer agent is the mixture of one or both arbitrary proportions in sodium allyl sulfonate, methallylsulfonic acid sodium, Thiovanic acid, thiohydracrylic acid, and its consumption is 0.17～0.22% of monomer total mass;
The preparation method of described low bleed shrinkage type polycarboxylic acid concrete water reducer, comprises the following steps:
1) at 50～55 DEG C of temperature, modified polyether TPEG is added to the water to stirring and dissolving;
2) in the solution obtaining to step 1), add initiator H
2o
2, stir 10～15min;
3) to step 2) drip respectively xitix, chain-transfer agent mixed aqueous solution and monomers B solution in the solution that obtains simultaneously;
Xitix, chain-transfer agent mixed aqueous solution time for adding are 2.5～3.0h; Monomers B solution time for adding is 2.0～2.5h;
4) dropwise and under said temperature, be incubated polymerase 10 .5～1.0h, be then cooled to 25～30 DEG C;
5) with alkaline solution regulator solution pH value to 6.0～8.0, obtain polycarboxylate water-reducer;
Described step 1) strength of solution is 65～70%;
In described step 4), after polyreaction, mending and adding water to solid content is 38～42%;
The sodium hydroxide solution that in described step 5), alkaline solution is 47%.
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| CN103030334B (en) * | 2012-12-11 | 2015-04-29 | 马清沛 | Polycarboxylic acid water reducing agent |
| CN103360554A (en) * | 2013-07-18 | 2013-10-23 | 安徽森普新型材料发展有限公司 | Synthesizing method of high-performance water reducing agent |
| CN103880317B (en) * | 2014-03-12 | 2016-08-24 | 江苏万邦新型建材有限公司 | Pile tube high-performance polycarboxylic acids water reducing agent |
| CN104761173B (en) * | 2014-12-23 | 2017-01-18 | 水利部交通运输部国家能源局南京水利科学研究院 | Polycarboxylate water reducer with good reducing effect and preparation method thereof |
| CN109942757A (en) * | 2017-12-20 | 2019-06-28 | 中冶建筑研究总院有限公司 | A kind of polycarboxylate water-reducer |
| CN113121754B (en) * | 2021-05-06 | 2023-08-01 | 钱倩 | Concrete workability improver, preparation method thereof, concrete additive and concrete |
| CN113816649B (en) * | 2021-09-24 | 2022-06-14 | 贵州石博士科技股份有限公司 | Shrinkage-reducing polycarboxylate superplasticizer and preparation method and application thereof |
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