CN102951865B - Air entraining type poly carboxylic acid high performance water reducing agent and preparation method thereof - Google Patents
Air entraining type poly carboxylic acid high performance water reducing agent and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to an air entraining type poly carboxylic acid high performance water reducing agent and a preparation method thereof. According to the water reducing agent, 0.25 mol of a monomer methyl alkenyl polyoxyethelene, allyl polyoxyethelene ether or polyoxypropylene ether with a polymerization degree of 30-60, 0.70 mol of a monomer methacrylic acid or acrylic acid, 0.18 mol of a monomer sodium methylallyl sulfonate, acrylamide or 2-acrylamide-methyl propanesulfonic acid, 0.05 mol of a monomer styrene or ethyl acetate, an initiator agent and a chain transfer agent are subjected to a thermal insulation reaction for 4-5 h at a temperature of 48-52 DEG C by adopting deionized water as a reaction medium to carry out copolymerization to obtain a polymer with a molecular weight of 60000-80000, cooling is performed to a temperature of less than 40 DEG C, and a 40% sodium hydroxide solution is added to adjust the pH value to 6-8 to obtain the finished product. The air entraining type poly carboxylic acid high performance water reducing agent has a high water reducing rate, wherein the water reducing rate can be 30% when the water reduced solid doping amount is 0.2%, and the air entraining of concrete can be 5-7% when the water reduced solid doping amount is 0.2% under the premise of no other air entraining agent compounding.
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 research work of air entrained type polycarboxylate high performance water-reducing agent and preparation method thereof.
Background technology
Water reducer refers to that can to keep cement paste, mortar and concrete work degree constant and significantly reduce the admixture of its mixing water content.It can significantly improve concrete intensity, improves concrete frost resistance and impermeability, and reduces the usage quantity of cement.
According to water reducer diminishing and enhancing ability, be divided into ordinary water-reducing agent (claim again fluidizer, water-reducing rate is not less than 8%), high efficiency water reducing agent (claim again superplasticizer, water-reducing rate is not less than 14%) and high-performance water reducing agent (water-reducing rate is not less than 25%).
Along with the continuous progress of 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 meet 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 mobility to meet 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 (as naphthalenesulfonate, melamine sulfonate, sulfamate etc.) is difficult to meet well these requirements.
Poly carboxylic acid series water reducer is the novel water reducer growing up in recent years.There are a lot of uniquenesses: and between different cement, have relatively better consistency; Even in the time of low-dosage, poly carboxylic acid series water reducer also can make concrete have high workability; And in the time of low water-cement ratio, there is low viscosity and good slump retention; 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; Do not use harmful starting material such as formaldehyde; Not chloride ion-containing, can not produce intergranular corrosion to building iron.
From twentieth century end, the concrete research of International Academic bound pair, the no longer concrete superstrength of simple pursuit, but gradually to high performance future development.High performance concrete refers to and meets mechanical property requirements, has the concrete of high workability, high-durability and high volume stability.Research shows: can greatly improve concrete endurance quality at the equally distributed micro-bubble of the appropriate introducing of inside concrete, but concrete strength is had to impact (the every raising 1% of air content, concrete strength approximately declines 4～5%).Nineteen nineties, domesticly also start to pay close attention to high performance concrete research, but on concrete engineering still mainly take concrete strength as unique standard for acceptance, and ignored concrete endurance quality, therefore, domestic cement water reducing agent product is take low air-entraining performance as main.In recent years, along with putting into operation in a large number of the engineerings such as high-speed railway, bridge spanning the sea, power station, harbour, concrete durability has been proposed to very high request, in the urgent need to researching and developing a kind of polycarboxylate high performance water-reducing agent product of research work of air entrained type.
In prior art, there is following several improving technology to polycarboxylate high performance water-reducing agent:
CN201110332112.3 has introduced a kind of synthetic method of universal polycarboxylic water reducer.This general polycarboxylate water-reducer is liquid, and solid content is 40%.It is under the effect of chain initiator, chain-transfer agent, to be carried out neutralizing the prepared water reducer that contains carboxyl, sulfonic group, polyoxyethylene base side chain after polymerization by monomers such as modification Soxylat A 25-7 or polyethenoxy ether and (methyl) vinylformic acid or methylene-succinic acid, methylpropene sodium sulfonates again.Universal polycarboxylic water reducer alkali content that the present invention prepares is low, water-reducing rate is high, add with gelling material weight ratio 0.25～1.0% fashionable, concrete rapid operation, cement mixture has high workability and high slump retaining and good workability.This polycarboxylate water-reducer product bleed is poor, and bubble size is large, inhomogeneous, affects bubble quality in concrete.
CN 201110207462.7 has introduced a kind of modification ethers polycarboxylic acid water reducing agent and preparation method thereof.The invention discloses a kind of modification ethers polycarboxylic acid water reducing agent, it is by 50%～95% methacrylic Soxylat A 25-7,4%～40% vinylformic acid and 1%～10%AMPS(2-acrylamide-2-methylpro panesulfonic acid) three kinds of monomers carry out free radical and cause copolymerization and form.Modification ethers polycarboxylic acid water reducing agent of the present invention, owing to having introduced methacrylic polyoxyethylene ether monomer, synthetic water reducer product is compared ethers polycarboxylic acid water reducing agent and is had higher water-reducing rate and function of slump protection, and the AMPS(2-acrylamide-2-methylpro panesulfonic acid of introducing) also further improve the water-reducing rate of product, the concrete of preparation have low-dosage, high workability, low slump through time loss, good workability and early strength fully, and product is improved greatly to the raw-material adaptive faculty of different sources.This polycarboxylate water-reducer product belongs to low research work of air entrained type, needs to improve by composite special air entrapment agent of later stage the bleed performance of product.
CN201210118358.5 has introduced a kind of polycarboxylate water-reducer and preparation method thereof.Its preparation method is by polyoxyethylene thiazolinyl, methylpropene sodium sulfonate and the vinylbenzene of vinylformic acid, prenol end-blocking, add in a certain amount of water according to a definite sequence, under the acting in conjunction of initiator and molecular weight regulator, radical polymerization at a certain temperature forms.This technique is simple, and product performance are single, and bleed is poor, to the bad adaptability of concrete raw material.
Summary of the invention
Main purpose of the present invention is to provide a kind of research work of air entrained type polycarboxylate high performance water-reducing agent and preparation method thereof, to overcome existing poly carboxylic acid series water reducer bleed poor performance, to introduce large, the inhomogeneous defect of bubble size in concrete.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of research work of air entrained type polycarboxylate high performance water-reducing agent, is characterized in that: comprising:
0.25mol monomer A,
0.70mol monomers B,
0.18mol monomer C,
0.05mol monomer D,
Take deionized water as reaction medium, with initiator, chain-transfer agent, insulation reaction 4～5h under 50 ± 2 ℃ of conditions, it is 60000～80000 polymkeric substance that copolymerization obtains molecular weight, then cools to below 40 ℃, adds liquid caustic soda regulation system pH value 6～8 and get final product;
The total consumption of described deionized water is 2.33 times of monomer total mass; Described initiator amount is 0.3～2.5% of reaction total monomer weight by weight, and the consumption of chain-transfer agent is 0.02～0.35% of reaction total monomer weight by weight;
Described monomer A is that the polymerization degree is 30～60 monomer methyl thiazolinyl polyoxyethylene, allyl polyethenoxy ether or polyethenoxy ether;
Described monomers B is methacrylic acid or vinylformic acid;
Described monomer C is methylpropene sodium sulfonate, acrylamide or 2-acrylamido-methyl propane sulfonic acid;
Described monomer D is vinylbenzene or ethyl acetate;
Described initiator is one or more mixing in ammonium persulphate, 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 40% sodium hydroxide solution.
In technique scheme, the consumption of monomer is the optimum feed stock ratio that participates in reaction, 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; Or increase the consumption of other monomers in order to improve the utilization ratio of some monomer, and then carry out raw material separation, but because must comprise the consumption that the present invention proposes, therefore be also equal to technical scheme of the present invention.
The preparation method of research work of air entrained type polycarboxylate high performance water-reducing agent of the present invention, comprises the following steps:
A, partial monosomy B, monomer C and monomer D are dissolved in deionized water, stir, obtain minor comonomer solution, stir stand-by;
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 50 ± 2 ℃, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1～2h, after reaction finishes, is cooled to below 40 ℃, add between liquid caustic soda regulation system pH value to 6～8, to obtain final product.
The amount of the monomers B further, adding in described step a is equivalent to the molar weight of twice monomer C.Its object is mainly to guarantee there is monomers B in whole reaction process, and namely acrylic or methacrylic acid, as main chain, causes new polyreaction, impels and reacts completely.
Beneficial effect of the present invention: research work of air entrained type polycarboxylate high performance water-reducing agent provided by the invention is in aqueous medium, take methacrylic acid or vinylformic acid as main chain, take the large monomer of unsaturated modified polyether as side chain, introduce the unsaturated minor comonomer of novel bleed, obtain thering is target molecular structure, molecular weight distribution, the research work of air entrained type polycarboxylate high performance water-reducing agent of functional group, this water reducer water-reducing rate is high (when the solid volume of folding is 0.2%, water-reducing rate can reach 30%), bleed excellent performance is (when the solid volume of folding is 0.2%, concrete 's air-containing can reach 5～7%), significantly improve concrete endurance quality, and between concrete raw material, there is adaptability widely.
Embodiment
For those skilled in the art are known and technical scheme clearly of the present invention more, spy provides preferred embodiment below, but technological thought of the present invention is not limited to following examples.
Embodiment mono-
0.25mol monomer A is that the polymerization degree is 30～60 methyl thiazolinyl polyoxyethylene;
0.70mol monomers B is methacrylic acid;
0.18mol monomer C is acrylamide;
0.05mol monomer D is ethyl acetate;
Initiator is Sodium Persulfate;
Chain-transfer agent is the mixture that Thiovanic acid mixes in the ratio of 1:2 with sodium bisulfite;
Preparation process:
A, the monomers B that is equivalent to the molar weight of twice monomer C, monomer C and monomer D are dissolved in deionized water, stir, and obtain minor comonomer solution, stir stand-by;
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 0.1% 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, initiator amount is 1.2% of reaction total monomer weight by weight, continues to stir and heats up; Treat that temperature rises to 50 ± 2 ℃, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, then continue insulation reaction 1.5h, after finishing, reaction is cooled to below 40 ℃, add between 40% sodium hydroxide solution regulation system pH value to 6～8, obtaining molecular weight is 60000～80000, the product that solid content is 30%.
In three steps, the total consumption of deionized water is 2.33 times of monomer total mass.
Embodiment bis-
0.25mol monomer A is that the polymerization degree is 30～60 allyl polyethenoxy ether;
0.70mol monomers B is methacrylic acid;
0.18mol monomer C is 2-acrylamido-methyl propane sulfonic acid;
0.05mol monomer D is ethyl acetate;
Initiator is the mixture that ammonium persulphate mixes in 1:1 ratio with Sodium Persulfate;
Chain-transfer agent is Thiovanic acid;
Preparation process:
A, the monomers B that is equivalent to the molar weight of twice monomer C, monomer C and monomer D are dissolved in deionized water, stir, and obtain minor comonomer solution, stir stand-by;
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, initiator amount is 1.5% of reaction total monomer weight by weight, continues to stir and heats up; Treat that temperature rises to 50 ± 2 ℃, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, then continue insulation reaction 1.5h, after finishing, reaction is cooled to below 40 ℃, add between 40% sodium hydroxide solution regulation system pH value to 6～8, obtaining molecular weight is 60000～80000, the product that solid content is 30%.
In three steps, the total consumption of deionized water is 2.33 times of monomer total mass.
Embodiment tri-
0.25mol monomer A is that the polymerization degree is 30～60 polyethenoxy ether;
0.70mol monomers B is vinylformic acid;
0.18mol monomer C is methylpropene sodium sulfonate;
0.05mol monomer D is vinylbenzene;
Initiator is hydrogen peroxide;
Chain-transfer agent is the mixture that Thiovanic acid mixes in 2:1 ratio with 2 mercaptopropionic acid;
Preparation process:
A, the monomers B that is equivalent to the molar weight of twice monomer C, monomer C and monomer D are dissolved in deionized water, stir, and obtain minor comonomer solution, stir stand-by;
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 0.25% 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, the monomers B that adds surplus and initiator (initiator amount by weight for react total monomer weight 2.2%), continue to stir and heat up, treat that temperature rises to 50 ± 2 ℃, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, then continue insulation reaction 1.5h, after finishing, reaction is cooled to below 40 ℃, add between 40% sodium hydroxide solution regulation system pH value to 6～8, obtaining molecular weight is 60000～80000, solid content is 30% product.
In three steps, the total consumption of deionized water is 2.33 times of monomer total mass.
Wherein the product of embodiment 1 (solid content: 30%) to carry out the test situation of performance comparison as follows with currently available products:
Currently available products source: the JJPC-C type polycarboxylate high performance water-reducing agent (solid content: 40%), represent with sample 1 that Chongqing Jian Jie Science and Technology Ltd. produces.
(GB8076-2008) test by " concrete admixture ".
1, water-reducing rate simultaneous test
Concrete mix and water-reducing rate test-results:
2, air content test
Concrete mix and air content test result:
3, concrete mix and relative endurance quality test-results:
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 exceedes 30%; There is more excellent bleed performance: under the prerequisite of composite other air entrapment agents not, when the solid volume of folding is 0.2%, concrete 's air-containing can reach 5～7%; Endurance performance of concrete is greatly improved, and after 200 freeze-thaw cycle, durability index has improved 8% relatively.
Claims (2)
1. a research work of air entrained type polycarboxylate high performance water-reducing agent, is characterized in that: by:
0.25mol monomer A,
0.70mol monomers B,
0.18mol monomer C,
0.05mol monomer D,
Take deionized water as reaction medium, with initiator, chain-transfer agent, insulation reaction 4～5h under 50 ± 2 ℃ of conditions, it is 60000～80000 polymkeric substance that copolymerization obtains molecular weight, then cools to below 40 ℃, adds liquid caustic soda regulation system pH value 6～8 and get final product;
The total consumption of described deionized water is 2.33 times of monomer total mass; Described initiator amount is 0.3～2.5% of reaction total monomer weight by weight, and the consumption of chain-transfer agent is 0.02～0.35% of reaction total monomer weight by weight;
Described monomer A is that the polymerization degree is 30～60 monomer methyl thiazolinyl polyoxyethylene, allyl polyethenoxy ether or polyethenoxy ether;
Described monomers B is methacrylic acid or vinylformic acid;
Described monomer C is methylpropene sodium sulfonate, acrylamide or 2-acrylamido-methyl propane sulfonic acid;
Described monomer D is vinylbenzene or ethyl acetate;
Described initiator is one or more mixing in ammonium persulphate, 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 40% sodium hydroxide solution;
Prepare by following concrete steps:
A, partial monosomy B, monomer C and monomer D are dissolved in deionized water, stir, obtain minor comonomer solution, stir stand-by;
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 50 ± 2 ℃, start synchronous uniform velocity and drip minor comonomer solution and chain-transfer agent solution, 3h drips off, and then continues insulation reaction 1～2h, after reaction finishes, is cooled to below 40 ℃, add between liquid caustic soda regulation system pH value to 6～8, to obtain final product.
2. research work of air entrained type polycarboxylate high performance water-reducing agent according to claim 1, is characterized in that: the amount of the monomers B adding in described step a is equivalent to the molar weight of twice monomer C.
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| CN101974135B (en) * | 2010-10-15 | 2013-03-06 | 北京工业大学 | Normal-temperature synthesis method for polycarboxylic acid water-reducing agent |
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| CN102286134A (en) * | 2011-06-09 | 2011-12-21 | 江苏天音化工有限公司 | Preparation method for high-performance water reducing agent |
| CN102627425A (en) * | 2012-04-20 | 2012-08-08 | 武汉汉星盛新型建材有限公司 | Polycarboxylic acid water reducing agent and preparation method thereof |
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Effective date of registration: 20200902 Address after: 333300 Tower Industrial Zone, Leping Industrial Park, Jiangxi, Jingdezhen Patentee after: LEPING LINGHANG NEW MATERIAL Co.,Ltd. Address before: Changshou District of Chongqing city in 401231 Qingfeng Glenn town dam Industrial Concentration Zone Patentee before: CHONGQING JIANJIE TECHNOLOGY Co.,Ltd. |