CN1702087A - Polyacrylic acid salts shrinkage-reducing-agent and method for making same - Google Patents
Polyacrylic acid salts shrinkage-reducing-agent and method for making same Download PDFInfo
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Abstract
An acrylate condensing agent and its preparation relates to additive of concrete. The invention comprises acroleic acid or methacrylic acid, phenylethene, initiating agent, chain-transferring agent, carbowax and catalyst and can get a linear polymer of high molecular weightcontaining polyoxyalkylenes chain. The invention has the advantages of low addition, low volatility, low reduction. The invention can be used in Portland cement concrete generally and is an ideal concrete condensing agent.
Description
Technical field:
The invention belongs to concrete structure and concrete works technical field, particularly concrete admixture.
Background technology:
Because concrete is easy to be shaped to the member of various size and shape, and characteristics such as intensity height, good endurance are arranged, and its starting material, as cement, gather materials and water etc. cheap and easy to get, so though concrete now still future all be the widest material of construction of purposes in the world.But concrete disadvantage is the fragility height, tensile strength is low, is easy to generate to shrink and crack or crackle occur under drying conditions, and these crackles or crack reduce concrete intensity and weather resistance, shorten concrete work-ing life, even influence concrete structural safety.Therefore, solve the cracking problem that concrete causes because of dry shrinkage is the problem that the building field of civil engineering is paid close attention to always.The dry way of shrinking of present domestic solution concrete has two kinds: a kind of is to mix swelling agent, and another kind is to mix fiber.For preventing concrete cracking, domestic life-time service swelling agent, the expansion that swelling agent produced is the contraction of compensating concrete partly or entirely, but swelling agent has stronger dependency to the extent of hydration of composition, envrionment temperature, humidity and the cement of cement, be difficult to control rate of expansion, even the aggravation crack on concrete.Expansive agent dosage is big in addition, wants contaminate environment during production, and the alkali in the swelling agent might cause alkali-aggregate reaction.Add fiber and just improved concrete tensile strength, do not reduce concrete shrinkage, while fiber price height, and have fiber and concrete compatibility problem, limited its popularization greatly.Economization agent is a kind of water soluble liq of low viscosity, when concrete is dry, reduces concrete contraction by the surface tension that reduces water in the pore.Can add in the concrete, also can be painted on concrete surface as surface treatment agent.Economization agent addition ratio swelling agent is little, and alkali content is low, has overcome the problem of the big and alkali of expansive agent dosage, and this admixture is a water soluble liq, can be in concrete homodisperse, overcome the compatibility problem between fiber and the concrete.At present both at home and abroad the chemical constitution of the economization agent that uses is mainly polyethers or polyethers derivative, monobasic or di-alcohols economization agent, alkamine economization agent, polyoxyethylene economization agent, alkyl Ammonia economization agent etc.The economization agent volume of this micromolecular amount is big, and volume is in 3～8% (in the weight of water), and volatilization is big, has a strong impact on the healthy of workman, and will influence concrete intensity." economization agent for concrete " that such as the Chinese patent publication number be CN1583648A formed according to the certainweight percentage mix by polyvinyl alcohol compounds, aliphatics glycol ether and hydroxide alkylamine.These are the compound of small molecular weight, and are volatile, can look into these compounds according to data and will reduce concrete intensity.And such economization agent volume is big, is about 3～5% of water weight.
Summary of the invention:
The objective of the invention is weak point, a kind of polyacrylic acid salts shrinkage-reducing-agent and preparation method thereof is provided at existing economization agent.Economization agent of the present invention is a kind of high molecular weight polymers, low volatilization, and volume is little, reduces effectively, does not reduce concrete intensity, even can also improve concrete intensity.
The object of the present invention is achieved like this: a kind of polyacrylic acid salts shrinkage-reducing-agent is made up of acrylic or methacrylic acid, vinylbenzene, initiator, chain-transfer agent, polyoxyethylene glycol and catalyzer, acrylic or methacrylic acid: vinylbenzene: initiator: chain-transfer agent: polyoxyethylene glycol: the mol ratio of catalyzer is 1: (0.0001～0.8): (0.00001～0.1): (0.001～10): (0.01～10): (0.0001～0.5).Its initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide or dilauroyl peroxide or the special fourth fat of peroxidation trimethylacetic acid or peroxy dicarbonate diisopropyl fat or peroxy dicarbonate two hexamethylene fat or different third hydrogen peroxide.Its chain-transfer agent is Virahol or methyl alcohol or acetone or acetaldehyde or trichloromethane or tetracol phenixin or lauryl mercaptan or sodium bisulfite.Its catalyzer is a phosphoric acid.The molecular weight of its polyoxyethylene glycol is 200～20000.Said components is by the inventive method, through polymerization, esterification and neutralization reaction, generates a kind of high-molecular weight, contains the comb-shaped polymer of polyoxyalkylene chain, and this polymkeric substance is polyacrylic acid salts shrinkage-reducing-agent of the present invention.
A kind of preparation method of polyacrylic acid salts shrinkage-reducing-agent, its processing step is as follows:
1. preparation monomer mixed solution
Be 1 in molar ratio at first: (0.0001～0.8) with acrylic or methacrylic acid, vinylbenzene and initiator: the mixed of (0.00001～0.1), stir, prepare monomer mixed solution.
2. carry out polyreaction
Go on foot the monomer mixed solution of preparing with the 1st, in 1～6 hour, slowly adding temperature while stirring and be 50～160 ℃, mol ratio is in 0.5～3 times the organic solvent of acrylic or methacrylic acid, after slowly adding, 0.001～10 times of chain-transfer agent that adds mol ratio more while stirring and be acrylic or methacrylic acid carried out polyreaction 1～4 hour, prepared lurid transparent polymer solution.Its organic solvent is benzene or toluene or dimethylbenzene or tetracol phenixin or ethyl acetate or ethyl acetate.
3. carry out esterification send out should
Go on foot in the polymers soln of preparing the 2nd, add mol ratio while stirring and be 0.01～10 times of acrylic or methacrylic acid, molecular weight is 0.0001～0.5 times the catalyzer that 200～20000 polyoxyethylene glycol and mol ratio are acrylic or methacrylic acid, under 60～160 ℃ of temperature, carried out esterification 1～8 hour, organic solvent and chain-transfer agent are reclaimed out in distillation simultaneously, can reuse, prepare brown xanchromatic esterification products at last.
4. carry out neutralization reaction
Go on foot in the esterification products of preparing the 3rd, add caustic soda soln while stirring, carry out neutralization reaction, and to regulate its pH value be 7～9, the comb-shaped polymer that just to prepare a kind of molecular-weight average be 2000～100000, contain polyoxyalkylene chain, wherein the quality of polyoxyalkylene chain is 50～90% of a whole polymer quality, and this polymkeric substance is polyacrylic acid salts shrinkage-reducing-agent of the present invention.
After the present invention adopts technique scheme, it is little that its invention product economization agent has a volume, volume is 0.5～2.5% of a water weight, volume less than existing economization agent 3.0～5.0%, low volatilization is reduced effectively, and does not reduce concrete intensity, and 8～18% water-reducing rate is arranged, and delayed coagulation is arranged.Therefore, product of the present invention be a kind of have simultaneously reduce, the multifunctional concrete admixture of diminishing and slow setting, be particularly suitable for the construction of mass concrete in summer.Show that according to test-results decrement can reach 70～80%, and the intensity of 7 days and 28 days is higher than blank concrete.And the concrete to different acidity, humidity and temperature all has the good effect of reducing.The inventive method has characteristics such as production technique is simple, easy and simple to handle, cost is low.The present invention can be widely used in portland-type cement concrete and the mortar, reinforcing bar there is not corrosion, also can spray to the surface of concrete or mortar member and goods, be suitable in the concrete construction engineerings such as factory building, road, bridge, tunnel, pond, dykes and dams, also being fit to the materials for wall production of articles, is modern optimal economization agent for concrete.
Description of drawings:
Fig. 1 is the decrement curve of economization agent of the present invention different volumes in mortar specimen;
Among the figure: a is the relative shrinkage curve of benchmark mortar;
B is the relative shrinkage curve that mixes the economization agent mortar of the present invention of 0.8% (by water);
C is the relative shrinkage curve that mixes the economization agent mortar of the present invention of 2.0% (by water);
D is the relative shrinkage curve that mixes the economization agent mortar of the present invention of 2.5% (by water).
Fig. 2 is sprayed on the decrement graphic representation on mortar specimen surface in the different concns aqueous solution for economization agent of the present invention.
Among the figure: a is the relative shrinkage curve of benchmark mortar specimen;
B sprays the relative shrinkage curve on mortar specimen surface at 13% the aqueous solution for economization agent of the present invention;
C is the relative shrinkage curve of economization agent of the present invention on 23% aqueous solution spraying mortar specimen surface,
Embodiment:
Below in conjunction with embodiment, further specify the present invention.
A kind of polyacrylic acid salts shrinkage-reducing-agent is formed vinylformic acid by vinylformic acid, vinylbenzene, Diisopropyl azodicarboxylate initiator, lauryl mercaptan chain-transfer agent, polyoxyethylene glycol and phosphoric acid catalyst: vinylbenzene: Diisopropyl azodicarboxylate: lauryl mercaptan: polyoxyethylene glycol: the mol ratio of phosphoric acid is 1: 0.1: 0.003: 0.5: 1.15: 0.1.The amount of the branch of its polyoxyethylene glycol is 400.Its synthetic processing step is as follows:
1. preparation monomer mixed solution
Earlier the Diisopropyl azodicarboxylate initiator of the vinylbenzene of the vinylformic acid of 1mol and 0.1mol and 0.003mol is mixed and stir, prepare monomer mixed solution.
2. carry out polymerization send out should
In 4 hours, it is in 70 ℃, the ethyl acetate organic solution of 3mol that the 1st monomer mixed solution prepared of step is added temperature while stirring, after interpolation finishes, add 0.5mol lauryl mercaptan chain-transfer agent more while stirring and carried out polyreaction 2 hours, prepare lurid transparent polymer solution at last.
3. carry out esterification
Go on foot in the polymers soln of preparing the 2nd, add 1.15mol, molecular weight while stirring and be 400 polyoxyethylene glycol and the phosphoric acid catalyst of 0.1mol, earlier under 71 ℃, carried out esterification 3 hours, under 98 ℃, carried out esterification 3 hours again, and ethyl acetate organic solution and lauryl mercaptan chain-transfer agent are reclaimed out in distillation, can reuse, make pale brown look esterification products at last.
4. carry out neutralization reaction
Go on foot in the esterification products of preparing the 3rd, add caustic soda soln while stirring and carry out neutralization reaction, and regulate the pH value 7, and the comb-shaped polymer that just to prepare a kind of molecular-weight average be 20000, contain polyoxyalkylene chain, wherein the quality of polyoxyalkylene chain is 70% of a whole polymer quality.
Polyacrylic acid salts shrinkage-reducing-agent to present embodiment carries out following test:
1. carry out the incorporation contraction test
In mortar specimen, mix 0.8%, 2.0% and 2.5% economization agent of the present invention respectively.The material of this test specimen is ground, a Chongqing dimension P.O.42.5 cement, and canal river sand, fineness modulus are 0.7, cement: sand is 1: 3, and water cement ratio is 0.6.Sample dimensions is 25 * 25 * 280mm
3Be placed on standard curing room maintenance form removal after a day, putting into temperature then is the contraction that 60% curing room is surveyed mortar specimen at 20 ± 1 ℃, relative humidity, and the shrinking percentage of its different volumes as shown in Figure 1.
As can be seen from Figure 1,3 days decrements of the test specimen of admixture 0.8% economization agent of the present invention can reach 80%, 28 day decrement and can reach 40%; 3 days decrements of the test specimen of admixture 2.5% can reach 90%, 28 day decrement and can reach 55%.Reduce effectively, reduce better effects if especially in early days.
2. carry out the strength trial of different volumes
Mortar strength under each volume of table 1
| Numbering | Volume (%) | 3 days | 7 days | 28 days | |||
| Anti-folding (Mpa) | Resistance to compression (MPa) | Anti-folding (MPa) | Resistance to compression (MPa) | Anti-folding (MPa) | Resistance to compression (MPa) | ||
| ????1 | ????0 | ????3.47 | ????11.4 | ????4.63 | ????18.1 | ????5.50 | ????26.7 |
| ????2 | ????0.8 | ????3.57 | ????12.1 | ????4.60 | ????17.2 | ????5.65 | ????30.4 |
| ????3 | ????2.0 | ????3.45 | ????11.9 | ????4.43 | ????17.9 | ????5.77 | ????28.9 |
| ????4 | ????2.5 | ????3.30 | ????11.4 | ????4.45 | ????19.5 | ????4.77 | ????26.8 |
In mortar specimen, mix 0.8%, 2.0% and 2.5% economization agent of the present invention respectively.The material of this test specimen is ground, a Chongqing dimension P.O.42.5 cement, and canal river sand, fineness modulus are 0.7, cement: sand is 1: 3, and water cement ratio is 0.6.Sample dimensions is 40 * 40 * 160mm
3, be placed on the standard curing room maintenance.The intensity of surveying its different volumes is as shown in table 1.
As can be seen from Table 1, admixture economization agent of the present invention is little to intensity effect, even can also improve concrete intensity.From economical and reduce effect and take all factors into consideration, mix water consumption 2.0% for best.
3. carry out surperficial spray test
Economization agent of the present invention is made into 23% and 13% the aqueous solution, sprays to the surface of mortar specimen respectively.The material of this test specimen be Chongqing tie up P.0.42.5 cement, canal river sand, fineness modulus are 0.7, cement: sand is 1: 3, water cement ratio is 0.6.Sample dimensions is 25 * 25 * 280mm
3Be placed on standard curing room maintenance form removal after a day, putting into temperature then is the contraction that 60% curing room is measured mortar specimen at 20 ± 1 ℃, relative humidity, and its different concns aqueous solution shrinking percentage as shown in Figure 2.
As can be seen from Figure 2, economization agent of the present invention is made into the aqueous solution is sprayed on the test specimen surface and has equally to have and significantly reduce effect, and also can be used as a kind of curing agent, reduced the consumption of economization agent like this, thereby reduced cost, reasonable future in engineering applications has been arranged.
4. carry out the test of cement paste diffusibleness
Economization agent of the present invention and West China high efficiency water reducing agent (high dense) FDN does clean slurry diffusibleness simultaneous test, and test-results is as shown in table 2, and the cement of this test is ground, Chongqing dimension P.O.42.5,300g, water 87ml.
The test of table 2 cement paste diffusibleness
| Economization agent of the present invention | West China high efficiency water reducing agent (high dense) FDN | ||
| Volume (%) | Diffusibleness (cm) | Volume (%) | Diffusibleness (cm) |
| ????0.5 | ????0 | ????- | ????- |
| ????0.8 | ????0 | ????- | ????- |
| ????1.2 | ????20.0 | ????0.3 | ????18.0 |
| ????2.0 | ????20.5 | ????0.4 | ????23.0 |
| ????3.0 | ????22.5 | ????0.5 | ????24.0 |
As can be seen from Table 2, economization agent of the present invention has certain water-reducing effect, and water-reducing effect is not obvious during low-dosage (＜1.2%), but volume surpasses at 1.2% o'clock, and water-reducing rate can reach 15～18%, continues to increase volume, and water-reducing rate improves little.Because economization agent of the present invention is a kind of tensio-active agent with wetting action, it can reduce the surface tension of water, has reduced the adhesive tension between the cement granules, and the water that a part is wrapped up by cement granules dissociates out, thereby has certain water-reducing effect.
5. carry out cement paste test time of coagulation
Carry out cement paste test time of coagulation of admixture economization agent of the present invention, test-results is as shown in table 3, and the cement that this test is adopted is ground, Chongqing dimension P.O.42.5, cement 300g, water 87ml.
Can find out that from table 3 economization agent of the present invention has delayed coagulation, along with the increasing of volume, its delayed coagulation strengthens, so economization agent of the present invention is particularly suitable for the mass concrete construction in summer.
The time of coagulation of cement paste under the various volumes of table 3
| Numbering | Volume (%) | Initial set (h) | Final set (h) |
| ????1 | ????- | ????4:00 | ????5:30 |
| ????2 | ????0.5 | ????5:20 | ????6:00 |
| ????3 | ????0.8 | ????6:10 | ????6:50 |
| ????4 | ????1.2 | ????6:50 | ????7:20 |
| ????5 | ????2.0 | ????7:30 | ????9:00 |
| ????6 | ????3.0 | ????8:00 | ????10:30 |
Claims (6)
1 one kinds of polyacrylic acid salts shrinkage-reducing-agents, it is characterized in that forming by acrylic or methacrylic acid, vinylbenzene, initiator, chain-transfer agent, polyoxyethylene glycol and catalyzer, acrylic or methacrylic acid: vinylbenzene: initiator: chain-transfer agent: polyoxyethylene glycol: the mol ratio of catalyzer is 1: 0.0001～0.8: 0.00001～0.1: 0.001～10: 0.01～10: 0.0001～0.5, and the molecular weight of its polyoxyethylene glycol is 200～20000.
2 according to the described polyacrylic acid salts shrinkage-reducing-agent of claim 1, it is characterized in that described initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide or dilauroyl peroxide or the special fourth fat of peroxidation trimethylacetic acid or peroxy dicarbonate diisopropyl fat or peroxy dicarbonate two hexamethylene fat or different third hydrogen peroxide; Described chain-transfer agent is Virahol or methyl alcohol or acetone or acetaldehyde or trichloromethane or tetracol phenixin or lauryl mercaptan or sodium bisulfite; Described catalyzer is a phosphoric acid.
3 according to claim 1 or 2 described polyacrylic acid salts shrinkage-reducing-agents, it is characterized in that a kind of polyacrylic acid salts shrinkage-reducing-agent is made up of vinylformic acid, vinylbenzene, Diisopropyl azodicarboxylate initiator, lauryl mercaptan chain-transfer agent, polyoxyethylene glycol and phosphoric acid catalyst, vinylformic acid: vinylbenzene: Diisopropyl azodicarboxylate: lauryl mercaptan: polyoxyethylene glycol: the mol ratio of phosphoric acid is 1: 0.1: 0.003: 0.5: 1.15: 0.1, the amount of the branch of its polyoxyethylene glycol was 400.
The preparation method of 4 one kinds of polyacrylic acid salts shrinkage-reducing-agents is characterized in that its processing step is as follows: (1) preparation monomer mixed solution
At first be 1: 0.0001～0.8: 0.00001～0.1 mixed in molar ratio, stir acrylic or methacrylic acid, vinylbenzene and initiator;
(2) carry out polyreaction
Go on foot the monomer mixed solution of preparing with (1), in 1～6 hour, slowly adding temperature while stirring and be 50～160 ℃, mol ratio is in 0.5～3 times the organic solvent of acrylic or methacrylic acid, after slowly adding, adding mol ratio more while stirring is 0.001～10 times of chain-transfer agent of acrylic or methacrylic acid, carries out polyreaction 1～4 hour;
(3) carry out esterification send out should
In (2) polymers soln of preparing, add mol ratio while stirring and be 0.01～10 times of acrylic or methacrylic acid, molecular weight is 0.0001～0.5 times the catalyzer that 200～20000 polyoxyethylene glycol and mol ratio are acrylic or methacrylic acid, under 60～160 ℃ of temperature, carried out esterification 1～8 hour, organic solvent and chain-transfer agent are reclaimed out in distillation simultaneously, can reuse;
(4) carry out neutralization reaction
In (3) esterification products of preparing, add caustic soda soln while stirring, carry out neutralization reaction, and to regulate its pH value be 7～9, the comb-shaped polymer that just to prepare a kind of molecular-weight average be 2000～100000, contain polyoxyalkylene chain, wherein the quality of polyoxyalkylene chain is 50～90% of a whole polymer quality.
5 preparation methods according to the described polyacrylic acid salts shrinkage-reducing-agent of claim 4 is characterized in that described organic solvent is benzene or toluene or dimethylbenzene or tetracol phenixin or ethyl acetate or ethyl acetate.
6 preparation methods according to claim 4 or 5 described polyacrylic acid salts shrinkage-reducing-agents is characterized in that a kind of preparation method of polyacrylic acid salts shrinkage-reducing-agent, and its processing step is as follows:
(1) preparation monomer mixed solution
Earlier the Diisopropyl azodicarboxylate initiator of the vinylbenzene of the vinylformic acid of 1mol and 0.1mol and 0.003mol is mixed and stir;
(2) carry out polymerization send out should
In 4 hours, it is in 70 ℃, the ethyl acetate organic solution of 3mol that (1) monomer mixed solution prepared of step is added temperature while stirring, add finish after, add 0.5mol lauryl mercaptan chain-transfer agent more while stirring and carried out polyreaction 2 hours;
(3) carry out esterification
Go on foot in the polymers soln of preparing (2), add 1.15mol, molecular weight while stirring and be 400 polyoxyethylene glycol and the phosphoric acid catalyst of 0.1mol, earlier under 71 ℃, carried out esterification 3 hours, under 98 ℃, carried out esterification 3 hours again, and distill and reclaim out ethyl acetate organic solution and lauryl mercaptan chain-transfer agent, can reuse;
(4) carry out neutralization reaction
Go on foot in the esterification products of preparing (3), add caustic soda soln while stirring and carry out neutralization reaction, and regulate the pH value 7, and the comb-shaped polymer that just to prepare a kind of molecular-weight average be 20000, contain polyoxyalkylene chain, wherein the quality of polyoxyalkylene chain is 70% of a whole polymer quality.
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| CN106186794B (en) * | 2016-07-04 | 2018-08-17 | 中交四航工程研究院有限公司 | A kind of high-effective concrete anti-cracking curing agent, preparation method and application |
| CN110746136A (en) * | 2019-09-27 | 2020-02-04 | 中建商品混凝土有限公司 | Shrinkage-reducing thickening type alkali-free liquid accelerator and preparation method and application thereof |
| CN111454014A (en) * | 2020-04-02 | 2020-07-28 | 厦门路桥翔通建材科技有限公司 | Mortar and concrete shrinkage reducing agent containing organic silicon and preparation method thereof |
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