CN104140220A - Concrete slump compensating agent and preparation method and application thereof - Google Patents
Concrete slump compensating agent and preparation method and application thereof Download PDFInfo
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- CN104140220A CN104140220A CN201410362627.1A CN201410362627A CN104140220A CN 104140220 A CN104140220 A CN 104140220A CN 201410362627 A CN201410362627 A CN 201410362627A CN 104140220 A CN104140220 A CN 104140220A
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Abstract
The invention discloses a concrete slump compensating agent and a preparation method and application of the concrete slump compensating agent. Styrene, sodium methylallyl sulfonate and monomethyl maleate are mixed and heated to 50 DEG C to 70 DEG C with water as a dispersion medium, 2-hydroxyethyl acrylate solution, initiator solution and molecular weight modifier solution are dropwise added, reaction continues for 1 h to 2 h after drop adding is completed, alkali is added to regulate the pH to 6 to 8, and then the slump compensating agent is obtained. The mass ratio of the monomethyl maleate, the styrene and the sodium methylallyl sulfonate is 1:1.2-1.6:0.6-0.8. Solution polymerization is adopted for the preparation method, and the preparation method is simpler, more reasonable and easier to operate compared with an existing ordinary slump compensating agent production technology; the temperature of the synthetic reaction is low, the synthetic technology is simple, and the slump compensating agent is easy to synthesize; in the application process, the slump compensating agent can be compatible with machine-made sand and high-slit-content gravel better, the slump compensating effect is obvious, and influence caused by weather is little.
Description
Technical field
The invention belongs to additive for building material field, be specifically related to a kind of concrete slump compensator and its preparation method and application.
Background technology
Since the sixties in 20th century, there are three kinds of high efficiency water reducing agents in foreign market, they are respectively benzene sulfonate formaldehyde condensation products, polycyclic aromatic hydrocarbon sulfonate formaldehyde condensation products and condensate of melamine sulfonate and formaldehyde, have brought thus the fast development of high efficiency water reducing agent exploitation with research.Develop rapidly the beginning of the nineties taking polyacrylate and graft copolymer thereof as the polycarboxylic acid series high efficiency water reducing agent of representative, and become the developing direction of 21 century high efficiency water reducing agent.In Practical Project, because the chemical composition of cement is different with firing process, the difference of the raw-material quality height difference of sandstone and construction environment (temperature and humidity etc.), cause the consistency variation of Water-reducing Admixtures To Cements, thereby reduce the concrete slump.The initial slump and Slump Time losing of Large directly have influence on concrete pumpability, mobility and water-retentivity.Improve the slump retaining of polycarboxylate water-reducer, have influence on the workability of high performance concrete.
The method that improves at present function of slump protection mainly contains following several: 1. use retardant and water reducer pair to mix, but excessive use retardant can affect construction speed and construction quality; 2. add water reducer two times, although can effectively increase the concrete slump, also can cause the super of admixture to be mixed simultaneously; 3. adopt multiple water reducer composite, but just sometimes can solve the problem of slump-loss.
A kind of preparation method of polycarboxylic acid high slump retaining agent is disclosed in CN 102093521A patent: adopt maleic anhydride and poly-second diester double esterification legal system for cross-linking monomer, with the copolymerization in redox system of macromole unsaturated polyether, generating portion is crosslinked.But esterification yield is not high, and, environmental protection not.
A kind of slow-release type polycarboxylate slump-retaining agent and preparation method thereof is disclosed in CN 102390950 patents: adopt unsaturated carboxylic acid polyoxyethylene glycol monoesters, unsaturated polyalkylene oxide base ether monoesters, unsaturated monocarboxylic acid and derivatives monomer thereof and unsaturated thiazolinyl sulfonic acid and sodium salt copolymerization thereof to mix.Can effectively solve sandstone material that silt content is large and the compatibility problem of water reducer, but its effectiveness is subject to the impact of temperature and pH larger.
A kind of preparation method of polycarboxylic acid slump retaining agent is disclosed in CN 102558454A patent; Formed by tail washings, unsaturated polyether and the acrylic acid copolymer derivative of producing propenal.Though can reduce the production cost of slump retaining agent, but it can not stop the absorption of the layered porous internal structure of clay, show when sandstone silt content is high, protect the effect of collapsing undesirable.
Because required river sand in concrete is in recent years used in a large number, therefore relevant company produces the Machine-made Sand that replaces river sand, and the silt content of existing sandstone is very high simultaneously, causes the effect of existing commercially available polycarboxylate water-reducer bad, and concrete slump is undesirable.
Summary of the invention
A kind of concrete slump compensator, its molecular weight is 25000～45000, molecular formula is:
In formula: m=40～60, k=45～70, p=10～30, q=60～100.
The preparation method of above-mentioned concrete slump compensator, comprises the following steps:
Vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl mix, be heated to 50～70 DEG C taking water as dispersion medium, drip Hydroxyethyl Acrylate solution, initiator solution and molecular-weight adjusting agent solution, dropwise rear continuation reaction 1～2h, add alkali to regulate pH to 6～8 to obtain slump compensator.
Press such scheme, the mass ratio of described maleic anhydride mono-methyl and vinylbenzene and methacrylic disulfonate acid is 1:1.2～1.6:0.6-0.8.
Press such scheme, described Hydroxyethyl Acrylate consumption accounts for 6～9%wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass, and 2～3h dropwises.
Press such scheme, described initiator is the mixture of ammonium persulphate and Potassium Persulphate, and ammonium persulphate and Potassium Persulphate mass ratio are 1:1～7; 0.8～1.5%wt%2～3h that the consumption of initiator accounts for vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass dropwises.
Press such scheme, described molecular weight regulator is Thiovanic acid and the mixture of-thiohydracrylic acid, and its mass ratio is 1:1～5; 0.08～0.36%wt%3-4h that the consumption of molecular weight regulator accounts for vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass dropwises.
The application of above-mentioned concrete slump compensator, adds the polycarboxylate water-reducer mix outer slump compensator of mixing 0.2～0.4wt% later in concrete preparation process.
The building-up process of concrete slump compensator of the present invention is as follows:
Beneficial effect of the present invention is:
The Hydroxyethyl Acrylate of introducing in molecular structure of the present invention is hydrolyzed to Carboxylic acid and alcohol under alkaline environment, and wherein carboxylic acid group can play slow setting and guarantor's effect of collapsing, and alcoholic extract hydroxyl group can play delayed coagulation; The maleic anhydride mono-methyl of introducing, wherein-COOH, can complexing Ca
2+, can effectively delay hydrated cementitious; The sulfonic acid group of introducing in molecular structure, can preferentially disperse cement granules, delays hydrated cementitious;
Preparation method is solution polymerization, compares simpler, reasonable, easy to operate with the production technique of existing general slump compensator; The temperature of building-up reactions is lower, and synthesis technique is simple, is easy to synthesize;
Better with the sandstone consistency of Machine-made Sand and high silt content in application process, slump compensation effect is obvious, and the impact of climate is little.
Embodiment
Following examples are explaination technical scheme of the present invention further, but not as the restriction of many present invention protection domain.
Slump compensator preparation process of the present invention is as follows:
Vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl are mixed, be heated to 50～70 DEG C taking water as dispersion medium, drip Hydroxyethyl Acrylate solution, initiator solution and molecular-weight adjusting agent solution, dropwise rear continuation reaction 1～2h, add alkali to regulate pH to 6～8 to obtain slump compensator.
Optimally, the mass ratio of maleic anhydride mono-methyl and vinylbenzene and methacrylic disulfonate acid is 1:1.2～1.6:0.6-0.8.
Optimally, Hydroxyethyl Acrylate consumption accounts for 6～9%wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass, and 2～3h dropwises.
Optimally, initiator is the mixture of ammonium persulphate and Potassium Persulphate, and ammonium persulphate and Potassium Persulphate mass ratio are 1:1～7; 0.8～1.5%wt%2～3h that the consumption of initiator accounts for vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass dropwises.
Optimally, molecular weight regulator is Thiovanic acid and the mixture of-thiohydracrylic acid, and its mass ratio is 1:1～5; 0.08～0.36%wt%3-4h that the consumption of molecular weight regulator accounts for vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass dropwises.
The application method of concrete slump compensator of the present invention: in concrete preparation process, add the later outer 60-120min of polycarboxylate water-reducer mix to mix the slump compensator of 0.2～0.4wt% outward.
Embodiment 1
Press maleic anhydride mono-methyl and prepare burden and mix with the mass ratio 1:1.2:0.8 of methacrylic disulfonate acid with vinylbenzene, be heated to 50 DEG C taking water as dispersion medium after constant temperature; Start to drip the 50wt% Hydroxyethyl Acrylate aqueous solution, 2.5wt% initiator solution (ammonium persulphate and Potassium Persulphate mass ratio are 1:3), the 2.5wt% molecular weight regulator aqueous solution (Thiovanic acid and β-mercaptopropionic acid mass ratio are 1:3); Wherein, the consumption of Hydroxyethyl Acrylate, initiator, molecular weight regulator accounts for respectively 6wt%, 0.8wt%, the 0.08wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl heavy amount, Hydroxyethyl Acrylate solution and initiator solution drip completely at 2h, and molecular-weight adjusting agent solution drips completely at 3h; Add adjusting PH with base=6, insulation 2h, obtains collapse protective poly-carboxylic acid water reducing agent solution.
Embodiment 2
Press maleic anhydride mono-methyl and prepare burden and mix with the mass ratio 1:1.6:0.6 of methacrylic disulfonate acid with vinylbenzene, be heated to 70 DEG C taking water as dispersion medium after constant temperature; Start to drip the 50wt% Hydroxyethyl Acrylate aqueous solution, 2.5wt% initiator solution (ammonium persulphate and Potassium Persulphate mass ratio are 1:1), the 2.5wt% molecular weight regulator aqueous solution (Thiovanic acid and β-mercaptopropionic acid mass ratio are 1:1); Wherein, the consumption of Hydroxyethyl Acrylate, initiator, molecular weight regulator accounts for respectively 9wt%, 1.5wt%, the 0.36wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl heavy amount, Hydroxyethyl Acrylate solution and initiator solution drip completely at 3h, and molecular-weight adjusting agent solution drips completely at 4h; Add adjusting PH with base=6, insulation 2h, obtains collapse protective poly-carboxylic acid water reducing agent solution.
Embodiment 3
Press maleic anhydride mono-methyl and prepare burden and mix with the mass ratio 1:1.4:0.7 of methacrylic disulfonate acid with vinylbenzene, be heated to 60 DEG C taking water as dispersion medium after constant temperature; Start to drip the 50wt% Hydroxyethyl Acrylate aqueous solution, 2.5wt% initiator solution (ammonium persulphate and Potassium Persulphate mass ratio are 1:7), the 2.5wt% molecular weight regulator aqueous solution (Thiovanic acid and β-mercaptopropionic acid mass ratio are 1:5); Wherein, the consumption of Hydroxyethyl Acrylate, initiator, molecular weight regulator accounts for respectively 7.5wt%, 1.1wt%, the 0.22wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl heavy amount, Hydroxyethyl Acrylate solution and initiator solution drip completely at 2h, and molecular-weight adjusting agent solution drips completely at 4h; Add adjusting PH with base=8, insulation 2h, obtains collapse protective poly-carboxylic acid water reducing agent solution.
Embodiment 4
Press maleic anhydride mono-methyl and prepare burden and mix with the mass ratio 1:1.35:0.65 of methacrylic disulfonate acid with vinylbenzene, be heated to 65 DEG C taking water as dispersion medium after constant temperature; Start to drip the 50wt% Hydroxyethyl Acrylate aqueous solution, 2.5wt% initiator solution (ammonium persulphate and Potassium Persulphate mass ratio are 1:4), the 2.5wt% molecular weight regulator aqueous solution (Thiovanic acid and β-mercaptopropionic acid mass ratio are 1:2); Wherein, the consumption of Hydroxyethyl Acrylate, initiator, molecular weight regulator accounts for respectively 6wt%, 1wt%, the 0.1wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl heavy amount, Hydroxyethyl Acrylate solution and initiator solution drip completely at 3h, and molecular-weight adjusting agent solution drips completely at 4h; Add adjusting PH with base=7, insulation 2h, obtains collapse protective poly-carboxylic acid water reducing agent solution.
Embodiment 5
Press maleic anhydride mono-methyl and prepare burden and mix with the mass ratio 1:1.5:0.75 of methacrylic disulfonate acid with vinylbenzene, be heated to 60 DEG C taking water as dispersion medium after constant temperature; Start to drip the 40wt% Hydroxyethyl Acrylate aqueous solution, 30wt% initiator solution (ammonium persulphate and Potassium Persulphate mass ratio are 1:5), the 30wt% molecular weight regulator aqueous solution (Thiovanic acid and β-mercaptopropionic acid mass ratio are 1:3); Wherein, the consumption of Hydroxyethyl Acrylate, initiator, molecular weight regulator accounts for respectively 8wt%, 1.2wt%, the 0.20wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl heavy amount, Hydroxyethyl Acrylate solution and initiator solution drip completely at 3h, and molecular-weight adjusting agent solution drips completely at 4h; Add adjusting PH with base=7, insulation 2h, obtains collapse protective poly-carboxylic acid water reducing agent solution.
Embodiment 6
Press maleic anhydride mono-methyl and prepare burden and mix with the mass ratio 1:1.4:0.65 of methacrylic disulfonate acid with vinylbenzene, be heated to 70 DEG C taking water as dispersion medium after constant temperature; Start to drip the 45wt% Hydroxyethyl Acrylate aqueous solution, 25wt% initiator solution (ammonium persulphate and Potassium Persulphate mass ratio are 1:6), the 25wt% molecular weight regulator aqueous solution (Thiovanic acid and β-mercaptopropionic acid mass ratio are 1:4); Wherein, the consumption of Hydroxyethyl Acrylate, initiator, molecular weight regulator accounts for respectively 9wt%, 1.3wt%, the 0.30wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl heavy amount, Hydroxyethyl Acrylate solution and initiator solution drip completely at 3h, and molecular-weight adjusting agent solution drips completely at 4h; Add adjusting PH with base=7, insulation 2h, obtains collapse protective poly-carboxylic acid water reducing agent solution.
Carry out the experiment of concrete application performance according to GB8076-2008.As shown in table 1.
Cement: 200kg, breeze: 80kg, flyash: 80kg, sand: 790kg, stone: 1080kg, water: 180kg.Wherein cement: the new P.O42.5 of China; Flyash: Yang Luo power plant secondary ash; Breeze: the new S95 level breeze of China.Test is carried out with reference to " concrete for hydraulic structure testing regulation ".
Table 1
The above example 1～6 of contrast can find out, add the concrete slump compensator that the method for the invention makes between 60～120min after fresh concrete mix is complete after, concrete 120min protect plasticity can significantly improve, and has good use value.
Claims (7)
1. a concrete slump compensator, is characterized in that molecular weight is 25000～45000, and molecular formula is:
Wherein, m=40～60, k=45～70, p=10～30, q=60～100.
2. the preparation method of concrete slump compensator described in claim 1, is characterized in that comprising the following steps:
Vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl mix, be heated to 50～70 DEG C taking water as dispersion medium, drip Hydroxyethyl Acrylate solution, initiator solution and molecular-weight adjusting agent solution, dropwise rear continuation reaction 1～2h, add alkali to regulate pH to 6～8 to obtain slump compensator.
3. the preparation method of concrete slump compensator as claimed in claim 2, the mass ratio that it is characterized in that described maleic anhydride mono-methyl and vinylbenzene and methacrylic disulfonate acid is 1:1.2～1.6:0.6-0.8.
4. the preparation method of concrete slump compensator as claimed in claim 2, is characterized in that described Hydroxyethyl Acrylate consumption accounts for 6～9%wt% of vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass, and 2～3h dropwises.
5. the preparation method of concrete slump compensator as claimed in claim 2, is characterized in that described initiator is the mixture of ammonium persulphate and Potassium Persulphate, and ammonium persulphate and Potassium Persulphate mass ratio are 1:1～7; 0.8～1.5%wt%2～3h that the consumption of initiator accounts for vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass dropwises.
6. the preparation method of concrete slump compensator as claimed in claim 2, is characterized in that described molecular weight regulator is Thiovanic acid and the mixture of-thiohydracrylic acid, and its mass ratio is 1:1～5; 0.08～0.36%wt%3-4h that the consumption of molecular weight regulator accounts for vinylbenzene, methacrylic disulfonate acid and maleic anhydride mono-methyl total mass dropwises.
7. the application of concrete slump compensator described in claim 1, is characterized in that adding polycarboxylate water-reducer mix later, to mix the described slump compensator of 0.2～0.4wt% in concrete preparation process.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102351999A (en) * | 2011-07-15 | 2012-02-15 | 清华大学 | Method for preparing nanoparticle water reducing agent |
| CN102603996A (en) * | 2012-02-28 | 2012-07-25 | 武汉理工大学 | Ether type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN103613307A (en) * | 2013-11-22 | 2014-03-05 | 武汉理工大学 | Slump type polycarboxylate superplasticizer and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351999A (en) * | 2011-07-15 | 2012-02-15 | 清华大学 | Method for preparing nanoparticle water reducing agent |
| CN102603996A (en) * | 2012-02-28 | 2012-07-25 | 武汉理工大学 | Ether type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN103613307A (en) * | 2013-11-22 | 2014-03-05 | 武汉理工大学 | Slump type polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20141112 |