CN111138589B - Concrete viscosity regulator and preparation method and application thereof - Google Patents
Concrete viscosity regulator and preparation method and application thereof Download PDFInfo
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- CN111138589B CN111138589B CN202010013868.0A CN202010013868A CN111138589B CN 111138589 B CN111138589 B CN 111138589B CN 202010013868 A CN202010013868 A CN 202010013868A CN 111138589 B CN111138589 B CN 111138589B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0045—Polymers chosen for their physico-chemical characteristics
- C04B2103/0053—Water-soluble polymers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention relates to a concrete viscosity regulator and a preparation method and application thereof. The raw materials of the concrete viscosity regulator comprise a monomer and an initiator; the monomers comprise unsaturated acid, unsaturated amide and unsaturated organosilicon monomer; the mass ratio of the unsaturated acid to the unsaturated amide to the unsaturated organosilicon monomer is 1: 1-3: 1-2; the dosage of the initiator accounts for 0.8 to 1.7 percent of the total mass of the monomers. The concrete viscosity regulator endows the concrete viscosity regulator with good affinity with cement particles and water reducing agent components in concrete by introducing hydration functional groups and silicon hydroxyl groups, so that the concrete viscosity regulator is better adapted to the alkaline environment of the concrete and is beneficial to improving the workability of the concrete.
Description
Technical Field
The invention relates to the field of concrete, in particular to a concrete viscosity regulator and a preparation method and application thereof.
Background
The concrete viscosity regulator is a kind of chemical additive for regulating concrete viscosity and improving concrete rheological property. The concrete viscosity regulator can greatly improve the construction performance of the concrete in the preparation of common low-grade concrete or high-strength and high-performance concrete, and greatly improves the working performance of the concrete while ensuring the mechanical property of the concrete.
The phenomenon that cement paste, mortar or concrete sinks solid components due to the difference in the density of cement particles, sand or stones from water and floats on the surface of water is called bleeding. Bleeding causes the surface strength of the concrete to decrease. The water can leave the bleeding channel in the floating process. These pores reduce the compactness of the concrete, so that chloride ions, sulfate, carbon dioxide and the like can enter the interior of the concrete more easily, and the durability of the concrete is seriously reduced. In addition, the water pockets formed by the bleeding water under the concrete also reduce the strength of the interface area between the aggregate and the set cement. In the self-compacting concrete, the bleeding can also lead to incomplete filling of the self-compacting concrete mold, thus causing the reduction of the structural strength. In pumping concrete, bleeding can cause the concrete to grab the bottom and block the pipe, thereby reducing production efficiency and increasing labor intensity of workers.
At present, inorganic materials such as silica fume, silica sol and stone powder are mostly adopted as concrete viscosity regulators for reducing the bleeding segregation phenomenon of cement paste, but more polymers such as natural polymers of rice hull ash, wen lian gum, cellulose ether, cellulose derivatives and the like are used. However, the substances have a certain compatibility problem with the water reducing agent, and influence the water reducing and slump retaining performances of the polycarboxylic acid water reducing agent.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a concrete viscosity regulator, which endows the regulator with good affinity with cement particles and water reducing agent components in concrete by introducing hydration functional groups and silicon hydroxyl groups, so that the regulator can better adapt to the alkaline environment of the concrete and is beneficial to improving the workability of the concrete.
The invention also provides a preparation method of the concrete viscosity regulator and application of the concrete viscosity regulator in concrete materials.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the concrete viscosity regulator comprises the raw materials of a monomer and an initiator;
the monomers comprise unsaturated acid, unsaturated amide and unsaturated organosilicon monomer;
the mass ratio of the unsaturated acid to the unsaturated amide to the unsaturated organosilicon monomer is 1: 1-3: 1-2;
the dosage of the initiator accounts for 0.8-1.7% of the total mass of the monomers.
Optionally, the unsaturated acid comprises at least one of acrylic acid, methacrylic acid, or itaconic acid.
Optionally, the unsaturated acid is acrylic acid.
Optionally, the unsaturated amide comprises at least one of acrylamide or N, N-dimethylacrylamide.
Optionally, the unsaturated amide is acrylamide.
Optionally, the unsaturated silicone monomer comprises methacryloxypropyltrimethoxysilane (KH 570).
Optionally, the initiator is selected from redox type initiators.
Optionally, the oxidation type initiator of the redox type initiator is selected from at least one of hydrogen peroxide, ammonium persulfate or potassium persulfate; the reduction type initiator of the redox type initiator is selected from at least one of vitamin C, D-sodium erythorbate or sodium hypophosphite.
Optionally, the oxidation initiator of the redox initiator is hydrogen peroxide.
Optionally, the reduction initiator of the redox-type initiator is sodium hypophosphite.
Optionally, the mass ratio of the oxidized initiator to the reduced initiator is 1-3: 1.
Different from traditional viscosity regulators such as cellulose and welan gum, the concrete viscosity regulator provided by the invention is a water-soluble high-molecular polymer formed by molecular structure design and polymerization, and can solve the problem of poor compatibility in the use process of the traditional viscosity regulator.
The concrete viscosity regulator provided by the invention introduces silicon hydroxyl group by taking unsaturated organosilicon monomer as a raw material, and has two main purposes: on one hand, the silicon hydroxyl can be condensed with the silicon hydroxyl on the surface of the cement particle, so that the silicon hydroxyl is firmly adsorbed on the surface of the cement particle; on the other hand, the viscosity regulator molecules or silicon hydroxyl groups among the molecules can also undergo condensation crosslinking in an alkaline environment, so that the water binding capacity of the viscosity regulator molecules is remarkably improved, and the workability of concrete is improved.
The concrete viscosity modifier provided by the invention introduces an amide group as a hydration functional group, and can expand in water by binding water, thereby playing roles in reducing the void ratio among particles and preventing the liquid from flowing, and reducing the bleeding phenomenon.
The concrete viscosity regulator provided by the invention selects unsaturated carboxylic acid to introduce carboxyl, can be adsorbed on a positively charged area on the surface of a cement particle through electrostatic attraction, and can also be adsorbed on a negatively charged area through calcium ion complexation, so that the concrete viscosity regulator can be well adsorbed on the surface of the cement particle, and thus, when a solution flows through gaps among the particles, the solution does not flow away with the particles.
According to another aspect of the present invention, there is provided a method for preparing any one of the concrete viscosity modifiers described above. The method comprises the following steps:
the reaction solution comprising the monomer and the initiator is polymerized under a non-oxidizing atmosphere.
Optionally, the temperature of the polymerization reaction is 40-60 ℃, and the reaction time is 7-10 h.
Optionally, the non-oxidizing atmosphere is selected from a nitrogen atmosphere and/or an inert gas atmosphere.
Optionally, the solvent of the reaction solution comprises at least one of N, N-dimethylformamide or water.
Optionally, the solvent of the reaction solution is N, N-dimethylformamide.
Optionally, the total concentration of the monomers in the reaction solution is from 20 wt.% to 40 wt.%.
Optionally, after the polymerization is completed, the method further comprises the steps of back precipitation, filtration, purification and drying.
Optionally, the back-precipitating comprises putting the reactant obtained by the polymerization in a poor solvent to precipitate.
As an embodiment of the present invention, the back-precipitating comprises pouring the reactant obtained by the polymerization into a poor solvent to be soaked.
Optionally, the poor solvent comprises acetone.
Optionally, the purification comprises extraction to remove unreacted monomer.
Optionally, the drying is vacuum drying at 20-40 ℃ to constant weight.
As an embodiment of the present invention, the purification comprises extraction removal of unreacted monomers with an extraction solvent.
Optionally, the extraction solvent comprises methanol.
As an embodiment of the present invention, a method for preparing a concrete viscosity modifier includes:
dissolving unsaturated acid and unsaturated amide in a solvent, stirring and heating to a set reaction temperature, continuously introducing non-oxidizing gas for a period of time, dropwise adding an unsaturated organic silicon monomer, adding an initiator, and carrying out polymerization reaction in a non-oxidizing atmosphere; after the polymerization is finished, pouring the reaction crude product into a large amount of poor solvent for fully soaking, filtering, then extracting by using an extraction solvent to remove unreacted monomers, drying in vacuum to constant weight, and storing in a dry environment.
According to another aspect of the invention, the application of any one of the concrete viscosity regulators in concrete materials is also provided.
Compared with the prior art, the invention has the beneficial effects that:
(1) the concrete viscosity regulator provided by the invention can be well dissolved in a polycarboxylic acid water reducing agent solution, obviously improves the workability of concrete under the condition of not influencing the water reducing and slump retaining performances of the polycarboxylic acid water reducing agent, and simultaneously reduces the sensitivity of the polycarboxylic acid water reducing agent to the change of water consumption.
(2) The concrete viscosity regulator provided by the invention is a water-soluble high polymer formed by molecular structure design polymerization, and the hydration functional group and the silicon hydroxyl group are introduced, so that the regulator has good affinity with cement particles and water reducing agent components in concrete, the problem of poor compatibility in the use process of the traditional viscosity regulator is solved, the traditional viscosity regulator is better adapted to the alkaline environment of the concrete, and the workability of the concrete is improved.
(3) The concrete viscosity regulator provided by the invention can solve the problems that the polycarboxylic acid high-performance water reducing agent is sensitive to the mixing amount and the water consumption, the concrete apparent bubbles are more, the loss after pumping is large and the like.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
Respectively weighing 10g of acrylic acid and 20g of acrylamide, dissolving in 150g of water, heating to the reaction temperature of 40 ℃ under stirring, and adding 0.63g (with the content of 30%) of oxidative initiator hydrogen peroxide; 20g of the silicone monomer KH570 and 0.19g of vitamin C were weighed out and dissolved in 50g of N, N-dimethylformamide.
And continuously introducing nitrogen into the aqueous solution of acrylic acid and acrylamide for 30min, dropwise adding an N, N-dimethylformamide solution of an organic silicon monomer KH570 and vitamin C, and continuously stirring and reacting for 8h under the protection of nitrogen to obtain an AA/AM/KH570 crude product.
Pouring the crude product into a large amount of acetone, soaking for 24h, and filtering; extracting with methanol to remove unreacted monomers; vacuum drying at 35 deg.C to remove methanol, and storing in a desiccator. Is denoted as T1#A viscosity modifier.
Example 2
Respectively weighing 10g of itaconic acid and 30g of N, N-dimethylacrylamide, dissolving in 150g of N, N-dimethylformamide, heating to the reaction temperature of 60 ℃ under stirring, and adding 0.5g of oxidative initiator ammonium persulfate; 15g of the organosilicon monomer KH570 and 0.25g D-sodium erythorbate were weighed out and dissolved in 50g of N, N-dimethylformamide.
And continuously introducing nitrogen into the N, N-dimethylformamide solution of acrylic acid and acrylamide for 30min, dropwise adding the N, N-dimethylformamide solution of an organic silicon monomer KH570 and D-sodium erythorbate, and continuously stirring and reacting for 7h under the protection of nitrogen to obtain an AA/AM/KH570 crude product.
Pouring the crude product into a large amount of acetone, soaking for 24h, and filtering; extracting with methanol to remove unreacted monomers; vacuum drying at 35 deg.C to remove methanol, and storing in a desiccator. Is denoted as T2#A viscosity modifier.
Example 3
Respectively weighing 20g of methacrylic acid and 20g of acrylamide, dissolving in 150g of N, N-dimethylformamide, heating to the reaction temperature of 50 ℃ under stirring, and adding 0.39g (the content is 30%) of oxidizing initiator potassium persulfate; 20g of the organosilicon monomer KH570 and 0.13g of sodium hypophosphite were weighed out and dissolved in 50g of N, N-dimethylformamide.
And continuously introducing nitrogen into the N, N-dimethylformamide solution of acrylic acid and acrylamide for 30min, dropwise adding the N, N-dimethylformamide solution of an organic silicon monomer KH570 and sodium hypophosphite, and continuously stirring and reacting for 10h under the protection of nitrogen to obtain an AA/AM/KH570 crude product.
Pouring the crude product into a large amount of acetone, soaking for 24h, and filtering; extracting with methanol to remove unreacted monomers; vacuum drying at 35 deg.C to remove methanol, and storing in a desiccator. Is denoted as T3#A viscosity modifier.
Experimental example 1 Effect of application of concrete viscosity modifier
The aggregate components of the concrete used in this example are shown in Table 1. The addition amount of the polycarboxylate superplasticizer is 2% of the dosage of the concrete viscosity modifier, the addition amount of the prepared viscosity modifier is 3% of that of the polycarboxylate superplasticizer, the application effect of the concrete viscosity modifier is considered, and the specific experimental data are listed in table 2.
In Table 2, the methods for measuring and calculating the spread, slump and strength refer to the methods described in GB/T50080-2002 and GB/T50081-2002.
TABLE 1 concrete solid content
Composition (I) | Cement | Fly ash | Mineral powder | Sand | (Stone) | Water (W) |
Dosage (kg/m)3) | 220 | 80 | 60 | 820 | 1050 | 160 |
Table 2 application effect test data of viscosity modifier
From the results in table 2, it can be seen that the concrete using the viscosity modifier provided by the present invention has more desirable expansion performance, strength and workability than the concrete using no viscosity modifier or using a common commercially available viscosity modifier.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (17)
1. The concrete viscosity regulator is characterized in that the raw materials of the concrete viscosity regulator comprise monomers and an initiator;
the monomer is unsaturated acid, unsaturated amide and unsaturated organosilicon monomer;
the mass ratio of the unsaturated acid to the unsaturated amide to the unsaturated organosilicon monomer is 1: 1-3: 1-2;
the unsaturated acid is itaconic acid;
the unsaturated amide is N, N-dimethylacrylamide;
the dosage of the initiator accounts for 0.8-1.7% of the total mass of the monomers.
2. The concrete viscosity modifier of claim 1, wherein the unsaturated silicone monomer comprises methacryloxypropyltrimethoxysilane.
3. The concrete viscosity modifier of claim 1, wherein the initiator is selected from the group consisting of redox initiators.
4. The concrete viscosity modifier of claim 3, wherein the oxidation initiator of the redox initiator is selected from at least one of hydrogen peroxide, ammonium persulfate or potassium persulfate.
5. The concrete viscosity modifier of claim 3, wherein the oxidation initiator of the redox initiator is hydrogen peroxide.
6. The concrete viscosity modifier of claim 4, wherein the reduced initiator of the redox initiator is selected from at least one of vitamin C, D-sodium erythorbate or sodium hypophosphite.
7. The concrete viscosity modifier of claim 4, wherein the reduced initiator of the redox initiator is sodium hypophosphite.
8. The concrete viscosity modifier according to claim 7, wherein the mass ratio of the oxidized initiator to the reduced initiator is 1 to 3: 1.
9. The method for preparing a concrete viscosity modifier according to any one of claims 1 to 8, comprising:
the reaction solution comprising the monomer and the initiator is polymerized under a non-oxidizing atmosphere.
10. The process according to claim 9, wherein the polymerization temperature is 40 ℃ to 60 ℃ and the reaction time is 7h to 10 h.
11. The method of claim 9, wherein the solvent of the reaction solution comprises at least one of N, N-dimethylformamide or water.
12. The method according to claim 9, wherein the solvent of the reaction solution is N, N-dimethylformamide.
13. The method according to claim 9, wherein the total concentration of the monomers in the reaction solution is 20 wt.% to 40 wt.%.
14. The process of claim 9, further comprising, after polymerization, settling, filtering, purifying, and drying.
15. The method of claim 14, wherein said back-precipitating comprises precipitating the reactants from the polymerization in a poor solvent.
16. The method of claim 14, wherein the purifying comprises stripping to remove unreacted monomer.
17. Use of the concrete viscosity modifier of any one of claims 1 to 8 in concrete materials.
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CN112812242B (en) * | 2021-01-14 | 2022-02-22 | 广东鼎基建材科技有限公司 | Viscosity regulator for concrete and preparation method thereof |
CN112851184A (en) * | 2021-01-28 | 2021-05-28 | 天津冶建特种材料有限公司 | Additive special for tailing sand concrete and preparation method thereof |
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US9416300B2 (en) * | 2011-01-16 | 2016-08-16 | Simpson Strong-Tie Company, Inc. | Low temperature curable adhesive compositions |
CN102492085A (en) * | 2011-12-06 | 2012-06-13 | 扬州大学 | Organosilicon-modified styrene-acrylic architectural waterproof latex and preparation method thereof |
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CN105669911B (en) * | 2016-01-14 | 2018-05-04 | 厦门路桥翔通建材科技有限公司 | A kind of concrete water conservation segregation reducing agent and preparation method thereof |
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