CN113292686B - Multifunctional concrete water-retaining agent and preparation method thereof - Google Patents
Multifunctional concrete water-retaining agent and preparation method thereof Download PDFInfo
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- 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
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- 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
- C04B2103/46—Water-loss or fluid-loss reducers, hygroscopic or hydrophilic agents, water retention agents
- C04B2103/465—Water-sorbing agents, hygroscopic or hydrophilic agents
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a multifunctional concrete water-retaining agent. Comprises the following components in parts by weight: 50-150 parts of unsaturated acid, 100-200 parts of unsaturated ester, 20-80 parts of glycol, 5-15 parts of sulfonate, 5-15 parts of alkylphenol polyoxyethylene ether, 1-10 parts of alkylolamide, 0.1-2 parts of oxidant, 0.1-2 parts of reducing agent, 1-10 parts of chain transfer agent and 500-1000 parts of deionized water. Has the advantages that: has a superposition effect with the water reducing component in a certain range, and has small influence on yield shear stress (softness) so as to improve the workability and not influence the strength. The working performance and the construction performance of the concrete are improved, meanwhile, the excellent service performance of the concrete is guaranteed, and the structural damage is reduced. The preparation method is simple, safe and pollution-free, does not need heating and pressurizing, has low requirement on equipment, short reaction time, excellent performance and remarkable economic benefit.
Description
Technical Field
The invention relates to the technical field of concrete water-retaining agents, in particular to a multifunctional concrete water-retaining agent and a preparation method thereof.
Background
The concrete water-retaining agent is also called thickening agent or tackifier, is an additive of a novel building material, can increase cohesiveness and cohesiveness of a cement cementing material, and improves the homogeneity and the performance of a hardened product of concrete. For example, the Chinese invention patent CN108298862A discloses a preparation method of a mortar thickening agent. The corn starch is used as a raw material, the substitution effect of the carboxymethyl starch is improved, and the carboxymethyl starch is used for preventing mortar from segregation and bleeding and preventing water from evaporating too fast or being absorbed too fast by a base material in the initial maintenance stage.
The concrete cohesiveness is improved by adopting thickening agents such as cellulose ether, starch, dextrin, sodium polyacrylate, polyvinyl alcohol and the like, and the limited water retention is ensured on the premise of sacrificing the consumption of polycarboxylic acid water reducing agent and slump retaining agent.
The traditional water-retaining agent utilizes the adsorbability group in the molecular structure, can be adsorbed on the surface of cement particles, and influences the acting force between the cement particles and water molecules, so that the dispersion effect of the water-reducing component is reduced while the viscosity of slurry is increased by the traditional water-retaining thickener.
Therefore, the traditional concrete water-retaining agent solves the technical problems that: (1) With the development of high-strength and high-performance concrete, the water-cement ratio is smaller and smaller, the free water of the concrete is less, the concrete is cracked due to the volume shrinkage in the hydration process, and the concrete water-retaining agent can reduce the water loss and effectively prevent the cracks from being generated. (2) The polycarboxylic acid high-performance water reducing agent has high water reducing performance and sensitivity to materials, and is easy to cause segregation, bleeding and slurry bleeding of concrete mixtures, so that the concrete mixtures lose workability. (3) The requirement of long-distance transportation of concrete is met, and the main reason for large slump loss of concrete is loss of free water. (4) The problem of the defects of the gradation and the mixing proportion of the sandstone materials is how to improve the pore distribution of the concrete by the water-retaining agent.
Meanwhile, in the face of the increasingly competitive additive market, and the situations that the concrete raw materials are lack, complex and poor in quality and the polycarboxylic acid water reducer is high in sensitivity, the multifunctional concrete water-retaining agent with simple production process, economy and environmental protection is provided, the water retention property, the slump retention property and the mechanical property of the concrete are improved, and the constructability and the durability of the concrete are ensured.
Disclosure of Invention
The invention aims to solve the technical problems of poor water retention, poor mixing ratio and gradation, sensitive admixture and the like of concrete, improve the working performance and the construction performance of the concrete, ensure the excellent service performance of the concrete and reduce structural diseases.
In order to realize the purpose, the invention adopts the following technical scheme to realize the purpose:
a multifunctional concrete water-retaining agent comprises the following components in parts by weight: 50-150 parts of unsaturated acid, 100-200 parts of unsaturated ester, 20-80 parts of glycol, 5-15 parts of sulfonate, 5-15 parts of alkylphenol polyoxyethylene ether, 1-10 parts of alkylolamide, 0.1-2 parts of oxidant, 0.1-2 parts of reducing agent, 1-10 parts of chain transfer agent and 500-1000 parts of deionized water.
Further, the unsaturated acid is one of acrylic acid and methacrylic acid; the unsaturated ester is one or more of methyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, 4-hydroxybutyl acrylate and n-butyl methacrylate; the sulfonate is selected from sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl diphenyl oxide disulfonate, sodium hexadecyl diphenyl oxide disulfonate, sodium methyl propylene sulfonate and alpha-sodium alkenyl sulfonate.
Further, the diol is one or more of diethylene glycol, dipropylene glycol, 1, 2-butanediol and 2, 3-butanediol.
Further, the alkylphenol polyoxyethylene is one of nonylphenol polyoxyethylene and octylphenol polyoxyethylene.
Further, the alkylolamide is one or more of alkylolamide phosphate and coconut oil fatty acid diethanolamide.
Further, the oxidant is one or more of ammonium persulfate, potassium persulfate, hydrogen peroxide and tert-butyl hydroperoxide.
Further, the reducing agent is one or more of sodium formaldehyde sulfoxylate, L-sodium ascorbate, E51 and ferrous sulfate.
Further, the chain transfer agent is sodium hypophosphite.
The invention also provides a preparation method of the multifunctional concrete water-retaining agent, which comprises the following steps:
s1, at normal temperature, putting deionized water, unsaturated acid, unsaturated ester, dihydric alcohol, sulfonate, alkylphenol polyoxyethylene ether and alkylolamide into a reaction kettle, and uniformly stirring to obtain a mixture of the components.
And S2, sequentially adding an oxidant, a reducing agent and a chain transfer agent into the mixture obtained in the S1, continuing stirring for 10 minutes, stopping stirring, and standing for reaction.
And S3, stirring when the reaction temperature in the step S2 rises to 60 ℃, stopping stirring after the temperature stops rising, continuously standing for reaction for 1h, and then preparing the concrete water-retaining agent.
(the temperature at which the temperature rise is stopped is related to the amount and type of the redox agent, and generally the temperature is 50-60 ℃, and the temperature rise is stopped when the temperature continues to rise by about 2 ℃ at most after the stirring is started.)
The invention also provides concrete added with the multifunctional concrete water-retaining agent, wherein the mixing amount of the water-retaining agent relative to the concrete raw materials is 0.05-0.1wt%.
The principle of the invention is as follows:
the unsaturated acid, the unsaturated ester, the diol and the amide used in the invention have high reaction activity, generate self-polymerization or crosslinking in a redox system, and wrap the nonionic surfactant (alkylolamide) therein to form a three-dimensional network structure. Namely, the viscosity of the aqueous phase system is increased by winding the molecular chain per se, and the molecular chain forms a three-dimensional structure in space. Dense carboxyl, hydroxyl, sulfonic group, amide and other groups contained in the molecular chain can tightly hold water molecules to play a role in water retention.
The three-dimensional network structure formed by winding the molecular chains, and the surfactant wrapped in the three-dimensional network structure can well form an interface among water, air and cement particles due to the action of interfacial activity, so that the plumpness of slurry is improved, and the wrapping property of concrete is improved.
The invention adopts alkylolamide as the nonionic surfactant, and because the alkylolamide molecule contains amide bonds, the alkylolamide has the advantages different from the traditional nonionic surfactant, has good dispersing performance and good foam stabilizing performance.
The chain transfer agent adopted by the invention is sodium hypophosphite which has different activity from the commonly used chain transfer agent, the commonly used chain transfer agent comprises isopropanol, sodium hypophosphite, mercaptoethanol, 3-mercaptopropionic acid, mercaptoacetic acid and the like, but the chain transfer activity of the isopropanol, the mercaptoethanol and the like is too high, and the method is not suitable for the standing reaction system.
The multifunctional concrete water-retaining agent prepared by the invention has different action mechanisms with the traditional water-retaining thickener, the traditional water-retaining thickener is easy to adsorb on the surface of cement particles to form bridging, the adsorption of water-reducing components by the cement particles is influenced, the viscosity of the system is increased, the dispersion effect of the water-reducing components is reduced, and the influence on the water-reducing rate is obvious. The multifunctional concrete water-retaining agent prepared by the invention belongs to a non-adsorption type, only acts on free water in concrete, and increases the water-retaining property of a free system by increasing the molecular chain of the multifunctional concrete water-retaining agent; the cohesiveness and cohesiveness of the cement binding material are improved, and meanwhile, the longitudinal dispersion of the binding material is promoted, so that the concrete mixture has the capability of keeping moisture in the construction process, and the working performance of the concrete is ensured.
Has the advantages that:
1. the water-retaining agent prepared by the invention does not influence the acting force between cement particles and water molecules, and the dispersing capacity of the water-reducing agent on the cement particles, the water-retaining agent plays a role in dispersing free water, has a superposition effect with water-reducing components in a certain range, and has small influence on yield shear stress (softness) so as to improve the workability and not influence the strength.
2. The multifunctional concrete water-retaining agent prepared by the invention has outstanding material effects on thick aggregates, large pores and slurry needing a stable suspension system with a certain consistency; at present, the sensitivity is fully verified, and the pump can still meet the requirement of pumping under the condition that the standard doping amount is increased by 20-50 percent, although the segregation exists, the ground is not grabbed, and the softness is good; the adaptability to river sand is verified, and the water retention and the pulp extraction capacity are obviously improved, so that the fluidity and the retentivity are improved; the verification shows that the concrete pump damage condition is greatly broken through. The working performance and the construction performance of the concrete are improved, meanwhile, the excellent service performance of the concrete is guaranteed, and the structural damage is reduced.
3. The multifunctional concrete water-retaining agent provided by the invention has the advantages of simple preparation method, safety, no pollution, no need of heating and pressurizing, low requirement on equipment, short reaction time, excellent performance and remarkable economic benefit.
Detailed Description
The technical solution of the present invention is further described in detail with reference to specific examples, but the present invention is not limited to the following technical solutions. The "parts" in the following examples may be in units of mass such as "Kg" or the like.
Example 1
Embodiment 1 provides a multifunctional concrete water-retaining agent, which is prepared from the following raw materials in parts by weight: 50 parts of acrylic acid, 120 parts of methyl acrylate, 30 parts of diethylene glycol, 5 parts of sodium dodecyl sulfate, 5 parts of sodium methyl propylene sulfonate, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of alkyl alcohol amide phosphate, 1 part of ammonium persulfate, 0.5 part of L-sodium ascorbate, 6 parts of sodium hypophosphite and 530 parts of deionized water.
A preparation method of a multifunctional concrete water-retaining agent comprises the following steps: at normal temperature, deionized water, acrylic acid, methyl acrylate, diethylene glycol, sulfonate, sodium dodecyl sulfate, sodium methyl acrylate sulfonate, nonylphenol polyoxyethylene ether and alkylolamide phosphate are put into a reaction kettle and stirred uniformly. After stirring evenly, sequentially adding ammonium persulfate, L-sodium ascorbate and sodium hypophosphite, continuing stirring for 10 minutes, stopping stirring, and standing for reaction. And starting stirring when the temperature rises to 60 ℃, stopping stirring after the temperature stops rising, and continuously standing for reaction for 1 hour.
Example 2
Example 2 provides a multifunctional concrete water-retaining agent, which has the same preparation steps as example 1, except that the multifunctional concrete water-retaining agent is composed of the following raw materials in parts by weight: 100 parts of methacrylic acid, 120 parts of hydroxyethyl acrylate, 50 parts of dipropylene glycol, 4 parts of sodium dodecyl benzene sulfonate, 4 parts of sodium dodecyl diphenyl ether disulfonate, 4 parts of sodium methyl propylene sulfonate, 5 parts of octyl phenol polyoxyethylene ether, 3 parts of alkylolamide phosphate, 1.5 parts of hydrogen peroxide, 0.5 part of E51, 6 parts of sodium hypophosphite and 695 parts of deionized water.
Example 3
Example 3 provides a multifunctional concrete water-retaining agent, which has the same preparation steps as example 1, except that the multifunctional concrete water-retaining agent consists of the following raw materials in parts by weight: 80 parts of methacrylic acid, 200 parts of hydroxyethyl acrylate, 80 parts of 1, 2-butanediol, 3 parts of hexadecyl diphenyl ether disulfonic acid, 5 parts of sodium methallyl sulfonate, 10 parts of octyl phenol polyoxyethylene ether, 5 parts of coconut oil fatty acid diethanolamide, 0.8 part of potassium persulfate, 1 part of L-sodium ascorbate, 0.2 part of ferrous sulfate, 8 parts of sodium hypophosphite and 910 parts of deionized water.
Example 4
Example 4 provides a multifunctional concrete water-retaining agent, which has the same preparation steps as example 1, except that no redox agent and no chain transfer agent are used, and the multifunctional concrete water-retaining agent is composed of the following raw materials in parts by weight: 50 parts of acrylic acid, 120 parts of methyl acrylate, 30 parts of diethylene glycol, 5 parts of sodium dodecyl sulfate, 5 parts of sodium methallyl sulfonate, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of alkylolamide phosphate and 530 parts of deionized water.
Performance test of multifunctional concrete water-retaining agent
In order to test the performance of the multifunctional concrete water-retaining agent disclosed in embodiments 1 to 4 of the invention, a concrete performance test is performed according to GB/T50080-2016 Standard for testing the Performance of common concrete mixtures and GB/T8076-2008 concrete Admixture.
Table 1: concrete mixing proportion
Table 2: admixture compounding mode
| Number of | Water reducing mother liquor/g | Sodium gluconate/g | Water retention agent/g | Water/g |
| Datum | 100 | 25 | 0 | 875 |
| A | 100 | 25 | 10 | 855 |
| B | 100 | 25 | 20 | 835 |
| C | 100 | 25 | 40 | 815 |
| D | 100 | 25 | 60 | 795 |
Adaptability verification of water-retaining agent
Table 3: adaptability verification data of water-retaining agent
Note: the data measured in the table correspond to the formula of the additive B, and the mixing amount of the water reducing agent is 2.1 percent.
And (4) conclusion: the data in table 1,3 illustrate that the water-retaining agent prepared by the present invention can significantly improve the working performance of concrete. The data of the first proportioning and the second proportioning prove that the concrete water-retaining agent has good improvement effect on the materials with thick aggregate, large pores and a stable suspension system with certain consistency required by slurry; the data of the ratio 1 and the ratio three prove that the concrete water-retaining agent has good improvement effect on river sand with less powder, round and smooth particles and poor water-retaining property; the data of the ratio 1 and the ratio three prove that the concrete water-retaining agent has a good improvement effect on the softness of high-grade concrete, and simultaneously the concrete strength is not influenced.
Sensitivity verification of water-retaining agent
Table 4: water retention agent sensitivity verification data
Note: the data measured in this table correspond to the additive formulation No. B, mix ratio 1.
And (4) conclusion: the data in Table 4 prove that even though segregation and bleeding exist under the condition of increasing the mixing amount of the water reducing agent by 3-4 points, the water reducing agent does not grab the ground, has good softness, can still meet the pumping requirement and reduces the sensitivity of the water reducing agent.
Verification of dosage of water-retaining agent
Table 5: verification data of water-retaining agent dosage
Note: the data measured in the table correspond to the mixing proportion of 1 and the admixture mixing amount of 2.3wt%.
And (4) conclusion: the data in Table 5 show that the optimal dosage of the concrete water-retaining agent is 20 kg-30 kg (with the dosage of 0.05-0.1 wt%), the water-retaining property is not obvious when the dosage is too low, the concrete is not obviously improved when the dosage is too high, the cost is wasted, and the concrete is not negatively influenced.
Mechanical property verification of water-retaining agent
Table 6: mechanical property test data of water-retaining agent
And (4) conclusion: the data in table 5 illustrate the effect of water-retaining agents on mechanical properties of concrete, and the use of water-retaining agents in concrete can improve the quality of concrete, including strength (compressive strength) and durability (tensile strength at cleavage, breaking strength).
In conclusion, it can be seen from tables 3-6 that the adaptability, sensitivity and mechanical properties of the water-retaining agent prepared by the invention are superior to those of the water-retaining agent without water-retaining agent.
Claims (7)
1. A preparation method of a multifunctional concrete water-retaining agent is characterized by comprising the following steps in parts by weight: 50-150 parts of unsaturated acid, 100-200 parts of unsaturated ester, 20-80 parts of glycol, 5-15 parts of sulfonate, 5-15 parts of alkylphenol polyoxyethylene ether, 1-10 parts of alkylolamide, 0.1-2 parts of oxidant, 0.1-2 parts of reducing agent, 1-10 parts of chain transfer agent and 500-1000 parts of deionized water;
the preparation method comprises the following steps:
s1, at normal temperature, putting deionized water, unsaturated acid, unsaturated ester, dihydric alcohol, sulfonate, alkylphenol polyoxyethylene ether and alkylolamide into a reaction kettle, and uniformly stirring to obtain a mixture of all components;
s2, sequentially adding an oxidant, a reducing agent and a chain transfer agent into the mixture obtained in the S1, continuing stirring for 10 minutes, stopping stirring, and standing for reaction;
s3, stirring is started when the reaction temperature in the step S2 rises to 60 ℃, stirring is stopped after the temperature stops rising, standing and reacting are continued for 1 hour, and then the concrete water-retaining agent is prepared;
the diol is one or more of diethylene glycol, dipropylene glycol, 1, 2-butanediol and 2, 3-butanediol;
the alkylphenol polyoxyethylene ether is one of nonylphenol polyoxyethylene ether and octylphenol polyoxyethylene ether.
2. The method for preparing the concrete water-retaining agent according to claim 1, wherein the unsaturated acid is one of acrylic acid and methacrylic acid; the unsaturated ester is one or more of methyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, 4-hydroxybutyl acrylate and n-butyl methacrylate; the sulfonate is selected from sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl diphenyl ether disulfonate, sodium hexadecyl diphenyl ether disulfonate, sodium methyl propylene sulfonate and alpha-sodium alkenyl sulfonate.
3. The preparation method of the concrete water-retaining agent according to claim 1, characterized in that the alkyl alcohol amide is one or more of alkyl alcohol amide phosphate and coconut oil fatty acid diethanol amide.
4. The preparation method of the concrete water-retaining agent according to claim 1, characterized in that the oxidant is one or more of ammonium persulfate, potassium persulfate, hydrogen peroxide and tert-butyl hydroperoxide.
5. The preparation method of the concrete water-retaining agent according to claim 1, wherein the reducing agent is one or more of sodium formaldehyde sulfoxylate, sodium L-ascorbate, E51 and ferrous sulfate.
6. The method for preparing the concrete water-retaining agent as claimed in claim 1, wherein the chain transfer agent is sodium hypophosphite.
7. A method for preparing the concrete water-retaining agent as claimed in any one of claims 1 to 6, wherein the amount of the water-retaining agent added is 0.05 to 0.1% relative to the concrete raw material.
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| CN112608420B (en) * | 2019-11-25 | 2022-02-18 | 科之杰新材料集团有限公司 | Preparation method of air-entraining type ester polycarboxylate superplasticizer |
| CN112608421B (en) * | 2019-11-25 | 2022-02-18 | 科之杰新材料集团有限公司 | Preparation method of air-entraining ether polycarboxylate superplasticizer |
| CN113999348A (en) * | 2021-11-24 | 2022-02-01 | 湖南金华达建材有限公司 | Viscosity reduction type ester ether copolymerization polycarboxylate superplasticizer and normal-temperature preparation method thereof |
| CN114349902B (en) * | 2021-12-14 | 2023-05-12 | 云南森博混凝土外加剂有限公司 | Stable foam type concrete air entraining agent and preparation method thereof |
| CN116023578B (en) * | 2023-02-17 | 2024-01-30 | 四川琪汇新材料有限责任公司 | Polyesterpolymer concrete water-retaining agent and preparation method thereof |
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