CN112778022A - Concrete curing agent and preparation method thereof - Google Patents
Concrete curing agent and preparation method thereof Download PDFInfo
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- CN112778022A CN112778022A CN202011494072.8A CN202011494072A CN112778022A CN 112778022 A CN112778022 A CN 112778022A CN 202011494072 A CN202011494072 A CN 202011494072A CN 112778022 A CN112778022 A CN 112778022A
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/65—Coating or impregnation with inorganic materials
- C04B41/68—Silicic acid; Silicates
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/04—Preventing evaporation of the mixing water
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5024—Silicates
Abstract
The invention discloses a concrete curing agent which comprises the following raw materials in parts by weight: 10-15 parts of paraffin emulsion, 10-20 parts of styrene-acrylic emulsion, 5-10 parts of repair microcapsule, 5-8 parts of sodium silicate, 5-8 parts of magnesium sulfate, 5-8 parts of aluminum sulfate, 4-10 parts of animal and plant fiber, 10-20 parts of methyl methacrylate, 1-1.5 parts of defoaming agent, 1-3 parts of flatting agent, 0.2-0.4 part of plasticizer and 20-30 parts of deionized water; the invention discloses a preparation process of the concrete curing agent, which is prepared by compounding inorganic components and organic components, is nontoxic, odorless and non-combustible, and is added with a repairing microcapsule, so that the mechanical property of concrete is improved while concrete cracks are repaired and bonded.
Description
Technical Field
The invention belongs to the technical field of concrete additives, and particularly relates to a concrete curing agent and a preparation method thereof.
Background
In the construction or production process of prefabricated materials of highways, airports and cement factories, a large amount of water is needed in the cement solidification and hardening process to carry out hydration reaction of the prefabricated materials, so the water retention and maintenance of a cement gelled structure body directly influences the quality of engineering or engineering prefabricated products. After concrete is poured, the curing period of 7-28 days is usually provided, and the shrinkage of concrete and the cracking caused by the shrinkage are persistent diseases of the quality of concrete engineering and are always concerned by academia and engineering. In order to prevent water from evaporating and losing in the curing process, conditions must be created to fully hydrate the cement in the construction process so as to ensure the strength of the concrete to be continuously increased.
The concrete curing method includes natural curing, curing with curing agent, and the like. The natural curing condition needs to continuously sprinkle a large amount of water on the surface of the concrete, the time and the labor are consumed, the traditional concrete curing agent adopts a protective film to cover the surface, and the water is prevented from volatilizing to the outside by the characteristics of no ventilation and no water permeation, but the air tightness is limited, the effect is difficult to obtain stable guarantee, the overall effect is not good, along with the continuous development of the technology, the macromolecule water-retaining agent and the silicate inorganic material are added into the concrete by the curing agent, but the existing curing agent has poor combining capacity with the concrete, so that the water-retaining effect is not ideal, and the product performance cannot meet the requirements of practical application.
Disclosure of Invention
The invention aims to provide a concrete curing agent and a preparation method thereof
The technical problems to be solved by the invention are as follows:
in the prior art, the concrete curing agent has low effective water retention rate, insufficient compressive strength ratio, no repair to micro-cracks and other problems, and unobvious curing effect on concrete.
The purpose of the invention can be realized by the following technical scheme:
the concrete curing agent comprises the following raw materials in parts by weight: 10-15 parts of paraffin emulsion, 10-20 parts of styrene-acrylic emulsion, 5-10 parts of repair microcapsule, 5-8 parts of sodium silicate, 5-8 parts of magnesium sulfate, 5-8 parts of aluminum sulfate, 4-10 parts of animal and plant fiber, 10-20 parts of methyl methacrylate, 1-1.5 parts of defoaming agent, 1-3 parts of flatting agent, 0.2-0.4 part of plasticizer and 20-30 parts of deionized water;
the concrete curing agent is prepared by the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min under the condition of a rotation speed of 200 plus materials and 400r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 1-2h under the condition of a constant rotation speed to obtain the concrete curing agent.
Further, the preparation method of the repair microcapsule comprises the following steps:
step S11, adding a formaldehyde solution with the mass fraction of 37% and urea into a beaker, stirring for 20-30min under the condition that the rotating speed is 200-300r/min, then adding triethanolamine into the beaker to adjust the pH value to 8-9 to obtain a solution A, transferring the solution A into a three-neck flask, heating under the condition of 70 ℃ water bath, carrying out reflux stirring at the rotating speed of 600r/min, and reacting for 1h to obtain a formaldehyde-urea prepolymer solution;
step S12, adding deionized water and sodium dodecyl benzene sulfonate into a beaker, stirring for 10min at the rotating speed of 60-100r/min, then adding n-octanol into the beaker to obtain a solution B, adding the solution B into a formaldehyde-urea prepolymer solution, simultaneously adding modified epoxy resin into the formaldehyde-urea prepolymer solution, reducing the water bath temperature from 70 ℃ to 50 ℃, carrying out reflux reaction for 30min at the rotating speed of 600r/min, then continuously dropwise adding a sulfuric acid solution with the volume fraction of 2% into the three-neck flask under the condition of constant rotating speed, detecting the pH value in the three-neck flask every 15min, stopping dropwise adding the sulfuric acid solution with the volume fraction of 2% into the three-neck flask until the pH value is 3, adjusting the water bath temperature to 70 ℃, curing for 2h at the rotating speed of 60r/min, then dropwise adding a sodium carbonate solution with the mass fraction of 25% into the three-neck flask, adjusting the pH value to 7-8, standing for 1-3h, cooling to room temperature, transferring to a beaker, washing with deionized water for 3 times, then carrying out vacuum filtration, and drying in a 60 ℃ oven for 10-14h to obtain the repairing microcapsule.
Further, the mass ratio of the formaldehyde solution with the mass fraction of 37% to the urea in the step S11 is 160-170:60-65, and the mass ratio of the deionized water to the sodium dodecyl benzene sulfonate in the step S12 is 280-300: 1.5, the addition amount of n-octanol is 10-20% of the mass of sodium dodecyl benzene sulfonate, and the mass ratio of the solution B, the formaldehyde-urea prepolymer solution and the modified epoxy resin is 300:250: 110-.
Further, the modified epoxy resin in step S12 is made by the steps of:
step S21, adding trifluoropropylmethyl cyclotrisiloxane, ethylenediamine and deionized water into a four-neck flask, controlling the temperature to be 60-70 ℃, starting nitrogen protection and stirring for 5-10h, heating to be 120 ℃ at 100-;
step S22, adding diphenylmethane diisocyanate into a four-neck flask, reacting for 10-13min at the temperature of 40-50 ℃ and the rotation speed of 300-;
and S23, adding epoxy resin E-51 into a three-neck flask, controlling the temperature to be 40-45 ℃, stirring for 20-30min under the condition of the rotation speed of 100-.
Further, in the step S21, the using ratio of the trifluoropropylmethylcyclotrisiloxane to the ethylenediamine to the deionized water to the silane coupling agent KH550 is 1 mol: 2 mol: 0.1-0.5 g: 3-5mL, the mass ratio of the diphenylmethane diisocyanate, the polyether glycol, the dibutyltin dilaurate and the intermediate a in the step S22 is 5-10:20:0.5-1:5, and the mass ratio of the epoxy resin E-51, the intermediate b, the n-butyl glycidyl ether and the diethylenetriamine in the step S23 is 5-10: 3: 3: 0.5-1.
Trifluoropropyl methyl cyclotrisiloxane is utilized to carry out ring-opening polymerization to prepare hydroxyl fluorosilicone oil, silane coupling agent KH550 is utilized to carry out end capping to prepare amino fluorosilicone oil, diphenylmethane diisocyanate and polyether glycol are used to react to prepare isocyanate group end capped prepolymer of fluorine-containing silicon polyurethane, then the prepolymer and epoxy resin are subjected to graft copolymerization reaction to generate epoxy resin containing fluorine and silicon, modified epoxy resin is used as a raw material of a repairing microcapsule and is wrapped by the urea-formaldehyde resin capsule wall generated by formaldehyde and urea to form a repairing microcapsule taking the modified epoxy resin as a core, the repairing microcapsule is added into a concrete curing agent, when the concrete has microcracks, the microcapsule is broken, the repairing agent inside the microcapsule flows out, the modified epoxy resin has strong caking property with the concrete, and the epoxy resin is modified to contain Si-O bonds on one hand, the modified epoxy resin has high adsorption capacity, film forming capacity, hardness, impact resistance, heat resistance and water resistance, and can repair and bond concrete cracks and improve the mechanical property of concrete.
Further, the leveling agent is an organic silicon leveling agent or an acrylic leveling agent.
Further, the plasticizer is dibutyl phthalate.
Further, the defoaming agent is a polyether defoaming agent or a silicone defoaming agent.
Furthermore, the animal and plant fibers are selected from one or more of gelatin, hydroxymethyl cellulose, hydroxyethyl cellulose and hydroxypropyl methyl cellulose which are mixed in any proportion.
Further, the preparation process of the concrete curing agent specifically comprises the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min under the condition of a rotation speed of 200 plus materials and 400r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 1-2h under the condition of a constant rotation speed to obtain the concrete curing agent.
The invention has the beneficial effects that:
the concrete curing agent provided by the invention is prepared by compounding inorganic components and organic components, is nontoxic, odorless and non-combustible, can quickly form a covering film on the surface of concrete, simultaneously reacts with free calcium hydroxide on the superficial layer of the surface of the concrete, is beneficial to improving the surface strength of the concrete, forms a self-dense and firm film on the surface, prevents the water evaporation of the concrete, thereby ensuring the hydration and achieving the purpose of self-curing, adopts the paraffin emulsion and the acrylic emulsion to compound, exerts the synergistic effect to improve the water retention performance of the finally prepared curing agent on the one hand, reduces the influence of the residue of the paraffin film on the surface performance of the concrete on the other hand, and adds sodium silicate to effectively permeate the surface of the concrete to react with a cement hydration product to generate calcium silicate which is insoluble in water and belongs to a nano material and can block capillary pores on the surface of the concrete, the aluminum sulfate and the magnesium sulfate can generate dihydrate gypsum with cement substances, the dihydrate gypsum can be crystallized and expanded in cement-concreting to help to block gaps on the surface of the concrete and reduce water evaporation inside the concrete, and the repairing microcapsules are added to repair and bond concrete cracks and improve the mechanical property of the concrete.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The concrete curing agent comprises the following raw materials in parts by weight: 10 parts of paraffin emulsion, 10 parts of styrene-acrylic emulsion, 5 parts of repair microcapsule, 5 parts of sodium silicate, 5 parts of magnesium sulfate, 5 parts of aluminum sulfate, 4 parts of animal and plant fibers, 10 parts of methyl methacrylate, 1 part of defoaming agent, 1 part of flatting agent, 0.2 part of plasticizer and 20 parts of deionized water;
the concrete curing agent is prepared by the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min at the rotating speed of 200r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 1h under the condition of unchanged rotating speed to obtain the concrete curing agent.
The preparation method of the repair microcapsule comprises the following steps:
step S11, adding a formaldehyde solution with the mass fraction of 37% and urea into a beaker, stirring for 20min at the rotating speed of 200r/min, then adding triethanolamine into the beaker to adjust the pH value to 8 to obtain a solution A, transferring the solution A into a three-neck flask, heating in a water bath condition at 70 ℃, carrying out reflux stirring at the rotating speed of 600r/min, and reacting for 1h to obtain a formaldehyde-urea prepolymer solution;
step S12, adding deionized water and sodium dodecyl benzene sulfonate into a beaker, stirring for 10min under the condition of a rotating speed of 60r/min, then adding n-octanol into the beaker to obtain a solution B, adding the solution B into a formaldehyde-urea prepolymer solution, simultaneously adding modified epoxy resin into the formaldehyde-urea prepolymer solution, reducing the water bath temperature from 70 ℃ to 50 ℃, carrying out reflux reaction for 30min under the condition of a rotating speed of 600r/min, then continuously dropwise adding a sulfuric acid solution with a volume fraction of 2% into the three-neck flask under the condition of a constant rotating speed, detecting the pH value in the three-neck flask every 15min, stopping dropwise adding a sulfuric acid solution with a volume fraction of 2% into the three-neck flask until the pH value is 3, adjusting the water bath temperature to 70 ℃, curing for 2h under the condition of a rotating speed of 60r/min, then dropwise adding a sodium carbonate solution with a mass fraction of 25% into the three-neck flask, adjusting the pH value to 7, standing for 1h, cooling to room temperature, transferring to a beaker, washing with deionized water for 3 times, then carrying out vacuum filtration, and drying in a 60 ℃ oven for 10h to obtain the repair microcapsule.
The mass ratio of the formaldehyde solution with the mass fraction of 37% to the urea in the step S11 is 160:60, and the mass ratio of the deionized water to the sodium dodecyl benzene sulfonate in the step S12 is 280: 1.5, the addition amount of n-octanol is 10% of the mass of sodium dodecyl benzene sulfonate, and the mass ratio of the solution B, the formaldehyde-urea prepolymer solution and the modified epoxy resin is 300:250: 110.
The modified epoxy resin in step S12 is prepared by the steps of:
step S21, adding trifluoropropylmethyl cyclotrisiloxane, ethylenediamine and deionized water into a four-neck flask, controlling the temperature to be 60 ℃, starting nitrogen protection and stirring for 5 hours, heating to 100 ℃, vacuumizing for 1 hour, dropwise adding a silane coupling agent KH550 into the four-neck flask under the constant temperature condition of 75 ℃, continuously reacting for 5 hours under the condition of the rotation speed of 200r/min, heating to 150 ℃, and vacuumizing for 3 hours to obtain an intermediate a;
step S22, adding diphenylmethane diisocyanate into a four-neck flask, reacting for 10min at the temperature of 40 ℃ and the rotation speed of 300r/min, then dropwise adding polyether glycol into the four-neck flask at the dropping speed of 1 drop/sec, heating to 60 ℃, adding dibutyltin dilaurate into the four-neck flask, introducing nitrogen, reacting for 2h at the rotation speed of 500r/min, cooling to 30 ℃, adding an intermediate a, heating to 75 ℃, and reacting for 1h at the rotation speed of 200r/min to obtain an intermediate b;
and step S23, adding epoxy resin E-51 into a three-neck flask, controlling the temperature to be 40 ℃, stirring for 20min at the rotation speed of 100r/min, adding the intermediate b under the protection of nitrogen, heating to 75 ℃, carrying out heat preservation reaction for 4h, adding n-butyl glycidyl ether and diethylenetriamine into the three-neck flask, stirring for 30min at room temperature under the condition that the rotation speed is not changed, vacuumizing to remove bubbles, curing for 4h in an oven at 80 ℃, and curing for 1h at 120 ℃ to obtain the modified epoxy resin.
In the step S21, the dosage ratio of the trifluoropropylmethyl cyclotrisiloxane to the ethylenediamine to the deionized water to the silane coupling agent KH550 is 1 mol: 2 mol: 0.1 g: 3mL, the mass ratio of the diphenylmethane diisocyanate, the polyether diol, the dibutyltin dilaurate to the intermediate a in step S22 is 5:20:0.5, and the mass ratio of the epoxy resin E-51, the intermediate b, the n-butyl glycidyl ether and the diethylenetriamine in step S23 is 5: 3: 3: 0.5.
the leveling agent is an organic silicon leveling agent, the plasticizer is dibutyl phthalate, the defoaming agent is a polyether defoaming agent, and the animal and plant fibers are gelatin.
Example 2
The concrete curing agent comprises the following raw materials in parts by weight: 12 parts of paraffin emulsion, 15 parts of styrene-acrylic emulsion, 8 parts of repair microcapsule, 7 parts of sodium silicate, 7 parts of magnesium sulfate, 7 parts of aluminum sulfate, 8 parts of animal and plant fibers, 15 parts of methyl methacrylate, 1.2 parts of defoaming agent, 2 parts of flatting agent, 0.3 part of plasticizer and 25 parts of deionized water;
the concrete curing agent is prepared by the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min at the rotating speed of 300r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 1.5h under the condition of unchanged rotating speed to obtain the concrete curing agent.
The preparation method of the repair microcapsule comprises the following steps:
step S11, adding a formaldehyde solution with the mass fraction of 37% and urea into a beaker, stirring for 25min at the rotating speed of 250r/min, then adding triethanolamine into the beaker to adjust the pH value to 8 to obtain a solution A, transferring the solution A into a three-neck flask, heating in a water bath condition at 70 ℃, carrying out reflux stirring at the rotating speed of 600r/min, and reacting for 1h to obtain a formaldehyde-urea prepolymer solution;
step S12, adding deionized water and sodium dodecyl benzene sulfonate into a beaker, stirring for 10min at a rotating speed of 80r/min, then adding n-octanol into the beaker to obtain a solution B, adding the solution B into a formaldehyde-urea prepolymer solution, simultaneously adding modified epoxy resin into the formaldehyde-urea prepolymer solution, reducing the water bath temperature from 70 ℃ to 50 ℃, carrying out reflux reaction for 30min at a rotating speed of 600r/min, then continuously dropwise adding a sulfuric acid solution with a volume fraction of 2% into the three-neck flask under the condition that the rotating speed is not changed, detecting the pH value in the three-neck flask every 15min, stopping dropwise adding the sulfuric acid solution with a volume fraction of 2% into the three-neck flask until the pH value is 3, adjusting the water bath temperature to 70 ℃, curing for 2h at a rotating speed of 60r/min, then dropwise adding a sodium carbonate solution with a mass fraction of 25% into the three-neck flask, adjusting the pH value to 7, standing for 1h, cooling to room temperature, transferring to a beaker, washing with deionized water for 3 times, then carrying out vacuum filtration, and drying in a 60 ℃ oven for 12h to obtain the repair microcapsule.
The mass ratio of the formaldehyde solution with the mass fraction of 37% to the urea in the step S11 is 165:62, and the mass ratio of the deionized water to the sodium dodecyl benzene sulfonate in the step S12 is 290: 1.5, the addition amount of n-octanol is 15% of the mass of sodium dodecyl benzene sulfonate, and the mass ratio of the solution B, the formaldehyde-urea prepolymer solution and the modified epoxy resin is 300:250: 115.
The modified epoxy resin in step S12 is prepared by the steps of:
step S21, adding trifluoropropylmethyl cyclotrisiloxane, ethylenediamine and deionized water into a four-neck flask, controlling the temperature to be 65 ℃, starting nitrogen protection and stirring for 8 hours, heating to 110 ℃, vacuumizing for 1.5 hours, dropwise adding a silane coupling agent KH550 into the four-neck flask under the constant temperature condition of 78 ℃, continuously reacting for 6 hours under the condition of the rotating speed of 250r/min, heating to 155 ℃, and vacuumizing for 4 hours to obtain an intermediate a;
step S22, adding diphenylmethane diisocyanate into a four-neck flask, reacting for 12min at the temperature of 45 ℃ and the rotation speed of 400r/min, then dropwise adding polyether glycol into the four-neck flask at the speed of 2 drops/sec, heating to 62 ℃, adding dibutyltin dilaurate into the four-neck flask, introducing nitrogen, reacting for 3h at the rotation speed of 700r/min, cooling to 33 ℃, adding an intermediate a, heating to 78 ℃, and reacting for 1.5h at the rotation speed of 250r/min to obtain an intermediate b;
and step S23, adding epoxy resin E-51 into a three-neck flask, controlling the temperature to be 42 ℃, stirring for 25min at the rotation speed of 150r/min, adding the intermediate b under the protection of nitrogen, heating to 78 ℃, carrying out heat preservation reaction for 5h, adding n-butyl glycidyl ether and diethylenetriamine into the three-neck flask, stirring for 45min at room temperature under the condition that the rotation speed is not changed, vacuumizing to remove bubbles, curing for 4h in an oven at 82 ℃, and curing for 1.5h at 125 ℃ to obtain the modified epoxy resin.
In the step S21, the dosage ratio of the trifluoropropylmethyl cyclotrisiloxane to the ethylenediamine to the deionized water to the silane coupling agent KH550 is 1 mol: 2 mol: 0.3 g: 4mL, the mass ratio of the diphenylmethane diisocyanate, the polyether diol, the dibutyltin dilaurate to the intermediate a in step S22 is 8:20:1, and the mass ratio of the epoxy resin E-51, the intermediate b, the n-butyl glycidyl ether and the diethylenetriamine in step S23 is 8: 3: 3: 0.7.
the leveling agent is an organic silicon leveling agent, the plasticizer is dibutyl phthalate, the defoaming agent is a polyether defoaming agent, and the animal and plant fibers are gelatin.
Example 3
The concrete curing agent comprises the following raw materials in parts by weight: 15 parts of paraffin emulsion, 20 parts of styrene-acrylic emulsion, 10 parts of repair microcapsule, 8 parts of sodium silicate, 8 parts of magnesium sulfate, 8 parts of aluminum sulfate, 10 parts of animal and plant fibers, 20 parts of methyl methacrylate, 1.5 parts of defoaming agent, 3 parts of flatting agent, 0.4 part of plasticizer and 30 parts of deionized water;
the concrete curing agent is prepared by the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min at the rotating speed of 400r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 2h under the condition of unchanged rotating speed to obtain the concrete curing agent.
The preparation method of the repair microcapsule comprises the following steps:
step S11, adding a formaldehyde solution with the mass percentage of 37% and urea into a beaker, stirring for 30min under the condition of the rotating speed of 300r/min, then adding triethanolamine into the beaker to adjust the pH value to 9 to obtain a solution A, transferring the solution A into a three-neck flask, heating under the condition of a water bath at 70 ℃, carrying out reflux stirring at the rotating speed of 600r/min, and reacting for 1h to obtain a formaldehyde-urea prepolymer solution;
step S12, adding deionized water and sodium dodecyl benzene sulfonate into a beaker, stirring for 10min under the condition of the rotating speed of 100r/min, then adding n-octanol into the beaker to obtain a solution B, adding the solution B into a formaldehyde-urea prepolymer solution, simultaneously adding modified epoxy resin into the formaldehyde-urea prepolymer solution, reducing the water bath temperature from 70 ℃ to 50 ℃, carrying out reflux reaction for 30min under the condition of the rotating speed of 600r/min, then continuously dropwise adding a sulfuric acid solution with the volume fraction of 2% into the three-neck flask under the condition of the unchanged rotating speed, detecting the pH value in the three-neck flask every 15min, stopping dropwise adding the sulfuric acid solution with the volume fraction of 2% into the three-neck flask until the pH value is 3, adjusting the water bath temperature to 70 ℃, curing for 2h under the condition of the rotating speed of 60r/min, then dropwise adding a sodium carbonate solution with the mass fraction of 25% into the three-neck flask, adjusting the pH value to 8, standing for 3h, cooling to room temperature, transferring to a beaker, washing with deionized water for 3 times, then carrying out vacuum filtration, and drying in an oven at 60 ℃ for 14h to obtain the repair microcapsule.
The mass ratio of the formaldehyde solution with the mass fraction of 37% to the urea in the step S11 is 170:65, and the mass ratio of the deionized water to the sodium dodecyl benzene sulfonate in the step S12 is 300: 1.5, the addition amount of n-octanol is 20% of the mass of sodium dodecyl benzene sulfonate, and the mass ratio of the solution B, the formaldehyde-urea prepolymer solution and the modified epoxy resin is 300:250: 120.
The modified epoxy resin in step S12 is prepared by the steps of:
step S21, adding trifluoropropylmethyl cyclotrisiloxane, ethylenediamine and deionized water into a four-neck flask, controlling the temperature to be 70 ℃, starting nitrogen protection and stirring for 10 hours, heating to 120 ℃, vacuumizing for 2 hours, dropwise adding a silane coupling agent KH550 into the four-neck flask under the constant temperature condition of 80 ℃, continuously reacting for 7 hours under the condition of the rotating speed of 300r/min, heating to 160 ℃, and vacuumizing for 5 hours to obtain an intermediate a;
step S22, adding diphenylmethane diisocyanate into a four-neck flask, reacting for 13min at the temperature of 50 ℃ and the rotation speed of 500r/min, then dropwise adding polyether glycol into the four-neck flask at the dropping speed of 3 drops/sec, heating to 65 ℃, adding dibutyltin dilaurate into the four-neck flask, introducing nitrogen, reacting for 4h at the rotation speed of 800r/min, cooling to 35 ℃, adding an intermediate a, heating to 80 ℃, and reacting for 2h at the rotation speed of 300r/min to obtain an intermediate b;
and step S23, adding epoxy resin E-51 into a three-neck flask, controlling the temperature to be 45 ℃, stirring for 30min at the rotation speed of 200r/min, adding the intermediate b under the protection of nitrogen, heating to 80 ℃, carrying out heat preservation reaction for 6h, adding n-butyl glycidyl ether and diethylenetriamine into the three-neck flask, stirring for 60min at room temperature under the condition that the rotation speed is not changed, vacuumizing to remove bubbles, curing for 4h in an oven at 85 ℃, and curing for 2h at 130 ℃ to obtain the modified epoxy resin.
In the step S21, the dosage ratio of the trifluoropropylmethyl cyclotrisiloxane to the ethylenediamine to the deionized water to the silane coupling agent KH550 is 1 mol: 2 mol: 0.5 g: 5mL, the mass ratio of the diphenylmethane diisocyanate, the polyether diol, the dibutyltin dilaurate to the intermediate a in the step S22 is 10:20:1:5, and the mass ratio of the epoxy resin E-51, the intermediate b, the n-butyl glycidyl ether and the diethylenetriamine in the step S23 is 10: 3: 3: 1.
the leveling agent is an organic silicon leveling agent, the plasticizer is dibutyl phthalate, the defoaming agent is a polyether defoaming agent, and the animal and plant fibers are gelatin.
Comparative example
The comparative example is a common concrete curing agent in the market.
The concrete curing agents of examples 1 to 3 and comparative example were subjected to performance tests according to JC901-2002 "Cement concrete curing agent" with the test results shown in the following table:
as can be seen from the above table, the concrete curing agents of examples 1-3 have better test results in the tests of effective water retention, 7d compressive strength ratio, 28-day compressive strength ratio, abrasion loss and solid content than the comparative examples, which shows that the concrete curing prepared by the invention has the characteristics of high water retention and improved mechanical properties of concrete.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. The concrete curing agent is characterized by comprising the following raw materials in parts by weight: 10-15 parts of paraffin emulsion, 10-20 parts of styrene-acrylic emulsion, 5-10 parts of repair microcapsule, 5-8 parts of sodium silicate, 5-8 parts of magnesium sulfate, 5-8 parts of aluminum sulfate, 4-10 parts of animal and plant fiber, 10-20 parts of methyl methacrylate, 1-1.5 parts of defoaming agent, 1-3 parts of flatting agent, 0.2-0.4 part of plasticizer and 20-30 parts of deionized water;
the concrete curing agent is prepared by the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min under the condition of a rotation speed of 200 plus materials and 400r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 1-2h under the condition of a constant rotation speed to obtain the concrete curing agent.
2. The concrete curing agent of claim 1, wherein the preparation method of the repair microcapsule comprises the following steps:
step S11, adding a formaldehyde solution with the mass fraction of 37% and urea into a beaker, stirring for 20-30min under the condition that the rotating speed is 200-300r/min, then adding triethanolamine into the beaker to adjust the pH value to 8-9 to obtain a solution A, transferring the solution A into a three-neck flask, heating under the condition of 70 ℃ water bath, carrying out reflux stirring at the rotating speed of 600r/min, and reacting for 1h to obtain a formaldehyde-urea prepolymer solution;
step S12, adding deionized water and sodium dodecyl benzene sulfonate into a beaker, stirring for 10min at the rotating speed of 60-100r/min, then adding n-octanol into the beaker to obtain a solution B, adding the solution B into a formaldehyde-urea prepolymer solution, simultaneously adding modified epoxy resin into the formaldehyde-urea prepolymer solution, reducing the water bath temperature from 70 ℃ to 50 ℃, carrying out reflux reaction for 30min at the rotating speed of 600r/min, then continuously dropwise adding a sulfuric acid solution with the volume fraction of 2% into the three-neck flask under the condition of constant rotating speed, detecting the pH value in the three-neck flask every 15min, stopping dropwise adding the sulfuric acid solution with the volume fraction of 2% into the three-neck flask until the pH value is 3, adjusting the water bath temperature to 70 ℃, curing for 2h at the rotating speed of 60r/min, then dropwise adding a sodium carbonate solution with the mass fraction of 25% into the three-neck flask, adjusting the pH value to 7-8, standing for 1-3h, cooling to room temperature, transferring to a beaker, washing with deionized water for 3 times, then carrying out vacuum filtration, and drying in a 60 ℃ oven for 10-14h to obtain the repairing microcapsule.
3. The concrete curing agent as defined in claim 2, wherein the mass ratio of the formaldehyde solution with 37% mass fraction to the urea in step S11 is 160-170:60-65, and the mass ratio of the deionized water to the sodium dodecylbenzenesulfonate in step S12 is 280-300: 1.5, the addition amount of n-octanol is 10-20% of the mass of sodium dodecyl benzene sulfonate, and the mass ratio of the solution B, the formaldehyde-urea prepolymer solution and the modified epoxy resin is 300:250: 110-.
4. The concrete curing agent of claim 2, wherein the modified epoxy resin in step S12 is prepared by the following steps:
step S21, adding trifluoropropylmethyl cyclotrisiloxane, ethylenediamine and deionized water into a four-neck flask, controlling the temperature to be 60-70 ℃, starting nitrogen protection and stirring for 5-10h, heating to be 120 ℃ at 100-;
step S22, adding diphenylmethane diisocyanate into a four-neck flask, reacting for 10-13min at the temperature of 40-50 ℃ and the rotation speed of 300-;
and S23, adding epoxy resin E-51 into a three-neck flask, controlling the temperature to be 40-45 ℃, stirring for 20-30min under the condition of the rotation speed of 100-.
5. The concrete curing agent of claim 4, wherein the trifluoropropylmethylcyclotrisiloxane, the ethylenediamine, the deionized water and the silane coupling agent KH550 are used in a ratio of 1 mol: 2 mol: 0.1-0.5 g: 3-5mL, the mass ratio of the diphenylmethane diisocyanate, the polyether glycol, the dibutyltin dilaurate and the intermediate a in the step S22 is 5-10:20:0.5-1:5, and the mass ratio of the epoxy resin E-51, the intermediate b, the n-butyl glycidyl ether and the diethylenetriamine in the step S23 is 5-10: 3: 3: 0.5-1.
6. The concrete curing agent of claim 1, wherein the leveling agent is an organic silicon leveling agent or an acrylic leveling agent; the plasticizer is dibutyl phthalate; the defoaming agent is a polyether defoaming agent or an organic silicon defoaming agent; the animal and plant fibers are selected from one or more of gelatin, hydroxymethyl cellulose, hydroxyethyl cellulose and hydroxypropyl methyl cellulose, and are mixed at any ratio.
7. The preparation process of the concrete curing agent according to claim 1, which is characterized by comprising the following steps:
firstly, adding a defoaming agent, a flatting agent and a plasticizer into a reactor, and uniformly stirring and mixing to obtain an organic auxiliary agent; adding sodium silicate, magnesium sulfate, aluminum sulfate and deionized water into a reactor, and uniformly stirring and mixing to obtain an inorganic auxiliary agent;
and secondly, sequentially adding the paraffin emulsion, the styrene-acrylic emulsion and the methyl methacrylate into a reaction kettle, stirring for 30min under the condition of a rotation speed of 200 plus materials and 400r/min, adding the organic auxiliary agent, the animal and plant fibers, the repairing microcapsule and the inorganic auxiliary agent into the reaction kettle, and mixing for 1-2h under the condition of a constant rotation speed to obtain the concrete curing agent.
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