CN110698845A - Preparation method of concrete curing agent - Google Patents
Preparation method of concrete curing agent Download PDFInfo
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- CN110698845A CN110698845A CN201910841981.5A CN201910841981A CN110698845A CN 110698845 A CN110698845 A CN 110698845A CN 201910841981 A CN201910841981 A CN 201910841981A CN 110698845 A CN110698845 A CN 110698845A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
-
- 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
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/46—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 organic materials
- C04B41/48—Macromolecular compounds
- C04B41/488—Other macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
- C04B41/4884—Polyurethanes; Polyisocyanates
-
- 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
- C04B41/62—Coating or impregnation with organic materials
- C04B41/63—Macromolecular 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
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
- C08F2/008—Processes of polymerisation cleaning reaction vessels using chemicals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
A preparation method of a concrete curing agent comprises the steps of reacting methyl methacrylate with organic montmorillonite under the action of an initiator to obtain a composite prepolymer; mixing the obtained composite prepolymer with polyether polyurethane resin and epoxy resin according to a weight ratio of 1-3: 5-8: 2-5, mixing to obtain a modified polyurethane emulsion; when in use, the modified polyurethane emulsion and the cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.1-0.5 of the curing agent for concrete. The beneficial effects are that solve present concrete curing agent under the condition of high temperature lack of water, the water loss is too fast, can't obtain supplementing, influences the problem of concrete quality.
Description
Technical Field
The invention belongs to the field of building materials, and particularly relates to a preparation method of a concrete curing agent.
Background
The performance of concrete as one of the building materials with large dosage and wide application in the building engineering depends on the composition and the proportion of the concrete raw materials and further depends on the maintenance after pouring. The concrete is not cured or not cured in place after being poured, so that the water in the concrete is evaporated to the outside through the fine capillary holes of the system, and various performance indexes of the concrete are reduced. The traditional concrete curing method mainly comprises water curing, steam curing, landfill curing, straw bag laying and plastic film laying, and the curing method is time-consuming, labor-consuming, energy-consuming, unstable in curing effect, low in protection rate and poor in curing effect, cannot effectively block water evaporation, and is especially suitable for high-temperature water-deficient areas.
The curing agent is applied to curing, after the concrete is constructed, a layer of chemical substance with film-forming property and permeability is sprayed or smeared on the surface of the concrete, and the chemical substance forms a layer of uniform and continuous compact film in a short time, so that the evaporation of water in the concrete is inhibited, and the full hydration of the cementing material is promoted. The invention patent with the application number of 201910332003.8 discloses a concrete curing agent which is obtained by mixing a polymer emulsion, a film forming agent and a penetrating agent, and the water loss is blocked by the film forming of the polymer emulsion. However, the concrete curing agent cannot effectively store water under the condition of high-temperature water shortage and rapid water loss, and secondary supplement is carried out.
Disclosure of Invention
The invention mainly aims to provide a concrete curing agent, which solves the problems that the existing concrete curing agent has too fast water loss under the condition of high temperature and water shortage, cannot be supplemented and influences the quality of concrete.
In order to achieve the technical effects, the invention adopts the following technical scheme:
(1) calcium hydroxide was added to methyl methacrylate, and the polymerization inhibitor was removed by distillation at 80 ℃.
(2) The organic montmorillonite was dried at 70 ℃ for 24 hours.
(3) Preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85. the washing solution is poured into a reaction kettle to be soaked for 12 hours and then washed with ethyl acetate for three times.
(4) Preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, standing is carried out for 24 hours, and water removal and filtration are carried out.
(5) 80-90 parts of methyl methacrylate, 10-20 parts of organic montmorillonite, and the amount of an initiator is N (methyl methacrylate): adding N (initiator) 8000:1 into a reaction kettle, and charging nitrogen for protection. And reacting for 2 hours at the stirring speed of 200-300 r/min and the temperature of 130 ℃ to obtain the composite prepolymer.
(6) And (3) mixing the composite prepolymer obtained in the step (5) with polyether polyurethane resin and epoxy resin according to a weight ratio of 1-3: 5-8: 2-5 to obtain the modified polyurethane emulsion.
When in use, the modified polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.1-0.5 of the curing agent is added to be used as a concrete curing agent to generate a crosslinking reaction to form a three-dimensional network structure.
Wherein the organic montmorillonite in the step (2) is quaternary ammonium salt modified montmorillonite, and the particle size is 2-8 microns;
the molecular weight of organisms in the composite prepolymer in the step (5) is 1000-2000;
in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 3000-4000, and the solid content is 45%; the epoxy resin is linear aliphatic epoxy resin, the molecular weight is 2000-3000, and the epoxy value is 0.25-0.45.
The invention has the beneficial effects that:
(1) the modified polyurethane emulsion obtained by compounding the polymer materials with the three structures can effectively absorb water, and can be supplemented when the water in the concrete is reduced; wherein the epoxy resin can slow down the cavity collapse caused by the output of water in the structure, thereby reducing the strength.
(2) The organic montmorillonite has a layered structure, is distributed in concrete, has a water-proof effect, and can reduce the influence of the external temperature change on the contraction and the like of the concrete under the high-temperature environment due to the heat insulation effect of the montmorillonite.
Detailed Description
For further understanding of the present invention, the following embodiments are provided to illustrate the technical solutions of the present invention in detail, and the scope of the present invention is not limited by the following embodiments.
Example 1
A preparation method of a concrete curing agent comprises the following steps: the method comprises the following steps:
(1) calcium hydroxide was added to methyl methacrylate, and the polymerization inhibitor was removed by distillation at 80 ℃.
(2) The organic montmorillonite was dried at 70 ℃ for 24 hours.
(3) Preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85. the washing solution is poured into a reaction kettle to be soaked for 12 hours and then washed with ethyl acetate for three times.
(4) Preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, standing is carried out for 24 hours, and water removal and filtration are carried out.
(5) 80 parts of methyl methacrylate, 20 parts of organic montmorillonite, and the amount of an initiator is N (methyl methacrylate): adding N (initiator) 8000:1 into a reaction kettle, and charging nitrogen for protection. Reacting for 2 hours at the stirring speed of 300 r/min and the temperature of 130 ℃ to obtain the composite prepolymer.
(6) And (3) mixing the composite prepolymer obtained in the step (5) with polyether polyurethane resin and epoxy resin according to the weight ratio of 1: 5: 2 mixing to obtain the modified polyurethane emulsion.
When in use, the modified polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.1, generating a crosslinking reaction to form a three-dimensional network structure.
Wherein the organic montmorillonite in the step (2) is quaternary ammonium salt modified montmorillonite with the particle size of 2 microns;
the molecular weight of organisms in the composite prepolymer in the step (5) is 1000;
in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 3000, and the solid content is 45%; the epoxy resin is linear aliphatic epoxy resin, and has a molecular weight of 2000 and an epoxy value of 0.25.
Example 2
A preparation method of a concrete curing agent comprises the following steps: the method comprises the following steps:
(1) calcium hydroxide was added to methyl methacrylate, and the polymerization inhibitor was removed by distillation at 80 ℃.
(2) The organic montmorillonite was dried at 70 ℃ for 24 hours.
(3) Preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85. the washing solution is poured into a reaction kettle to be soaked for 12 hours and then washed with ethyl acetate for three times.
(4) Preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, standing is carried out for 24 hours, and water removal and filtration are carried out.
(5) 90 parts of methyl methacrylate, 10 parts of organic montmorillonite, and the amount of an initiator is N (methyl methacrylate): adding N (initiator) 8000:1 into a reaction kettle, and charging nitrogen for protection. Reacting for 2 hours at the stirring speed of 200 r/min and the temperature of 130 ℃ to obtain the composite prepolymer.
(6) And (3) mixing the composite prepolymer obtained in the step (5) with polyether polyurethane resin and epoxy resin according to the weight ratio of 3: 8: 5 mixing to obtain the modified polyurethane emulsion.
When in use, the modified polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.5, generating a crosslinking reaction to form a three-dimensional network structure.
Wherein the organic montmorillonite in the step (2) is quaternary ammonium salt modified montmorillonite with the particle size of 8 microns;
the molecular weight of organisms in the composite prepolymer in the step (5) is 2000;
in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 4000, and the solid content is 45%; the epoxy resin is linear aliphatic epoxy resin, and has a molecular weight of 3000 and an epoxy value of 0.45.
Example 3
A preparation method of a concrete curing agent comprises the following steps: the method comprises the following steps:
(1) calcium hydroxide was added to methyl methacrylate, and the polymerization inhibitor was removed by distillation at 80 ℃.
(2) The organic montmorillonite was dried at 70 ℃ for 24 hours.
(3) Preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85. the washing solution is poured into a reaction kettle to be soaked for 12 hours and then washed with ethyl acetate for three times.
(4) Preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, standing is carried out for 24 hours, and water removal and filtration are carried out.
(5) 85 parts of methyl methacrylate, 15 parts of organic montmorillonite, and the amount of an initiator is N (methyl methacrylate): adding N (initiator) 8000:1 into a reaction kettle, and charging nitrogen for protection. Reacting for 2 hours at the stirring speed of 200-300 r/min and the temperature of 130 ℃ to obtain the composite prepolymer.
(6) Mixing the composite prepolymer obtained in the step (5) with polyether polyurethane resin and epoxy resin according to the weight ratio of 2: 6: 3 mixing to obtain the modified polyurethane emulsion.
When in use, the modified polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.4, generating a crosslinking reaction to form a three-dimensional network structure.
Wherein the organic montmorillonite in the step (2) is quaternary ammonium salt modified montmorillonite with the particle size of 5 microns;
the molecular weight of organisms in the composite prepolymer in the step (5) is 1500;
in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 3500, and the solid content is 45%; the epoxy resin is linear aliphatic epoxy resin, and has a molecular weight of 2500 and an epoxy value of 0.35.
Comparative example 1
A preparation method of a concrete curing agent comprises the following steps: the method comprises the following steps:
(1) calcium hydroxide was added to methyl methacrylate, and the polymerization inhibitor was removed by distillation at 80 ℃.
(2) The organic montmorillonite was dried at 70 ℃ for 24 hours.
(3) Preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85. the washing solution is poured into a reaction kettle to be soaked for 12 hours and then washed with ethyl acetate for three times.
(4) Preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, standing is carried out for 24 hours, and water removal and filtration are carried out.
(5) 80 parts of methyl methacrylate, 20 parts of organic montmorillonite, and the amount of an initiator is N (methyl methacrylate): adding N (initiator) 8000:1 into a reaction kettle, and charging nitrogen for protection. Reacting for 2 hours at the stirring speed of 300 r/min and the temperature of 130 ℃ to obtain the composite prepolymer.
(6) Mixing the composite prepolymer obtained in the step (5) with polyether polyurethane resin according to the weight ratio of 1: 5 mixing to obtain the modified polyurethane emulsion.
When in use, the modified polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.1, generating a crosslinking reaction to form a three-dimensional network structure.
Wherein the organic montmorillonite in the step (2) is quaternary ammonium salt modified montmorillonite with the particle size of 2 microns;
the molecular weight of organisms in the composite prepolymer in the step (5) is 1000;
in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 3000, and the solid content is 45%; .
Comparative example 2
A preparation method of a concrete curing agent comprises the following steps: the method comprises the following steps:
(1) calcium hydroxide was added to methyl methacrylate, and the polymerization inhibitor was removed by distillation at 80 ℃.
(3) Preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85. the washing solution is poured into a reaction kettle to be soaked for 12 hours and then washed with ethyl acetate for three times.
(4) Preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, standing is carried out for 24 hours, and water removal and filtration are carried out.
(5) 80 parts by weight of methyl methacrylate, and the amount of an initiator is N (methyl methacrylate): adding N (initiator) 8000:1 into a reaction kettle, and charging nitrogen for protection. The reaction was carried out at 130 ℃ for 2 hours at a stirring speed of 300 rpm to obtain a prepolymer.
(6) And (3) mixing the prepolymer obtained in the step (5), polyether polyurethane resin and epoxy resin according to the weight ratio of 1: 5: 2 mixing to obtain the modified polyurethane emulsion.
When in use, the modified polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.1, generating a crosslinking reaction to form a three-dimensional network structure.
Wherein the molecular weight of the organism in the composite prepolymer in the step (5) is 1000;
in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 3000, and the solid content is 45%; the epoxy resin is linear aliphatic epoxy resin, and has a molecular weight of 2000 and an epoxy value of 0.25.
Comparative example 3
Example 1 of the invention patent application No. 201910332003.8 was used as comparative example 3
The materials obtained in examples and comparative examples were subjected to performance tests, and the results are shown in tables 1 and 2.
TABLE 1
TABLE 2
As can be seen from Table 1, the properties of examples 1 to 3 are significantly higher than those of comparative examples 1 and 2, and when the epoxy resin is not added in comparative example 1, the properties are reduced, wherein the compressive strength is reduced significantly; the document 2 is not added with the organic montmorillonite, so that the water retention rate and the osmotic pressure ratio are obviously reduced, and the organic montmorillonite has a barrier effect on water.
As can be seen from Table 2, when curing is performed at 60 degrees, the comparative examples have lower performance than the present invention, so that the present invention has significant advantages in high temperature environment.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It should be understood by those skilled in the art that the above embodiments do not limit the scope of the present invention in any way, and all technical solutions obtained by using equivalent substitution methods fall within the scope of the present invention.
Claims (4)
1. A preparation method of a concrete curing agent is characterized by comprising the following steps: the method comprises the following steps: (1) adding calcium hydroxide into methyl methacrylate, and distilling at 80 ℃ to remove a polymerization inhibitor; (2) drying organic montmorillonite at 70 deg.C for 24 hr; (3) preparing washing liquid of a reaction kettle, wherein the proportion of the washing liquid is V (dichlorodimethylsilane): v (ethyl acetate) ═ 15: 85 parts by weight; pouring the washing liquid into a reaction kettle, soaking for 12 hours, and then washing with ethyl acetate for three times; (4) preparing an initiator, wherein the initiator adopts stannous octoate and a toluene solution, the concentration of the solution is 0.1g/ml, a small amount of calcium hydride is added into the toluene solvent before preparation, the mixture is kept stand for 24 hours, and water and filtration are carried out; (5) 80-90 parts of methyl methacrylate, 10-20 parts of organic montmorillonite, and the amount of an initiator is N (methyl methacrylate): putting N (initiator) 8000:1 into a reaction kettle, charging nitrogen for protection, and reacting for 2 hours at the stirring speed of 200-300 r/min and the temperature of 130 ℃ to obtain a composite prepolymer; (6) and (3) mixing the composite prepolymer obtained in the step (5) with polyether polyurethane resin and epoxy resin according to a weight ratio of 1-3: 5-8: 2-5, mixing to obtain a modified polyurethane emulsion;
when in use, the polyurethane emulsion obtained in the step (6) and cyclohexane dimethylene diisocyanate are mixed according to the weight ratio of 10: 0.1-0.5 of the curing agent for concrete.
2. The method for preparing a concrete curing agent according to claim 1, wherein the concrete curing agent comprises: the organic montmorillonite in the step (2) is quaternary ammonium salt modified montmorillonite, and the particle size is 2-8 microns.
3. The method for preparing a concrete curing agent according to claim 1, wherein the concrete curing agent comprises: the molecular weight of organisms in the composite prepolymer in the step (5) is 1000-2000.
4. The method for preparing a concrete curing agent according to claim 1, wherein the concrete curing agent comprises: in the step (6), the polyether polyurethane resin is aliphatic polyurethane, the molecular weight is 3000-4000, and the solid content is 45%; the epoxy resin is linear aliphatic epoxy resin, the molecular weight is 2000-3000, and the epoxy value is 0.25-0.45.
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