CN114163577A - Viscosity-reducing water reducer and preparation method and application thereof - Google Patents
Viscosity-reducing water reducer and preparation method and application thereof Download PDFInfo
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- CN114163577A CN114163577A CN202111292019.4A CN202111292019A CN114163577A CN 114163577 A CN114163577 A CN 114163577A CN 202111292019 A CN202111292019 A CN 202111292019A CN 114163577 A CN114163577 A CN 114163577A
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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
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated 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
- 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
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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Abstract
The invention relates to a viscosity-reducing water reducer and a preparation method and application thereof, wherein the viscosity-reducing water reducer comprises a structural unit A derived from polyether monomers, a structural unit B derived from acrylic monomers, a structural unit C derived from methyl methacrylate monomers, a structural unit D derived from 2-acrylamido-2-methylpropanesulfonic acid monomers and a structural unit E derived from polyether amine monomers, wherein the molar ratio of the structural unit B to the structural unit A is 2.0-4.0:1, the molar ratio of the structural unit C to the structural unit A is 0.07-0.10:1, and the molar ratio of the structural unit D to the structural unit A is 0.50-0.70: 1. According to the viscosity-reducing water reducer, the functionalization of the polycarboxylic acid water reducer is realized by introducing functional groups with different functions, controlling the polymerization degree of the main chain, the length of the side chain and the like, the high strength of concrete is realized, the viscosity of the concrete is reduced, the expansion degree of the concrete is improved, and the flow velocity of the concrete is accelerated, so that the working performance of the concrete is improved, and the construction requirements are met.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a viscosity-reducing water reducer and a preparation method and application thereof.
Background
In recent years, with the rapid development of the building industry, high-performance concrete gradually enters various concrete projects by virtue of the characteristics of high strength, compact and hard structure, good mechanical property, volume stability, durability and the like, and becomes the main direction of the development of modern concrete technology. At present, some super high-rise buildings with large span and important buildings with special functional requirements continuously appear, and high-strength-grade concrete enters the construction market by virtue of the characteristics of high strength, good integrity and small self weight. Because the concrete strength is mainly improved by reducing the water-cement ratio at present, the problems of high viscosity, low flow rate and the like of high-grade concrete in application can occur, further the construction problems exist in the processes of stirring, transportation, pumping and the like, and the development of high-strength concrete is limited. The polycarboxylate superplasticizer is a comb copolymer with a main chain containing carboxyl and grafted polyoxyethylene side chains, and the superior performance of the polycarboxylate superplasticizer brings great convenience in the field of concrete, but still has many problems. For example, on the premise of improving the requirement on the quality of concrete, the polycarboxylate superplasticizer needs to maintain good fluidity and workability in the aspect of concrete construction performance, is suitable for long-distance transportation and is easy for pumping construction, but the concrete bleeding can be caused by excessively high mixing amount of the polycarboxylate superplasticizer; the addition of excessive retarding component can result in excessive setting time of the concrete and delay construction progress. Therefore, the research and development of the polycarboxylate superplasticizer with viscosity reducing performance have great significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the viscosity-reducing water reducer, and the preparation method and the application thereof, which can realize high strength of concrete, and can lower the viscosity of the concrete and improve the working performance of the concrete, thereby meeting the construction requirements.
The first aspect of the invention provides a viscosity-reducing water reducer, which comprises a structural unit A derived from polyether monomers, a structural unit B derived from acrylic monomers, a structural unit C derived from methyl methacrylate monomers, a structural unit D derived from 2-acrylamido-2-methylpropanesulfonic acid monomers and a structural unit E derived from polyether amine monomers, wherein the molar ratio of the structural unit B to the structural unit A is (2.0-4.0):1, the molar ratio of the structural unit C to the structural unit A is (0.07-0.10):1, and the molar ratio of the structural unit D to the structural unit A is (0.50-0.70): 1.
According to some embodiments of the invention, the molar ratio of structural unit B to structural unit a is (2.9-3.4):1, e.g. 2.95:1, 3.03:1, 3.05:1, 3.07:1, 3.10:1, 3.13:1, 3.15:1, 3.17:1, 3.20:1, 3.23:1, 3.25:1, 3.27:1, 3.30:1 or any value in between. In some embodiments, the molar ratio of structural unit B to structural unit A is (3.0-3.35): 1.
According to some embodiments of the invention, the molar ratio of structural unit C to structural unit a is (0.075 to 0.085):1, e.g., 0.0755:1, 0.0760:1, 0.077:1, 0.078:1, 0.079:1, 0.0805:1, 0.0805:1, 0.0810:1, 0.0815:1, 0.0820:1, 0.0825:1, 0.0830:1, 0.0835:1, 0.0840:1, 0.0845:1, or any value therebetween. In some embodiments, the molar ratio of structural unit C to structural unit A is (0.080-0.085): 1.
According to some embodiments of the invention, the molar ratio of structural unit D to structural unit a is (0.55-0.62):1, e.g. 0.56:1, 0.57:1, 0.58:1, 0.591:1, 0.593:1, 0.595:1, 0.597:1, 0.60:1, 0.603:1, 0.605:1, 0.607:1, 0.61:1, 0.613:1, 0.615:1, 0.617:1 or any value in between. In some embodiments, the molar ratio of structural unit D to structural unit A is (0.59-0.62): 1.
According to some embodiments of the invention, the molar ratio of structural unit E to structural unit a is (0.18-0.25):1, e.g. 0.19:1, 0.195:1, 0.203:1, 0.205:1, 0.207:1, 0.210:1, 0.213:1, 0.215:1, 0.217:1, 0.220:1, 0.225:1, 0.23:1, 0.235:1, 0.240:1, 0.245:1 or any value in between. In some embodiments, the molar ratio of structural unit E to structural unit A is (0.2-0.23): 1. In some embodiments, the molar ratio of structural unit E to structural unit A is (0.2-0.21): 1.
According to some embodiments of the present invention, the polyether monomer is selected from prenyl polyoxyethylene ether, preferably one or more selected from TPEG-1200, TPEG-2400, TPEG-4000, and more preferably TPEG-1200. According to the invention, the viscosity reduction water reducer prepared by selecting TPEG-1200 has obvious improvement on the viscosity performance of concrete.
According to some embodiments of the invention, the methyl methacrylate-based monomer is selected from methyl methacrylate and/or methyl acrylate.
According to some embodiments of the invention, the 2-acrylamido-2-methylpropanesulfonic acid-based monomer is selected from one or more of 2-acrylamido-2-methylpropanesulfonic acid, tetrahydrobenzoic acid, and lignosulfonic acid;
according to some embodiments of the invention, the acrylic monomer is selected from methacrylic acid and/or acrylic acid.
According to some embodiments of the invention, the polyetheramine monomer is selected from one or more of MA-240, MA-223, and MA-1100.
The second aspect of the invention provides a preparation method of a viscosity-reducing water reducer, which comprises the following steps:
s1: providing a mixture I containing a polyether monomer, a polyether amine monomer, an initiator and a solvent, a mixture II containing a reducing agent, a chain transfer agent and a solvent, and a mixture III containing a methyl methacrylate monomer, an acrylic monomer, a 2-acrylamido-2-methylpropanesulfonic acid monomer and a solvent;
s2: simultaneously adding the mixture II and the mixture III into the mixture I for polymerization reaction to obtain a polymerization reaction product;
s3: mixing the polymerization reaction product obtained in the step S2 with a pH regulator to obtain the viscosity-reducing water reducer;
the polyether monomer is 32.50-36.50 parts by weight, the acrylic monomer is 5.50-8.00 parts by weight, the methyl methacrylate monomer is 0.20-0.30 part by weight, and the 2-acrylamide-2-methylpropanesulfonic acid monomer is 3.00-4.00 parts by weight.
According to some embodiments of the present invention, the polyether monomer is 33.50 parts to 36.50 parts, such as 33.7 parts, 33.9 parts, 34.0 parts, 34.5 parts, 34.7 parts, 35.0 parts, 35.3 parts, 35.5 parts, 35.7 parts, 35.9 parts, 36.1 parts, 36.3 parts, 36.4 parts, 36.45 parts, or any value therebetween, in parts by weight. In some embodiments, the polyether monomer is 35.0 parts to 36.50 parts by weight.
According to some embodiments of the invention, the acrylic monomer is 6.0 parts to 7.5 parts, such as 6.1 parts, 6.2 parts, 6.3 parts, 6.4 parts, 6.55 parts, 6.6 parts, 6.65 parts, 6.7 parts, 6.75 parts, 6.8 parts, 6.85 parts, 6.9 parts, 6.95 parts, 7.1 parts, 7.2 parts, 7.3 parts, 7.4 parts, or any value therebetween, in parts by weight. In some embodiments, the acrylic monomer is 6.5 parts to 7.0 parts by weight.
According to some embodiments of the present invention, the methyl methacrylate-based monomer is 0.22 parts to 0.26 parts, such as 0.25 parts, 0.231 parts, 0.235 parts, 0.237 parts, 0.239 parts, 0.24 parts, 0.243 parts, 0.245 parts, 0.247 parts, 0.249 parts, 0.255 parts, or any value therebetween, by weight parts. In some embodiments, the methyl methacrylate-based monomer is 0.23 parts to 0.25 parts by weight.
According to some embodiments of the invention, the 2-acrylamido-2-methylpropanesulfonic acid-based monomer is from 3.20 parts to 3.70 parts, for example, 3.3 parts, 3.4 parts, 3.45 parts, 3.53 parts, 3.55 parts, 3.57 parts, 3.59 parts, 3.6 parts, 3.61 parts, 3.63 parts, 3.65 parts, 3.67 parts, 3.69 parts, 3.73 parts, 3.75 parts, or any value therebetween, by weight parts. In some embodiments, the 2-acrylamido-2-methylpropane sulfonic acid-based monomer is from 3.50 parts to 3.70 parts by weight.
According to some embodiments of the invention, the polyetheramine-based monomer is 1.30 parts to 1.70 parts, such as 1.37 parts, 1.39 parts, 1.40 parts, 1.42 parts, 1.45 parts, 1.47 parts, 1.49 parts, 1.52 parts, 1.55 parts, 1.57 parts, 1.60 parts, 1.65 parts, 1.67 parts, or any value therebetween, by weight parts. In some embodiments, the polyetheramine monomer is 1.35 parts to 1.50 parts by weight.
According to some embodiments of the invention, the initiator is 0.25 to 0.75 parts, such as 0.3 parts, 0.4 parts, 0.5 parts, 0.65 parts, 0.7 parts, or the like, by weight parts. According to some embodiments of the invention, the initiator is 0.35 to 0.60 parts by weight.
According to some embodiments of the invention, the reducing agent is 0.10 to 0.50 parts, such as 0.13 parts, 0.17 parts, 0.19 parts, 0.3 parts, 0.4 parts, or the like, by weight parts. According to some embodiments of the invention, the reducing agent is 0.15 to 0.20 parts by weight.
According to some embodiments of the invention, the chain transfer agent is 0.50 to 0.80 parts, such as 0.55 parts, 0.60 parts, 0.65 parts, or 0.75 parts, etc., by weight parts. According to some embodiments of the invention, the chain transfer agent is 0.50 to 0.70 parts by weight.
According to some embodiments of the invention, the pH adjusting agent is 19.50 to 26.50 parts, such as 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, or the like, by weight parts.
According to some embodiments of the invention, the solvent is 21.25-37.15 parts, such as 22 parts, 24 parts, 26 parts, 28 parts, 30 parts, 33 parts, 35 parts, or the like, by weight parts.
According to some embodiments of the present invention, in step S1, providing the mixture I including the polyether-based monomer, the polyetheramine-based monomer, the initiator and the solvent includes mixing the polyether macromonomer, the polyetheramine-based monomer, the solvent and the initiator, preferably at 20 ℃ to 30 ℃, until dissolved, to obtain the mixture I.
According to some embodiments of the present invention, providing mixture II comprising a reducing agent, a chain transfer agent, and a solvent in step S1 includes mixing the reducing agent, the chain transfer agent, and the solvent uniformly to obtain mixture II.
According to some embodiments of the present invention, providing the mixture III including the methyl methacrylate monomer, the acrylic monomer, the 2-acrylamido-2-methylpropanesulfonic acid monomer, and the solvent in step S1 includes uniformly mixing the methyl methacrylate monomer, the acrylic monomer, the 2-acrylamido-2-methylpropanesulfonic acid, and the solvent to obtain the mixture III.
According to some embodiments of the present invention, in step S2, the addition time of mixture III is 3-4h, and the addition time of mixture II is controlled to be greater than the addition time of mixture III, preferably greater than the addition time of mixture III by 0.3-0.7 h. According to some embodiments of the invention, the addition time of the mixture III is 3 h. According to some embodiments of the invention, the addition time of the mixture II is 3.5 h.
According to the preparation method of the viscosity-reducing water reducer, the mixture II and the mixture III are uniformly dripped into the container filled with the mixture I within the dripping time of 3.5 hours and 3 hours respectively, so that the viscosity-reducing water reducer is remarkably improved in the aspect of concrete viscosity performance.
According to some embodiments of the invention, the temperature of the polymerization reaction in step S2 is 15 ℃ to 40 ℃, preferably 20 ℃ to 30 ℃. According to some embodiments of the invention, in step S2, the polymerization reaction time is 1h to 5 h.
According to some embodiments of the invention, in step S3, the polymerization reaction product obtained in step S2 is mixed with a pH regulator to adjust the pH to 5-7, so as to obtain the viscosity-reducing water reducer.
According to some embodiments of the invention, the method comprises the following specific steps:
t1: uniformly mixing a polyether macromonomer, a polyether amine monomer, deionized water and an initiator to obtain a mixture I;
t2: uniformly mixing a reducing agent, a chain transfer agent and deionized water to obtain a mixture II;
t3: uniformly mixing methyl methacrylate monomers, acrylic acid monomers, 2-acrylamide-2-methylpropanesulfonic acid monomers and deionized water to obtain a mixture III;
t4: and (3) respectively and simultaneously dripping the mixture II and the mixture III into a container filled with the mixture I for a certain time at a certain temperature, uniformly mixing, keeping the temperature for 2 hours, and adding a certain amount of pH regulating solution to obtain the viscosity-reducing water reducer.
According to some embodiments of the invention, in step T4, the mixture II and the mixture III are respectively added dropwise into a container filled with the mixture I at a certain temperature and for a certain time, the mixture is uniformly mixed and then kept for 2 hours, and a certain amount of pH regulating solution is added to obtain the viscosity-reducing water reducer.
According to some embodiments of the invention, in step T4, preferably at a temperature of 20 ℃ to 30 ℃, mixture II and mixture III are uniformly dripped into a container filled with mixture I for 3.5 hours and 3 hours respectively, the mixture is uniformly mixed and then is kept at the temperature for 2 hours, and a certain amount of pH regulating solution is added to obtain the viscosity-reducing water reducer.
According to some embodiments of the invention, in step T4, preferably at a temperature of 20 ℃ to 30 ℃, mixture II and mixture III are uniformly dripped into a container filled with mixture I for 3.5 hours and 3 hours respectively, the mixture is uniformly mixed and then kept at the temperature for 2 hours, and a certain amount of pH regulating solution is added, preferably the pH is regulated to 5-7, so as to obtain the viscosity-reducing water reducer.
According to some embodiments of the present invention, the polyether monomer is selected from prenyl polyoxyethylene ether, preferably one or more selected from TPEG-1200, TPEG-2400, TPEG-4000, and more preferably TPEG-1200.
According to some embodiments of the invention, the methyl methacrylate-based monomer is selected from methyl methacrylate and/or methyl acrylate.
According to some embodiments of the invention, the 2-acrylamido-2-methylpropanesulfonic acid-based monomer is selected from one or more of 2-acrylamido-2-methylpropanesulfonic acid, tetrahydrobenzoic acid, and lignosulfonic acid.
According to some embodiments of the invention, the acrylic monomer is selected from methacrylic acid and/or acrylic acid.
According to some embodiments of the invention, the polyetheramine monomer is selected from one or more of MA-240, MA-223, and MA-1100.
According to some embodiments of the invention, the initiator is selected from one or more of potassium persulfate, hydrogen peroxide, sodium persulfate, and ammonium persulfate.
According to some embodiments of the invention, the reducing agent is selected from one or more of ascorbic acid and sodium bisulfite.
According to some embodiments of the invention, the chain transfer agent is selected from one or more of beta-mercaptopropionic acid, 3-mercaptoacetic acid, and 3-mercaptopropionic acid.
According to some embodiments of the invention, the pH adjusting agent is selected from one or more of a potassium hydroxide solution, a sodium hydroxide solution and a sodium bicarbonate solution at a mass concentration of 25% to 35%.
According to some embodiments of the invention, the solvent is selected from water.
The third aspect of the invention provides the viscosity-reducing water reducer prepared by the method of the second aspect.
The fourth aspect of the invention provides the application of the viscosity-reducing water-reducing agent of the first aspect or the viscosity-reducing water-reducing agent prepared by the method of the second aspect in concrete.
The invention synthesizes the viscosity-reducing water reducer with viscosity-reducing function by copolymerization under the action of redox system initiation, chain transfer agent and the like. The viscosity reduction water reducer is applied to concrete engineering, after the polycarboxylic acid superplasticizer is adsorbed on the surface of cement particles, a layer of hydrophobization solvolysis layer can be formed on the surface of the cement particles by virtue of a special hydrophobic group on the structure of the polycarboxylic acid superplasticizer, and a hydrophilic solvolysis layer formed by polyoxyethylene ether side chains can form a water film layer with certain mechanical strength on the surface of the cement particles under the combined action of the hydrophobization solvolysis layer and the hydrophilic solvolysis layer, so that free water among the cement particles can be released, the floc structure of the cement particles can be damaged, the lubricating effect between the cement particles and aggregate is improved, the viscosity of concrete is reduced, and the flow rate of the concrete is improved.
Compared with the prior art, the invention has the following advantages:
(1) the viscosity reduction water reducer provided by the invention can obviously improve the viscosity performance of concrete under the condition of low doping amount.
(2) The invention has simple synthesis process and lower cost requirement.
Detailed Description
The invention will now be further illustrated by means of specific examples, but it will be understood that the scope of the invention is not limited thereto.
The starting materials used in the examples and comparative examples were commercially available and analytically pure, unless otherwise specified.
The viscosity-reducing water reducer is mainly prepared from the following components in parts by weight through solution polymerization: 32.50-36.50 parts of polyether monomer, 0.20-0.30 part of methyl methacrylate monomer, 3.00-4.00 parts of 2-acrylamide-2-methylpropanesulfonic acid monomer, 5.50-8.00 parts of acrylic monomer, 1.30-1.70 parts of polyether amine monomer, 0.25-0.75 part of initiator, 0.10-0.50 part of reducing agent, 0.50-0.80 part of chain transfer agent, 19.50-26.50 parts of pH adjusting solution and 21.25-37.15 parts of deionized water.
In the embodiment of the invention, the pH adjusting solution is a sodium hydroxide (NaOH) solution with the mass fraction of 30%.
The polyether macromonomer used in the embodiment of the present invention is: isopentenol polyoxyethylene ether (TPEG-1200, weight average molecular weight 1200); the functional small monomer is: methyl methacrylate, 2-acrylamido-2-methylpropanesulfonic acid, acrylic acid and polyetheramine (MA-240, weight average molecular weight 240); the initiator is as follows: hydrogen peroxide solution with mass fraction of 35%; the reducing agent is: ascorbic acid (VC); the chain transfer agent is: beta-mercaptopropionic acid.
Example 1
The main components of the synthesized viscosity-reducing water reducer comprise: 32.50 parts of polyether macromonomer, 0.20 part of methyl methacrylate monomer, 3.00 parts of 2-acrylamide-2-methylpropanesulfonic acid monomer, 5.50 parts of acrylic monomer, 1.30 parts of polyether amine monomer, 0.25 part of initiator, 0.10 part of reducing agent, 0.50 part of chain transfer agent, 19.50 parts of pH regulating solution and 37.15 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) 32.50 parts of prenol polyoxyethylene ether (TPEG-1200) and polyether amine (MA-240)
Placing 1.30 parts of hydrogen peroxide and 0.25 part of hydrogen peroxide into a reaction flask A, heating to 20-30 ℃ for dissolution, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.10 part of ascorbic acid (VC), 0.50 part of beta-mercaptopropionic acid and 20.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.20 part of Methyl Methacrylate (MMA), 5.50 parts of Acrylic Acid (AA), 3.00 parts of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS) and 17.15 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 19.50 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 2
The main components of the synthesized viscosity-reducing water reducer comprise: the modified polyether comprises, by weight, 33.50 parts of a polyether macromonomer, 0.22 part of a methyl methacrylate monomer, 3.20 parts of a 2-acrylamido-2-methylpropanesulfonic acid monomer, 6.00 parts of an acrylic monomer, 1.35 parts of a polyetheramine monomer, 0.30 part of an initiator, 0.15 part of a reducing agent, 0.55 part of a chain transfer agent, 20.00 parts of a pH adjusting solution and 34.73 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) placing 33.50 parts of prenyl polyoxyethylene ether (TPEG-1200), 1.35 parts of polyetheramine (MA-240) and 0.30 part of hydrogen peroxide in a reaction flask A, heating to 20-30 ℃ for dissolving, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.15 part of ascorbic acid (VC), 0.55 part of beta-mercaptopropionic acid and 20.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.22 part of methyl methacrylate, 6.00 parts of acrylic acid, 3.20 parts of 2-acrylamido-2-methylpropanesulfonic acid and 14.73 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 20.00 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 3
The main components of the synthesized viscosity-reducing water reducer comprise: by weight, 34.10 parts of polyether macromonomer, 0.20 part of methyl methacrylate monomer, 3.25 parts of 2-acrylamide-2-methylpropanesulfonic acid monomer, 6.25 parts of acrylic acid monomer, 1.35 parts of polyether amine monomer, 0.35 part of initiator, 0.15 part of reducing agent, 0.55 part of chain transfer agent, 21.50 parts of pH regulating solution and 32.30 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) 34.10 parts of prenyl polyoxyethylene ether (TPEG-1200) and polyether amine (MA-240)
Placing 1.35 parts of hydrogen peroxide and 0.35 part of hydrogen peroxide into a reaction flask A, heating to 20-30 ℃ for dissolution, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.15 part of ascorbic acid (VC), 0.55 part of beta-mercaptopropionic acid and 20.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.20 part of methyl methacrylate, 6.25 parts of acrylic acid, 3.25 parts of 2-acrylamido-2-methylpropanesulfonic acid and 12.30 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 21.50 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 4
The main components of the synthesized viscosity-reducing water reducer comprise: according to parts by weight, 35.20 parts of polyether macromonomer, 0.24 part of methyl methacrylate monomer, 3.55 parts of 2-acrylamide-2-methylpropanesulfonic acid monomer, 6.85 parts of acrylic acid monomer, 1.40 parts of polyether amine monomer, 0.45 part of initiator, 0.18 part of reducing agent, 0.60 part of chain transfer agent, 22.60 parts of pH regulating solution and 28.93 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) placing 35.20 parts of prenyl polyoxyethylene ether (TPEG-1200), 1.40 parts of polyetheramine (MA-240) and 0.45 part of hydrogen peroxide in a reaction flask A, heating to 20-30 ℃ for dissolving, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.18 part of ascorbic acid (VC), 0.60 part of beta-mercaptopropionic acid and 20.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.24 part of methyl methacrylate, 6.85 parts of acrylic acid, 3.55 parts of 2-acrylamido-2-methylpropanesulfonic acid and 8.93 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, uniformly and simultaneously dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 22.60 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 5
The main components of the synthesized viscosity-reducing water reducer comprise: the polyether comprises, by weight, 35.20 parts of a polyether macromonomer, 0.24 part of a methyl methacrylate monomer, 3.65 parts of a 2-acrylamido-2-methylpropanesulfonic acid monomer, 6.97 parts of an acrylic monomer, 1.46 parts of a polyetheramine monomer, 0.49 part of an initiator, 0.20 part of a reducing agent, 0.70 part of a chain transfer agent, 24.65 parts of a pH adjusting solution and 26.44 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) placing 35.20 parts of prenyl polyoxyethylene ether (TPEG-1200), 1.46 parts of polyetheramine (MA-240) and 0.49 part of hydrogen peroxide in a reaction flask A, heating to 20-30 ℃ for dissolving, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.20 part of ascorbic acid (VC), 0.70 part of beta-mercaptopropionic acid and 15.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.24 part of methyl methacrylate, 6.97 parts of acrylic acid, 3.65 parts of 2-acrylamido-2-methylpropanesulfonic acid and 11.44 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 24.65 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 6
The main components of the synthesized viscosity-reducing water reducer comprise: 35.80 parts of polyether macromonomer, 0.24 part of methyl methacrylate monomer, 3.75 parts of 2-acrylamide-2-methylpropanesulfonic acid monomer, 7.25 parts of acrylic monomer, 1.51 parts of polyether amine monomer, 0.55 part of initiator, 0.20 part of reducing agent, 0.75 part of chain transfer agent, 25.00 parts of pH regulating solution and 24.95 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) 35.80 parts of prenyl alcohol polyoxyethylene ether (TPEG-1200), 1.51 parts of polyether amine (MA-240) and 0.55 part of hydrogen peroxide are placed in a reaction flask A, heated to 20-30 ℃ to be dissolved, and uniformly mixed to obtain a mixture I.
(2) And (3) placing 0.20 part of ascorbic acid (VC), 0.75 part of beta-mercaptopropionic acid and 15.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.24 part of methyl methacrylate, 7.25 parts of acrylic acid, 3.75 parts of 2-acrylamido-2-methylpropanesulfonic acid and 9.95 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 25.00 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 7
The main components of the synthesized viscosity-reducing water reducer comprise: the polyether comprises, by weight, 36.00 parts of a polyether macromonomer, 0.26 part of a methyl methacrylate monomer, 3.80 parts of a 2-acrylamido-2-methylpropanesulfonic acid monomer, 7.50 parts of an acrylic monomer, 1.58 parts of a polyetheramine monomer, 0.60 part of an initiator, 0.20 part of a reducing agent, 0.75 part of a chain transfer agent, 25.63 parts of a pH adjusting solution and 23.68 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) placing 36.00 parts of prenyl polyoxyethylene ether (TPEG-1200), 1.58 parts of polyetheramine (MA-240) and 0.60 part of hydrogen peroxide in a reaction flask A, heating to 20-30 ℃ for dissolving, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.20 part of ascorbic acid (VC), 0.75 part of beta-mercaptopropionic acid and 10.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.26 part of methyl methacrylate, 7.50 parts of acrylic acid, 3.80 parts of 2-acrylamido-2-methylpropanesulfonic acid and 13.68 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 25.63 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 8
The main components of the synthesized viscosity-reducing water reducer comprise: the modified polyether comprises, by weight, 36.50 parts of a polyether macromonomer, 0.28 part of a methyl methacrylate monomer, 3.80 parts of a 2-acrylamido-2-methylpropanesulfonic acid monomer, 8.00 parts of an acrylic monomer, 1.65 parts of a polyetheramine monomer, 0.70 part of an initiator, 0.20 part of a reducing agent, 0.75 part of a chain transfer agent, 26.20 parts of a pH adjusting solution and 21.92 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) placing 36.50 parts of prenyl polyoxyethylene ether (TPEG-1200), 1.65 parts of polyetheramine (MA-240) and 0.70 part of hydrogen peroxide in a reaction flask A, heating to 20-30 ℃ for dissolving, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.20 part of ascorbic acid (VC), 0.75 part of beta-mercaptopropionic acid and 10.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.28 part of methyl methacrylate, 8.00 parts of acrylic acid, 3.80 parts of 2-acrylamido-2-methylpropanesulfonic acid and 11.92 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, simultaneously and uniformly dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 26.20 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
Example 9
The main components of the synthesized viscosity-reducing water reducer comprise: the polyether comprises, by weight, 36.50 parts of a polyether macromonomer, 0.30 part of a methyl methacrylate monomer, 4.00 parts of a 2-acrylamido-2-methylpropanesulfonic acid monomer, 8.00 parts of an acrylic monomer, 1.70 parts of a polyetheramine monomer, 0.75 part of an initiator, 0.20 part of a reducing agent, 0.80 part of a chain transfer agent, 26.50 parts of a pH adjusting solution and 21.25 parts of deionized water.
The preparation method for synthesizing the viscosity-reducing water reducer comprises the following steps:
(1) placing 36.50 parts of prenyl polyoxyethylene ether (TPEG-1200), 1.70 parts of polyetheramine (MA-240) and 0.75 part of hydrogen peroxide in a reaction flask A, heating to 20-30 ℃ for dissolving, and uniformly mixing to obtain a mixture I.
(2) And (3) placing 0.20 part of ascorbic acid (VC), 0.80 part of beta-mercaptopropionic acid and 10.00 parts of deionized water into a reaction flask B at normal temperature, and uniformly mixing to obtain a mixture II.
(3) Under the condition of normal temperature, 0.30 part of methyl methacrylate, 8.00 parts of acrylic acid, 4.00 parts of 2-acrylamido-2-methylpropanesulfonic acid and 11.25 parts of deionized water are placed in a reaction flask C and uniformly mixed to obtain a mixture III.
(4) Keeping the temperature at 20-30 ℃, uniformly and simultaneously dropwise adding the mixture II and the mixture III in the reaction flask B and the reaction flask C into the flask A filled with the mixture I within 3.5h and 3.0h, continuously preserving the temperature for 2h after dropwise adding is finished, and adding 26.50 parts of pH regulating solution to obtain the target viscosity-reducing water reducer, wherein the solid content of the viscosity-reducing water reducer is 45%.
The viscosity-reducing water reducer of the embodiment 1 to the embodiment 9 is supplemented with a certain amount of water to prepare a solid content of about 40 percent, and the solid content is applied to concrete cement-based materials, and the addition amount of the solid content is 0.30 to 0.50 percent of the cementing materials.
The fluidity test and the concrete performance test are carried out on the cement paste of the viscosity reduction water reducer of the embodiments 1 to 9 by referring to the national standards GB/T8077-2012 and GB 8076-:
TABLE 1 Effect of different Synthesis conditions on product Properties
As is clear from examples 1 to 5 in the No. 1, under the synthesis conditions, when the molar ratio of methyl methacrylate to prenyl polyoxyethylene ether (TPEG-1200) is 0.07 to 0.09 (example 5), the viscosity-reducing water-reducing agent synthesized in example 5 is synthesized, and when the mixing amount is 0.35%, the viscosity-reducing water-reducing agent synthesized in example 5 can be confirmed to have a good viscosity-reducing effect by the cement paste fluidity and the air space time data shown in Table 1.
As is clear from examples 3 to 5 in the No. 2, the viscosity reducing water reducing agent synthesized in example 5 has a good viscosity reducing effect under the synthesis conditions when the molar ratio of 2-acrylamido-2-methylpropanesulfonic acid to prenyl alcohol polyoxyethylene ether (TPEG-1200) is 0.58 to 0.62, as shown by the fluidity of cement paste and the time data of the flowing space in Table 1.
As is clear from examples 5 to 7 in No. 3, the viscosity-reducing water-reducing agent synthesized in example 5 has a good viscosity-reducing effect under the synthesis conditions when the molar ratio of the amount of acrylic acid incorporated to the amount of prenyl polyoxyethylene ether (TPEG-1200) incorporated is 3.00 to 3.50, as shown by the cement paste fluidity and the head space time data in Table 1.
As is clear from examples 5 to 9 in No. 4, the viscosity-reducing water-reducing agent synthesized in example 5 has a good viscosity-reducing effect under the synthesis conditions when the molar ratio of the polyether amine (M-240) to the prenyl polyoxyethylene ether (TPEG-1200) is 0.20 to 0.22, as shown by the cement neat paste fluidity and the head space time data in Table 1.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not set any limit to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A viscosity-reducing water reducer comprises a structural unit A derived from polyether monomers, a structural unit B derived from acrylic monomers, a structural unit C derived from methyl methacrylate monomers, a structural unit D derived from 2-acrylamido-2-methylpropanesulfonic acid monomers and a structural unit E derived from polyetheramine monomers,
wherein the molar ratio of the structural unit B to the structural unit A is (2.0-4.0):1, the molar ratio of the structural unit C to the structural unit A is (0.07-0.10):1, and the molar ratio of the structural unit D to the structural unit A is (0.50-0.70): 1.
2. The viscosity-reducing water reducer according to claim 1, wherein the molar ratio of the structural unit B to the structural unit A is (2.9-3.4):1, preferably (3.0-3.35): 1;
and/or the molar ratio of structural units C to A is (0.075 to 0.085):1, preferably (0.080 to 0.085): 1;
and/or the molar ratio of structural units D to structural units A is (0.55-0.62):1, preferably (0.59-0.62): 1.
3. The viscosity-reducing water-reducing agent according to claim 1 or 2, wherein the molar ratio of the structural unit E to the structural unit A is (0.18-0.25):1, preferably (0.2-0.23):1, and more preferably (0.2-0.21): 1.
4. The viscosity-reducing water reducer according to any one of claims 1 to 3, wherein the polyether monomer is selected from prenyl polyoxyethylene ether, preferably from one or more of TPEG-1200, TPEG-2400 and TPEG-4000, and more preferably from TPEG-1200;
and/or the methyl methacrylate monomer is selected from methyl methacrylate and/or methyl acrylate;
and/or the 2-acrylamido-2-methylpropanesulfonic acid monomer is selected from 2-acrylamido-2-methylpropanesulfonic acid;
and/or the acrylic monomer is selected from methacrylic acid and/or acrylic acid;
and/or the polyetheramine monomer is selected from one or more of MA-240, MA-223 and MA-1100.
5. The preparation method of the viscosity-reducing water reducer comprises the following steps:
s1: providing a mixture I containing a polyether monomer, a polyether amine monomer, an initiator and a solvent, a mixture II containing a reducing agent, a chain transfer agent and a solvent, and a mixture III containing a methyl methacrylate monomer, an acrylic monomer, a 2-acrylamido-2-methylpropanesulfonic acid monomer and a solvent;
s2: simultaneously adding the mixture II and the mixture III into the mixture I for polymerization reaction to obtain a polymerization reaction product;
s3: mixing the polymerization reaction product obtained in the step S2 with a pH regulator to obtain the viscosity-reducing water reducer;
the polyether monomer is 32.50-36.50 parts by weight, the acrylic monomer is 5.50-8.00 parts by weight, the methyl methacrylate monomer is 0.20-0.30 part by weight, and the 2-acrylamide-2-methylpropanesulfonic acid monomer is 3.00-4.00 parts by weight.
6. The method according to claim 5, wherein the polyether monomer is 33.50 to 36.50 parts by weight, preferably 35.0 to 36.50 parts by weight;
and/or the acrylic monomer is 6.0 to 7.5 parts, preferably 6.5 to 7.0 parts;
and/or the methyl methacrylate monomer is 0.22 to 0.26, preferably 0.23 to 0.25;
and/or the 2-acrylamide-2-methylpropanesulfonic acid monomer is 3.20 to 3.70 parts, preferably 3.50 to 3.70 parts.
7. The method according to claim 5 or 6, characterized in that the polyetheramine monomer is present in an amount of 1.30 parts to 1.70 parts, preferably 1.35 parts to 1.50 parts;
and/or the initiator is 0.25-0.75 parts, preferably 0.35-0.60 parts;
and/or the reducing agent is 0.10-0.50 parts, preferably 0.15-0.20 parts;
and/or the chain transfer agent is 0.50 to 0.80 part, preferably 0.50 to 0.70 part;
and/or the pH regulator is 19.50-26.50 parts;
and/or the solvent is 21.25-37.15 parts.
8. The method according to any one of claims 5 to 7, wherein in step S2, the addition time of mixture III is 3 to 4 hours, and the addition time of mixture II is controlled to be greater than the addition time of mixture III, preferably greater than the addition time of mixture III by 0.3 to 0.7 hours;
and/or in step S2, the temperature of the polymerization reaction is 15-40 ℃, preferably 20-30 ℃, and the reaction time is 1-5 h.
9. The process according to any one of claims 5 to 8, wherein the polyether monomer is selected from prenyl polyoxyethylene ethers, preferably from one or more of TPEG-1200, TPEG-2400, TPEG-4000, more preferably from TPEG-1200;
and/or the methyl methacrylate monomer is selected from methyl methacrylate and/or methyl acrylate;
and/or the 2-acrylamido-2-methylpropanesulfonic acid monomer is selected from 2-acrylamido-2-methylpropanesulfonic acid;
and/or the acrylic monomer is selected from methacrylic acid and/or acrylic acid;
and/or the polyetheramine monomer is selected from one or more of MA-240, MA-223 and MA-1100;
and/or the initiator is selected from one or more of potassium persulfate, hydrogen peroxide, sodium persulfate and ammonium persulfate;
and/or the reducing agent is selected from one or more of ascorbic acid and sodium bisulfite;
and/or the chain transfer agent is selected from one or more of beta-mercaptopropionic acid, 3-mercaptoacetic acid and 3-mercaptopropionic acid;
and/or the pH regulator is selected from one or more of potassium hydroxide solution, sodium hydroxide solution and sodium bicarbonate solution with the mass concentration of 25-35%;
and/or the solvent is selected from water.
10. Use of a viscosity reducing water reducer according to any one of claims 1 to 4 or prepared according to the method of any one of claims 5 to 9 in concrete.
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| CN116253842A (en) * | 2023-05-10 | 2023-06-13 | 山东大明精细化工有限公司 | Thickened oil viscosity reducer for displacement of reservoir oil and synthesis method |
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| CN116253842A (en) * | 2023-05-10 | 2023-06-13 | 山东大明精细化工有限公司 | Thickened oil viscosity reducer for displacement of reservoir oil and synthesis method |
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