CN113527593B - High-performance polycarboxylate superplasticizer and preparation method thereof - Google Patents
High-performance polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN113527593B CN113527593B CN202111041879.0A CN202111041879A CN113527593B CN 113527593 B CN113527593 B CN 113527593B CN 202111041879 A CN202111041879 A CN 202111041879A CN 113527593 B CN113527593 B CN 113527593B
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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
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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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
Abstract
The invention discloses a preparation method of a high-performance polycarboxylate water reducer, which takes isopentenyl polyethylene glycol and unsaturated acid monomers as main raw materials, adds unsaturated acid ester, acrylamide and cationic monomers, and prepares the polycarboxylate water reducer through free radical polymerization and siloxane grafting. The invention is prepared from the following raw materials in parts by weight: 60-100 parts of isopentene polyethylene glycol, 7-20 parts of unsaturated acid monomer, 1.0-5.0 parts of acrylamide, 1.0-10 parts of dimethylaminoethyl methacrylate, 0.5-5.0 parts of methacryloyloxyethyl trimethyl ammonium chloride, 1.0-6.0 parts of siloxane, 0.5-1.5 parts of oxidant, 0.3-1.0 part of reducing agent, 0.35-1.0 part of chain transfer agent and a proper amount of deionized water. The process flow is simple and easy to operate, and the synthesized water reducer has the functions of mud resistance and cement early strength improvement.
Description
Technical Field
The invention relates to the field of concrete admixtures in building materials, and particularly relates to a high-performance polycarboxylic acid water reducing agent and a preparation method thereof.
Background
The polycarboxylate superplasticizer is a water-soluble high polymer with a comb-shaped structure, is formed by copolymerizing unsaturated monomers containing carboxyl and other monomers, has excellent performance, and is called as a high-performance water reducing agent. However, the common water reducing agent often has certain retardation, and influences the early strength development of concrete. The main retarding mechanism is that high-density carboxylic acid groups generate a complex with free Ca2+ in the early stage of cement hydration and precipitate on the surface of cement particles to delay cement hydration, thereby reducing the early strength of cement. And the adaptability of the polycarboxylate superplasticizer to cement clay is poor, and the performance of the powdery polycarboxylate superplasticizer is affected by moisture.
Patent CN108192039A discloses a method for preparing a rapid hardening super early strength polycarboxylate water reducer, which is prepared by introducing monomers such as unsaturated alcohol amine ester, dimethylaminoethyl methacrylate and triallylamine and copolymerizing at room temperature to obtain the water reducer. The water reducing agent reduces the initial setting and final setting time of cement. But the effect of improving the early strength is not very significant. And the preparation reaction time of the unsaturated alcohol amine ester is long, the temperature is high, and the control is difficult. Patent CN112708044A discloses a method for preparing an ether anti-mud type super-early-strength polycarboxylate water reducer, which accelerates cement hydration to improve the early strength of cement and shows good mud resistance by introducing methoxy polyethylene glycol-acrylamide as a side chain and introducing cations.
In order to solve the problems, ester groups, amide groups, cations and siloxane can be introduced into the molecular structure of the water reducing agent. The ester group and the amide group can reduce the proportion of the carboxylic acid groups in the molecular chain, so that the adsorption of the initial carboxylic acid groups by the clay is reduced. And the ester group and the amide group can be hydrolyzed in an alkaline environment, so that the number of carboxylic acid groups is increased, and the concrete can still keep better fluidity. The siloxane is grafted to the molecular structure of the water reducing agent, so that the polycarboxylic acid water reducing agent powder has better fluidity and moisture resistance.
Therefore, the proper groups are introduced into the molecular structure of the polycarboxylic acid water reducing agent, and the performance of the water reducing agent is greatly influenced.
Disclosure of Invention
The invention aims to provide a high-performance polycarboxylate superplasticizer and a preparation method thereof, which solve one or more of the problems in the prior art.
According to one aspect of the invention, the high-performance polycarboxylate superplasticizer comprises the following components in parts by weight: 60-100 parts of isopentenyl polyethylene glycol, 7-20 parts of unsaturated acid monomers, 1.0-5.0 parts of acrylamide, 1.0-10 parts of dimethylaminoethyl methacrylate, 0.5-5.0 parts of methacryloyloxyethyl trimethyl ammonium chloride, 1.0-6.0 parts of siloxane, 0.5-1.5 parts of oxidant, 0.3-1.0 part of reducing agent, 0.35-1.0 part of chain transfer agent and 140 parts of deionized water 130-ion.
In certain embodiments, the unsaturated acid monomer is methacrylic acid or acrylic acid.
In certain embodiments, the siloxane is trimethylmethoxysilane or trimethylethoxysilane.
In certain embodiments, the prenyl polyethylene glycol has a molecular weight of 2400 g/mol.
In certain embodiments, the chain transfer agent is 3-mercaptopropionic acid.
In certain embodiments, the oxidizing agent is hydrogen peroxide, t-butanol peroxide, or ammonium persulfate.
In certain embodiments, the reducing agent is ascorbic acid or sodium formaldehyde sulfoxylate.
According to another aspect of the invention, the preparation method of the high-performance polycarboxylate superplasticizer comprises the following steps:
(1) adding isopentene polyethylene glycol, dimethylaminoethyl methacrylate, an oxidant and deionized water into a flask, stirring to completely dissolve, and heating to 60 ℃;
(2) mixing and stirring unsaturated acid monomers, a chain transfer agent, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride and deionized water to prepare a dropping liquid A; mixing and stirring a reducing agent and deionized water to prepare a dropping liquid B;
(3) dropwise adding a dropping liquid A and a dropping liquid B into the flask obtained in the step (1); the dropping of the dropping liquid A is finished within 180 minutes of 150 plus, and the dropping of the dropping liquid B is finished within 210 minutes of 180 plus; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
(4) carrying out water bath at 60 ℃, dropwise adding the solution D into a flask filled with the siloxane solution while stirring, wherein the dropwise adding time is 1h, and keeping the temperature for 0.5 h;
(5) adding a 30% sodium hydroxide solution into the solution for neutralization, and enabling the pH of the solution to be neutral to obtain a novel high-performance polycarboxylate superplasticizer mother solution;
(6) freeze drying the mother liquid and making powder.
The invention provides a high-performance polycarboxylate water reducer and a preparation method thereof, which have the advantages that a material A (unsaturated acid monomers, acrylamide, methacryloxyethyl trimethyl ammonium chloride and a chain transfer agent are dissolved in deionized water) and a material B (a reducing agent and the deionized water) are simultaneously dripped into a backing material (isopentenyl polyethylene glycol, hydrogen peroxide and water) at a constant speed, and after free radical polymerization and reaction, the polycarboxylate water reducer is subjected to in-situ grafting modification on siloxane to obtain a final product. The process operation is simple, the reaction condition is easy to control, the product performance is stable, the product is a non-toxic and harmless water-soluble polymer, and the preparation method is simple and reasonable, high in efficiency and low in cost.
Dimethyl aminoethyl methacrylate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride and siloxane can introduce siloxane, ester groups, amide groups and cations into the molecular structure of the water reducing agent; the introduction of the siloxane structure can play a role in flame retardance in the synthesis production process and the functions of preventing fouling and moisture hardening in the storage process of the polycarboxylate superplasticizer powder; ester groups and amide groups are introduced into the molecular structure, and the introduction of the groups can improve the mud resistance of the water reducing agent and improve the early strength of cement to a certain extent. The polycarboxylate superplasticizer prepared by the method has the advantages of good mud resistance, high early strength, easiness in storage and low possibility of deterioration.
Detailed Description
The present invention will be described in further detail below with reference to examples.
The invention provides a preparation method of a high-performance polycarboxylic acid water reducing agent, which comprises the following raw materials in parts by weight: 60-100 parts of isopentenyl polyethylene glycol, 7-20 parts of unsaturated acid monomer, 3.0-10.0 parts of acrylamide, 5-15 parts of dimethylaminoethyl methacrylate, 1.0-6.0 parts of methacryloyloxyethyl trimethyl ammonium chloride, 1.0-6.0 parts of siloxane, 0.5-1.5 parts of oxidant, 0.3-1.0 part of reducing agent, 0.35-1.0 part of chain transfer agent and 140 parts of deionized water 130-containing materials (the solid content of the prepared mother liquor is 40%).
The unsaturated acid monomer comprises any one of methacrylic acid and acrylic acid; the siloxane is any one of trimethyl methoxy silane and trimethyl ethoxy silane; the molecular weight of the isopentenyl polyethylene glycol is 2400 g/mol.
The chain transfer agent is 3-mercaptopropionic acid; the oxidant is one of hydrogen peroxide, tert-butyl peroxide or ammonium persulfate; the reducing agent is one of ascorbic acid and sodium formaldehyde sulfoxylate.
The preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
the method comprises the following steps: adding isopentene polyethylene glycol, dimethylaminoethyl methacrylate and an oxidant into a flask, adding deionized water, stirring to completely dissolve, and heating to 60 ℃;
step two: mixing and stirring unsaturated acid monomers, a chain transfer agent, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride and deionized water to prepare a dropping liquid A; mixing and stirring a reducing agent and deionized water to prepare a dropping liquid B;
step three: dropwise adding a dropping liquid A and a dropping liquid B into the flask obtained in the step one; the dropping of the dropping liquid A is finished in 180 minutes after 150 and 210 minutes after 180; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
step four: carrying out water bath at 60 ℃, dropwise adding the solution D into a flask filled with the siloxane solution while stirring, wherein the dropwise adding time is 1h, and keeping the temperature for 0.5 h;
step five: adding a 30% sodium hydroxide solution into the solution for neutralization to enable the pH of the solution to be neutral, and finally obtaining a solution which is a novel high-performance polycarboxylate superplasticizer mother solution;
step six: freeze drying the mother liquid and making powder.
Example 1
The invention provides a high-performance polycarboxylic acid water reducing agent, which comprises the following raw materials in parts by weight: 72 parts of isopentene polyethylene glycol, 9 parts of acrylic acid, 1.0 part of acrylamide, 2.4 parts of dimethylaminoethyl methacrylate, 0.8 part of methacryloyloxyethyl trimethyl ammonium chloride, 1.0 part of trimethylethoxysilane, 0.8 part of hydrogen peroxide, 0.3 part of ascorbic acid, 0.4 part of 3-mercaptopropionic acid and 130 parts of deionized water.
The preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
the method comprises the following steps: adding 72 parts of isopentenyl polyethylene glycol, 2.4 parts of dimethylaminoethyl methacrylate and 0.8 part of hydrogen peroxide into a flask, adding deionized water, stirring to completely dissolve, and heating to 60 ℃;
step two: mixing 9 parts of acrylic acid, 0.4 part of 3-mercaptopropionic acid, 1.0 part of acrylamide, 0.8 part of methacryloyloxyethyl trimethyl ammonium chloride and deionized water, and stirring to prepare a dropping liquid A; mixing 0.3 part of ascorbic acid and deionized water and stirring to prepare a dropping liquid B;
step three: dropwise adding a dropping liquid A and a dropping liquid B into the flask obtained in the step one; the dropping of the dropping liquid A is finished within 180 minutes, and the dropping of the dropping liquid B is finished within 210 minutes; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
step four: carrying out water bath at 60 ℃, dropwise adding the solution D into a flask containing 1.0 part of trimethylethoxysilane while stirring, wherein the dropwise adding time is 1h, and carrying out heat preservation for 0.5 h;
step five: adding 30% sodium hydroxide solution into the solution for neutralization to make the pH of the solution neutral, and finally obtaining PC1 solution;
step six: the PC1 solution was freeze-dried and made into powder.
Example 2
The invention provides a high-performance polycarboxylic acid water reducing agent, which comprises the following raw materials in parts by weight: 72 parts of isopentene polyethylene glycol, 9 parts of acrylic acid, 2.0 parts of acrylamide, 3.8 parts of dimethylaminoethyl methacrylate, 1.6 parts of methacryloyloxyethyl trimethyl ammonium chloride, 1.6 parts of trimethylethoxysilane, 0.8 part of hydrogen peroxide, 0.3 part of ascorbic acid, 0.4 part of 3-mercaptopropionic acid and 130 parts of deionized water.
The preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
the method comprises the following steps: adding 72 parts of isopentenyl polyethylene glycol, 3.8 parts of dimethylaminoethyl methacrylate and 0.8 part of hydrogen peroxide into a flask, adding deionized water, stirring to completely dissolve, and heating to 60 ℃;
step two: mixing 9 parts of acrylic acid, 0.4 part of 3-mercaptopropionic acid, 2.0 parts of acrylamide, 1.6 parts of methacryloyloxyethyl trimethyl ammonium chloride and deionized water, and stirring to prepare a dropping liquid A; mixing 0.3 part of ascorbic acid and deionized water and stirring to prepare a dropping liquid B;
step three: and (4) dropwise adding a dropping liquid A and a dropping liquid B into the flask in the step one. The dropping of the dropping liquid A is finished within 180 minutes, and the dropping of the dropping liquid B is finished within 210 minutes; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
step four: carrying out water bath at 60 ℃, adding the solution D dropwise into a flask containing 1.6 parts of trimethylethoxysilane for 1 hour while stirring, and keeping the temperature for 0.5 hour;
step five: adding 30% sodium hydroxide solution into the solution for neutralization to make the pH of the solution neutral, and finally obtaining PC2 solution;
step six: the PC1 solution was freeze-dried and made into powder.
Example 3
The invention provides a high-performance polycarboxylic acid water reducing agent, which comprises the following raw materials in parts by weight: 96 parts of isopentenyl polyethylene glycol, 17 parts of methacrylic acid, 1.4 parts of acrylamide, 3.2 parts of dimethylaminoethyl methacrylate, 1.1 parts of methacryloyloxyethyl trimethyl ammonium chloride, 1.2 parts of trimethyl methoxy silane, 1.0 part of hydrogen peroxide, 0.4 part of ascorbic acid, 0.5 part of 3-mercaptopropionic acid and 130 parts of deionized water.
The preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
the method comprises the following steps: adding 96 parts of isopentenyl polyethylene glycol, 3.2 parts of dimethylaminoethyl methacrylate and 1.0 part of hydrogen peroxide into a flask, adding deionized water, stirring to completely dissolve, and heating to 60 ℃;
step two: mixing 17 parts of methacrylic acid, 0.5 part of 3-mercaptopropionic acid, 1.4 parts of acrylamide, 1.1 parts of methacryloyloxyethyl trimethyl ammonium chloride and deionized water, and stirring to prepare a dropping liquid A; mixing 0.4 part of ascorbic acid and deionized water and stirring to prepare a dropping liquid B;
step three: and (4) dropwise adding a dropping liquid A and a dropping liquid B into the flask in the step one. The dropwise addition of the dropping solution A was completed within 180 minutes, and the dropwise addition of the dropping solution B was completed within 210 minutes. After the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
step four: carrying out water bath at 60 ℃, dropwise adding the solution D into a flask containing 1.2 parts of trimethylethoxysilane while stirring, wherein the dropwise adding time is 1h, and carrying out heat preservation for 0.5 h;
step five: adding 30% sodium hydroxide solution into the solution for neutralization to make the pH of the solution neutral, and finally obtaining PC3 solution;
step six: the PC3 solution was freeze-dried and made into powder.
Example 4
The invention provides a high-performance polycarboxylic acid water reducing agent, which comprises the following raw materials in parts by weight: 96 parts of isopentenyl polyethylene glycol, 17 parts of methacrylic acid, 2.8 parts of acrylamide, 5.0 parts of dimethylaminoethyl methacrylate, 2.2 parts of methacryloyloxyethyl trimethyl ammonium chloride, 2.4 parts of trimethyl methoxy silane, 1.0 part of hydrogen peroxide, 0.4 part of ascorbic acid, 0.5 part of 3-mercaptopropionic acid and 130 parts of deionized water.
The preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
the method comprises the following steps: adding 96 parts of isopentenyl polyethylene glycol, 5.0 parts of dimethylaminoethyl methacrylate and 1.0 part of hydrogen peroxide into a flask, adding deionized water, stirring to completely dissolve, and heating to 60 ℃;
step two: mixing 17 parts of methacrylic acid, 0.5 part of 3-mercaptopropionic acid, 2.8 parts of acrylamide, 2.2 parts of methacryloyloxyethyl trimethyl ammonium chloride and deionized water, and stirring to prepare a dropping liquid A; mixing 0.4 part of ascorbic acid and deionized water and stirring to prepare a dropping liquid B;
step three: and (4) dropwise adding a dropping liquid A and a dropping liquid B into the flask in the step one. The dropping of the dropping liquid A is finished within 180 minutes, and the dropping of the dropping liquid B is finished within 210 minutes; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
step four: carrying out water bath at 60 ℃, dropwise adding the solution D into a flask containing 2.4 parts of trimethylethoxysilane while stirring, wherein the dropwise adding time is 1h, and carrying out heat preservation for 0.5 h;
step five: adding 30% sodium hydroxide solution into the solution for neutralization to make the pH of the solution neutral, and finally obtaining PC4 solution;
step six: the PC4 solution was freeze-dried and made into powder.
Example 5
The invention provides a high-performance polycarboxylic acid water reducing agent, which comprises the following raw materials in parts by weight: 96 parts of isopentenyl polyethylene glycol, 15 parts of acrylic acid, 2.8 parts of acrylamide, 6.0 parts of dimethylaminoethyl methacrylate, 2.2 parts of methacryloyloxyethyl trimethyl ammonium chloride, 3.3 parts of trimethyl methoxy silane, 1.0 part of hydrogen peroxide, 0.4 part of ascorbic acid, 0.5 part of 3-mercaptopropionic acid and 130 parts of deionized water.
The preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
the method comprises the following steps: 96 parts of isopentenyl polyethylene glycol, 5.0 parts of dimethylaminoethyl methacrylate and 1.0 part of hydrogen peroxide are added into a flask, and then deionized water is added, stirred and dissolved completely, and heated to 60 ℃.
Step two: mixing and stirring 15 parts of acrylic acid, 0.5 part of 3-mercaptopropionic acid, 2.8 parts of acrylamide, 2.2 parts of methacryloyloxyethyl trimethyl ammonium chloride and deionized water to prepare a dropping liquid A; mixing 0.4 part of ascorbic acid and deionized water and stirring to prepare a dropping liquid B;
step three: and (4) dropwise adding a dropping liquid A and a dropping liquid B into the flask in the step one. The dropping of the dropping liquid A is finished within 180 minutes, and the dropping of the dropping liquid B is finished within 210 minutes; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
step four: carrying out water bath at 60 ℃, dropwise adding the solution D into a flask containing 2.4 parts of trimethylethoxysilane while stirring, wherein the dropwise adding time is 1h, and carrying out heat preservation for 0.5 h;
step five: adding 30% sodium hydroxide solution into the solution for neutralization to make the pH of the solution neutral, and finally obtaining PC5 solution;
step six: the PC5 solution was freeze-dried and made into powder.
Comparative example 1
The preparation process was the same as in example 1 except that the raw materials contained no dimethylaminoethyl methacrylate, acrylamide, methacryloyloxyethyl trimethylammonium chloride, and siloxane, to obtain a PC6 solution.
Comparative example 2
The procedure was as in example 1 except that the starting material contained no siloxane to give a solution of PC 7.
Comparative example 3
The preparation process was the same as in example 3 except that the raw materials contained no dimethylaminoethyl methacrylate and silicone, to obtain a PC8 solution.
Comparative example 4
The preparation process was the same as in example 3 except that acrylamide and methacryloyloxyethyl trimethylammonium chloride were not contained in the raw materials, to obtain a PC9 solution.
The samples obtained in examples 1-5 and comparative examples 1-4 were compared by using standard cement, the water cement ratio was 0.25, and the water reducing agent folded solid content was 0.09% of the cement content.
TABLE 1 comparison of the results of the fluidity tests of the polycarboxylate superplasticizers cement paste of each example and comparative example
As can be seen from Table 1, the polycarboxylate water reducer prepared by the method disclosed by the invention is added into the cement paste, so that the cement paste has better fluidity, and after 20min, the cement paste fluidity is not changed greatly, so that the water reducer can keep good fluidity of the cement paste. The fluidity of the cement paste is greatly improved by adding the water reducing agent of dimethylaminoethyl methacrylate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride and siloxane.
TABLE 2 Effect of the polycarboxylate Water reducers of the examples and comparative examples on the compressive Strength of Cement Net slurries
It can be seen from Table 2 that the compressive strengths of the cements of examples 1-5 are all superior to those of comparative example 1. The water reducing agent prepared by the method is improved in early strength of cement. The polycarboxylate superplasticizer prepared by the invention has the capability of improving the early strength of cement.
Table 3. flow properties of concrete with 1% montmorillonite added.
As can be seen from Table 3, when the amount of montmorillonite added is 1%, the net slurry fluidity of examples 1-5 is significantly higher than that of comparative examples 1-4, indicating that the polycarboxylic acid water reducing agent prepared by the present invention has good soil resistance.
The foregoing is only a preferred form of the invention and it should be noted that several similar variations and modifications could be made by one skilled in the art without departing from the inventive concept and these should also be considered within the scope of the invention.
Claims (8)
1. The high-performance polycarboxylate superplasticizer is characterized by comprising the following components in parts by weight: 60-100 parts of isopentenyl polyethylene glycol, 7-20 parts of unsaturated acid monomers, 1.0-5.0 parts of acrylamide, 1.0-10 parts of dimethylaminoethyl methacrylate, 0.5-5.0 parts of methacryloyloxyethyl trimethyl ammonium chloride, 1.0-6.0 parts of siloxane, 0.5-1.5 parts of oxidant, 0.3-1.0 part of reducing agent, 0.35-1.0 part of chain transfer agent and 140 parts of deionized water 130-ion.
2. The high-performance polycarboxylate superplasticizer according to claim 1, wherein said unsaturated acid monomer is methacrylic acid or acrylic acid.
3. The high-performance polycarboxylate water reducer according to claim 1, characterized in that the siloxane is trimethylmethoxysilane or trimethylethoxysilane.
4. The high-performance polycarboxylate superplasticizer according to claim 1, wherein the molecular weight of said prenyl polyethylene glycol is 2400 g/mol.
5. The high-performance polycarboxylate water reducer according to claim 1, characterized in that the chain transfer agent is 3-mercaptopropionic acid.
6. The high-performance polycarboxylate water reducer according to claim 1, characterized in that the oxidant is hydrogen peroxide, tert-butyl peroxide or ammonium persulfate.
7. The high-performance polycarboxylate water reducer according to claim 1, characterized in that the reducing agent is ascorbic acid or sodium formaldehyde sulfoxylate.
8. The preparation method of the high-performance polycarboxylate water reducer as defined in any one of claims 1-7, characterized by comprising the following steps:
(1) adding isopentenyl polyethylene glycol, dimethylaminoethyl methacrylate, an oxidant and deionized water into a flask, stirring to completely dissolve, and heating to 60 ℃;
(2) mixing and stirring unsaturated acid monomers, a chain transfer agent, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride and deionized water to prepare a dropping liquid A; mixing and stirring a reducing agent and deionized water to prepare a dropping liquid B;
(3) dropwise adding a dropping liquid A and a dropping liquid B into the flask obtained in the step (1); the dropping of the dropping liquid A is finished within 180 minutes of 150 plus, and the dropping of the dropping liquid B is finished within 210 minutes of 180 plus; after the dripping is finished, keeping the temperature for 0.5h to obtain a solution D;
(4) carrying out water bath at 60 ℃, dropwise adding the solution D into a flask filled with the siloxane solution while stirring, wherein the dropwise adding time is 1h, and keeping the temperature for 0.5 h;
(5) adding a sodium hydroxide solution with the concentration of 30% into the solution for neutralization, and enabling the pH of the solution to be neutral to obtain a novel high-performance polycarboxylate superplasticizer mother solution;
(6) freeze drying the mother liquid and making powder.
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Denomination of invention: A high-performance polycarboxylate water reducer and its preparation method Effective date of registration: 20230727 Granted publication date: 20211119 Pledgee: Jiangsu Rudong Rural Commercial Bank Co.,Ltd. Xindian Sub branch Pledgor: JIANGSU VIRGINIA CONSTRUCTION MATERIALS CO.,LTD. Registration number: Y2023980049886 |
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