CN110172128B - Brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer and preparation method thereof - Google Patents
Brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer and preparation method thereof Download PDFInfo
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- CN110172128B CN110172128B CN201910382696.1A CN201910382696A CN110172128B CN 110172128 B CN110172128 B CN 110172128B CN 201910382696 A CN201910382696 A CN 201910382696A CN 110172128 B CN110172128 B CN 110172128B
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/1416—Monomers containing oxygen in addition to the ether oxygen, e.g. allyl glycidyl ether
-
- 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
-
- 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
-
- 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
- C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/1416—Monomers containing oxygen in addition to the ether oxygen, e.g. allyl glycidyl ether
- C08F216/1425—Monomers containing side chains of polyether groups
- C08F216/1433—Monomers containing side chains of polyethylene oxide groups
Abstract
A brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer and a preparation method thereof are disclosed: the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer is obtained by taking ammonium persulfate as an initiator, maleic anhydride, vinyl triethoxysilane and allyl alcohol polyoxyethylene ether as monomers and mercaptopropionic acid as a chain transfer agent through addition polymerization. The brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer has a good viscosity-reducing effect in a cementing material.
Description
Technical Field
The invention relates to a polycarboxylic acid water reducing agent for concrete and a preparation method thereof, in particular to a polycarboxylic acid high-efficiency viscosity-reducing water reducing agent capable of obviously reducing the concrete viscosity with low water-gel ratio and multiple gelling components and a preparation method thereof.
Background
The water reducing agent is used as a key component of concrete and plays a decisive role in the workability of fresh concrete and various performances of hardened concrete.
At present, the most widely used is a polycarboxylic acid (PCE) water reducing agent, and the mixing amount of the PCE water reducing agent is 15-20 times of that of common concrete in a low water-cement ratio and complex gelling component system. However, concrete with low water-gel ratio and complex gel component system still has the defects of high viscosity and low fluidity, and brings extremely adverse effects on stirring, pumping and forming.
The traditional PCE molecule is of a comb-shaped structure, a main chain is connected through a C-C bond, anchoring groups such as carboxyl, sulfonic acid group and the like exist on the main chain of the molecule, the anchoring groups can be adsorbed on the surfaces of gelling component particles, and hydrophilic long side chains can provide steric hindrance to form a polymer adsorption layer with a certain thickness. When the particles of the gelling component are close to each other, the steric hindrance effect provided by the side chains can prevent the particles from approaching each other and agglomerating, thereby playing a role in dispersing the particles and reducing the viscosity of the system. According to the action mechanism of the comb-type PCE, for the purposes of reducing viscosity and improving fluidity of a complex gel component system with low water-gel ratio, the adsorption effect and the steric effect of the PCE need to be further enhanced, and the agglomeration of gel component particles, particularly auxiliary gel material particles, is prevented.
Disclosure of Invention
The invention aims to solve the technical problems that the defects of high viscosity and poor workability of the existing low water-cement ratio and complex gelled component system concrete are overcome, and the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer for the low water-cement ratio and complex gelled component system concrete and the preparation method thereof are provided.
The invention solves the technical problems by adopting the technical scheme that a brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer has the following general formula of a brush type molecular structure:
wherein a, b and c respectively represent the polymerization degree of each monomer in the polymer, and a: b: c = 1-5: 3-7: 1-5.
The brush type polycarboxylic acid high-efficiency viscosity-reducing water-reducing agent has the weight-average molecular weightM wIs 6000 to 18000 (preferably 8000 to 15000).
The preparation method of the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer comprises the steps of carrying out addition polymerization reaction in deionized water by taking Ammonium Persulfate (APS) as an initiator, Maleic Anhydride (MAH), Vinyl Triethoxysilane (VTEO) and allyl Alcohol Polyoxyethylene Ether (APEG) as monomers and mercaptopropionic acid as a chain transfer agent.
The weight ratio of the raw materials is 0.1-10 parts (preferably 0.5-8 parts; more preferably 1.0-6.0; even more preferably 2.0-5.0), 3-30 parts (preferably 5-25 parts; more preferably 8-20; even more preferably 10-15), 1-20 parts (preferably 2-15 parts; more preferably 4-12; even more preferably 6-10), 50-200 parts (preferably 60-180 parts; more preferably 80-160; even more preferably 90-150), 0.1-2 parts (preferably 0.3-1.6 parts; more preferably 0.5-1.2; even more preferably 0.7-1.0) of mercaptopropionic acid, and 60-80 parts (preferably 65-75 parts; more preferably 68-72) of deionized water.
Further, the specific operation steps are as follows:
(1) dissolving ammonium persulfate in deionized water to prepare an initiator solution;
(2) dissolving mercaptopropionic acid in deionized water to prepare a chain transfer agent solution;
(3) placing a four-neck flask containing allyl alcohol polyoxyethylene ether, maleic anhydride, vinyl triethoxy silicon, deionized water and a stirrer into an oil bath pot, heating to a specified temperature, uniformly dropwise adding an initiator solution and a chain transfer agent solution by using a peristaltic pump, and after dropwise adding, continuously preserving heat for 2-4 hours to perform addition polymerization;
(4) cooling the reaction product to below 40 ℃, and adding alkali (preferably NaOH) to adjust the pH value to 6-7 (preferably 7).
Further, in the step (1), the dropping rate of the initiator solution is 1-2 mL/min.
Further, in the step (2), the dropping rate of the chain transfer agent solution is 0.8-1.5 mL/min.
Further, in the step (3), the reaction temperature is 60-90 ℃.
Further, in the step (3), the initiator solution and the chain transfer agent solution are simultaneously dropped.
The technical principle of the invention is as follows: synthesizing the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer through chemical design.
The applicant finds out through research that: the degree of dispersion of the cementitious constituent particles and the surface tension of the liquid phase of the cementitious material are closely related to the viscosity of the concrete. The dispersion degree of the gelling component particles mainly depends on the interaction force and the steric hindrance effect among the particles, so that the electrostatic repulsion and the steric hindrance effect among the particles are improved, and the dispersion degree of the gelling component particles can be effectively improved; the surface tension of the liquid phase of the cementitious material is directly related to the surface activity of the additives used, etc.
Based on the research results, the invention prepares the brush type polycarboxylate superplasticizer with short main chain and long side chain by controlling the synthesis process on the basis of improving the electrostatic repulsion and the steric hindrance effect among the gelled component particles and the surface activity of the polycarboxylate superplasticizer, improves the adsorptivity of the main chain by using the monomer with high adsorption group density, improves the surface activity of the polycarboxylate superplasticizer by using the monomer with high surface activity, further reduces the viscosity of concrete and improves the fluidity.
The mixing amount of the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer is 1-3% of the total mass of the cementing material.
The brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer can be mixed with at least one additive known in the prior art for use, and comprises an early strength agent, an air entraining agent, a defoaming agent, a shrinkage reducing agent, an expanding agent and the like.
The molecular structure of the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer has the structural characteristics of short main chain and relatively longer side chain, has smaller hydrodynamic volume compared with comb type PCE, shows higher molecular degree of freedom in pore solution of a gelling component, and stretches molecular chains of the water reducer to expose more carboxyl and silicon hydroxyl, thereby being beneficial to forming a compact adsorption layer on the surface of the gelling component by the PCE and increasing the adsorption number of the PCE on the surface of the gelling component; and because the molecular weight is smaller, the brush type PCE has high surface activity and can obviously reduce the surface tension of the liquid phase of the gelled material.
The preparation method of the invention is based on the chemical design synthesis theory, and the length of the main chain and the density of the side chain are controlled; maleic anhydride with high carboxyl density and silane coupling agent containing silicon hydroxyl are adopted to enhance the adsorption capacity of the polycarboxylate superplasticizer on the surface of the gelling component; silane coupling agent containing double bonds is introduced into the main chain of the polycarboxylate superplasticizer through addition polymerization, so that the surface activity of the polycarboxylate superplasticizer is improved, and the surface tension of a liquid phase of a cementing material system is obviously reduced.
Compared with the existing water reducing agent, the invention has the following advantages: (1) the water reducing agent has a unique brush structure and has strong adsorption and steric effect; (2) the invention has the advantages of simple synthesis method, strong operability, low production cost and little environmental pollution; (3) the water reducing agent prepared by the method has the advantages of good viscosity reduction in a complex gelling component system, high water reducing rate, low mixing amount, good adaptability and the like.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, which is defined in the appended claims, as may be amended by those skilled in the art upon reading the present invention.
Example 1
Dissolving 1g of APS in deionized water to prepare an initiator solution, and dissolving 0.39g of mercaptopropionic acid in water to prepare a chain transfer agent solution; placing a four-neck flask containing 100g of APEG, 12g of MAH, 5g of VTEO, 100g of deionized water and a stirrer into an oil bath kettle, heating to 65 ℃, and then uniformly dropwise adding an initiator solution and a chain transfer agent solution by using a peristaltic pump; wherein the dropping rate of the initiator solution is about 1 mL/min, the dropping rate of the chain transfer agent solution is about 0.8 mL/min, and the temperature is kept for 4 hours after the dropping is finished; then, cooling the reaction product to 40 ℃, adding NaOH to adjust the pH value to 7, and obtaining the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer.
Example 2
Dissolving 6.8g of APS in deionized water to prepare an initiator solution, and dissolving 1.23g of mercaptopropionic acid in water to prepare a chain transfer agent solution; a four-neck flask containing 180g of APEG, 25g of MAH, 8g of VTEO, 220g of deionized water and a stirrer is placed in an oil bath kettle, and after the temperature is raised to 85 ℃, a peristaltic pump is used for uniformly dripping an initiator solution and a chain transfer agent solution. Wherein the dropping speed of the initiator solution is about 2 mL/min, the dropping speed of the chain transfer agent solution is about 1.2 mL/min, and the heat preservation is continued for 3h after the dropping is finished. And finally, cooling the reaction product to 39 ℃, and adding NaOH to adjust the pH value to 7 to obtain the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer.
Example 3
4.6g of APS was dissolved in deionized water to make an initiator solution, and 0.99g of mercaptopropionic acid was dissolved in water to make a chain transfer agent solution. Secondly, a four-neck flask containing 120g of APEG, 17.16g of MAH, 1.85g of VTEO, 160g of deionized water and a stirrer is placed in an oil bath kettle, and after the temperature is raised to 75 ℃, a peristaltic pump is used for uniformly dripping an initiator solution and a chain transfer agent solution. Wherein the dropping speed of the initiator solution is about 1.2 mL/min, the dropping speed of the chain transfer agent solution is about 1.2 mL/min, and the heat preservation is continued for 2.5h after the dropping is finished. And finally, cooling the reaction product to below 38 ℃, and adding NaOH to adjust the pH value to 6.9 to obtain the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer.
Comparative application example a commercial Sika ViscoCrete 3301 comb polycarboxylate water reducer was used. The materials used were cement and silica fume with a pH value of 42.5, a water-to-gel ratio of 0.18, a silica fume mixing amount of 20%, and a water reducing agent mixing amount of 2%. The PCE sample is added in 0.1mol/L NaNO3After the solution is fully dissolved, filtering the solution through a 0.22 mu m needle filter, and determining the molecular weight of the water reducing agent by adopting a Waters 1515 type gel permeation chromatograph of the United states Waters company; the surface tension of the water reducing agent solution with the concentration of 10 percent is tested by adopting an automatic control tensiometer of A-601 model of KINO company in America; carrying out total organic carbon content test by adopting a Sievers InnovOx total organic carbon analyzer of GE company in America, and calculating the adsorption amount of the water reducing agent on the surface of the gelled material particles according to the test result; the fluidity and the water reduction rate were carried out according to the relevant specifications of GB8076-2008 "concrete admixture Specification", using rheological parameters measured in a RheoPlus QC type coaxial cylindrical rheometer from Anton Paar, Germany.
TABLE 1 comparison table of physicochemical property tests of examples 1-3 and comparative application examples
TABLE 2 comparison of basic Performance tests of examples 1-3 and comparative application examples
As can be seen from Table 1, (1) the weight-average molecular mass was measuredM w10933-13159, the molecular weights of the examples are all smaller than those of the comparative examples, and the examples are proved to be brush structures with short main chains and long side chains; (2) the surface tension of the solution in the examples is 29.80 to 30.18 mN · m-1Lower than in the comparative example; (3) in the embodiment, the adsorption capacity of the cement-silica fume system with low water-cement ratio is 4.56-5.33 mg/g, which is obviously larger than that of the comparative example. As can be seen from the results of table 2, (1) the initial fluidity of the example was significantly increased by about 50 mm compared to the comparative example, showing excellent water-reducing effect; (2) the yield stress of the embodiment is 1.27-1.39 Pa, the equivalent plastic viscosity is 2.22-2.45 Pa.s, the comparative yield stress is reduced by 7.94-15.89%, the plastic viscosity is reduced by 59.84-63.61%, and the brush type polycarboxylate water reducer has obvious viscosity reduction and water reduction effects on a cement-silica fume system with a low water-cement ratio.
Claims (11)
1. The brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer is characterized in that: the general formula of the brush type molecular structure is as follows:
in the formula, a, b and c respectively represent the polymerization degree of each monomer in a polymer, wherein a: b: c = 1-10: 1-5;
the preparation method of the brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer comprises the following steps: performing addition polymerization reaction in deionized water by using ammonium persulfate as an initiator, maleic anhydride, vinyl triethoxysilane and allyl alcohol polyoxyethylene ether as monomers and mercaptopropionic acid as a chain transfer agent; the weight ratio of the raw materials is 0.1-10 parts of ammonium persulfate, 3-30 parts of maleic anhydride, 1-20 parts of vinyl triethoxysilane, 50-200 parts of allyl alcohol polyoxyethylene ether, 0.1-2 parts of mercaptopropionic acid and 60-80 parts of deionized water.
2. The brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 1, which is characterized by comprising, by weight, 0.5-8 parts of ammonium persulfate, 5-25 parts of maleic anhydride, 2-15 parts of vinyltriethoxysilane, 60-180 parts of allyl alcohol polyoxyethylene ether, 0.3-1.6 parts of mercaptopropionic acid and 65-75 parts of deionized water.
3. The brush type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 2, which is characterized by comprising, by weight, 1.0-6.0 parts of ammonium persulfate, 8-20 parts of maleic anhydride, 4-12 parts of vinyltriethoxysilane, 80-160 parts of allyl alcohol polyoxyethylene ether, 0.5-1.2 parts of mercaptopropionic acid and 68-72 parts of deionized water.
4. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) dissolving ammonium persulfate in deionized water to prepare an initiator solution;
(2) dissolving mercaptopropionic acid in deionized water to prepare a chain transfer agent solution;
(3) placing a four-neck flask containing allyl alcohol polyoxyethylene ether, maleic anhydride, vinyl triethoxy silicon, deionized water and a stirrer into an oil bath pot, heating to a specified temperature, uniformly dropwise adding an initiator solution and a chain transfer agent solution by using a peristaltic pump, and after dropwise adding, continuously preserving heat for 2-4 hours to perform addition polymerization;
(4) and cooling the reaction product to below 40 ℃, and adding alkali to adjust the pH value to 6-7.
5. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 4, which is characterized by comprising the following steps: in the step (1), the dropping rate of the initiator solution is 1-2 mL/min.
6. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 4 or 5, which is characterized by comprising the following steps: in the step (2), the dropping rate of the chain transfer agent solution is 0.8-1.5 mL/min.
7. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 4 or 5, which is characterized by comprising the following steps: in the step (3), the reaction temperature is 60-90 ℃.
8. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 6, which is characterized by comprising the following steps: in the step (3), the reaction temperature is 60-90 ℃.
9. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 4 or 5, which is characterized by comprising the following steps: in the step (3), the initiator solution and the chain transfer agent solution are simultaneously dropped.
10. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 6, which is characterized by comprising the following steps: in the step (3), the initiator solution and the chain transfer agent solution are simultaneously dropped.
11. The preparation method of the brush-type polycarboxylic acid high-efficiency viscosity-reducing water reducer according to claim 7, which is characterized by comprising the following steps: in the step (3), the initiator solution and the chain transfer agent solution are simultaneously dropped.
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| CN111019057B (en) * | 2019-12-06 | 2023-01-17 | 湖北工业大学 | Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN110982019A (en) * | 2019-12-06 | 2020-04-10 | 湖北工业大学 | High-viscosity-reduction type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN110790529B (en) * | 2019-12-11 | 2021-12-03 | 广东科隆智谷新材料股份有限公司 | High-strength concrete viscosity-reducing water reducer and preparation method thereof |
| CN111154052B (en) * | 2020-01-09 | 2021-03-23 | 湖南大学 | Viscosity reducer for ultra-high performance concrete and preparation method and application thereof |
| CN111808244B (en) * | 2020-08-21 | 2022-08-30 | 湖南加美乐素新材料股份有限公司 | Polycarboxylate superplasticizer with high water reduction and high adaptability and preparation method thereof |
| CN113968695B (en) * | 2021-09-24 | 2023-01-10 | 中核混凝土股份有限公司 | Method for manufacturing viscosity-reducing dispersive concrete |
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