CN109400821B - Concrete bleeding-resistant inhibitor with water reducing function and preparation method thereof - Google Patents
Concrete bleeding-resistant inhibitor with water reducing function and preparation method thereof Download PDFInfo
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- CN109400821B CN109400821B CN201811301988.XA CN201811301988A CN109400821B CN 109400821 B CN109400821 B CN 109400821B CN 201811301988 A CN201811301988 A CN 201811301988A CN 109400821 B CN109400821 B CN 109400821B
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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
Abstract
The invention discloses a concrete bleeding-resistant inhibitor with a water reducing function and a preparation method thereof, wherein the bleeding-resistant inhibitor is mainly prepared by carrying out aqueous solution free radical polymerization on a polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof, a cross-linking agent, an oxidizing agent, a reducing agent, a chain transfer agent and deionized water at 15-30 ℃, then adding sodium hydroxide solution to adjust the pH value, and then supplementing water. The preparation method is used for production at normal temperature, a heat source is not needed, equipment is simple, pollution is avoided, production efficiency is high, the bleeding-resistant inhibitor can effectively solve the problems that the existing polycarboxylate superplasticizer is poor in water retention and water absorption performance, poor in workability and prone to bleeding and bottom scratching, has excellent thickening and water retention performances, and can greatly reduce construction difficulty.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to a concrete bleeding-resistant inhibitor with a water reducing function and a preparation method thereof.
Background
The polycarboxylic acid high-performance water reducing agent has a series of excellent performances of high water reducing rate, low mixing amount, strong adaptability, small loss, environmental protection and the like, is widely applied to the engineering fields of real estate buildings, railways, highways, bridges, water conservancy, hydropower and the like, is gradually becoming the most widely applied concrete admixture in China instead of other products at present, and is suitable for the development of high-performance concrete.
Although the excellent water reducing performance of the polycarboxylic acid water reducing agent is widely accepted by the industry at present, due to the change of cement, the difference of the quality of pulverized materials such as coal ash and the like, the poor grading of aggregate and the like, the polycarboxylic acid water reducing agent also has the phenomena of too fast slump loss, poor workability, bleeding and bottom grabbing in practical application, and the working performance of concrete is reduced. In engineering application, different varieties of polycarboxylic acid water reducers and various chemical additives for adjusting viscosity are frequently considered to be compounded for use, such as xanthan gum, welan gum, cellulose ether, polyacrylamide, polyvinyl alcohol and the like, the viscosity of a mixture can be increased, a good tackifying effect can be achieved when the mixing amount is small, the improvement effect on the viscosity of concrete is obvious, and the phenomena of bottom grabbing and bleeding of the concrete can be obviously reduced. However, from the practical engineering point of view, most viscosity regulators have compatibility problems with polycarboxylic acid water reducing agents. On one hand, flocculation and delamination phenomena are easy to occur in the compounding and storage process of the viscosity regulator and the polycarboxylate superplasticizer, so that the storage stability is poor; on the other hand, the addition of the viscosity modifier can affect the dispersibility of the polycarboxylate superplasticizer and even reduce the concrete fluidity in severe cases.
Aiming at the problems, at present, many researchers prepare thickening and water-retaining polycarboxylic acid water reducing agents through molecular structure design to solve the problems of concrete bleeding, bottom grabbing and the like, but the problems of complex process, high production cost and the like exist.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a concrete bleeding-resistant inhibitor with a water reducing function and a preparation method thereof, the concrete bleeding-resistant inhibitor with the water reducing function can be prepared at the normal temperature of 15-30 ℃, and the bleeding-resistant inhibitor can effectively solve the problems of poor water retention and water absorption performance, poor workability and easiness in bleeding and bottom grabbing of the existing polycarboxylic acid water reducing agent.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 300-360 parts of unsaturated polyether macromonomer, 50-100 parts of unsaturated carboxylic acid, 20-30 parts of unsaturated amide, 3-8 parts of unsaturated sulfonic acid or salt thereof, 0.5-3.0 parts of cross-linking agent, 4-6 parts of oxidant, 0.5-1.5 parts of reducing agent, 1.0-1.5 parts of chain transfer agent and 450-500 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0: 7.0-8.0: 2.0-3.0: 0.2-0.5: 0.02-0.05.
Further, the feed comprises the following raw materials in parts by mass: 330 parts of unsaturated polyether macromonomer, 76.5 parts of unsaturated carboxylic acid, 30 parts of unsaturated amide, 6.8 parts of unsaturated sulfonic acid or salt thereof, 0.8 part of cross-linking agent, 4.9 parts of oxidizing agent, 0.73 part of reducing agent, 1.32 parts of chain transfer agent and 485 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.45:2.2:0.24:0.038.
Further, the unsaturated polyether macromonomer is one or two of allyl alcohol polyoxyethylene ether, isoamylol polyoxyethylene ether and isobutenol polyoxyethylene ether, and the molecular weight of the unsaturated polyether macromonomer is 2400-3000.
Further, the unsaturated carboxylic acid is one or two of acrylic acid, methacrylic acid, maleic anhydride and fumaric acid.
Further, the unsaturated amide is one or two of acrylamide, methacrylamide, N-dimethylacrylamide, N-methylolacrylamide and N-isopropylacrylamide.
Further, the unsaturated sulfonic acid or the salt thereof is one or two of 2-acrylamide-2-methylpropanesulfonic acid, sodium methallyl sulfonate, sodium allyl sulfonate and sodium p-styrene sulfonate.
Further, the cross-linking agent is one or two of N, N-methylene bisacrylamide, polyethylene glycol 400 diacrylate and polyethylene glycol 400 dimaleate; the chain transfer agent is one or two of thioglycolic acid, mercaptopropionic acid, mercaptoethanol, methyl mercaptopropionate, ethyl mercaptopropionate and isooctyl mercaptopropionate.
Further, the oxidant is one or two of hydrogen peroxide, ammonium persulfate, potassium persulfate, sodium persulfate and tert-butyl hydroperoxide.
Further, the reducing agent is at least two of vitamin C, rongalite, ferrous sulfate heptahydrate, sodium hydrosulfite, sodium thiosulfate, sodium hypophosphite, sodium bisulfite and sodium metabisulfite.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) sequentially adding unsaturated polyether macromonomer, unsaturated amide, unsaturated sulfonic acid or salt thereof, oxidant and deionized water into a reaction kettle, stirring and dissolving to prepare a mixed bottom material solution with the mass fraction of 50-60%;
(2) mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution A with the mass fraction of 1.0-2.0%; mixing unsaturated carboxylic acid, a cross-linking agent and deionized water to prepare a solution B with the mass fraction of 50-70%;
(3) and (2) dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 15-30 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5-3.0 h, dropwise adding the solution A for 5-10 min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0-2.5 h, ensuring that the solution A is later than the solution B is completely dropwise added, continuously stirring for 1.0-1.5 h after the dropwise adding of the two solutions is completed, finally adjusting the pH value of the solution to be 5.0-7.0 by using a sodium hydroxide solution with the mass fraction of 30%, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt%.
The beneficial effects produced by adopting the scheme are as follows:
(1) the anti-bleeding inhibitor utilizes the highly active carbon-carbon double bond in the functional monomerThe self-polymerization and the copolymerization are used for effectively improving the molecular mass of the polymer so as to improve the tackifying performance of the thickening agent; simultaneously, a large amount of-SO is in the molecular structure3H. -COOH and-CONH2The high water absorption group and the certain net structure can play roles of water retention, thickening, adhesion and the like, and can improve interaction among concrete particles, thereby increasing the strength and toughness of the concrete, and leading the concrete to have good workability, no bleeding, no bottom grabbing, high strength and stronger thickening and water retention performances.
(2) The crosslinking agent of the invention firstly carries out partial crosslinking on unsaturated carboxylic acid, the crosslinked copolymer can be hydrolyzed under the cement alkaline environment, the crosslinking chemical bond is broken, each molecule which is crosslinked is released, and the water reducing agent molecule with dispersion effect is continuously released, thereby continuously supplementing the water reducing agent which is adsorbed and covered by hydrate, achieving the effect of slow release and having excellent long-acting slump retentivity. The bleeding-resistant inhibitor can not only keep the slump of the ready-mixed concrete after long-time transportation, but also avoid the evaporation of mixing water caused by long-time transportation at high temperature.
(3) According to the concrete bleeding resistance inhibitor, polymer molecules form a high-water-absorption three-dimensional network structure, when the concrete bleeding resistance inhibitor is used, the concrete mixture is good in workability, good in flowability and strong in bleeding resistance, the slurry structure is more compact through the coordination and promotion effect among the components, and more chemical bonds with stronger binding force are generated among cement hydrated particles to replace Van der Waals force, so that the bonding force of a cementing material is improved, the strength of cement and concrete is improved, the quality and performance of the concrete material are improved, and the cohesiveness and pumpability of the concrete mixture are improved.
(4) The bleeding-resistant inhibitor prepared by the invention can be compounded with a common high-performance water reducing agent for use, has good compatibility and storage stability, does not cause flocculation and delamination phenomena of traditional viscosity regulators such as xanthan gum, welan gum, cellulose ether, polyacrylamide, polyvinyl alcohol and the like, can obviously improve the adaptability of concrete and obviously reduce the slump loss of the concrete, and simultaneously has the advantages of high strength, good durability, no segregation and no bleeding.
(5) The preparation method of the invention adopts a normal temperature process, does not need a heat source, has the advantages of simple production process, easy control of reaction, low cost and the like, and simultaneously, the prepared anti-bleeding inhibitor not only has higher water reducing rate, but also can effectively improve the workability and slump retention of the concrete and improve the strength of the concrete.
Detailed Description
Example 1
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 300 parts of prenyl alcohol polyoxyethylene ether, 68 parts of acrylic acid, 21 parts of acrylamide, 5.7 parts of 2-acrylamide-2-methylpropanesulfonic acid, 0.72 part of N, N-methylene bisacrylamide, 2.4 parts of hydrogen peroxide, 2.1 parts of potassium persulfate, 0.35 part of vitamin C, 0.25 part of sodium bisulfite, 1.2 parts of mercaptopropionic acid and 465 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.55:2.33:0.22:0.037.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) adding 300g of prenyl alcohol polyoxyethylene ether with the molecular weight of 2400, 21g of acrylamide, 5.7g of 2-acrylamide-2-methylpropanesulfonic acid, 2.4g of hydrogen peroxide, 2.1g of potassium persulfate and 290g of deionized water into a reaction kettle in sequence, and stirring and dissolving uniformly to obtain a mixed base material solution;
(2) mixing 0.35g of vitamin C, 0.25g of sodium bisulfite, 1.2g of mercaptopropionic acid and 130g of deionized water to prepare a mixed solution A; mixing 68g of acrylic acid, 0.72g of N, N-methylene bisacrylamide and 45g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 25 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5h, dropwise adding the solution A for 5min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0h, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1.5h after the dropwise adding of the two solutions is completed, finally, regulating the pH value of the solution to be 5.0-7.0 by using 30% of sodium hydroxide solution, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-1).
Example 2
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 360 parts of prenyl alcohol polyoxyethylene ether, 95 parts of methacrylic acid, 30 parts of methacrylamide, 6 parts of sodium methallyl sulfonate, 3.2 parts of polyethylene glycol 400 diacrylate, 2.4 parts of hydrogen peroxide, 2.4 parts of ammonium persulfate, 0.55 part of vitamin C, 0.35 part of sodium thiosulfate, 0.72 part of thioglycolic acid, 0.6 part of mercaptopropionic acid and 480 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.36:2.35:0.25:0.042.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) adding 360g of prenyl alcohol polyoxyethylene ether with the molecular weight of 2400, 30g of methacrylamide, 6g of sodium methylacrylsulfonate, 2.4g of hydrogen peroxide, 2.4g of ammonium persulfate and 285g of deionized water into a reaction kettle in sequence, and stirring and dissolving uniformly to obtain a mixed base material solution;
(2) mixing 0.55g of vitamin C, 0.35g of sodium thiosulfate, 0.72g of thioglycolic acid, 0.6g of mercaptopropionic acid and 155g of deionized water to prepare a mixed solution A; mixing 95g of methacrylic acid, 3.2g of polyethylene glycol 400 diacrylate and 40g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 20 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5h, dropwise adding the solution A for 8min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0h, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1.5h after the dropwise adding of the two solutions is completed, finally, regulating the pH value of the solution to be 5.0-7.0 by using 30% of sodium hydroxide solution, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-2).
Example 3
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 330 parts of prenyl alcohol polyoxyethylene ether, 55 parts of acrylic acid, 20 parts of methacrylic acid, 20 parts of acrylamide, 5 parts of N, N-dimethylacrylamide, 6.5 parts of sodium p-styrene sulfonate, 3.6 parts of polyethylene glycol 400 dimaleate, 2.1 parts of hydrogen peroxide, 3 parts of sodium persulfate, 1.2 parts of rongalite, 1.45 parts of mercaptopropionic acid and 470 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.24:2.41:0.23:0.044.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) sequentially adding 330g of prenyl alcohol polyoxyethylene ether with the molecular weight of 2400, 20g of acrylamide, 5g of N, N-dimethylacrylamide, 6.5g of sodium p-styrenesulfonate, 2.1g of hydrogen peroxide, 3g of sodium persulfate and 290g of deionized water into a reaction kettle, and uniformly stirring and dissolving to obtain a mixed base material solution;
(2) mixing 1.2g of rongalite, 1.45g of mercaptopropionic acid and 140g of deionized water to prepare a mixed solution A; mixing 55g of acrylic acid, 20g of methacrylic acid, 3.6g of polyethylene glycol 400 dimaleate and 40g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed base material solution prepared in the step (1) at the temperature of 20 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 3 hours, dropwise adding the solution A for 6min, then dropwise adding the solution B into the mixed base material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.5 hours, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1 hour after the two solutions are dropwise added, finally, regulating the pH value of the solution to be 5.0-7.0 by using a sodium hydroxide solution with the mass fraction of 30%, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-3).
Example 4
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 300 parts of isobutylene polyoxyethylene ether, 42 parts of acrylic acid, 34 parts of maleic anhydride, 27.5 parts of N, N-dimethylacrylamide, 6.2 parts of 2-acrylamide-2-methylpropanesulfonic acid, 2.4 parts of polyethylene glycol 400 diacrylate, 3.2 parts of hydrogen peroxide, 1.8 parts of ammonium persulfate, 0.7 part of rongalite, 0.3 part of sodium metabisulfite, 1.26 parts of isooctyl mercaptopropionate and 490 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.44:2.22:0.24:0.038.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) adding 300g of isobutenol polyoxyethylene ether with the molecular weight of 2400, 27.5g of N, N-dimethylacrylamide, 6.2g of 2-acrylamide-2-methylpropanesulfonic acid, 3.2g of hydrogen peroxide, 1.8g of ammonium persulfate and 285g of deionized water into a reaction kettle in sequence, and stirring and dissolving uniformly to obtain a mixed bottom material solution;
(2) mixing 0.7g of rongalite, 0.3g of sodium metabisulfite, 1.26g of isooctyl mercaptopropionate and 155g of deionized water to prepare a mixed solution A; mixing 42g of acrylic acid, 34g of maleic anhydride, 2.4g of polyethylene glycol 400 diacrylate and 50g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed base material solution prepared in the step (1) at the temperature of 15 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 3 hours, dropwise adding the solution A for 6 minutes, then dropwise adding the solution B into the mixed base material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.5 hours, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1 hour after the two solutions are dropwise added, finally, regulating the pH value of the solution to be 5.0-7.0 by using a sodium hydroxide solution with the mass fraction of 30%, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-4).
Example 5
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 200 parts of prenyl alcohol polyoxyethylene ether, 120 parts of isobutenyl alcohol polyoxyethylene ether, 59.6 parts of acrylic acid, 16.5 parts of fumaric acid, 25 parts of methacrylamide, 3 parts of N-hydroxymethyl acrylamide, 5.2 parts of allyl propanesulfonic acid, 3.5 parts of polyethylene glycol 400 dimaleate, 3.6 parts of tert-butyl hydroperoxide, 1.2 parts of ammonium persulfate, 0.32 part of vitamin C, 0.3 part of sodium hydrosulfite, 0.01 part of ferrous sulfate heptahydrate, 1.5 parts of mercaptoethanol and 495 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.27:2.43:0.27:0.044.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) adding 200g of prenyl alcohol polyoxyethylene ether with the molecular weight of 2400, 120g of isobutenyl alcohol polyoxyethylene ether with the molecular weight of 2400, 25g of methacrylamide, 3g of N-hydroxymethyl acrylamide, 5.2g of allyl propanesulfonic acid, 3.6g of tert-butyl hydroperoxide, 1.2g of ammonium persulfate and 290g of deionized water into a reaction kettle in sequence, and stirring and dissolving uniformly to obtain a mixed primer solution;
(2) mixing 0.32g of vitamin C, 0.3g of sodium hydrosulfite, 0.01g of ferrous sulfate heptahydrate, 1.5g of mercaptoethanol and 155g of deionized water to prepare a mixed solution A; mixing 59.6g of acrylic acid, 16.5g of fumaric acid, 3.5g of polyethylene glycol 400 dimaleate and 50g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 25 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5h, dropwise adding the solution A for 8min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0h, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1.5h after the dropwise adding of the two solutions is completed, finally, regulating the pH value of the solution to be 5.0-7.0 by using 30% of sodium hydroxide solution, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-5).
Example 6
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 300 parts of allyl alcohol polyoxyethylene ether, 25 parts of acrylic acid, 60 parts of maleic anhydride, 18.5 parts of acrylamide, 5.6 parts of N-isopropyl acrylamide, 5 parts of sodium allylsulfonate, 2.6 parts of polyethylene glycol 400 dimaleate, 3.6 parts of hydrogen peroxide, 1.8 parts of ammonium persulfate, 1.25 parts of rongalite, 1.26 parts of mercaptopropionic acid and 475 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.67:2.48:0.28:0.035.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) adding 300g of allyl alcohol polyoxyethylene ether with the molecular weight of 2400, 18.5g of acrylamide, 5.6g of N-isopropyl acrylamide, 5g of sodium allylsulfonate, 3.6g of hydrogen peroxide, 1.8g of ammonium persulfate and 285g of deionized water into a reaction kettle in sequence, and stirring and dissolving uniformly; obtaining mixed bottom material solution;
(2) mixing 1.25g of rongalite, 1.26g of mercaptopropionic acid and 135g of deionized water to prepare a mixed solution A; mixing 25g of acrylic acid, 60g of maleic anhydride, 2.6g of polyethylene glycol 400 dimaleate and 55g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed base material solution prepared in the step (1) at the temperature of 20 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 3 hours, dropwise adding the solution A for 5min, then dropwise adding the solution B into the mixed base material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.5 hours, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1 hour after the two solutions are dropwise added, finally, regulating the pH value of the solution to be 5.0-7.0 by using a sodium hydroxide solution with the mass fraction of 30%, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-6).
Example 7
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 330 parts of isobutylene alcohol polyoxyethylene ether, 60 parts of acrylic acid, 16.5 parts of methacrylic acid, 30 parts of N, N-dimethylacrylamide, 6.8 parts of sodium p-styrenesulfonate, 0.8 part of N, N-methylene bisacrylamide, 4.9 parts of tert-butyl hydroperoxide, 0.72 part of vitamin C, 0.01 part of ferrous sulfate, 1.32 parts of ethyl mercaptopropionate and 485 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.45:2.2:0.24:0.038.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) sequentially adding 330g of isobutenol polyoxyethylene ether with the molecular weight of 2400, 30g of N, N-dimethylacrylamide, 6.8g of sodium p-styrene sulfonate, 4.9g of tert-butyl hydroperoxide and 285g of deionized water into a reaction kettle, and stirring and dissolving uniformly to obtain a mixed bottom material solution; (ii) a
(2) Mixing 0.72g of vitamin C, 0.01g of ferrous sulfate, 1.32g of ethyl mercaptopropionate and 140g of deionized water to prepare a mixed solution A; mixing 60g of acrylic acid, 16.5g of methacrylic acid, 0.8g of N, N-methylene bisacrylamide and 60g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 15 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5h, dropwise adding the solution A for 5min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0h, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1.5h after the dropwise adding of the two solutions is completed, finally, regulating the pH value of the solution to be 5.0-7.0 by using 30% of sodium hydroxide solution, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-7).
Example 8
A concrete bleeding-resistant inhibitor with a water reducing function comprises the following raw materials in parts by weight: 200 parts of prenyl alcohol polyoxyethylene ether, 120 parts of allyl alcohol polyoxyethylene ether, 55 parts of acrylic acid, 20 parts of maleic anhydride, 22 parts of acrylamide, 6 parts of 2-acrylamide-2-methylpropanesulfonic acid, 2.8 parts of polyethylene glycol 400 diacrylate, 2.4 parts of hydrogen peroxide, 2.6 parts of sodium persulfate, 0.5 part of vitamin C, 0.2 part of sodium hypophosphite, 1.58 parts of thioglycolic acid and 480 parts of deionized water; unsaturated polyether macromonomer, unsaturated carboxylic acid, unsaturated amide, unsaturated sulfonic acid or salt thereof and crosslinking agent, wherein the mass ratio of the substances is as follows: 1.0:7.25:2.32:0.22:0.041.
The preparation method of the concrete anti-bleeding inhibitor with the water reducing function comprises the following steps:
(1) sequentially adding 200g of prenyl alcohol polyoxyethylene ether with the molecular weight of 2400, 120g of allyl alcohol polyoxyethylene ether with the molecular weight of 2400, 22g of acrylamide, 6g of 2-acrylamide-2-methylpropanesulfonic acid, 2.4g of hydrogen peroxide, 2.6g of sodium persulfate and 280g of deionized water into a reaction kettle, and stirring and dissolving uniformly to obtain a mixed bottom material solution;
(2) mixing 0.5g of vitamin C, 0.2g of sodium hypophosphite, 1.58g of thioglycolic acid and 150g of deionized water to prepare a mixed solution A; mixing 55g of acrylic acid, 20g of maleic anhydride, 2.8g of polyethylene glycol 400 diacrylate and 50g of deionized water to prepare a mixed solution B;
(3) and (2) firstly, dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 30 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5h, dropwise adding the solution A for 9min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0h, ensuring that the solution A is later than the solution B and is completely dropwise added, continuously stirring for 1.5h after the dropwise adding of the two solutions is completed, finally, regulating the pH value of the solution to be 5.0-7.0 by using 30% of sodium hydroxide solution, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt% (the product number is PCE-TJ-8).
Test examples
The invention relates to a concrete bleeding-resistant inhibitor with a water reducing function, which can be compounded with a common high-performance water reducing agent according to a certain mass proportion, wherein the compounded water reducing agent has the same using method as a conventional polycarboxylic acid water reducing agent, namely, the compounded water reducing agent is added into concrete, and the mixing amount of the compounded water reducing agent is 1.0-2.5 percent (mass percentage mixing amount) of a cementing material. The following concrete application performance and mechanical property test experiments are carried out on the anti-bleeding inhibitor prepared by the invention:
firstly, concrete application performance tests are carried out according to GB/T50080-2002 Standard for Performance test methods of common concrete mixtures, and the mixing proportion of the concrete is shown in Table 1.
Secondly, polycarboxylic acid series TZ-GC high-water-reducing type mother liquor, TZ-GZ polycarboxylic acid high-performance slump retaining agent mother liquor and sodium gluconate retarder which are produced by Sichuan same-boat chemical technology Limited are respectively adopted, the mixture and the concrete bleeding-resistant inhibitor synthesized in the examples 1-8 are prepared into a compound product according to the mass ratio of 13:1 for experiment, the bleeding-resistant inhibitor is not doped in a blank control experiment, and the compound scheme is shown in table 2.
And thirdly, during concrete performance test, the mixing amount of the water reducer is 1.5 percent (mass percentage mixing amount) of the cementing material, the slump and the expansion degree of the concrete mixture are respectively recorded in units of mm when the concrete mixture is tested initially, 1h, 2h and 3h, and the concrete states at the initial time and 3h are respectively recorded. The mechanical properties of the concrete are tested according to GB/T50081-2002 'test method for mechanical properties of common concrete', the 3d, 7d and 28d compressive strengths of the concrete are tested, and the test results are shown in Table 3.
TABLE 1 concrete test mix ratio (kg/m)3)
| Grade | Water (W) | Cement (C) | Fly ash (F) | Coarse sand (S1) | Fine sand (S2) | Egg broken stone (G) |
| C30 | 160 | 270 | 60 | 680 | 200 | 1050 |
Table 2 compounding scheme (g)
| High water reduction (GC) | Slump retaining agent (GZ) | Sodium gluconate (PN) | Anti-bleeding inhibitor (TJ) | Water (W) |
| 180 | 50 | 30 | 20 | 720 |
TABLE 3 concrete workability test
From the concrete test results shown in table 3, the concrete bleeding-resistant inhibitor with the water-reducing function synthesized in embodiments 1 to 8 of the invention enables the concrete to have good wrapping property, no bleeding, no bottom grabbing, high strength, good thickening and water-retaining properties, good workability and high slump-retaining property after 3 hours, maintain good fluidity, be suitable for long-distance transportation and be easy for pumping construction.
Claims (7)
1. The concrete bleeding-resistant inhibitor with the water reducing function is characterized by comprising the following raw materials in parts by weight: 300-360 parts of unsaturated polyether macromonomer, 50-100 parts of unsaturated carboxylic acid, 20-30 parts of unsaturated amide, 3-8 parts of unsaturated sulfonic acid or salt thereof, 0.5-3.0 parts of cross-linking agent, 4-6 parts of oxidant, 0.5-1.5 parts of reducing agent, 1.0-1.5 parts of chain transfer agent and 450-500 parts of deionized water; the unsaturated polyether macromonomer, the unsaturated carboxylic acid, the unsaturated amide, the unsaturated sulfonic acid or the salt thereof and the crosslinking agent are mixed according to the mass ratio of: 1.0: 7.0-8.0: 2.0-3.0: 0.2-0.5: 0.02-0.05, wherein the chain transfer agent is one or two of methyl mercaptopropionate, ethyl mercaptopropionate and isooctyl mercaptopropionate, the unsaturated polyether macromonomer is one or two of allyl alcohol polyoxyethylene ether and methacrylate alcohol polyoxyethylene ether, the molecular weight of the unsaturated polyether macromonomer is 2400-3000, the unsaturated amide is one or two of methacrylamide, N-dimethylacrylamide, N-hydroxymethyl acrylamide and N-isopropylacrylamide, and the crosslinking agent is one or two of polyethylene glycol 400 diacrylate and polyethylene glycol 400 dimaleate.
2. The concrete bleeding inhibitor with the water reducing function according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 330 parts of unsaturated polyether macromonomer, 76.5 parts of unsaturated carboxylic acid, 30 parts of unsaturated amide, 6.8 parts of unsaturated sulfonic acid or salt thereof, 0.8 part of cross-linking agent, 4.9 parts of oxidizing agent, 0.73 part of reducing agent, 1.32 parts of chain transfer agent and 485 parts of deionized water; the unsaturated polyether macromonomer, the unsaturated carboxylic acid, the unsaturated amide, the unsaturated sulfonic acid or the salt thereof and the crosslinking agent are mixed according to the mass ratio of: 1.0:7.45:2.2:0.24:0.038.
3. The concrete antisecretory inhibitor having a water-reducing function according to claim 1 or 2, wherein the unsaturated carboxylic acid is one or two of acrylic acid, methacrylic acid, maleic anhydride and fumaric acid.
4. The concrete anti-bleeding inhibitor with water-reducing function according to claim 1 or 2, wherein the unsaturated sulfonic acid or its salt is one or two of 2-acrylamide-2-methylpropanesulfonic acid, sodium methallyl sulfonate, sodium allyl sulfonate and sodium p-styrenesulfonate.
5. The water-reducing concrete bleeding inhibitor according to claim 1 or 2, wherein the oxidizing agent is one or two of hydrogen peroxide, ammonium persulfate, potassium persulfate, sodium persulfate and tert-butyl hydroperoxide.
6. The concrete anti-bleeding inhibitor with water-reducing function according to claim 1 or 2, wherein the reducing agent is at least two of vitamin C, rongalite, ferrous sulfate heptahydrate, sodium hydrosulfite, sodium thiosulfate, sodium hypophosphite, sodium bisulfite and sodium metabisulfite.
7. The method for preparing the concrete anti-bleeding inhibitor with the water reducing function according to any one of claims 1 to 6, comprising the steps of:
(1) sequentially adding unsaturated polyether macromonomer, unsaturated amide, unsaturated sulfonic acid or salt thereof, oxidant and deionized water into a reaction kettle, stirring and dissolving to prepare a mixed bottom material solution with the mass fraction of 50-60%;
(2) mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution A with the mass fraction of 1.0-2.0%; mixing unsaturated carboxylic acid, a cross-linking agent and deionized water to prepare a solution B with the mass fraction of 50-70%;
(3) and (2) dropwise adding the solution A into the mixed bottom material solution prepared in the step (1) at the temperature of 15-30 ℃ in the reaction kettle, controlling the dropwise adding time of the solution A to be 2.5-3.0 h, dropwise adding the solution A for 5-10 min, then dropwise adding the solution B into the mixed bottom material solution prepared in the step (1), controlling the dropwise adding time of the solution B to be 2.0-2.5 h, ensuring that the solution A is later than the solution B is completely dropwise added, continuously stirring for 1.0-1.5 h after the dropwise adding of the two solutions is completed, finally adjusting the pH value of the solution to be 5.0-7.0 by using a sodium hydroxide solution with the mass fraction of 30%, supplementing water, and uniformly stirring to obtain the anti-bleeding inhibitor with the solid content of 40 wt%.
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