CN111217966A - Viscosity-reducing early-strength concrete water reducer and preparation method thereof - Google Patents

Viscosity-reducing early-strength concrete water reducer and preparation method thereof Download PDF

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CN111217966A
CN111217966A CN202010159772.5A CN202010159772A CN111217966A CN 111217966 A CN111217966 A CN 111217966A CN 202010159772 A CN202010159772 A CN 202010159772A CN 111217966 A CN111217966 A CN 111217966A
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reaction
monomer
dropping liquid
reaction monomer
deionized water
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宋欣
倪涛
汪咏梅
刘昭洋
田献文
康静
王进春
刘翠芬
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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
    • C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
    • C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
    • C08F290/06—Polymers provided for in subclass C08G
    • C08F290/062—Polyethers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • 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 provides a viscosity-reducing early-strength concrete water reducer and a preparation method thereof, and provides a structural formula of the viscosity-reducing early-strength concrete water reducer. The preparation method comprises the following steps: putting the reaction monomer A, the chain transfer agent and deionized water into a reaction kettle, and heating and stirring uniformly; dissolving a reaction monomer B in deionized water to obtain a dropping liquid X; dissolving a reaction monomer C in deionized water to obtain a dropping liquid Y; heating the temperature of the reaction kettle to 55-65 ℃, adding an initiator into the reaction kettle, stirring, then beginning to dropwise add liquid X, Y, wherein the dropwise adding time is 1.5-2.5h, continuing to perform heat preservation reaction after dropwise adding, and then cooling in an ice water bath to terminate the reaction, wherein the obtained product is the viscosity-reducing early-strength concrete water reducer. The invention has the advantages of both early strength and viscosity reduction effects, and good water reduction effect, thereby shortening the turnover period of the die and realizing the steaming-free and pressure-steaming-free single-double-free process.

Description

Viscosity-reducing early-strength concrete water reducer and preparation method thereof
Technical Field
The invention relates to a concrete water reducing agent, in particular to a viscosity-reducing early-strength concrete water reducing agent. The invention also relates to a preparation method of the viscosity-reducing early-strength concrete water reducer
Background
In recent years, large-scale construction projects in China are continuously eager for using precast concrete. Precast concrete is also required to have a certain early strength development rate to improve the turnover rate of the formwork or to be suitable for use in a low temperature environment, extending its production cycle to a cold season. The high-strength concrete pipe pile is a product which is developed rapidly in a short period of time and has a wide application range, has the advantages of high strength, strong bearing capacity, convenience in application and the like, and is applied to many fields. For the production, it is desirable to reduce some steam-curing steps to achieve zero energy consumption. At present, the early strength type polycarboxylate superplasticizer generally adopts a superplasticizer with longer side chain and shorter main chain, so that the shape of molecules is changed from comb type to inverted T type, and the length of the side chain exceeds the length of the main chain. However, since the water-gel ratio of high-strength concrete is low, the viscosity of concrete is high, and the viscosity of concrete is high due to the long side chain of the common early-strength water reducing agent. However, the side chain of the general viscosity reduction type water reducing agent is short, so that the effect of early strength cannot be achieved, and even concrete retardation may be caused.
The inventors searched the following related patent documents: CN104193913A discloses an early strength polycarboxylate concrete water reducer and a preparation method thereof, wherein a macromonomer isobutylene alcohol polyoxyethylene ether and water are heated and heated; after stirring and completely dissolving, heating to 65-80 ℃, then respectively dropwise adding acrylic acid, sodium methallylsulfonate, and an aqueous solution of an early strength monomer containing an amido group and an initiator solution, and dropwise adding for 2-3 h; and (3) preserving the heat for 2-3h after the dropwise addition is finished, cooling to room temperature, and neutralizing by using organic alkali to adjust the pH value to 7-8 to obtain the early-strength polycarboxylate concrete water reducer. CN103772624A discloses an early strength polycarboxylate concrete water reducer and a preparation method thereof, which comprises the steps of heating and heating up isobutenol polyoxyethylene ether and water; after stirring and completely dissolving, heating to 70 ℃, adding sodium methallyl sulfonate as a molecular weight regulator and an early strength functional monomer, stirring and dissolving, keeping the temperature at 70 ℃, respectively and simultaneously dripping an aqueous solution obtained by diluting acrylic acid with water and an aqueous solution of initiator ammonium persulfate into a reaction container, finishing dripping within 2-3h, keeping the temperature for 2h, cooling the system to about 25-40 ℃, and neutralizing by using monoethanolamine or diethanolamine to regulate the pH value to 7-8 to obtain the early strength polycarboxylate concrete water reducer. CN103011660A discloses a preparation method and a construction method for preparing a concrete water reducing agent and a concrete early strength agent by using the water reducing agent, and the preparation method comprises the following process steps: polyethylene glycol monomethyl ether acrylate: sodium methallyl sulfonate: methyl acrylate: preparing methacrylic acid into aqueous solution according to a certain molar ratio for one-time feeding; heating in water bath, and carrying out heat preservation reaction after the initiator is added dropwise; after the reaction is finished, cooling to room temperature, and adjusting the pH value of the mixed solution by using a sodium hydroxide solution to prepare the polyester polycarboxylic acid water reducing agent.
The technologies can simultaneously achieve the early strength and viscosity reduction effects of the concrete water reducing agent, have good water reducing effects, and do not provide a specific guidance scheme.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a viscosity-reducing early-strength concrete water reducer which has both early strength and viscosity-reducing effects and has a good water-reducing effect, so that the turnover period of a mold is shortened, and steam curing and pressure steam single-double-free processes are avoided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the technical scheme of the viscosity-reduction early-strength concrete water reducer is that the viscosity-reduction early-strength concrete water reducer has the following structural formula:
Figure BDA0002405333280000021
a is an integer of 3-7, b is an integer of 10-21, c is an integer of 5-10;
the structural formula of A is:
Figure BDA0002405333280000022
n is an integer of 15 to 25;
the structural formula of B is:
Figure BDA0002405333280000031
R1is H or CH3；
The structural formula of C is:
Figure BDA0002405333280000032
R2is H, CH3And CH2CH3；R3And R4Are respectively C1-3An alkyl group.
Through the active polymerization of the controllable free radicals, the molecular configuration of the water reducing agent is as follows: the molecular side chain of the water reducing agent is longer than the main chain.
Figure BDA0002405333280000033
The molecular weight of the viscosity-reducing early-strength water reducer is 9000-15000.
A preparation method of a viscosity-reducing early-strength concrete water reducer comprises the following technical steps: putting a reaction monomer A, a chain transfer agent and deionized water into a reaction kettle, heating and stirring uniformly, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1 (0.6-0.8); dissolving the reaction monomer B in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1 (1.1-1.5); dissolving a reaction monomer C in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1 (7-11); heating the temperature of the reaction kettle to 55-65 ℃, adding an initiator into the reaction kettle, stirring for 1-2 min, starting (or simultaneously) dropwise adding the dropwise adding liquid X and the dropwise adding liquid Y, wherein the dropwise adding completion time of the dropwise adding liquid X and the dropwise adding liquid Y is 1.5-2.5h, continuing to perform heat preservation reaction at 55-65 ℃ for 0.5-2h after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining the viscosity-reducing early-strength concrete water reducer (product).
The reaction monomer A refers to the structural formula of the A, the reaction monomer B refers to the structural formula of the B, the reaction monomer C refers to the structural formula of the C, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1 (2-4) to 0.1-0.6; the amount (mass) of the initiator is 0.06-0.4% of the total mass of the monomers; the chain transfer agent is one of dithio phenylacetate pyridinium chloride, dithio benzoate butyric acid and dithio benzoate propionamide, and the dosage (mass) of the chain transfer agent is 0.4-1.5% of the total monomer mass. The total monomers comprise a reaction monomer A, a reaction monomer B and a reaction monomer C. The initiator is one of azodiisopropyl amidine oxazoline hydrochloride (namely VA044), azodiisobutyl amidine hydrochloride and azodiisopropyl imidazoline.
The structural formula of the dithiophenylacetate pyridinium chloride is shown as a formula I:
Figure BDA0002405333280000041
the structural formula of the dithiobenzoate butyric acid is shown as a formula II:
Figure BDA0002405333280000042
the structural formula of the dithio-benzoate propionamide is shown as a formula III:
Figure BDA0002405333280000043
among the above technical solutions, the preferable technical solutions can be seen in examples 1 to 5. The above-mentioned reactive monomer A, reactive monomer B, reactive monomer C and chain transfer agent are commercially available products. Reactive monomer A may be purchased from macromonomer manufacturers.
According to the invention, the molecular structure and molecular weight of the polycarboxylate superplasticizer are controlled, and the viscosity reduction and early strength groups are added, so that the water reducer product with both early strength and viscosity reduction effects is obtained. According to the high molecular structure design theory, a special polyether macromonomer A with a viscosity reduction function and a macromonomer C with an early strength function are introduced into a molecular structure, and a polycarboxylate superplasticizer molecule with a specific molecular structure and a specific molecular weight is obtained through controllable free radical polymerization, so that the concrete has higher early strength and lower viscosity. Referring to the test later in the specification, the concrete evaluation data show that compared with the commercial early-strength water reducing agent, the viscosity-reducing early-strength water reducing agent provided by the invention has the advantages that the T500 flow rate is obviously higher, the viscosity-reducing effect is achieved, and the strength is not reduced in 12h, 7d and 28 d. Compared with the commercially available viscosity reduction type water reducer, the strength of the viscosity reduction early-strength water reducer is obviously improved within 12h, 7d and 28d, and the T500 flow rate is not reduced.
In conclusion, the viscosity-reducing early-strength concrete water reducer prepared by the invention has good early strength and viscosity-reducing effects and good water-reducing effect. The method is applied to the precast concrete, promotes the early strength development of the concrete, shortens the turnover period of the mould, and realizes the steam-curing-free and pressure-steam-free single-double-free process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b): the viscosity-reducing early-strength concrete water reducer has the following structural formula:
Figure BDA0002405333280000051
a is an integer of 3-7, b is an integer of 10-21, c is an integer of 5-10 (a can be 4, b can be 12, c can be 8);
the structural formula of A is:
Figure BDA0002405333280000061
n is an integer from 15 to 25 (n may be 18);
the structural formula of B is:
Figure BDA0002405333280000062
R1is H or CH3；
The structural formula of C is:
Figure BDA0002405333280000063
R2is H, CH3And CH2CH3；R3And R4Are respectively C1-3Alkyl (R)2Can be CH3Or CH2CH3，R3And R4May be respectively C2Alkyl groups).
Through the active polymerization of the controllable free radicals, the molecular configuration of the water reducing agent is as follows: the molecular side chain of the water reducing agent is longer than the main chain.
Figure BDA0002405333280000064
The molecular weight of the viscosity-reducing early-strength water reducer is 9000-15000 (10000 can be adopted as the molecular weight).
Example 1: the preparation method of the viscosity-reducing early-strength concrete water reducer comprises the following process steps: putting 96g of reaction monomer A, 0.94g of chain transfer agent dithiobenzoate butyric acid and 65g of deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.67; dissolving a reaction monomer B, namely 17.29g of acrylic acid, in 25g of deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.45; dissolving 3.4g of a reaction monomer C, namely 3.4g of 2-acrylamide-2-methylpropanesulfonic acid in 35g of deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 10.29; heating the temperature of a reaction kettle to 55 ℃, adding an initiator, namely 0.32g of azodiisopropyl amidine oxazoline hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.5h, continuing to perform heat preservation reaction at 55 ℃ for 1.5h after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer (product); the structural formula of the reaction monomer A is shown in the specification, n is 18, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:2.4: 0.16; the using amount of the initiator is 0.27 percent of the total monomer mass; the amount of chain transfer agent used was 0.81% of the total monomer mass.
Example 2: the preparation method of the viscosity-reducing early-strength concrete water reducer comprises the following process steps: putting 96g of reaction monomer A, 1.23g of chain transfer agent dithiobenzoate butyric acid and 78g of deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.8; dissolving a reaction monomer B, namely 20.14g of acrylic acid, in 25g of deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.24; dissolving 4.6g of a reaction monomer C, namely 4.6g of 2-acrylamide-2-ethyl-2-methylpropanesulfonic acid in 35g of deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 7.61; heating the temperature of a reaction kettle to 60 ℃, adding an initiator, namely 0.43g of azobisisobutylamidine hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.0h, continuing to perform heat preservation reaction at 60 ℃ for 1h after the dropwise adding is completed, and then cooling in an ice-water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer (product); the structural formula of the reaction monomer A is shown in the specification, n is 20, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:3.1: 0.22; the amount of the initiator is 0.36 percent of the total monomer mass; the amount of the chain transfer agent is the total amount of the monomer1.0% of the bulk mass. In this example, the reactive monomer C is 2-acrylamido-2-ethyl-2-methylpropanesulfonic acid, see the formula of the reactive monomer C, R2Is CH3；R3Is C1Alkyl (i.e. alkyl of the general formula n ═ 1), R4Are respectively C2Alkyl (i.e., an alkyl group of the formula wherein n is 2).
Example 3: the preparation method of the viscosity-reducing early-strength concrete water reducer comprises the following process steps: putting 96g of reaction monomer A, 1.46g of chain transfer agent dithiobenzoate propionamide and 78g of deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.8; dissolving a reaction monomer B, namely 20.62g of acrylic acid in 25g of deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.21; dissolving 3.2g of a reaction monomer C, namely 3.2g of 2-acrylamide-2-diethyl-propanesulfonic acid in 35g of deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 10.94; heating the temperature of a reaction kettle to 60 ℃, adding an initiator, namely 0.45g of azodiisopropyl amidine oxazoline hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 1.5h, continuing to perform heat preservation reaction for 1h at 60 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer (product); the structural formula of the reaction monomer A is shown in the specification, n is 25, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:3.77: 0.19; the using amount of the initiator is 0.38 percent of the total monomer mass; the amount of chain transfer agent used was 1.2% of the total monomer mass. In this example, the reactive monomer C is 2-acrylamido-2-diethyl-propanesulfonic acid, see the formula for reactive monomer C, R2Is CH2CH3；R3And R4Are respectively C2Alkyl (i.e., an alkyl group of the formula wherein n is 2).
Example 4: the preparation method of the viscosity-reducing early-strength concrete water reducer comprises the following process steps: putting 96g of reaction monomer A, 0.67g of chain transfer agent dithiobenzoate propionamide and 68g of deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.7; dissolving a reaction monomer B, namely 19.32g of acrylic acid, in 25g of deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.29; dissolving 3.6g of a reaction monomer C, namely 3.6g of 2-acrylamide-2-diethyl-propanesulfonic acid in 35g of deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 9.72; heating the temperature of a reaction kettle to 60 ℃, adding an initiator, namely 0.48g of azodiisopropyl amidine oxazoline hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.0h, continuing to perform heat preservation reaction for 1h at 60 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer (product); the structural formula of the reaction monomer A is shown in the specification, n is 15, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:2.3: 0.14; the initiator amount is 0.4 percent of the total monomer mass; the amount of chain transfer agent used was 0.56% of the total monomer mass.
Example (b): 5 the preparation method of the viscosity-reducing early-strength concrete water reducer comprises the following process steps: putting 96g of reaction monomer A, 1.38g of chain transfer agent dithiobenzoate butyric acid and 60g of deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.62; dissolving a reaction monomer B, namely 17.29g of acrylic acid, in 25g of deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.45; dissolving 3.4g of a reaction monomer C, namely 3.4g of 2-acrylamide-2-methylpropanesulfonic acid in 35g of deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 10.29; heating the temperature of a reaction kettle to 55 ℃, adding an initiator, namely 0.46g of azodiisopropyl amidine oxazoline hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.0h, continuing to perform heat preservation reaction for 1h at 55 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer (product); the structural formula of the reaction monomer A is shown in the specification, n is 18, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:2.4: 0.15; the using amount of the initiator is 0.39 percent of the total monomer mass; the amount of chain transfer agent used was 1.2% of the total monomer mass.
The following are the experimental part of the invention:
the molecular weights of the products of examples 1 to 5 of the present invention are shown in Table 1, and the viscosity-reducing early-strength water-reducing agent synthesized in examples 1 to 5 of the present invention was compared with commercially available early-strength water-reducing agents and viscosity-reducing water-reducing agents. Concrete was prepared according to the formulation shown in Table 2 below, and slump, t500 and 12h, and 7d and 28d strength of the concrete were measured.
TABLE 1 examples Water reducing agent molecular weight
Example additives Molecular weight
Example 1 13628
Example 2 10536
Example 3 9462
Example 4 14397
Example 5 11561
TABLE 2 concrete mix proportion (C50)
Cement Fly ash Coarse sand Fine sand Stone (stone) Water (W)
432 108 450 198 1034 165
TABLE 3 evaluation results of concrete
Figure BDA0002405333280000101
As can be seen from the water reducer molecular weight data in the embodiment shown in Table 1, the water reducer molecular weight in all the embodiments is controlled between 9000 and 15000, so that the water reducer side chain is ensured to be shorter, the viscosity reduction effect is achieved, the main chain of the water reducer is ensured to be shorter than the side chain, the molecules are in an inverted T-shaped structure and have the early strength effect, the amino group introduced into the molecular structure can also have the early strength effect, and the phosphate group in the monomer A can also have a part of the viscosity reduction effect.
As can be seen from the concrete evaluation data in Table 3, compared with the commercially available early strength water reducing agent, the viscosity-reducing early strength water reducing agent of the invention has a significantly faster T500 flow rate, achieves the effect of viscosity reduction, and has no decrease in strength for 12h, 7d and 28 d. Compared with the commercially available viscosity-reducing water reducer, the viscosity-reducing early-strength water reducer disclosed by the invention has the advantages that the strength of 12h, 7d and 28d is obviously improved, and the T500 flow rate is not reduced.
In conclusion, the viscosity-reducing early-strength concrete water reducer prepared by the invention has good early strength and viscosity-reducing effects and good water-reducing effect. The method is applied to the precast concrete, promotes the early strength development of the concrete, shortens the turnover period of the mould, and realizes the steam-curing-free and pressure-steam-free single-double-free process.

Claims (10)

1. The viscosity-reducing early-strength concrete water reducer is characterized by having the following structural formula:
Figure FDA0002405333270000011
a is an integer of 3-7, b is an integer of 10-21, c is an integer of 5-10;
the structural formula of A is:
Figure FDA0002405333270000012
n is an integer of 15 to 25;
the structural formula of B is:
Figure FDA0002405333270000013
R1is H or CH3；
The structural formula of C is:
Figure FDA0002405333270000014
R2is H, CH3And CH2CH3；R3And R4Are respectively C1-3An alkyl group.
2. The viscosity-reducing early-strength concrete water reducer according to claim 1, wherein the molecular configuration of the water reducer is as follows through controlled radical living polymerization: the molecular side chain of the water reducing agent is longer than the main chain.
Figure FDA0002405333270000015
3. The viscosity-reducing early-strength concrete water-reducing agent according to claim 1, wherein the molecular weight of the viscosity-reducing early-strength water-reducing agent is 9000-15000.
4. A preparation method of a viscosity-reducing early-strength concrete water reducer is characterized by comprising the following process steps: putting a reaction monomer A, a chain transfer agent and deionized water into a reaction kettle, heating and stirring uniformly, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1 (0.6-0.8); dissolving the reaction monomer B in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1 (1.1-1.5); dissolving a reaction monomer C in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1 (7-11); heating the temperature of a reaction kettle to 55-65 ℃, adding an initiator into the reaction kettle, stirring for 1-2 min, then starting dropwise adding a dropwise adding liquid X and a dropwise adding liquid Y, wherein the dropwise adding completion time of the dropwise adding liquid X and the dropwise adding liquid Y is 1.5-2.5h, continuing to perform heat preservation reaction at 55-65 ℃ for 0.5-2h after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer;
the reaction monomer A refers to the structural formula of the A, the reaction monomer B refers to the structural formula of the B, the reaction monomer C refers to the structural formula of the C, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1 (2-4) to 0.1-0.6; the amount of the initiator is 0.06-0.4% of the total monomer mass; the chain transfer agent is one of dithiophenylacetate pyridinium chloride, dithiobenzoate butyric acid and dithiobenzoate propionamide, the dosage of the chain transfer agent is 0.4-1.5% of the total monomer mass, and the total monomer comprises a reaction monomer A, a reaction monomer B and a reaction monomer C;
the structural formula of the dithiophenylacetate pyridinium chloride is shown as a formula I:
Figure FDA0002405333270000021
the structural formula of the dithiobenzoate butyric acid is shown as a formula II:
Figure FDA0002405333270000022
the structural formula of the dithio-benzoate propionamide is shown as a formula III:
Figure FDA0002405333270000031
5. the method for preparing the viscosity-reducing early strength concrete water reducer according to claim 4, wherein the initiator is one of azodiisopropylamidine hydrochloride, azobisisobutylamidine hydrochloride and azodiisopropylimidazoline.
6. The preparation method of the viscosity-reducing early-strength concrete water reducer according to claim 4, characterized by comprising the following process steps: putting a reaction monomer A, a chain transfer agent dithiobenzoate butyric acid and deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.67; dissolving a reaction monomer B, namely acrylic acid in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.45; dissolving a reaction monomer C, namely 2-acrylamide-2-methylpropanesulfonic acid, in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 10.29; heating the temperature of a reaction kettle to 55 ℃, adding an initiator namely azodiisopropyl amidine oxazoline hydrochloride into the reaction kettle, stirring for 1min, then beginning to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.5h, continuing to perform heat preservation reaction for 1.5h at 55 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer; the structural formula of the reaction monomer A is shown in the specification, n is 18, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:2.4: 0.16; the using amount of the initiator is 0.27 percent of the total monomer mass; the amount of chain transfer agent used was 0.81% of the total monomer mass.
7. The preparation method of the viscosity-reducing early-strength concrete water reducer according to claim 4, characterized by comprising the following process steps: putting a reaction monomer A, a chain transfer agent dithiobenzoate butyric acid and deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.8; dissolving a reaction monomer B, namely acrylic acid in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.24; dissolving a reaction monomer C, namely 2-acrylamide-2-ethyl-2-methylpropanesulfonic acid, in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 7.61; heating the temperature of a reaction kettle to 60 ℃, adding an initiator namely azodiisobutyl amidine hydrochloride into the reaction kettle, stirring for 1min, then beginning to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.0h, continuing to perform heat preservation reaction for 1h at 60 ℃ after the dropwise adding is completed, and then cooling in an ice-water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer; the structural formula of the reaction monomer A is shown in the specification, n is 20, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:3.1: 0.22; the amount of the initiator is 0.36 percent of the total monomer mass; the amount of chain transfer agent used was 1.0% of the total monomer mass.
8. The preparation method of the viscosity-reducing early-strength concrete water reducer according to claim 4, characterized by comprising the following process steps: putting a reaction monomer A, a chain transfer agent dithiobenzoate propionamide and deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.8; dissolving a reaction monomer B, namely acrylic acid in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.21; dissolving a reaction monomer C, namely 2-acrylamide-2-diethyl-propanesulfonic acid in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 10.94; heating the temperature of a reaction kettle to 60 ℃, adding an initiator, namely azodiisopropylamidine oxazoline hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 1.5h, continuing to perform heat preservation reaction for 1h at 60 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer; the structural formula of the reaction monomer A is shown in the specification, n is 25, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:3.77: 0.19; the using amount of the initiator is 0.38 percent of the total monomer mass; the amount of chain transfer agent used was 1.2% of the total monomer mass.
9. The preparation method of the viscosity-reducing early-strength concrete water reducer according to claim 4, characterized by comprising the following process steps: putting a reaction monomer A, a chain transfer agent dithiobenzoate propionamide and deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.7; dissolving a reaction monomer B, namely acrylic acid in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.29; dissolving a reaction monomer C, namely 2-acrylamide-2-diethyl-propanesulfonic acid in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 9.72; heating the temperature of a reaction kettle to 60 ℃, adding an initiator, namely azodiisopropylamidine oxazoline hydrochloride, into the reaction kettle, stirring for 1min, then starting to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.0h, continuing to perform heat preservation reaction for 1h at 60 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity-reducing early-strength concrete water reducer; the structural formula of the reaction monomer A is shown in the specification, n is 15, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:2.3: 0.14; the initiator amount is 0.4 percent of the total monomer mass; the amount of chain transfer agent used was 0.56% of the total monomer mass.
10. The preparation method of the viscosity-reducing early-strength concrete water reducer according to claim 4, characterized by comprising the following process steps: putting a reaction monomer A, a chain transfer agent dithiobenzoate butyric acid and deionized water into a reaction kettle, heating and uniformly stirring, wherein the mass ratio of the sum of the mass of the reaction monomer A and the chain transfer agent to the mass of the deionized water is 1: 0.62; dissolving a reaction monomer B, namely acrylic acid in deionized water to obtain a dropping liquid X, wherein the mass ratio of the reaction monomer B to the deionized water in the dropping liquid X is 1: 1.45; dissolving a reaction monomer C, namely 2-acrylamide-2-methylpropanesulfonic acid, in deionized water to obtain a dropping liquid Y, wherein the mass ratio of the reaction monomer C to the deionized water in the dropping liquid Y is 1: 10.29; heating the temperature of a reaction kettle to 55 ℃, adding an initiator namely azodiisopropyl amidine oxazoline hydrochloride into the reaction kettle, stirring for 1min, then beginning to dropwise add a dropping liquid X and a dropping liquid Y, wherein the dropwise adding completion time of the dropping liquid X and the dropping liquid Y is 2.0h, continuing to perform heat preservation reaction for 1h at 55 ℃ after the dropwise adding is completed, and then cooling in an ice water bath to terminate the reaction, thus obtaining a product, namely the viscosity reduction early strength type concrete water reducer; the structural formula of the reaction monomer A is shown in the specification, n is 18, and the molar ratio of the reaction monomer A to the reaction monomer B to the reaction monomer C is 1:2.4: 0.15; the using amount of the initiator is 0.39 percent of the total monomer mass; the amount of chain transfer agent used was 1.2% of the total monomer mass.
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CN116102691A (en) * 2023-04-17 2023-05-12 石家庄市长安育才建材有限公司 Viscosity-reducing water reducer for high-strength concrete and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116102691A (en) * 2023-04-17 2023-05-12 石家庄市长安育才建材有限公司 Viscosity-reducing water reducer for high-strength concrete and preparation method thereof
CN116102691B (en) * 2023-04-17 2023-08-08 石家庄市长安育才建材有限公司 Viscosity-reducing water reducer for high-strength concrete and preparation method thereof

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