CN114230730A - Concrete slump retaining agent and preparation method and application thereof - Google Patents

Concrete slump retaining agent and preparation method and application thereof Download PDF

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Publication number
CN114230730A
CN114230730A CN202111631692.6A CN202111631692A CN114230730A CN 114230730 A CN114230730 A CN 114230730A CN 202111631692 A CN202111631692 A CN 202111631692A CN 114230730 A CN114230730 A CN 114230730A
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parts
acid
slump retaining
retaining agent
concrete
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李卫
黄小文
张静
孟祥杰
赵潜
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Chongqing Jianyan Kezhijie Building Materials Co ltd
Chongqing Kzj New Materials Co ltd
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Chongqing Jianyan Kezhijie Building Materials Co ltd
Chongqing Kzj New Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2688Copolymers containing at least three different monomers
    • C04B24/2694Copolymers containing at least three different monomers containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F292/00Macromolecular compounds obtained by polymerising monomers on to inorganic materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/308Slump-loss preventing agents

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention provides a concrete slump retaining agent and a preparation method and application thereof. The slump retaining agent comprises the following preparation raw materials in parts by weight: 1.5-3 parts of graphene oxide; 15-18 parts of 2-chloroacrylic acid; 18-21 parts of solid alkali; 330-460 parts of methyl allyl polyoxyethylene ether or isopentenyl polyoxyethylene ether; 1.8-6.4 parts of an initiator; 3-6 parts of a chain transfer agent; 0.4-1.4 parts of a reducing agent; 6-22 parts of an olefine acid compound; 23-46 parts of acrylate compound and 400-500 parts of water. The slump retaining agent disclosed by the invention can be stably adsorbed on the surface of cement particles, the hydration reaction is delayed, the time-lapse loss of concrete is effectively reduced, and the dispersion performance is improved through the carboxylated graphene template effect, so that the dispersibility of the slump retaining agent on a slurry system is improved, and the slump retaining effect of concrete is enhanced.

Description

Concrete slump retaining agent and preparation method and application thereof
Technical Field
The invention belongs to the technical field of concrete building materials, and particularly relates to a concrete slump retaining agent and a preparation method and application thereof.
Background
In recent years, the quality of sandstone raw materials is rapidly reduced due to mass exploitation in China, excellent and even qualified sandstone aggregates are gradually depleted, and high-mud content sandstone and machine-made sand are often adopted to fill the aggregate. The absorption rate and the absorption capacity of the high-mud-content sand to the slump retaining agent, particularly the polycarboxylic acid slump retaining agent are faster and larger than those of a cementing material system, and compared with natural sand, the mechanical sand has the advantages of poor gradation, large fineness modulus and rough surface, and can increase the flow resistance after concrete is mixed, so that the concrete has poor flow property and slump retaining property. Along with the popularization and application of the premixed concrete, the raw material problem of the concrete and the requirement of long-distance transportation cause that the construction performance of the concrete is gradually reduced, and the quality of the concrete can not be well ensured in the construction process. In addition, the great slump loss of the concrete in the construction process is a particularly serious problem, so that the engineering hidden danger is greatly increased, and the service life of the engineering is greatly shortened. The research and development of High Performance Concrete (HPC), also known as HPC (high Performance concrete), is now well appreciated by all countries, and can be summarized as follows: the concrete with the composite performance and homogeneity requirement can be obtained without adopting the traditional raw materials and the common mixing, pouring and curing methods. These properties include: (1) the pressure is easy to pour, and the pressure pump does not separate when in pressure pumping; (2) the mechanical property of the long-age is improved; (3) high early strength; (4) high toughness; (5) volume stability; (6) long life in harsh environments. The high-performance concrete not only has excellent construction performance, but also has better durability, can effectively prolong the service life of infrastructure and reduce huge maintenance cost. Therefore, the first link in developing high-performance concrete is to develop a slump retaining agent with good slump retaining effect, workability and sensitivity.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a concrete slump retaining agent and a preparation method and application thereof. The technical scheme of the invention is as follows:
in a first aspect, the invention provides a concrete slump retaining agent, which comprises the following preparation raw materials in parts by weight: 1.5-3 parts of graphene oxide; 15-18 parts of 2-chloroacrylic acid; 18-21 parts of solid alkali; 330-460 parts of methyl allyl polyoxyethylene ether or isopentenyl polyoxyethylene ether; 1.8-6.4 parts of an initiator; 3-6 parts of a chain transfer agent; 0.4-1.4 parts of a reducing agent; 6-22 parts of an olefine acid compound; 23-46 parts of acrylate compound and 400-500 parts of water.
Further, the 2-chloroacrylic acid is replaced by 2-chloroacrylic acid methyl ester, 3-chloroacrylic acid and cis-3-chloroacrylic acid.
Further, the solid alkali is sodium hydroxide and potassium hydroxide.
Further, the average molecular weight of the methallyl polyoxyethylene ether is 1964-2756, and the structural formula is as follows:
Figure BDA0003440420100000021
wherein n is 43-61.
Further, the average molecular weight of the isopentene polyoxyethylene ether is 1980-2772, and the structural formula is as follows:
Figure BDA0003440420100000022
wherein m is 43-61.
Further, the initiator is one of hydrogen peroxide, ammonium persulfate, potassium persulfate or sodium persulfate, and azobisisobutyronitrile.
Further, the chain transfer agent is selected from one or more of the following: isopropanol, phosphorous acid and hypophosphorous acid and salts thereof (sodium hypophosphite, potassium hypophosphite, etc.), sulfurous acid, bisulfite, hyposulfurous acid and metabisulfite and salts thereof (sodium sulfite, sodium bisulfite, preferably sodium dithionite, sodium metabisulfite, potassium sulfite, potassium bisulfite, potassium dithionite, potassium metabisulfite, etc.), mercaptoethanol, mercaptoglycerol, mercaptoacetic acid, mercaptopropionic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid, thiomalic acid, 2-mercaptoethanesulfonic acid and salts thereof.
Further, the reducing agent is vitamin C, oxalic acid, ferrous sulfate, cuprous sulfate, oxalic acid, sodium bisulfite, sodium sulfite, glucose, fructose, ethylenediamine, diphenylamine, sodium monohydrogen phosphate or potassium monohydrogen phosphate.
Further, the olefinic acid compound is one or more of acrylic acid, methacrylic acid, crotonic acid, maleic acid, itaconic acid, citraconic acid and fumaric acid, or one or more of monovalent metal salt, divalent metal salt, ammonium salt and organic amine salt of the compounds, or one or more of acid anhydride of the compounds.
Further, the acrylate compound is at least one of hydroxymethyl acrylate, hydroxyethyl acrylate and hydroxypropyl acrylate.
In a second aspect, the invention provides a preparation method of a concrete slump retaining agent, which comprises the following steps:
step 1, uniformly mixing graphene oxide and water, and adding solid alkali to react with 2-chloroacrylic acid to prepare a carboxylated graphene dispersion liquid;
step 2, adding methyl allyl polyoxyethylene ether or isopentenyl polyoxyethylene ether into the carboxylated graphene dispersion liquid, uniformly mixing, adding an initiator, and uniformly mixing;
step 3, respectively preparing a chain transfer agent, a reducing agent mixed aqueous solution I and an acrylic acid compound and acrylate compound mixed aqueous solution II; and (3) dropping the aqueous solution I and the aqueous solution II into the mixed solution obtained in the step (2) at the temperature below 45 ℃, controlling the dropping time of the aqueous solution I and the aqueous solution II to be 2-3.5 h, carrying out heat preservation reaction for 1-2 h after the dropping is finished, and adjusting the pH to be 6.8-7.2 by using a pH regulator after the reaction is finished.
Preferably, the carboxylated graphene dispersion liquid prepared in the step 1 is prepared by an ultrasonic method, and the control parameters are as follows: the ultrasonic frequency is 20 +/-1 kHz, the ultrasonic power is 3000W, and the time is 2-3 h.
In a third aspect, the invention provides a concrete material comprising the slump retaining agent.
Compared with the prior art, the invention has the following outstanding advantages and positive effects:
the slump retaining agent can delay hydration reaction, effectively reduce the loss of concrete over time, has good dispersion performance and enhances the slump retaining effect of the concrete. In addition, the preparation method of the slump retaining agent is simple and feasible, the polymerization reaction can be carried out at normal temperature or low temperature, the condition is mild, and the popularization is easy.
Detailed Description
In the description of the present invention, it is to be noted that those whose specific conditions are not specified in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present invention will be described in further detail with reference to specific embodiments thereof to assist those skilled in the art in providing a more complete, accurate and thorough understanding of the inventive concept and aspects thereof, and the scope of the present invention includes, but is not limited to, the following examples, and any modifications in the details and form of the technical aspects thereof that fall within the spirit and scope of the present application are intended to be included therein.
In the following examples, the average molecular weight of methallyl polyoxyethylene ether is 1964-2756, and the structural formula is as follows:
Figure BDA0003440420100000041
wherein n is 43-61. The average molecular weight of the isopentene polyoxyethylene ether is 1980-2772, and the structural formula is as follows:
Figure BDA0003440420100000051
wherein m is 43-61. Since the polyether polymer herein is a continuous polymer in a range, the molecular weight is an average molecular weight, generally 2400.
Example 1
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 330 parts of methyl allyl polyoxyethylene ether, 400 parts of water, 3 parts of thioglycollic acid, 6 parts of acrylic acid, 23 parts of hydroxyethyl acrylate, 1.8 parts of hydrogen peroxide, 0.4 part of vitamin C, 1.5 parts of graphene oxide, 18 parts of caustic soda flakes and 15 parts of 2-chloroacrylic acid.
The preparation method comprises the following steps:
(1) adding 1.5 parts by weight of graphene oxide and 300 parts by weight of water into a reaction kettle, opening a high-power industrial continuous flow energy-gathering type ultrasonic dispersion machine, and controlling the parameters as follows: carrying out ultrasonic treatment for 15min at an ultrasonic frequency of 20 +/-1 kHz and an ultrasonic power of 3000W, then adding 18 parts by weight of caustic soda flakes and 15 parts by weight of 2-chloroacrylic acid, and continuing to carry out ultrasonic treatment for 2h to obtain a carboxylated graphene dispersion liquid;
(2) adding 330 parts by weight of methyl allyl polyoxyethylene ether into a reaction kettle, stirring, mixing and dissolving at the normal temperature of 25 ℃, and adding 1.8 parts by weight of hydrogen peroxide;
(3) sequentially dropwise adding a solution I into the material obtained in the step (2): 3 parts by weight of thioglycolic acid, 0.4 part by weight of vitamin C and 60 parts by weight of water; solution II: 6 parts by weight of acrylic acid, 23 parts by weight of hydroxyethyl acrylate and 40 parts by weight of water; and after dropwise adding for 2h, preserving the heat below 45 ℃ for 1h for carrying out an aging reaction, and then neutralizing with an alkali solution until the pH value is 6.8, thus obtaining the concrete slump retaining agent.
Example 2
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 370 parts of methyl allyl polyoxyethylene ether, 440 parts of water, 4 parts of isopropanol, 8 parts of fumaric acid, 29 parts of hydroxyethyl acrylate, 2.2 parts of ammonium persulfate, 0.8 part of sodium bisulfite, 2 parts of graphene oxide, 19 parts of caustic soda flakes and 16 parts of methyl 2-chloroacrylate.
The specific preparation method is the same as that of example 1.
Example 3
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 410 parts of methyl allyl polyoxyethylene ether, 500 parts of water, 4.8 parts of mercaptopropionic acid, 10 parts of citraconic acid, 39 parts of hydroxypropyl acrylate, 2.6 parts of hydrogen peroxide, 0.4 part of ferrous sulfate, 3 parts of graphene oxide, 20 parts of caustic soda flakes and 18 parts of 2-chloroacrylic acid.
The specific preparation method is the same as that of example 1.
Example 4
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 350 parts of isopentenyl polyoxyethylene ether, 420 parts of water, 0.5 part of oxalic acid, 2 parts of hydrogen peroxide, 3.2 parts of mercaptoethanol, 7 parts of maleic acid, 25 parts of hydroxymethyl acrylate, 2 parts of graphene oxide, 19 parts of caustic soda flakes and 16 parts of 2-chloroacrylic acid.
The specific preparation method is the same as that of example 1.
Example 5
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 360 parts of isopentene polyoxyethylene ether, 430 parts of water, 0.8 part of sodium bisulfite, 2.2 parts of ammonium persulfate, 3.6 parts of potassium hypophosphite, 7 parts of methacrylic acid, 25 parts of hydroxyethyl acrylate, 2 parts of graphene oxide, 19 parts of caustic soda flakes and 16 parts of 2-chloroacrylic acid.
The specific preparation method is the same as that of example 1.
Example 6
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 360 parts of isopentene polyoxyethylene ether, 430 parts of water, 0.9 part of ethylenediamine, 2 parts of azobisisobutyronitrile, 4 parts of thiomalic acid, 8 parts of crotonic acid, 23 parts of hydroxypropyl acrylate, 2.5 parts of graphene oxide, 20 parts of caustic soda flakes and 17 parts of 2-chloroacrylic acid.
The specific preparation method is the same as that of example 1.
Example 7
The embodiment provides a concrete slump retaining agent and a preparation method thereof, wherein the concrete slump retaining agent is prepared from the following raw material components in parts by weight: 400 parts of isopentene polyoxyethylene ether, 490 parts of water, 4.2 parts of potassium dithionite, 3 parts of hydrogen peroxide, 1.2 parts of fructose, 12 parts of itaconic acid, 40 parts of hydroxypropyl acrylate, 3 parts of graphene oxide, 21 parts of caustic soda flakes and 18 parts of 2-chloroacrylic acid.
The specific preparation method is the same as that of example 1.
Comparative example 1
A commercially available polycarboxylic slump retaining agent, model SPS-100, was used.
Comparative example 2
A commercially available polycarboxylic acid slump retaining agent model MOLE a 018 was used.
Comparative example 3
The difference between the raw material components and the raw material components in the concrete slump retaining agent and the preparation method of the concrete slump retaining agent is that no graphene oxide exists.
The preparation method comprises the following steps:
(1) adding 320 parts by weight of water into a reaction kettle, adding 19 parts by weight of caustic soda flakes and 16 parts by weight of 2-chloroacrylic acid, opening a high-power industrial-grade continuous flow energy-gathering type ultrasonic dispersion machine, and controlling the parameters as follows: ultrasonic frequency is 20 +/-1 kHz, ultrasonic power is 3000W, and ultrasonic is carried out for 2 hours to obtain dispersion liquid;
(2) adding 350 parts by weight of isopentenyl polyoxyethylene ether into the dispersion, stirring, mixing and dissolving at the normal temperature of 25 ℃, and adding 2 parts by weight of hydrogen peroxide;
(3) sequentially dropwise adding a solution I into the material obtained in the step (2): 3.2 parts by weight of mercaptoethanol, 0.5 part by weight of oxalic acid and 60 parts by weight of water; solution II: 7 parts by weight of maleic acid, 25 parts by weight of hydroxymethyl acrylate, 40 parts by weight of water; and after dropwise adding for 2h, preserving the heat below 45 ℃ for 1h for carrying out an aging reaction, and then neutralizing with an alkali solution until the pH value is 6.8, thus obtaining the concrete slump retaining agent.
Comparative example 4
The comparative example provides a concrete slump retaining agent and a preparation method thereof, and the raw material components are the same as those in example 4.
The preparation method comprises the following steps:
(1) adding 350 parts by weight of isopentenyl polyoxyethylene ether and 220 parts by weight of water into a reaction kettle, stirring, mixing and dissolving at normal temperature of 25 ℃, and adding 2 parts by weight of hydrogen peroxide;
(2) sequentially dropwise adding a solution I into the material obtained in the step (1): 3.2 parts by weight of mercaptoethanol, 0.5 part by weight of oxalic acid and 60 parts by weight of water; solution II: 7 parts by weight of maleic acid, 25 parts by weight of hydroxymethyl acrylate, 40 parts by weight of water; after dropwise adding for 2h, preserving the heat below 45 ℃ for 1h for aging reaction;
(3) adding 2 parts by weight of graphene oxide and 100 parts by weight of water into a reaction kettle, opening a high-power industrial continuous flow energy-gathering type ultrasonic dispersion machine, and controlling the parameters as follows: carrying out ultrasonic treatment for 15min at an ultrasonic frequency of 20 +/-1 kHz and an ultrasonic power of 3000W, then adding 19 parts by weight of caustic soda flakes and 16 parts by weight of 2-chloroacrylic acid, and continuing to carry out ultrasonic treatment for 2h to obtain a carboxylated graphene dispersion liquid; and (3) adding the material obtained in the step (2), and then neutralizing with an alkali solution until the pH value is 6.8, so as to obtain the concrete slump retaining agent.
Comparative example 5
The comparative example provides a concrete slump retaining agent and a preparation method thereof, and the difference between the raw material components and the example 4 is as follows: 5 parts of graphene oxide.
The preparation method comprises the following steps:
(1) adding 5 parts by weight of graphene oxide and 320 parts by weight of water into a reaction kettle, opening a high-power industrial-grade continuous flow energy-gathering type ultrasonic dispersion machine, and controlling the parameters as follows: carrying out ultrasonic treatment for 15min at an ultrasonic frequency of 20 +/-1 kHz and an ultrasonic power of 3000W, then adding 19 parts by weight of caustic soda flakes and 16 parts by weight of 2-chloroacrylic acid, and continuing to carry out ultrasonic treatment for 2h to obtain a carboxylated graphene dispersion liquid;
(2) adding 350 parts by weight of isopentenyl polyoxyethylene ether into a reaction kettle, stirring, mixing and dissolving at normal temperature of 25 ℃, and adding 2 parts by weight of hydrogen peroxide;
(3) sequentially dropwise adding a solution I into the material obtained in the step (2): 3.2 parts by weight of mercaptoethanol, 0.5 part by weight of oxalic acid, and 60 parts by weight of water; solution II: 7 parts by weight of maleic acid, 25 parts by weight of hydroxymethyl acrylate, 40 parts by weight of water; and after dropwise adding for 2h, preserving the heat below 45 ℃ for 1h for carrying out an aging reaction, and then neutralizing with an alkali solution until the pH value is 6.8, thus obtaining the concrete slump retaining agent.
Comparative example 6
The comparative example provides a concrete slump retaining agent and a preparation method thereof, and the difference between the raw material components and the example 4 is as follows: and replacing 2 parts by weight of graphene oxide with 2 parts by weight of graphene. The preparation method is the same as example 4.
A comparison experiment is carried out on the concrete slump retaining agent synthesized in the examples 1-7 and the comparative examples 3-6, and a polycarboxylic acid slump retaining agent with high slump retaining capacity and sold SPS-100 model and MOLE A018 model, wherein Qingpeng P & O42.5R cement, machine-made mountain sand with the mud content of 2.3 percent and the fineness modulus of 3.2, and continuous graded broken stones with the nominal grain diameter of 5-10mm and 10-20mm and the mud content of 0.6 percent are used as materials, the mixing amount is 0.3 percent (bending and fixing mixing amount) of the mass of the cement, and the concrete loss of 3 hours is tested according to the detection method provided by GB8076-2008 concrete admixture.
The concrete formulation for the test is shown in table 1:
TABLE 1 concrete Components Table
Raw materials Cement Machine-made sand Small stone Big stone Tap water
For one side useAmount/kg 320 780 310 805 165
The loss of each slump retaining agent over time at 3h as measured by the test is shown in Table 2:
TABLE 2 test results of examples and comparative examples
Figure BDA0003440420100000101
As can be seen from the test data in the table above:
under the condition of the same mixing amount, compared with a comparative example 1 and a comparative example 2, after the slump retaining agent prepared by the invention is added, the slump of concrete is stably maintained within 200 +/-5 mm within 180min, the slump retaining performance is excellent, and the samples of the comparative examples have the obvious phenomenon of insufficient slump retaining time and are not beneficial to construction.
Compared with a comparative example 3, the invention uses graphene oxide, the comparative example 3 does not use graphene oxide, which causes poor loss with time, the slump retaining agent polymer lacks the introduction of carboxylated graphene, the graphene bridging effect and the template effect are avoided, the hydration reaction can not be delayed, the dispersion performance can not be improved, and the loss with time is large;
compared with the comparative example 4, the hydroxylated graphene is added after the carboxylic acid is synthesized, the hydroxylated graphene introduced with the alkenyl group cannot participate in free radical polymerization, and the carboxylated graphene cannot be introduced into the slump retaining agent polymer, so that the loss is large over time;
compared with the comparative example 5, the condition of poor loss with time can be caused by increasing the weight part of the graphene oxide beyond 1.5-3, the ultrasonic treatment effect of the probe is poor due to excessive graphene oxide, the probe cannot be effectively dispersed, the amount of the graphene oxide with a flocculation structure is large, the effective amount of the hydroxylated graphene is reduced, and the loss is large;
compared with the comparative example 6, the graphene oxide is replaced by graphene, and the hydroxylation and the alkenyl can not be carried out in the hydroxylation process, and the carboxylated graphene can not be introduced into the slump retaining agent polymer, so that the loss is large;
in conclusion, the concrete slump retaining agent can be effectively used as a concrete special slump retaining agent and has an excellent slump retaining effect.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A concrete slump retaining agent is characterized in that: the slump retaining agent comprises the following preparation raw materials in parts by weight: 1.5-3 parts of graphene oxide; 15-18 parts of 2-chloroacrylic acid; 18-21 parts of solid alkali; 330-460 parts of methyl allyl polyoxyethylene ether or isopentenyl polyoxyethylene ether; 1.8-6.4 parts of an initiator; 3-6 parts of a chain transfer agent; 0.4-1.4 parts of a reducing agent; 6-22 parts of an olefine acid compound; 23-46 parts of acrylate compound and 400-500 parts of water.
2. The concrete slump retaining agent as claimed in claim 1, wherein: the 2-chloroacrylic acid is replaced by 2-chloroacrylic acid methyl ester, 3-chloroacrylic acid and cis-3-chloroacrylic acid.
3. The concrete slump retaining agent as claimed in claim 1, wherein: the average molecular weight of the methyl allyl polyoxyethylene ether is 1964-2756, and the structural formula is as follows:
Figure FDA0003440420090000011
wherein n is 43-61; the average molecular weight of the isopentene polyoxyethylene ether is 1980-2772, and the structural formula is as follows:
Figure FDA0003440420090000012
wherein m is 43-61.
4. The concrete slump retaining agent as claimed in claim 1, wherein: the initiator is one of hydrogen peroxide, ammonium persulfate, potassium persulfate or sodium persulfate and azobisisobutyronitrile.
5. The concrete slump retaining agent as claimed in claim 1, wherein: the chain transfer agent is selected from one or more of the following: isopropanol, phosphorous acid and hypophosphorous acid and salts thereof, sulfurous acid, bisulfite, dithionous acid and metabisulfite and salts thereof, mercaptoethanol, thioglycerol, thioglycolic acid, mercaptopropionic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid, thiomalic acid, 2-mercaptoethanesulfonic acid and salts thereof.
6. The concrete slump retaining agent as claimed in claim 1, wherein: the reducing agent is vitamin C, oxalic acid, ferrous sulfate, cuprous sulfate, oxalic acid, sodium bisulfite, sodium sulfite, glucose, fructose, ethylenediamine, diphenylamine, sodium monohydrogen phosphate or potassium monohydrogen phosphate.
7. The concrete slump retaining agent as claimed in claim 1, wherein: the olefine acid compound is one or more of acrylic acid, methacrylic acid, crotonic acid, maleic acid, itaconic acid, citraconic acid and fumaric acid, one or more of monovalent metal salt, divalent metal salt, ammonium salt and organic amine salt of the compound, or one or more of anhydride of the compound.
8. The concrete slump retaining agent as claimed in claim 1, wherein: the acrylate compound is at least one of hydroxymethyl acrylate, hydroxyethyl acrylate and hydroxypropyl acrylate.
9. The method for preparing a concrete slump retaining agent as claimed in any one of claims 1 to 8, wherein: the method comprises the following steps:
step 1, uniformly mixing graphene oxide and water, and adding solid alkali to react with 2-chloroacrylic acid to prepare a carboxylated graphene dispersion liquid;
step 2, adding methyl allyl polyoxyethylene ether or isopentenyl polyoxyethylene ether into the carboxylated graphene dispersion liquid, uniformly mixing, adding an initiator, and uniformly mixing;
step 3, respectively preparing a chain transfer agent, a reducing agent mixed aqueous solution I and an acrylic acid compound and acrylate compound mixed aqueous solution II; and (3) dropping the aqueous solution I and the aqueous solution II into the mixed solution obtained in the step (2) at the temperature below 45 ℃, controlling the dropping time of the aqueous solution I and the aqueous solution II to be 2-3.5 h, carrying out heat preservation reaction for 1-2 h after the dropping is finished, and adjusting the pH to be 6.8-7.2 by using a pH regulator after the reaction is finished.
10. A concrete material characterized by: comprises the slump retaining agent as claimed in any one of claims 1 to 8 or obtained by the preparation method as claimed in claim 9.
CN202111631692.6A 2021-12-28 2021-12-28 Concrete slump retaining agent and preparation method and application thereof Pending CN114230730A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925301A (en) * 2022-05-27 2023-04-07 福建省磐石混凝土工程有限公司 Concrete waste slurry treatment process and concrete preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106478895A (en) * 2016-10-09 2017-03-08 武汉工程大学 Compound polycarboxylate water-reducer of a kind of graphene oxide and preparation method thereof
CN107311569A (en) * 2017-07-19 2017-11-03 太原理工大学 Carboxyl-functional graphene oxide high performance concrete and preparation method thereof
CN108609897A (en) * 2018-05-18 2018-10-02 萧县沃德化工科技有限公司 A kind of preparation method of graphite oxide ene-type polycarboxylate water-reducer
CN109020414A (en) * 2018-10-22 2018-12-18 太原理工大学 A kind of complex cement adsorbing material and preparation method thereof
CN112759726A (en) * 2021-01-21 2021-05-07 深圳港创建材股份有限公司 Graphene oxide modified slump retaining mother solution, and preparation method and use method thereof
CN116239729A (en) * 2022-12-27 2023-06-09 重庆建研科之杰建材有限公司 Low-sensitivity concrete slump retaining agent and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106478895A (en) * 2016-10-09 2017-03-08 武汉工程大学 Compound polycarboxylate water-reducer of a kind of graphene oxide and preparation method thereof
CN107311569A (en) * 2017-07-19 2017-11-03 太原理工大学 Carboxyl-functional graphene oxide high performance concrete and preparation method thereof
CN108609897A (en) * 2018-05-18 2018-10-02 萧县沃德化工科技有限公司 A kind of preparation method of graphite oxide ene-type polycarboxylate water-reducer
CN109020414A (en) * 2018-10-22 2018-12-18 太原理工大学 A kind of complex cement adsorbing material and preparation method thereof
CN112759726A (en) * 2021-01-21 2021-05-07 深圳港创建材股份有限公司 Graphene oxide modified slump retaining mother solution, and preparation method and use method thereof
CN116239729A (en) * 2022-12-27 2023-06-09 重庆建研科之杰建材有限公司 Low-sensitivity concrete slump retaining agent and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925301A (en) * 2022-05-27 2023-04-07 福建省磐石混凝土工程有限公司 Concrete waste slurry treatment process and concrete preparation method thereof

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