CN114436577A - Preparation method of plastic ultrahigh-performance concrete - Google Patents
Preparation method of plastic ultrahigh-performance concrete Download PDFInfo
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- CN114436577A CN114436577A CN202210274239.2A CN202210274239A CN114436577A CN 114436577 A CN114436577 A CN 114436577A CN 202210274239 A CN202210274239 A CN 202210274239A CN 114436577 A CN114436577 A CN 114436577A
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/022—Carbon
- C04B14/024—Graphite
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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
- C04B24/168—Polysaccharide derivatives, e.g. starch sulfate
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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
- C08F290/08—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 side groups
- C08F290/10—Polymers provided for in subclass C08B
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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
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00008—Obtaining or using nanotechnology related materials
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a preparation method of plastic ultrahigh-performance concrete, which comprises the steps of uniformly mixing 300-350 parts of cement, 400-420 parts of quartz sand, 100-105 parts of mineral powder, 70-90 parts of nano silica fume, 4-5 parts of water reducing agent, 55-65 parts of steel fiber and 1-1.5 parts of sulfonated graphene, adding water, continuously stirring in a stirrer for 5-10 min, and preparing the plastic ultrahigh-performance concrete after uniform stirring; the sulfonated graphene in the ultra-high performance concrete prepared by the invention can be bonded on the surface of the sulfonated graphene through hydrogen bonds and ester bonds with water reducing agent molecules, and the dispersing performance of the sulfonated graphene is improved by reducing the Van der Waals force among sulfonated graphene sheets, so that the ultra-high performance concrete is in a plastic state, the application scene of the ultra-high performance concrete can be obviously increased, and the mechanical property, the stability and the durability of the ultra-high performance concrete can be enhanced.
Description
Technical Field
The invention belongs to the technical field of concrete, and particularly relates to a preparation method of plastic ultrahigh-performance concrete.
Background
The working state of the existing ultra-high performance concrete is self-leveling slurry, when in engineering application or product production, a template is needed to be poured, and the template is removed after initial setting, so that the concrete can be shaped. As the template is always provided with gaps, slurry is easy to flow out, waste is large, the precision is not high, and the error is generally 0.5-1 cm. In order to solve the problem, the plastic ultrahigh-performance concrete can be directly shaped without a mould, is used for engineering application such as structure reinforcement, special-shaped member or sculpture manufacture and the like, has controllable precision and less material waste, and the finished product performance reaches or exceeds the performance of the original ultrahigh-performance concrete.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of plastic ultrahigh-performance concrete.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of plastic ultrahigh-performance concrete comprises the following steps:
according to the weight parts, 300-350 parts of sand-doped cement, 400-420 parts of quartz sand, 100-105 parts of mineral powder, 70-90 parts of nano silica fume, 4-5 parts of water reducing agent, 55-65 parts of steel fiber and 1-1.5 parts of sulfonated graphene are uniformly mixed, 100-150 parts of water is added, the mixture is placed into a stirrer to be continuously stirred for 5-10 min, and the ultrahigh-performance concrete is prepared after uniform stirring, wherein the working performance of the ultrahigh-performance concrete is in a plastic state, and the performances of the ultrahigh-performance concrete after final setting are superior to those of the conventional ultrahigh-performance concrete.
The water reducing agent is prepared by the following steps:
s1: adding cyclodextrin and p-toluenesulfonic acid into a reaction container, stirring and dissolving, adding maleic anhydride, continuously stirring, heating to 80 ℃, reacting for 7-8 hours, precipitating after the reaction is finished, and washing to obtain a maleic anhydride cyclodextrin polymer;
s2: and (2) placing the prepared maleic anhydride cyclodextrin polymer into a reaction kettle, adding a proper amount of hydroxyethyl acrylate, sodium allylsulfonate, an initiator ammonium persulfate and deionized water, reacting for 5-6 hours at 88 ℃ to obtain a mixture, cooling to room temperature after the reaction is finished, neutralizing the pH value of the mixture to be 7 by using a 20% sodium hydroxide solution, and uniformly stirring to obtain the water reducer.
The quantity ratio of the cyclodextrin to the maleic anhydride is 1: 1-6.
The weight ratio of the maleic anhydride cyclodextrin polymer hydroxyethyl acrylate to the sodium allylsulfonate substance is 1: 0.5.
The grain size of the quartz sand is 1.18-0.3 mm, and the grain size of the nano silica fume is 10-2 nm.
The sulfonated graphene is prepared by the following steps:
slowly adding the oxidizing sulfonating agent into the organic material at the temperature of 50-100 ℃ for reaction for 1-40 h, and after the reaction is finished, raising the reaction temperature to 150-220 ℃ for continuous reaction for 1-40 h, so that the oxidizing sulfonating agent and the organic material are fully reacted to prepare the sulfonated graphene.
The oxidative sulfonating agent is selected from: a compound of the general formula R-SO 3H, wherein R is selected from F, Cl, Br; h2SO4, HCl, HF, or a combination thereof.
The organic material is a combination of one or more of an organic high molecular material and an organic small molecular material, the organic high molecular material is selected from high molecular poly alkyne and polyolefin containing halogen elements, and the organic small molecular material is selected from straight-chain hydrocarbon containing 10-30 carbon atoms.
The working performance of the concrete prepared by compounding the sulfonated graphene and the water reducing agent is in a plastic state.
The sulfonated graphene obtained by the reaction of the oxidative sulfonating agent and the organic material in the reaction medium can be bonded on the surface of the sulfonated graphene through hydrogen bonds and ester bonds with water reducing agent molecules, so that the van der Waals force between sulfonated graphene sheets can be reduced, and the dispersion performance of the sulfonated graphene is improved.
In order to make the organic material in an amorphous state, so that loose graphene material is easily formed for further sulfonation and delamination, and a proper reaction speed is obtained, and the reaction is not too violent to cause safety problems, the invention mixes substances at a lower temperature of 50-100 ℃, and then forms a layered sulfonated graphene sheet with uniform properties at a higher temperature of 180 ℃.
Further, the water reducing agent is prepared by the following steps:
s1: adding cyclodextrin and p-toluenesulfonic acid into a reaction container, stirring and dissolving, adding maleic anhydride, continuously stirring, heating to 80 ℃, reacting for 7-8 hours, precipitating after the reaction is finished, and washing to obtain a maleic anhydride cyclodextrin polymer;
s2: putting the prepared maleic anhydride cyclodextrin polymer into a reaction kettle, adding a proper amount of hydroxyethyl acrylate, sodium allylsulfonate, an initiator ammonium persulfate and deionized water, reacting for 5-6 hours at 88 ℃ to obtain a mixture, cooling to room temperature after the reaction is finished, neutralizing the pH value of the mixture to be 7 by using a 20% sodium hydroxide solution, and uniformly stirring to obtain the water reducer; the quantity ratio of the cyclodextrin to the maleic anhydride is 1: 1-6; the weight ratio of the maleic anhydride cyclodextrin polymer hydroxyethyl acrylate to the sodium allylsulfonate substance is 1: 0.5.
When the water reducing agent is used in the ultra-high performance concrete, a small amount of micro holes are uniformly distributed on the surface of the ultra-high performance concrete, and the small holes have small aperture, so that the water reducing agent has good water reducing performance and certain air entraining effect, and thus the workability of the ultra-high performance concrete mixture can be improved, bleeding can be reduced, and the durability of the ultra-high performance concrete can be improved.
The invention has the beneficial effects that:
the invention can obviously improve the mechanical property of the ultra-high performance concrete by adding the sulfonated graphene as the filler of the ultra-high performance concrete, firstly, the prepared sulfonated graphene with large spacing, by the self-contained structure with larger interlayer spacing, the cyclodextrin macromonomer is wound on the surface of the sulfonated graphene due to the long chain function, under the condition that ammonium persulfate is used as an initiator, a long-chain structure is formed, and can be combined with water reducing agent molecules on the surface of sulfonated graphene through hydrogen bonds and ester bonds, so that the van der Waals force among sulfonated graphene sheets can be reduced, the dispersion performance of the sulfonated graphene is improved, and the ultrahigh-performance concrete is in a plastic state, furthermore, the application scenes of the ultra-high performance concrete, such as fields of special-shaped members, engineering construction, sculpture manufacturing and the like, can be obviously increased, and the mechanical property, the stability and the durability of the ultra-high performance concrete can be enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 1
The sulfonated graphene comprises the following steps:
slowly adding the oxidative sulfonating agent into the organic material at the temperature of 75 ℃ for reaction for 20 hours, and after the reaction is finished, raising the reaction temperature to 185 ℃ for continuous reaction for 20 hours, so that the oxidative sulfonating agent and the organic material are fully reacted to prepare the sulfonated graphene.
Example 2
A preparation method of plastic ultrahigh-performance concrete comprises the following steps:
according to the weight portion, 300 portions of cement, 400 portions of quartz sand, 100 portions of mineral powder, 70 portions of nano silica fume, 4 portions of water reducing agent, 55 portions of steel fiber and 1 portion of sulfonated graphene are uniformly mixed, 100 portions of water are added, the mixture is placed into a stirrer to be continuously stirred for 5min, and the ultrahigh-performance concrete is prepared after uniform stirring.
The water reducing agent is prepared by the following steps:
firstly, adding cyclodextrin and p-toluenesulfonic acid into a reaction vessel, stirring and dissolving, then adding maleic anhydride, continuously stirring, heating to 80 ℃, reacting for 7.5 hours, precipitating after the reaction is finished, and washing to obtain a maleic anhydride cyclodextrin polymer; and (2) placing the prepared maleic anhydride cyclodextrin polymer into a reaction kettle, adding a proper amount of hydroxyethyl acrylate, sodium allylsulfonate, an initiator ammonium persulfate and deionized water, reacting for 5.5 hours at 88 ℃ to obtain a mixture, cooling to room temperature after the reaction is finished, neutralizing the pH value of the mixture to be 7 by using a 20% sodium hydroxide solution, and uniformly stirring to obtain the water reducer.
Example 3
A preparation method of plastic ultrahigh-performance concrete comprises the following steps:
according to the weight parts, 320 parts of cement, 410 parts of quartz sand, 105 parts of mineral powder, 80 parts of nano silica fume, 4 parts of water reducing agent, 60 parts of steel fiber and 1.2 parts of sulfonated graphene are uniformly mixed, 130 parts of water is added, the mixture is placed into a stirrer to be continuously stirred for 8min, and the ultrahigh-performance concrete is prepared after uniform stirring.
The water reducing agent is prepared by the following steps:
firstly, adding cyclodextrin and p-toluenesulfonic acid into a reaction vessel, stirring and dissolving, then adding maleic anhydride, continuously stirring, heating to 80 ℃, reacting for 7.5 hours, precipitating after the reaction is finished, and washing to obtain a maleic anhydride cyclodextrin polymer; and (2) placing the prepared maleic anhydride cyclodextrin polymer into a reaction kettle, adding a proper amount of hydroxyethyl acrylate, sodium allylsulfonate, an initiator ammonium persulfate and deionized water, reacting for 5.5 hours at 88 ℃ to obtain a mixture, cooling to room temperature after the reaction is finished, neutralizing the pH value of the mixture to be 7 by using a 20% sodium hydroxide solution, and uniformly stirring to obtain the water reducer.
Example 4
A preparation method of plastic ultrahigh-performance concrete comprises the following steps:
according to the weight parts, 350 parts of cement, 420 parts of quartz sand, 105 parts of mineral powder, 90 parts of nano silica fume, 5 parts of water reducing agent, 65 parts of steel fiber and 1.5 parts of sulfonated graphene are uniformly mixed, 150 parts of water is added, the mixture is placed into a stirrer to be stirred for 10min, and the ultrahigh-performance concrete is prepared after uniform stirring.
The water reducing agent is prepared by the following steps:
firstly, adding cyclodextrin and p-toluenesulfonic acid into a reaction vessel, stirring and dissolving, then adding maleic anhydride, continuously stirring, heating to 80 ℃, reacting for 7.5 hours, precipitating after the reaction is finished, and washing to obtain a maleic anhydride cyclodextrin polymer; and (2) placing the prepared maleic anhydride cyclodextrin polymer into a reaction kettle, adding a proper amount of hydroxyethyl acrylate, sodium allylsulfonate, an initiator ammonium persulfate and deionized water, reacting for 5.5 hours at 88 ℃ to obtain a mixture, cooling to room temperature after the reaction is finished, neutralizing the pH value of the mixture to be 7 by using a 20% sodium hydroxide solution, and uniformly stirring to obtain the water reducer.
Comparative example 1
This comparative example compares to example 4 without the addition of sulfonated graphene.
Comparative example 2
Compared with example 4, the graphene oxide prepared by the Hummers method is used for replacing sulfonated graphene.
The compressive strength and the flexural strength of the concrete prepared in examples 2-4 and comparative examples 1-2 were tested according to GB/T50081-2002 Standard test methods for mechanical Properties of ordinary concrete, at least 3 test pieces were molded per group in the sizes of 100mm × 100mm × 100mm, 100mm × 100mm × 300mm, and the mechanical properties were tested after curing to a age of 28 days.
As can be seen from the table, the ultra-high performance concrete prepared by the embodiment of the invention has excellent mechanical properties.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The preparation method of the plastic ultrahigh-performance concrete is characterized by comprising the following steps of: the method comprises the following steps:
uniformly mixing 300-350 parts of cement, 400-420 parts of quartz sand, 100-105 parts of mineral powder, 70-90 parts of nano silica fume, 4-5 parts of water reducing agent, 55-65 parts of steel fiber and 1-1.5 parts of sulfonated graphene by weight, adding 100-150 parts of water, stirring in a stirrer for 5-10 min, and preparing the plastic ultrahigh-performance concrete after uniform stirring;
the water reducing agent is prepared by the following steps:
s1: adding cyclodextrin and p-toluenesulfonic acid into a reaction container, stirring and dissolving, adding maleic anhydride, continuously stirring, heating to 80 ℃, reacting for 7-8 hours, precipitating after the reaction is finished, and washing to obtain a maleic anhydride cyclodextrin polymer;
s2: and (2) placing the prepared maleic anhydride cyclodextrin polymer into a reaction kettle, adding a proper amount of hydroxyethyl acrylate, sodium allylsulfonate, an initiator ammonium persulfate and deionized water, reacting for 5-6 hours at 88 ℃ to obtain a mixture, cooling to room temperature after the reaction is finished, neutralizing the pH value of the mixture to be 7 by using a 20% sodium hydroxide solution, and uniformly stirring to obtain the water reducer.
2. The method of preparing a plastic ultra-high performance concrete according to claim 1, characterized in that: the quantity ratio of the cyclodextrin to the maleic anhydride is 1: 1-6.
3. The method of preparing a plastic ultra-high performance concrete according to claim 1, characterized in that: the weight ratio of the maleic anhydride cyclodextrin polymer hydroxyethyl acrylate to the sodium allylsulfonate substance is 1: 0.5.
4. The method of preparing a plastic ultra-high performance concrete according to claim 1, characterized in that: the grain size of the quartz sand is 1.18-0.3 mm, and the grain size of the nano silica fume is 10-2 nm.
5. The method of preparing a plastic ultra-high performance concrete according to claim 1, characterized in that: the sulfonated graphene is prepared by the following steps:
slowly adding the oxidizing sulfonating agent into the organic material at the temperature of 50-100 ℃ for reaction for 1-40 h, and after the reaction is finished, raising the reaction temperature to 150-220 ℃ for continuous reaction for 1-40 h, so that the oxidizing sulfonating agent and the organic material are fully reacted to prepare the sulfonated graphene.
6. The method of preparing a plastic ultra-high performance concrete according to claim 5, characterized in that: the oxidative sulfonating agent is selected from: a compound of the general formula R-SO 3H, wherein R is selected from F, Cl, Br; h2SO4, HCl, HF, or a combination thereof.
7. The method of preparing a plastic ultra-high performance concrete according to claim 5, characterized in that: the organic material is a combination of one or more of an organic high molecular material and an organic small molecular material, the organic high molecular material is selected from high molecular polyacetylene and polyolefin containing halogen elements, and the organic small molecular material is selected from straight-chain hydrocarbon containing 10-30 carbon atoms.
8. The method of producing a plastic ultra high performance concrete according to any one of claims 1 to 7, characterized in that: the working performance of the ultra-high performance concrete prepared by compounding the sulfonated graphene and the water reducing agent is in a plastic state.
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