CN113416016B - Concrete anti-shrinkage carbon-based nano reinforcing agent and preparation method thereof - Google Patents
Concrete anti-shrinkage carbon-based nano reinforcing agent and preparation method thereof Download PDFInfo
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- CN113416016B CN113416016B CN202110728818.5A CN202110728818A CN113416016B CN 113416016 B CN113416016 B CN 113416016B CN 202110728818 A CN202110728818 A CN 202110728818A CN 113416016 B CN113416016 B CN 113416016B
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention relates to a concrete dry shrinkage resistant carbon-based nano reinforcing agent and a preparation method thereof, wherein the concrete dry shrinkage resistant carbon-based nano reinforcing agent comprises the following components in percentage by mass: 1-10% of modified silica fume dispersion liquid, 1-12% of modified super absorbent resin microspheres, 0.3-5% of graphene oxide and the balance of deionized water. The concrete anti-shrinkage carbon-based nano reinforcing agent provided by the invention is prepared from the raw materials of silica fume, carbide slag and the like, solid wastes are reasonably utilized, certain economic benefit can be brought, and the concrete anti-shrinkage carbon-based nano reinforcing agent is added into concrete, so that not only can the shrinkage be reduced, but also the strength of the concrete can be improved.
Description
Technical Field
The invention belongs to the technical field of compositions of mortar, concrete or artificial stone containing inorganic binders, and particularly relates to a concrete dry shrinkage resistant carbon-based nano reinforcing agent and a preparation method thereof.
Background
When concrete is in a dry environment, moisture continuously dissipates from inside to outside, and the phenomenon of volume shrinkage is called concrete shrinkage. Concrete shrinkage can deform the concrete structure, affecting the durability of the concrete. To counteract this potential hazard, internal curing is often used to reduce the shrinkage of the concrete, such as adding superabsorbent to provide additional curing water, but the strength of the concrete to which the superabsorbent is added is often reduced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a concrete anti-shrinkage carbon-based nano reinforcing agent and a preparation method thereof aiming at the defects in the prior art.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the concrete dry shrinkage resistant carbon-based nano reinforcing agent is prepared from the following components in percentage by mass: 1-10% of modified silica fume dispersion liquid, 1-12% of modified super absorbent resin microspheres, 0.3-5% of graphene oxide and the balance of deionized water.
According to the scheme, the modified silica fume dispersion liquid comprises the following components in percentage by mass: 20-40% of silica fume, 5-10% of carbide slag, 40-60% of deionized water, 1-12% of phenyltriethoxysilane and 5-30% of absolute ethyl alcohol; the preparation method comprises the following steps: adding carbide slag and deionized water into silica fume, ultrasonically stirring for 15-30 min to obtain a uniform dispersion liquid, standing for 0.5-1 h, then dropwise adding phenyltriethoxysilane dissolved in absolute ethyl alcohol into the uniform dispersion liquid, and stirring for 2h at the temperature of 20-40 ℃ to obtain the calcium carbide powder. The modified silica fume dispersion liquid can ensure that the graphene oxide can be stably dispersed in concrete.
According to the scheme, siO in the silica fume 2 85 to 95 percent by mass and 0.1 to 100 mu m of particle size.
According to the scheme, ca (OH) in the carbide slag 2 The mass fraction of (A) is 70-90%.
According to the scheme, the modified super absorbent resin microsphere comprises the following raw material components in percentage by mass: 20-40% of super water-absorbent resin microspheres, 1-5% of surface modifier and 40-60% of water; the preparation method comprises the following steps: adding the surface modifier and water into the super absorbent resin microspheres, stirring and then ultrasonically dispersing for 15-30 min to obtain the super absorbent resin microspheres. The modification by the method can ensure that the super absorbent resin microspheres are stably dispersed on the surface of the graphene oxide.
According to the scheme, the super absorbent resin microspheres are acrylic acid-acrylamide copolymer resin microspheres, and the particle size of the super absorbent resin microspheres is 50-3000 nm. The super absorbent resin microspheres are used for reducing the drying shrinkage of concrete.
According to the scheme, the surface modifier is one of naphthalene sulfonate (such as 1-sodium naphthalene sulfonate) and sodium p-styrene sulfonate. The surface modifier is used for grafting a certain benzene ring on the super water-absorbent resin microsphere, so that the super water-absorbent resin can be stably dispersed on the surface of the graphene oxide.
According to the scheme, the graphene oxide is layered graphene oxide, the O/C atomic ratio is 0.25-0.35, and the specific surface area is 300-1000 m 2 (iv) g. The graphene oxide contains carboxyl, hydroxyl, carbonyl and epoxy groups. Application of graphene oxide toThe strength of the concrete is improved.
The invention also comprises a preparation method of the concrete anti-shrinkage carbon-based nano reinforcing agent, which comprises the following specific steps:
1) Weighing raw materials in proportion for later use;
2) Mixing the modified silica fume dispersion liquid and the modified super absorbent resin microspheres, and ultrasonically dispersing for 10-15 min to prepare uniform mixed dispersion liquid;
3) Mixing graphene oxide and deionized water according to a mass ratio of 1: 100-1000, adding the mixture into the mixed dispersion liquid obtained in the step 2) after ultrasonic dispersion is carried out for 10-15 min, and carrying out uniform ultrasonic dispersion to obtain the concrete anti-dry shrinkage carbon-based nano reinforcing agent.
The use method of the concrete dry shrinkage resistant carbon-based nano reinforcing agent specifically comprises the following steps: the concrete anti-dry shrinkage carbon-based nano reinforcing agent is doped into concrete, wherein the doping amount is 8-18% (weight percentage based on cement).
Firstly, pretreating the surface of silica fume by using carbide slag, then modifying the silica fume by using phenyl triethoxysilane, then assembling the silica fume dispersion liquid modified by using the phenyl triethoxysilane and graphene oxide through non-covalent modification so as to stably disperse the graphene oxide, and then adding the phenyl-modified super-absorbent resin microspheres into the assembly to obtain an assembly. The assembly is added into concrete, wherein the stably dispersed graphene oxide can play a role in improving the strength of the concrete, and the super water-absorbent resin microspheres in the assembly can play a role in resisting drying shrinkage.
The invention has the beneficial effects that: 1. the anti-shrinkage carbon-based nano reinforcing agent for concrete provided by the invention is added into concrete, so that the shrinkage can be reduced, and the strength can be improved; 2. the preparation method of the concrete dry shrinkage resistant carbon-based nano reinforcing agent provided by the invention takes the silica fume, the carbide slag and the like as raw materials, reasonably utilizes solid wastes, and can bring certain economic benefits.
Drawings
Fig. 1 is a schematic structural view of the concrete anti-shrinkage carbon-based nano reinforcing agent prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
SiO in silica fume used in the embodiment of the invention 2 Has a mass fraction of 94% and an average particle diameter of 0.37 μm, wherein Ca (OH) in the carbide slag is 2 The mass fraction of the acrylic acid-acrylamide copolymerized resin microspheres is 76%, the particle size of the acrylic acid-acrylamide copolymerized resin microspheres is 200nm, the graphene oxide is layered graphene oxide, the O/C atomic ratio is 0.3, and the specific surface area is 500m 2 /g。
Example 1
A concrete anti-shrinkage carbon-based nano reinforcing agent is prepared by the following specific steps:
A. adding 56 parts of deionized water and 10 parts of carbide slag into 34 parts of silica fume, ultrasonically dispersing for 20min, and standing for 40min to obtain uniform silica fume dispersion subjected to surface pretreatment;
B. 8 parts of phenyl triethoxy silane is dissolved in 30 parts of absolute ethyl alcohol and is dripped into the silicon ash dispersion liquid subjected to surface pretreatment, and the mixture is stirred for 2 hours at the temperature of 30 ℃ to obtain modified silicon ash dispersion liquid;
C. adding 1 part of surface modifier (sodium p-styrene sulfonate) and 59 parts of water into 40 parts of acrylic acid-acrylamide copolymer resin microspheres, stirring, and ultrasonically dispersing for 20min to obtain modified super absorbent resin microspheres;
D. weighing the following raw materials: 2% of modified silica fume dispersion liquid, 5% of modified super absorbent resin microspheres, 0.5% of graphene oxide and 92.5% of deionized water;
E. and mixing the modified silica fume dispersion liquid and the modified super absorbent resin microspheres, performing ultrasonic dispersion for 15min to prepare a uniform dispersion liquid, dissolving graphene oxide in deionized water, adding the graphene oxide into the uniform dispersion liquid after performing ultrasonic dispersion for 15min, and performing ultrasonic dispersion uniformly to obtain the concrete anti-drying shrinkage carbon-based nano reinforcing agent.
The concrete dry shrinkage resistant carbon-based nano reinforcing agent prepared in the embodiment is doped into concrete, wherein the doping amount is 12% (weight percentage based on cement), and the concrete raw material ratio is as follows: 13.50 parts of ordinary portland cement, 1.62 parts of concrete anti-dry carbon shrinkage nano reinforcing agent, 9 parts of slag, 67.6 parts of standard sand, 8.21 parts of water and 0.07 part of water reducing agent (the concrete without the concrete anti-dry carbon shrinkage nano reinforcing agent is used as blank comparison). The concrete strength is detected according to a GB/T17671-1999 method, the concrete shrinkage is detected according to a GB/T29417-2012 method, and through the test, the 28-day compressive strength of a blank sample is 32MPa, the shrinkage is 0.15%, the 28-day compressive strength of a concrete sample added with the concrete anti-shrinkage carbon-based nano reinforcing agent prepared in the embodiment is 44.5MPa, the shrinkage is 0.078%, and compared with the blank sample, the shrinkage is reduced by 48%.
Fig. 1 is a schematic structural diagram of the concrete dry shrinkage resistant carbon-based nano-reinforcing agent prepared in this embodiment, in which SAP is super water-absorbent resin, and silica fume modified by phenyl and super water-absorbent resin microspheres are stably dispersed on the surface of graphene oxide through pi-pi stacking.
Comparative example 1
The modified super absorbent resin microspheres in the example 1 are replaced by equivalent unmodified super absorbent resin microspheres, the concrete dry shrinkage resistant carbon-based nano reinforcing agent is prepared by the same method as the example 1, concrete is prepared, and the 28-day compressive strength of the obtained concrete sample is 28.5MPa.
Example 2
A concrete anti-shrinkage carbon-based nano reinforcing agent is prepared by the following specific steps:
A. adding 55 parts of deionized water and 9 parts of carbide slag into 36 parts of silica fume, performing ultrasonic dispersion for 20min, and standing for 40min to obtain uniform silica fume dispersion subjected to surface pretreatment;
B. 6 parts of phenyltriethoxysilane is dissolved in 28 parts of absolute ethanol and is dripped into the silicon ash dispersion liquid subjected to surface pretreatment, and the mixture is stirred for 2 hours at 30 ℃ to obtain modified silicon ash dispersion liquid;
C. adding 2 parts of surface modifier (1-sodium naphthalene sulfonate) and 60 parts of water into 38 parts of acrylic acid-acrylamide copolymer resin microspheres, stirring, and performing ultrasonic dispersion for 20min to obtain modified super absorbent resin microspheres;
D. weighing the following raw materials: 2% of modified silica fume dispersion liquid, 6% of modified super absorbent resin microspheres, 0.8% of graphene oxide and 91.2% of deionized water;
E. and mixing the modified silica fume dispersion liquid and the modified super absorbent resin microspheres, performing ultrasonic dispersion for 15min to prepare a uniform dispersion liquid, dissolving graphene oxide in deionized water, performing ultrasonic dispersion for 15min, adding the graphene oxide into the uniform dispersion liquid, and performing ultrasonic dispersion uniformly to obtain the concrete anti-drying shrinkage carbon-based nano reinforcing agent.
The concrete dry shrinkage resistant carbon-based nano reinforcing agent prepared in the embodiment is doped into concrete, wherein the doping amount is 9% (weight percentage based on cement), and the concrete raw material ratio is as follows: 13.6 parts of ordinary portland cement, 1.22 parts of concrete anti-dry carbon shrinkage nano reinforcing agent, 9 parts of slag, 67.8 parts of standard sand, 8.31 parts of water and 0.07 part of water reducing agent (the concrete without the concrete anti-dry carbon shrinkage nano reinforcing agent is used as blank comparison). The concrete strength is detected according to a GB/T17671-1999 method, the concrete shrinkage is detected according to a GB/T29417-2012 method, and through the test, the 28-day compressive strength of a blank sample is 32MPa, the shrinkage is 0.15%, the 28-day compressive strength of a concrete sample added with the concrete anti-shrinkage carbon-based nano reinforcing agent prepared by the embodiment is 43MPa, the shrinkage is 0.083%, and compared with the blank sample, the shrinkage is reduced by 45%.
Comparative example 2
The modified super absorbent resin microspheres in the example 2 are replaced by the same amount of unmodified super absorbent resin microspheres, the concrete dry shrinkage resistant carbon-based nano reinforcing agent is prepared by the same method in the example 2, concrete is prepared, and the 28-day compressive strength of the obtained concrete sample is 29MPa.
Claims (8)
1. The concrete dry shrinkage resistant carbon-based nano reinforcing agent is characterized by comprising the following components in percentage by mass: 1-10% of modified silica fume dispersion liquid, 1-12% of modified super absorbent resin microspheres, 0.3-5% of graphene oxide and the balance of deionized water;
the modified silica fume dispersion liquid comprises the following components in percentage by mass: 20-40% of silica fume, 5-10% of carbide slag, 40-60% of deionized water, 1-12% of phenyltriethoxysilane and 5-30% of absolute ethyl alcohol; the preparation method comprises the following steps: adding carbide slag and deionized water into silica fume, ultrasonically stirring for 15-30 min to obtain a uniform dispersion liquid, standing for 0.5-1 h, then dropwise adding phenyltriethoxysilane dissolved in absolute ethyl alcohol into the uniform dispersion liquid, and stirring for 2h at the temperature of 20-40 ℃ to obtain the calcium carbide powder;
the modified super absorbent resin microsphere comprises the following raw material components in percentage by mass: 20-40% of super water-absorbent resin microspheres, 1-5% of surface modifier and 40-60% of water; the preparation method comprises the following steps: adding the surface modifier and water into the super absorbent resin microspheres, stirring and then ultrasonically dispersing for 15-30 min to obtain the super absorbent resin microspheres.
2. The concrete dry-shrink-resistant carbon-based nanoenhancer as claimed in claim 1, wherein SiO in the silica fume is SiO 2 85 to 95 percent by mass and 0.1 to 100 mu m of particle size.
3. The concrete dry shrinkage resistant carbon-based nano reinforcing agent as claimed in claim 1, wherein Ca (OH) in the carbide slag 2 The mass fraction of (A) is 70-90%.
4. The concrete dry shrinkage resistant carbon-based nano reinforcing agent as claimed in claim 1, wherein the super water absorbent resin microspheres are acrylic acid-acrylamide copolymer resin microspheres, and the particle size of the super water absorbent resin microspheres is 50-3000 nm.
5. The concrete dry shrinkage-resistant carbon-based nano reinforcing agent as claimed in claim 1, wherein the surface modifier is one of naphthalene sulfonate and sodium p-styrene sulfonate.
6. The concrete dry shrinkage-resistant carbon-based nano reinforcing agent as claimed in claim 1, wherein the graphene oxide is a layered graphene oxide, the atomic ratio of O/C is 0.25-0.35, and the specific surface area is 300-1000 m 2 /g。
7. A preparation method of the concrete dry shrinkage resistant carbon-based nano reinforcing agent as claimed in any one of claims 1 to 6, is characterized by comprising the following specific steps:
1) Weighing raw materials in proportion for later use;
2) Mixing the modified silica fume dispersion liquid and the modified super absorbent resin microspheres, and ultrasonically dispersing for 10-15 min to prepare uniform mixed dispersion liquid;
3) Mixing graphene oxide and deionized water according to a mass ratio of 1: 100-1000, adding the mixture into the mixed dispersion liquid obtained in the step 2) after ultrasonic dispersion is carried out for 10-15 min, and carrying out uniform ultrasonic dispersion to obtain the concrete anti-dry shrinkage carbon-based nano reinforcing agent.
8. The use method of the concrete dry-shrinkage-resistant carbon-based nano reinforcing agent as claimed in any one of claims 1 to 6, wherein the concrete dry-shrinkage-resistant carbon-based nano reinforcing agent is mixed into concrete in an amount of 8 to 18%.
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| CN107056183A (en) * | 2017-01-23 | 2017-08-18 | 常州第六元素材料科技股份有限公司 | A kind of graphene oxide concrete composite material of chloride-penetration resistance and preparation method thereof |
| CN107382205A (en) * | 2017-08-16 | 2017-11-24 | 西安建筑科技大学 | A kind of super high strength high performance fiber concrete of C160 strength grades and preparation method thereof |
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| CN106587691A (en) * | 2016-10-28 | 2017-04-26 | 同济大学 | Method for preparing modified micro particles coated with graphene oxide |
| EP3640223A1 (en) * | 2018-10-16 | 2020-04-22 | Graphenano S.L. | Graphenic nanomaterials for the improvement of cementitious materials |
| CN112723788A (en) * | 2021-01-15 | 2021-04-30 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Efficient water-saving maintenance material |
| CN112939499A (en) * | 2021-01-29 | 2021-06-11 | 南京工业大学 | Preparation method and application of modified silica fume material |
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| CN107056183A (en) * | 2017-01-23 | 2017-08-18 | 常州第六元素材料科技股份有限公司 | A kind of graphene oxide concrete composite material of chloride-penetration resistance and preparation method thereof |
| CN107382205A (en) * | 2017-08-16 | 2017-11-24 | 西安建筑科技大学 | A kind of super high strength high performance fiber concrete of C160 strength grades and preparation method thereof |
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