CN112047674B - Material for wave wall - Google Patents
Material for wave wall Download PDFInfo
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- CN112047674B CN112047674B CN202010731679.7A CN202010731679A CN112047674B CN 112047674 B CN112047674 B CN 112047674B CN 202010731679 A CN202010731679 A CN 202010731679A CN 112047674 B CN112047674 B CN 112047674B
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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
- C04B28/02—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 containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
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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
- C04B14/026—Carbon of particular shape, e.g. nanotubes
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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
- C04B24/10—Carbohydrates or derivatives thereof
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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
- C04B2111/20—Resistance against chemical, physical or biological attack
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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
Abstract
The invention discloses a material for a wave wall, which comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent; wherein the nano composite temperature-sensitive hydrogel is cyclodextrin modified graphene type nano hydrogel. The nano composite temperature-sensitive hydrogel disclosed by the invention can be used for rapidly absorbing redundant moisture in concrete, preventing the moisture from entering capillary holes of raw materials such as slurry and the like, so that the concrete is frosted and cracked, the freeze-thaw resistance of the concrete for the wave wall is improved, the nano composite temperature-sensitive hydrogel can be used as a wear-resistant agent to improve the wear resistance of the concrete, and the economic effect of a concrete material is improved.
Description
Technical Field
The invention relates to the field of concrete for coastal protection. More particularly, the present invention relates to a material for a wave wall.
Background
The slope dikes arranged on two sides of the coast are important hydraulic engineering in coastal port engineering, and a wave wall is usually arranged on the top of each slope dike for ensuring the safety of the slope dike structure and the stability of a water area in a port, so that the effective elevation of the top of each slope dike can be improved, and the impact strength of sea wave breaking on the slope dikes is weakened. The wave wall is actually the concrete water retaining wall for preventing waves from crossing the top of the dike, and because the environment is severe, the wave wall is damaged to a certain extent by wind waves, seawater impact and temperature change, so that the performance of frost resistance, wear resistance and the like of hydraulic concrete for manufacturing the wave wall is higher in requirement, and the damage to the wave wall caused by various environmental factors is resisted.
The concrete raw materials include cement mortar and orthopaedics, cement mortar and aggregate are all porous bodies with micro pores, and all have certain hydroscopicity, in order to guarantee the workability among the raw materials of the concrete, a certain amount of water is usually required to be added, the total amount of the water is required to be larger than the hydration water of the cement, in the stirring and manufacturing process of the concrete, the redundant water can enter the capillary pores of the cement mortar and the aggregate and is retained in the capillary pores, and the retained water is the main internal cause of causing the concrete to be damaged and cracked by freezing: the water retained in the capillary holes is frozen and becomes solid when meeting the cold, the volume is increased, and the expansive force is generated, so that the structure in the rigid capillary holes is damaged, and finally the concrete is cracked by freezing.
In the prior art, the water consumption of concrete is reduced by adding the water reducing agent, and the excessive water entering the capillary pores is reduced, so that the aim of improving the frost resistance of the concrete is fulfilled; however, the introduction of the water reducing agent has a plurality of technical problems, such as the sensitivity to cement and admixture causes the addition amount of the water reducing agent to be not controlled, the water reducing agent can influence the slump of concrete, and in addition, the addition of the water reducing agent can prolong the curing time; in addition, in order to ensure the wear resistance of the concrete, a wear-resistant additive is additionally added to improve the wear resistance of the concrete, the addition of the wear-resistant additive can increase the preparation cost of the concrete and reduce the economic benefit of the concrete, and meanwhile, the compounding effect of the wear-resistant additive and the water reducing agent is poor; finally, the concrete in the prior art has poor improvement effects on frost resistance and wear resistance.
Therefore, it is highly desirable to provide a new concrete material for making a wave wall, which can significantly improve the frost resistance and wear resistance of the concrete.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a material for wave-retaining walls, which can improve the frost resistance and wear resistance of concrete by introducing the nano composite temperature-sensitive hydrogel, and solves the technical problem that the frost resistance and wear resistance of concrete in the prior art are not well improved.
To achieve these objects and other advantages in accordance with the present invention, there is provided a material for a wave barrier, comprising the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent;
wherein the nano composite temperature-sensitive hydrogel is cyclodextrin modified graphene type nano hydrogel.
Preferably, the preparation method of the material for the wave barrier and the nano composite temperature-sensitive hydrogel comprises the following steps:
step a, dissolving 4 parts of cyclodextrin in deionized water according to parts by weight to prepare a cyclodextrin water solution with the concentration of 0.01 g/mL; taking 2.5 parts of glycidyl methacrylate, adding the glycidyl methacrylate into a cyclodextrin water solution under the protection of nitrogen atmosphere, and fully stirring the mixture for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, taking 50 parts of graphene oxide aqueous solution with the concentration of 0.7mg/mL, placing the graphene oxide aqueous solution in an ice water bath, introducing nitrogen into the graphene oxide aqueous solution, adding 1 part of N-isopropylacrylamide into the graphene oxide aqueous solution under the protection of nitrogen atmosphere, and stirring the graphene oxide aqueous solution for 30min under the ice water bath to obtain a second solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of initiator and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the initiator is added, the first solution is dropwise added into the second solution after stirring for 10min, and after the first solution is added, the stirring is continued for 20min to obtain a reaction solution;
and d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube to obtain the product.
Preferably, the material for the wave wall, the first sediment is purified, specifically: d, dissolving the first sediment obtained in the step d by using deionized water at 5 ℃, filling the first sediment into a dialysis bag for dialysis treatment, transferring the solution in the dialysis bag into a centrifugal tube after 6 hours, centrifuging the solution at 40 ℃ for 5 minutes, pouring out a second supernatant in the centrifugal tube while the solution is hot, and collecting a second sediment in the centrifugal tube to obtain the nano composite temperature-sensitive hydrogel; wherein the cut-off molecular weight of the dialysis bag is 7000, and the dialysis external liquid is deionized water.
Preferably, the preparation method of the material for the wave wall and the graphene oxide aqueous solution comprises the following steps:
putting 70 parts by weight of concentrated sulfuric acid into a reaction vessel in an ice-water bath, adding 3 parts by weight of graphite powder into the concentrated sulfuric acid while stirring, continuing to stir for 10min after the graphite powder is added, then sequentially adding 1.5 parts by weight of sodium nitrate and 9 parts by weight of potassium permanganate into the concentrated sulfuric acid, continuing to stir for 20min, transferring the reaction vessel to an oil bath at 40 ℃, continuing to stir for 1h, dropwise adding 150 parts by weight of deionized water into the reaction vessel, heating the oil bath to 90 ℃, continuing to stir until the solution in the reaction vessel is yellow, stopping heating and cooling to room temperature, then adding 500 parts by weight of deionized water into the reaction vessel, stirring for 30min, adding 20 parts by weight of 30% hydrogen peroxide into the reaction vessel, stirring for 20min, standing for 30h, pouring out a third supernatant in the reaction vessel, and sequentially adding 5% by weight of dilute hydrochloric acid, Washing the lower layer mixture for 2 times by using distilled water, then carrying out centrifugal treatment, collecting a third deposit in a centrifugal tube, dispersing the third deposit in deionized water, and adjusting the concentration of the third deposit to be 0.7mg/mL to obtain the graphene oxide aqueous solution.
Preferably, the cyclodextrin of the material for the wave-retaining wall is hydroxypropyl-beta-cyclodextrin.
Preferably, the material for the wave wall is prepared by adopting a calcium sulphoaluminate CAS concrete expanding agent as an expanding agent.
Preferably, the initiator of the material for the wave wall is one of potassium persulfate, sodium persulfate and lauroyl peroxide.
The invention at least comprises the following beneficial effects:
1. according to the invention, the nano composite temperature-sensitive hydrogel is introduced into the concrete, so that excessive moisture in the concrete can be quickly absorbed, the moisture is prevented from entering capillary holes of raw materials such as slurry and the like, the concrete is frosted and cracked, the freeze-thaw resistance of the concrete for the wave barrier wall is improved, the nano composite temperature-sensitive hydrogel can be used as a wear-resistant agent to improve the wear resistance of the concrete, and the economic effect of the concrete material is improved; in addition, the nano composite temperature-sensitive hydrogel does not have any influence on the performance of other raw materials of concrete;
2. dissolving glycidyl methacrylate in an aqueous solution of cyclodextrin to prepare a first solution, dissolving N-isopropylacrylamide in an aqueous solution of graphene oxide to prepare a second solution, and when the first solution is added into the second solution, reacting the glycidyl methacrylate with the N-isopropylacrylamide, so that the cyclodextrin and the graphene oxide are added to the hydrogel for modification, and the temperature sensitivity and the mechanical property of the hydrogel are improved, thereby achieving the technical effect of simultaneously improving the freeze-thaw resistance and the wear resistance of concrete;
the epoxy group of glycidyl acrylate is subjected to ring-opening crosslinking, cyclodextrin is remained on a high molecular chain in the in-situ synthesis process of hydrogel, the cyclodextrin has excellent hydrophilicity, the ratio of hydrophilic groups to hydrophobic groups on the high molecular chain can be greatly improved, the number of hydrogen bonds formed by the cyclodextrin and water is increased, therefore, the water absorption rate is improved, when the temperature is higher than the low critical transition temperature, the hydrogen bonds are destroyed, water molecules are quickly released, the swelling ratio is quickly reduced, the response rate of the hydrogel to the temperature is accelerated, meanwhile, the cyclodextrin has a large cavity, so that the hydrogel provides more water containing sites, excessive water can be more quickly absorbed, the introduction of the cyclodextrin enables the hydrogel to have better temperature sensitivity, and the water balance in a concrete system can be more quickly regulated; in addition, the cyclodextrin has better biocompatibility, so that the hydrogel can be better fused with other raw materials of concrete;
meanwhile, the N-isopropylacrylamide is modified by graphene oxide, and the graphene oxide is loaded on the N-isopropylacrylamide to provide an active covalent crosslinking site and a physical crosslinking site, so that the finally prepared composite hydrogel simultaneously has physical crosslinking and chemical crosslinking inside, has a uniform three-dimensional network structure and higher crosslinking density, improves the extensibility and mechanical strength of the hydrogel, and further improves the temperature sensitivity of the hydrogel; when the hydrogel expands due to water absorption and contracts due to water release under the change of temperature, energy dissipation can be performed through the fracture of covalent bonds and the fracture of hydrogen bonds, the fracture of the hydrogel caused by local stress concentration is avoided, and the mechanical property of the hydrogel can be enhanced by the graphene oxide, so that the hydrogel plays a role of an anti-wear agent.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
< example 1>
The invention provides a material for a wave wall, which comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent; wherein the nano composite temperature-sensitive hydrogel is cyclodextrin modified graphene type nano hydrogel.
The preparation method of the nano composite temperature-sensitive hydrogel comprises the following steps:
step a, dissolving 4 parts of cyclodextrin in deionized water according to parts by weight to prepare a cyclodextrin water solution with the concentration of 0.01 g/mL; taking 2.5 parts of glycidyl methacrylate, adding the glycidyl methacrylate into a cyclodextrin water solution under the protection of nitrogen atmosphere, and fully stirring the mixture for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, taking 50 parts of graphene oxide aqueous solution with the concentration of 0.7mg/mL, placing the graphene oxide aqueous solution in an ice water bath, introducing nitrogen into the graphene oxide aqueous solution, adding 1 part of N-isopropylacrylamide into the graphene oxide aqueous solution under the protection of nitrogen atmosphere, and stirring the graphene oxide aqueous solution for 30min under the ice water bath to remove bubbles in the structure to obtain a second solution;
the preparation method of the graphene oxide aqueous solution comprises the following steps: putting 70 parts by weight of concentrated sulfuric acid into a reaction vessel in an ice-water bath, adding 3 parts by weight of graphite powder into the concentrated sulfuric acid while stirring, continuing to stir for 10min after the graphite powder is added, then sequentially adding 1.5 parts by weight of sodium nitrate and 9 parts by weight of potassium permanganate into the concentrated sulfuric acid, continuing to stir for 20min, transferring the reaction vessel to an oil bath at 40 ℃, continuing to stir for 1h, dropwise adding 150 parts by weight of deionized water into the reaction vessel, heating the oil bath to 90 ℃, continuing to stir until the solution in the reaction vessel is yellow, stopping heating and cooling to room temperature, then adding 500 parts by weight of deionized water into the reaction vessel, stirring for 30min, adding 20 parts by weight of 30% hydrogen peroxide into the reaction vessel, stirring for 20min, standing for 30h, pouring out a third supernatant in the reaction vessel, and sequentially adding 5% by weight of dilute hydrochloric acid, Washing the lower layer mixture for 2 times by using distilled water, then carrying out centrifugal treatment, collecting a third deposit in a centrifugal tube, dispersing the third deposit in deionized water, and adjusting the concentration of the third deposit to be 0.7mg/mL to obtain a graphene oxide aqueous solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of potassium persulfate and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the potassium persulfate is added, stirring for 10min, then adding the first solution into the second solution, and after the first solution is added, continuously stirring for 20min to obtain a reaction solution;
and d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube.
Wherein the cyclodextrin is hydroxypropyl-beta-cyclodextrin; the expanding agent is a calcium sulphoaluminate CAS concrete expanding agent.
< example 2>
The invention provides a material for a wave wall, which comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent; wherein the nano composite temperature-sensitive hydrogel is cyclodextrin modified graphene type nano hydrogel.
The preparation method of the nano composite temperature-sensitive hydrogel comprises the following steps:
step a, dissolving 4 parts of cyclodextrin in deionized water according to parts by weight to prepare a cyclodextrin water solution with the concentration of 0.01 g/mL; taking 2.5 parts of glycidyl methacrylate, adding the glycidyl methacrylate into a cyclodextrin water solution under the protection of nitrogen atmosphere, and fully stirring the mixture for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, taking 50 parts of graphene oxide aqueous solution with the concentration of 0.7mg/mL, placing the graphene oxide aqueous solution in an ice water bath, introducing nitrogen into the graphene oxide aqueous solution, adding 1 part of N-isopropylacrylamide into the graphene oxide aqueous solution under the protection of nitrogen atmosphere, and stirring the graphene oxide aqueous solution for 30min under the ice water bath to remove bubbles in the structure to obtain a second solution;
the preparation method of the graphene oxide aqueous solution comprises the following steps: putting 70 parts by weight of concentrated sulfuric acid into a reaction vessel in an ice-water bath, adding 3 parts by weight of graphite powder into the concentrated sulfuric acid while stirring, continuing to stir for 10min after the graphite powder is added, then sequentially adding 1.5 parts by weight of sodium nitrate and 9 parts by weight of potassium permanganate into the concentrated sulfuric acid, continuing to stir for 20min, transferring the reaction vessel to an oil bath at 40 ℃, continuing to stir for 1h, dropwise adding 150 parts by weight of deionized water into the reaction vessel, heating the oil bath to 90 ℃, continuing to stir until the solution in the reaction vessel is yellow, stopping heating and cooling to room temperature, then adding 500 parts by weight of deionized water into the reaction vessel, stirring for 30min, adding 20 parts by weight of 30% hydrogen peroxide into the reaction vessel, stirring for 20min, standing for 30h, pouring out a third supernatant in the reaction vessel, and sequentially adding 5% by weight of dilute hydrochloric acid, Washing the lower layer mixture for 2 times by using distilled water, then carrying out centrifugal treatment, collecting a third deposit in a centrifugal tube, dispersing the third deposit in deionized water, and adjusting the concentration of the third deposit to be 0.7mg/mL to obtain a graphene oxide aqueous solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of lauroyl peroxide and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the addition of the lauroyl peroxide is finished, the first solution is dropwise added into the second solution after stirring for 10min, and after the addition of the first solution is finished, the stirring is continued for 20min to obtain a reaction solution;
d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube;
e, dissolving the first sediment obtained in the step d by using deionized water at 5 ℃, filling the first sediment into a dialysis bag for dialysis treatment, transferring the solution in the dialysis bag into a centrifugal tube after 6 hours, centrifuging the solution at 40 ℃ for 5 minutes, pouring a second supernatant in the centrifugal tube while the solution is hot, and collecting a second sediment in the centrifugal tube to obtain the nano composite temperature-sensitive hydrogel; wherein the cut-off molecular weight of the dialysis bag is 7000, and the dialysis external liquid is deionized water.
Wherein the cyclodextrin is hydroxypropyl-beta-cyclodextrin; the expanding agent is a calcium sulphoaluminate CAS concrete expanding agent.
< comparative example 1>
The material for the wave-retaining wall comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of water reducing agent, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent.
< comparative example 2>
The material for the wave-retaining wall comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent;
the preparation method of the nano temperature-sensitive hydrogel comprises the following steps:
step a, adding 2.5 parts by weight of methacrylic acid glycidyl into an aqueous solution under the protection of nitrogen atmosphere, and fully stirring for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, under the protection of nitrogen atmosphere, adding 1 part of N-isopropylacrylamide into the aqueous solution, and stirring the aqueous solution for 30min in an ice-water bath to obtain a second solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of initiator and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the initiator is added, the first solution is dropwise added into the second solution after stirring for 10min, and after the first solution is added, the stirring is continued for 20min to obtain a reaction solution;
d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube;
e, dissolving the first sediment obtained in the step d by using deionized water at 5 ℃, filling the first sediment into a dialysis bag for dialysis treatment, transferring the solution in the dialysis bag into a centrifugal tube after 6 hours, centrifuging the solution at 40 ℃ for 5 minutes, pouring a second supernatant in the centrifugal tube while the solution is hot, and collecting a second sediment in the centrifugal tube to obtain the nano composite temperature-sensitive hydrogel; wherein the cut-off molecular weight of the dialysis bag is 7000, and the dialysis external liquid is deionized water.
< comparative example 3>
The material for the wave-retaining wall comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent;
the preparation method of the nano composite temperature-sensitive hydrogel comprises the following steps:
step a, dissolving 4 parts of cyclodextrin in deionized water according to parts by weight to prepare a cyclodextrin water solution with the concentration of 0.01 g/mL; taking 2.5 parts of glycidyl methacrylate, adding the glycidyl methacrylate into a cyclodextrin water solution under the protection of nitrogen atmosphere, and fully stirring the mixture for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, under the protection of nitrogen atmosphere, adding 1 part of N-isopropylacrylamide into the aqueous solution, and stirring the aqueous solution for 30min in an ice-water bath to obtain a second solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of initiator and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the initiator is added, the first solution is dropwise added into the second solution after stirring for 10min, and after the first solution is added, the stirring is continued for 20min to obtain a reaction solution;
d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube;
e, dissolving the first sediment obtained in the step d by using deionized water at 5 ℃, filling the first sediment into a dialysis bag for dialysis treatment, transferring the solution in the dialysis bag into a centrifugal tube after 6 hours, centrifuging the solution at 40 ℃ for 5 minutes, pouring a second supernatant in the centrifugal tube while the solution is hot, and collecting a second sediment in the centrifugal tube to obtain the nano composite temperature-sensitive hydrogel; wherein the cut-off molecular weight of the dialysis bag is 7000, and the dialysis external liquid is deionized water.
< comparative example 4>
The material for the wave-retaining wall comprises the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent;
the preparation method of the nano composite temperature-sensitive hydrogel comprises the following steps:
step a, adding 2.5 parts by weight of methacrylic acid glycidyl into an aqueous solution under the protection of nitrogen atmosphere, and fully stirring for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, taking 50 parts of graphene oxide aqueous solution with the concentration of 0.7mg/mL, placing the graphene oxide aqueous solution in an ice water bath, introducing nitrogen into the graphene oxide aqueous solution, adding 1 part of N-isopropylacrylamide into the graphene oxide aqueous solution under the protection of nitrogen atmosphere, and stirring the graphene oxide aqueous solution for 30min under the ice water bath to remove bubbles in the structure to obtain a second solution;
the preparation method of the graphene oxide aqueous solution comprises the following steps: putting 70 parts by weight of concentrated sulfuric acid into a reaction vessel in an ice-water bath, adding 3 parts by weight of graphite powder into the concentrated sulfuric acid while stirring, continuing to stir for 10min after the graphite powder is added, then sequentially adding 1.5 parts by weight of sodium nitrate and 9 parts by weight of potassium permanganate into the concentrated sulfuric acid, continuing to stir for 20min, transferring the reaction vessel to an oil bath at 40 ℃, continuing to stir for 1h, dropwise adding 150 parts by weight of deionized water into the reaction vessel, heating the oil bath to 90 ℃, continuing to stir until the solution in the reaction vessel is yellow, stopping heating and cooling to room temperature, then adding 500 parts by weight of deionized water into the reaction vessel, stirring for 30min, adding 20 parts by weight of 30% hydrogen peroxide into the reaction vessel, stirring for 20min, standing for 30h, pouring out a third supernatant in the reaction vessel, and sequentially adding 5% by weight of dilute hydrochloric acid, Washing the lower layer mixture for 2 times by using distilled water, then carrying out centrifugal treatment, collecting a third deposit in a centrifugal tube, dispersing the third deposit in deionized water, and adjusting the concentration of the third deposit to be 0.7mg/mL to obtain a graphene oxide aqueous solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of initiator and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the initiator is added, the first solution is dropwise added into the second solution after stirring for 10min, and after the first solution is added, the stirring is continued for 20min to obtain a reaction solution;
d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube;
e, dissolving the first sediment obtained in the step d by using deionized water at 5 ℃, filling the first sediment into a dialysis bag for dialysis treatment, transferring the solution in the dialysis bag into a centrifugal tube after 6 hours, centrifuging the solution at 40 ℃ for 5 minutes, pouring a second supernatant in the centrifugal tube while the solution is hot, and collecting a second sediment in the centrifugal tube to obtain the nano composite temperature-sensitive hydrogel; wherein the cut-off molecular weight of the dialysis bag is 7000, and the dialysis external liquid is deionized water.
< test >
Preparing materials according to the formulas provided by the embodiments 1-2 and the comparative examples 1-4 respectively, mixing the materials, stirring for 3min by a forced stirrer, and discharging to obtain concrete samples corresponding to the embodiments 1-2 and the comparative examples 1-4;
the compressive strength of several concrete samples corresponding to the above examples 1-2 and comparative examples 1-4 was tested according to the concrete structure design Specification (GB/T50010); as shown in table 1:
TABLE 1 compressive Strength of concrete
As can be seen from table 1, compared with comparative examples 1 to 4, the concrete prepared from the concrete material provided in embodiments 1 to 2 of the present invention has better compressive property, the hydrogel modified by cyclodextrin and graphene oxide is introduced into the concrete material, the internal moisture of the concrete system is regulated and controlled from the preparation process of the concrete, and the excessive moisture is regulated while the workability of each component of the concrete is ensured, so as to prevent the moisture from entering into the capillary pores of the raw materials such as slurry, and further achieve the technical effect of improving the compressive property of the concrete product.
The anti-abrasion performance of the concrete samples of the examples 1 to 2 and the comparative examples 1 to 4 was tested according to the Experimental regulations on Hydraulic concrete (DL/T5150-2001), and the results are shown in Table 2; adjusting an electromagnetic relay speed regulator of an anti-abrasion tester in the testing process, adjusting the rotation speed to 1200r/min (the water flow speed corresponding to the surface of the concrete sample is 1.8m/s), and adopting 67 steel balls with the diameter of 19 mm;
the frost resistance of several concrete samples corresponding to the above examples 1-2 and comparative examples 1-4 was tested according to the concrete frost resistance test equipment (JGT 243-2009) and the aerated concrete frost resistance test method GBT 11973-1997, and the results are shown in 2;
the durability of the concrete samples of examples 1 to 2 and comparative examples 1 to 4 was measured according to the technical specification for durability of concrete for hydraulic engineering (DB32_ T2333-2013), and the results are shown in FIG. 2.
TABLE 2 concrete Performance test results
As can be seen from table 2, compared with comparative examples 1 to 4, the concrete prepared from the concrete material provided in embodiments 1 to 2 of the present invention has better frost resistance, wear resistance and durability, and the hydrogel modified by cyclodextrin and graphene oxide can significantly improve various properties of the concrete, achieve the C45 standard, achieve the frost resistance level of F250, meet the design requirement of 50 years, and can be used in a seawater splash zone with a higher environmental level.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (6)
1. The material for the wave-retaining wall is characterized by comprising the following raw materials in parts by weight: 15 parts of cement, 25 parts of basalt broken stone, 30 parts of river sand, 0.5 part of nano composite temperature-sensitive hydrogel, 0.3 part of polyvinyl alcohol fiber, 5 parts of water, 1.5 parts of slag powder and 0.2 part of expanding agent;
wherein the nano composite temperature-sensitive hydrogel is cyclodextrin modified graphene type nano hydrogel;
the preparation method of the nano composite temperature-sensitive hydrogel comprises the following steps:
step a, dissolving 4 parts of cyclodextrin in deionized water according to parts by weight to prepare a cyclodextrin water solution with the concentration of 0.01 g/mL; taking 2.5 parts of glycidyl methacrylate, adding the glycidyl methacrylate into a cyclodextrin water solution under the protection of nitrogen atmosphere, and fully stirring the mixture for 30min under the protection of nitrogen atmosphere to obtain a first solution;
b, taking 50 parts of graphene oxide aqueous solution with the concentration of 0.7mg/mL, placing the graphene oxide aqueous solution in an ice water bath, introducing nitrogen into the graphene oxide aqueous solution, adding 1 part of N-isopropylacrylamide into the graphene oxide aqueous solution under the protection of nitrogen atmosphere, and stirring the graphene oxide aqueous solution for 30min under the ice water bath to obtain a second solution;
c, placing the second solution obtained in the step b in an ice water bath, and sequentially adding 0.05 part of initiator and the first solution obtained in the step a into the second solution under the protection of nitrogen atmosphere, wherein after the initiator is added, the first solution is dropwise added into the second solution after stirring for 10min, and after the first solution is added, the stirring is continued for 20min to obtain a reaction solution;
and d, placing the reaction liquid obtained in the step c into a water bath at 60 ℃, placing the reaction liquid into a sealed container, replacing air in the sealed container with nitrogen, stirring the reaction liquid for reaction for 20 hours to obtain a product mixed liquid, transferring the product mixed liquid into a centrifugal tube, centrifuging the product mixed liquid for 5 minutes at 40 ℃, pouring a first supernatant in the centrifugal tube while the product mixed liquid is hot, and collecting a first sediment in the centrifugal tube to obtain the product.
2. Material for retaining walls according to claim 1, characterized in that the first deposit is subjected to a purification treatment, in particular: d, dissolving the first sediment obtained in the step d by using deionized water at 5 ℃, filling the first sediment into a dialysis bag for dialysis treatment, transferring the solution in the dialysis bag into a centrifugal tube after 6 hours, centrifuging the solution at 40 ℃ for 5 minutes, pouring out a second supernatant in the centrifugal tube while the solution is hot, and collecting a second sediment in the centrifugal tube to obtain the nano composite temperature-sensitive hydrogel; wherein the cut-off molecular weight of the dialysis bag is 7000, and the dialysis external liquid is deionized water.
3. The material for the wave wall according to claim 1, wherein the preparation method of the graphene oxide aqueous solution comprises the following steps:
putting 70 parts by weight of concentrated sulfuric acid into a reaction vessel in an ice-water bath, adding 3 parts by weight of graphite powder into the concentrated sulfuric acid while stirring, continuing to stir for 10min after the graphite powder is added, then sequentially adding 1.5 parts by weight of sodium nitrate and 9 parts by weight of potassium permanganate into the concentrated sulfuric acid, continuing to stir for 20min, transferring the reaction vessel to an oil bath at 40 ℃, continuing to stir for 1h, dropwise adding 150 parts by weight of deionized water into the reaction vessel, heating the oil bath to 90 ℃, continuing to stir until the solution in the reaction vessel is yellow, stopping heating and cooling to room temperature, then adding 500 parts by weight of deionized water into the reaction vessel, stirring for 30min, adding 20 parts by weight of 30% hydrogen peroxide into the reaction vessel, stirring for 20min, standing for 30h, pouring out a third supernatant in the reaction vessel, and sequentially adding 5% by weight of dilute hydrochloric acid, Washing the lower layer mixture for 2 times by using distilled water, then carrying out centrifugal treatment, collecting a third deposit in a centrifugal tube, dispersing the third deposit in deionized water, and adjusting the concentration of the third deposit to be 0.7mg/mL to obtain the graphene oxide aqueous solution.
4. The material for a wall of claim 3, wherein the cyclodextrin is hydroxypropyl- β -cyclodextrin.
5. The material for a raised wall as claimed in claim 1, wherein the swelling agent is a calcium sulfoaluminate CAS type concrete swelling agent.
6. The material for a retaining wall according to claim 1, wherein the initiator is one of potassium persulfate, sodium persulfate, and lauroyl peroxide.
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| PCT/CN2021/097428 WO2022022050A1 (en) | 2020-07-27 | 2021-05-31 | Material for wave wall |
| ZA2022/04480A ZA202204480B (en) | 2020-07-27 | 2022-04-21 | Material for wave wall |
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| CN112047674B (en) * | 2020-07-27 | 2022-02-11 | 中国港湾工程有限责任公司 | Material for wave wall |
| CN114933844B (en) * | 2022-03-30 | 2023-06-06 | 哈尔滨工程大学 | Preparation method of cyclodextrin modified graphene oxide composite coating |
| CN115259783A (en) * | 2022-06-28 | 2022-11-01 | 江苏苏博特新材料股份有限公司 | High-magnesium low-heat anti-cracking cement for hydraulic large-volume concrete and preparation method thereof |
| CN115340316A (en) * | 2022-09-05 | 2022-11-15 | 新特新材料集团(河南)股份有限公司 | Cavitation erosion resistant and abrasion resistant agent for hydraulic concrete and preparation method thereof |
| CN115353700B (en) * | 2022-09-22 | 2023-08-01 | 浙江智峰科技有限公司 | High-strength nano aerogel building material and preparation method thereof |
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