CN116768554B - Superfine mineral admixture self-compacting high-performance concrete and preparation method thereof - Google Patents

Superfine mineral admixture self-compacting high-performance concrete and preparation method thereof Download PDF

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CN116768554B
CN116768554B CN202310487109.1A CN202310487109A CN116768554B CN 116768554 B CN116768554 B CN 116768554B CN 202310487109 A CN202310487109 A CN 202310487109A CN 116768554 B CN116768554 B CN 116768554B
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罗乃将
朱宝贵
纪小敏
蒋文
孙赛寅
袁乾国
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Yancheng Fuqi Concrete Co ltd
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Abstract

The invention discloses a self-compacting high-performance concrete of an ultrafine mineral admixture and a preparation method thereof, and relates to the technical field of concrete. According to the preparation method, calcium-aluminum layered double hydroxide can be used as an aerogel supporting structure, triethoxysilyl butyraldehyde, 2-amino-4-hydroxy-1, 4-succinic acid and 2, 4-dihydroxyphenethylamine are used for grafting modification, and then the self-made hydrogel is prepared by crosslinking with formaldehyde, so that the viscosity of an aqueous phase system is increased, meanwhile, water molecules are tightly grasped, the water retention effect is achieved, meanwhile, carboxyl groups can be anchored and attached to cement particles, and a benzene ring structure is used, so that the dispersion among cement particles is improved, and a good slump retaining effect is achieved; then pressurizing to promote hydrogel to permeate and wrap recycled aggregate and mineral admixture, reducing pores among materials, converting the hydrogel into aerogel in the curing process, generating micro-expansion effect, filling micro-cracks generated by hardening, and further densifying the concrete.

Description

Superfine mineral admixture self-compacting high-performance concrete and preparation method thereof
Technical Field
The invention relates to the technical field of concrete, in particular to superfine mineral admixture self-compacting high-performance concrete and a preparation method thereof.
Background
The concrete is a mixture which is formed by mixing cementing materials, granular aggregates, water and chemical additives and mineral admixtures which are required to be added according to a proper proportion, or a composite material with a stacking structure is formed after hardening. The existing concrete has high curing strength and good durability, but is easy to cause the problems of bubbles, cavities and the like, and most of the concrete needs to be subjected to vibration compaction operation during grouting. However, in the actual operation process, the concrete has poor vibration compacting effect due to the grouting structure, shape and the like.
An important criterion for measuring the performance of fresh concrete is the workability of the concrete, including the fluidity, cohesiveness and water retention of the concrete, and slump is one of the quantitative indicators for measuring the degree of slump, and is used for judging whether normal construction is possible. For commercial concrete, the mixing plant is typically located at the edge of the city and the concrete is left for a period of time from completion of the mixing to transportation to the site to the start of the construction, which can easily lead to slump loss of the concrete. Meanwhile, the bleeding segregation phenomenon of the concrete is easy to occur, so that the working performance of the concrete is reduced, and the hole knitting rib exposing phenomenon occurs.
Disclosure of Invention
The invention aims to provide a self-compacting high-performance concrete of an ultrafine mineral admixture and a preparation method thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the self-compacting high-performance concrete mainly comprises self-made hydrogel, the superfine mineral admixture, recycled aggregate and cement.
Further, the self-made hydrogel is prepared by calcining calcium oxide and aluminum hydroxide to prepare tricalcium aluminate, then carrying out ion exchange with sodium dodecyl sulfate to prepare calcium aluminum layered double hydroxide, and then carrying out grafting modification by using triethoxysilyl butyraldehyde, 2-amino-4-hydroxy-1, 4-succinic acid and 2, 4-dihydroxyphenethylamine, and then carrying out crosslinking with formaldehyde to prepare the self-made hydrogel.
Further, the preparation method of the self-compacting high-performance concrete by the superfine mineral admixture comprises the following preparation steps:
(1) Mixing sodium dodecyl sulfate and deionized water according to a mass ratio of 1:16.4, adding a sodium hydroxide solution until the pH value of the solution is 10-12, adding tricalcium aluminate with the mass of 0.2-0.3 times that of the sodium dodecyl sulfate, sealing in a nitrogen atmosphere, placing in a water bath with the temperature of 20-30 ℃, performing ultrasonic treatment for 10-12 hours at 400-500W, placing in a water bath with the temperature of 65 ℃, and aging for 24 hours to obtain a calcium aluminum layered double hydroxide solution;
(2) Pretreating the calcium-aluminum layered double hydroxide solution to obtain a pretreated layered product; mixing methanol, 2-amino-4-hydroxy-1, 4-succinic acid, triethylamine and a pretreated lamellar material according to the mass ratio of 10:0.4:1:0.4-14:0.6:1:0.4, stirring for 30min at 100-200 rpm, reacting for 50-70 min at room temperature, cooling to 10-15 ℃, adding sodium borohydride with the mass of 0.1 times of the pretreated lamellar material, reacting for 50-70 min at room temperature, adding deionized water with the mass of 80 times of the pretreated lamellar material, continuously stirring for 10min, washing for 3 times by using dichloromethane, suction filtering, and drying for 10h at 60 ℃ to obtain an intermediate A;
(3) Mixing an intermediate A, acetone, 2- (7-aza-benzotriazol) -N, N, N ', N' -tetramethyl urea hexafluorophosphate, triethylamine and 2, 4-dihydroxyphenethylamine according to the mass ratio of 1:28:1.1:2.2:1.2-1:34:1.1:2.2:2.0, stirring for 14-18 h at 80-100 rpm, filtering, adding ethyl acetate with 199 times of the mass of the intermediate A, performing ultrasonic treatment for 20min at 400-500W, washing, and drying at 60 ℃ for 10h to obtain an amidated lamellar compound;
(4) Mixing the amidated lamellar compound and ethyl acetate according to the mass ratio of 1:16-1:20, heating to 50-60 ℃, filtering while the mixture is hot, adding methanesulfonic acid with the mass of 0.2-0.4 times that of the amidated lamellar compound, reacting for 1-2 h, and drying at 80 ℃ for 24h to obtain a modified lamellar compound;
(5) Mixing the modified lamellar matter, formaldehyde, deionized water and anhydrous sodium carbonate, stirring at 100-200 rpm for 30min, and standing in a water bath at 85 ℃ for 5d to obtain self-made hydrogel; placing the self-made hydrogel in ethanol with the mass 2-3 times of that of the self-made hydrogel, standing for 3d, and replacing the ethanol once a day to obtain wet gel;
(6) Mixing the superfine mineral admixture, the recycled aggregate and the wet gel according to the mass ratio of 10:6:20-20:15:40, uniformly stirring, pressurizing to 3-5 MPa, performing ultrasonic treatment for 30min at 400-500W, adding the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid high-efficiency water reducer according to the mass ratio of 30:32:15:1-40:50:30:18:3, and uniformly mixing the fine aggregate and the superfine mineral admixture according to the mass ratio of 30:10-40:20 to obtain the self-compacting high-performance concrete of the superfine mineral admixture.
Further, the preparation method of the tricalcium aluminate in the step (1) comprises the following steps: mixing calcium oxide and aluminum hydroxide according to a mass ratio of 1:0.93, uniformly stirring, tabletting and forming, calcining for 4-5 hours at 1350 ℃, grinding for 5 minutes at 30-50 m/min, tabletting and forming, calcining for 4-5 hours at 1350 ℃, and repeating the process until the color of the product becomes light green, thus obtaining the tricalcium aluminate.
Further, the preparation method of the pretreated layered product in the step (2) comprises the following steps: adding toluene with 7-10 times of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1h, adding hydrochloric acid with 0.01-0.03 time of sodium dodecyl sulfate and 1.5-2.3 times of triethoxysilyl butyraldehyde with the mass fraction of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1h, transferring into a water bath kettle with the temperature of 90 ℃ for reacting for 22-26h, cooling to room temperature, washing with ethanol for 3 times, carrying out suction filtration, washing with deionized water for 3 times, carrying out suction filtration, and drying at the temperature of 65 ℃ for 10h.
Further, the washing in the step (3) comprises the following specific steps: washing with 5% hydrochloric acid for 4 times, deionized water for 1 time, saturated sodium bicarbonate for 3 times, and deionized water for 2 times.
Further, the mass ratio of the modified layered product, formaldehyde, deionized water and anhydrous sodium carbonate in the step (5) is 1:0.4:0.6:0.0005-1:0.6:1.2:0.00.
Further, the preparation method of the superfine mineral admixture in the step (6) comprises the following steps: mixing the fly ash, the blast furnace slag powder, the silica fume and the grinding aid according to the mass ratio of 35:20:30:0.08-45:30:35:0.2, grinding until the volume average diameter D (4, 3) of the particles is 150nm, and preparing the superfine mineral admixture by using the grinding aid with the mass ratio of 12:6:6:3:60-16:10:10:7:70 of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water.
Compared with the prior art, the invention has the following beneficial effects:
Firstly, calcium oxide and aluminum hydroxide are utilized to carry out tabletting and calcination to prepare tricalcium aluminate, an ion exchange method is adopted to obtain calcium aluminum layered double hydroxide intercalated with sodium dodecyl sulfate, the calcium aluminum layered double hydroxide can carry out hydration reaction with calcium sulfate mixed in cement, the calcium aluminum layered double hydroxide can be effectively filled in a hole seam of concrete, and certain expansion occurs along with the progress of the hydration reaction, so that the self-shrinkage of the concrete in the early stage of hardening is prevented, and a compact cement stone structure is formed; then utilizing the silicon-oxygen bond of triethoxy silicon-based butyraldehyde to graft on calcium aluminum layered double hydroxide, reacting aldehyde group with amino of 2-amino-4-hydroxy-1, 4-succinic acid, and generating an amide structure by carboxyl of 2-amino-4-hydroxy-1, 4-succinic acid and amino of 2, 4-dihydroxyphenethylamine, and generating sulfonic acid group after the carbonyl of amide is sulfonated; the calcium-aluminum layered double hydroxide is used as a supporting point and is crosslinked with formaldehyde to form hydrogel, the viscosity of a water phase system is increased through the winding of a molecular chain, meanwhile, groups such as carboxyl, hydroxyl, sulfonic acid group, amide and the like contained in the molecular chain can tightly grasp water molecules to play a role in retaining water, meanwhile, carboxyl can be anchored and attached to cement particles, and the benzene ring structure at the tail end of a long chain is beneficial to improving the dispersion among cement particles, so that the fluidity of slurry is prevented from being influenced by the aggregation of the cement particles, and the agglomeration of the later stage of particles caused by the winding of a long-chain branched chain can be reduced to play a role in retaining slump well.
Secondly, the hydrogel can more effectively permeate into the pores of the recycled aggregate, the mineral admixture and the fly ash under the action of pressure, the surface is uniformly coated, capillary pores and microcracks are filled, meanwhile, the structure of the coated material is round, the pores among the materials are reduced, and the compact structure of the concrete is further improved; then in the curing process, the hydrogel slowly releases water, cracks formed by self shrinkage of the concrete are reduced, the compact structure of the concrete is further improved, the hydrogel, the recycled aggregate, the mineral admixture and the fly ash form aerogel with a three-dimensional network structure along with the reduction of the water, and in the process of transforming the aerogel by the hydrogel, a certain micro-expansion effect is generated, and micro-cracks generated by hardening are filled, so that the purpose of hole sealing is achieved; meanwhile, in addition, the calcium aluminum layered double hydroxide can be used as an aerogel supporting structure, so that the influence on the compactness of concrete caused by shrinkage of the aerogel in the transformation process is prevented.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the following specific test methods of each index of the self-compacting high-performance concrete of the superfine mineral admixture prepared in the following examples:
And (3) water retention: the clotting time test was performed with reference to GB/T50080 for examples of the same quality as for comparative examples.
Slump loss protection: slump tests were performed with reference to DL/T5117 for examples of the same quality as comparative examples.
Self-compaction: concrete prepared in examples and comparative examples was poured into 150 mm. Times.150 mm cube test pieces, which were cured under standard conditions for 28 days, and concrete filling properties and clearance passage properties were measured with reference to CESC 203:203:2006.
Example 1
(1) Mixing calcium oxide and aluminum hydroxide according to a mass ratio of 1:0.93, uniformly stirring, tabletting and forming, calcining at 1350 ℃ for 4 hours, grinding for 5 minutes at 30m/min, tabletting and forming, calcining at 1350 ℃ for 4 hours, and repeating the above processes until the color of the product becomes light green to obtain tricalcium aluminate;
(2) Mixing sodium dodecyl sulfate and deionized water according to a mass ratio of 1:16.4, adding a sodium hydroxide solution until the pH value of the solution is 10, adding tricalcium aluminate with the mass of 0.2 times that of the sodium dodecyl sulfate, sealing in a nitrogen atmosphere, placing in a water bath at 20 ℃, performing 400W ultrasonic treatment for 10 hours, placing in a water bath at 65 ℃, and aging for 24 hours to obtain a calcium aluminum layered double hydroxide solution; adding toluene with the mass of 7 times of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1 hour, adding hydrochloric acid with the mass fraction of 36% and with the mass fraction of 0.01 time of sodium dodecyl sulfate and triethoxy silicon-based butyraldehyde with the mass of 1.5 time of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1 hour, transferring into a water bath kettle with the temperature of 90 ℃, reacting for 22 hours, cooling to room temperature, washing with ethanol for 3 times, carrying out suction filtration, washing with deionized water for 3 times, carrying out suction filtration, and drying at the temperature of 65 ℃ for 10 hours to obtain a pretreated lamellar substance;
(3) Mixing methanol, 2-amino-4-hydroxy-1, 4-succinic acid, triethylamine and a pretreated lamellar material according to the mass ratio of 10:0.4:1:0.4, stirring for 30min at 100rpm, reacting at room temperature for 50min, cooling to 10 ℃, adding sodium borohydride with the mass of 0.1 times of the pretreated lamellar material, reacting at room temperature for 50min, adding deionized water with the mass of 80 times of the pretreated lamellar material, continuously stirring for 10min, washing for 3 times with dichloromethane, suction filtering, and drying at 60 ℃ for 10h to obtain an intermediate A;
(4) Mixing an intermediate A, acetone, 2- (7-aza-benzotriazol) -N, N, N ', N' -tetramethyl urea hexafluorophosphate, triethylamine and 2, 4-dihydroxyphenethylamine according to the mass ratio of 1:28:1.1:2.2:1.2, stirring for 14h at 80rpm, filtering, adding ethyl acetate which is 199 times the mass of the intermediate A, performing ultrasonic treatment for 20min at 400W, washing with hydrochloric acid with the mass fraction of 5% for 4 times, washing with deionized water for 1 time, washing with saturated sodium bicarbonate for 3 times, washing with deionized water for 2 times, and drying at 60 ℃ for 10h to obtain an amidated lamellar compound;
(5) Mixing the amidated lamellar compound and ethyl acetate according to the mass ratio of 1:16, heating to 50 ℃, filtering while the mixture is hot, adding methanesulfonic acid with the mass of 0.2 times that of the amidated lamellar compound, reacting for 1h, and drying at 80 ℃ for 24h to obtain a modified lamellar compound;
(6) Mixing the modified lamellar matter, formaldehyde, deionized water and anhydrous sodium carbonate according to the mass ratio of 1:0.4:0.6:0.0005, stirring at 100rpm for 30min, and standing in a water bath at 85 ℃ for 5d to obtain self-made hydrogel; placing the self-made hydrogel in ethanol with the mass of 2 times of that of the self-made hydrogel, standing for 3d, and replacing the ethanol once a day to obtain wet gel;
(7) Mixing fly ash, blast furnace slag powder, silica fume and grinding aid according to a mass ratio of 35:20:30:0.08, grinding until the volume average diameter D (4, 3) of particles is 150nm, wherein the mass ratio of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water in the grinding aid is 12:6:6:3:60, so as to prepare an ultrafine mineral admixture; mixing the superfine mineral admixture, the recycled aggregate and the wet gel according to the mass ratio of 10:6:20, uniformly stirring, pressurizing to 3MPa, performing 400W ultrasonic treatment for 30min, adding the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid high-efficiency water reducer according to the mass ratio of 30:32:15:6:1, and uniformly mixing the fine aggregate and the superfine mineral admixture according to the mass ratio of 30:10 to obtain the self-compacting high-performance concrete of the superfine mineral admixture.
Example 2
(1) Mixing calcium oxide and aluminum hydroxide according to a mass ratio of 1:0.93, uniformly stirring, tabletting and forming, calcining at 1350 ℃ for 4.5 hours, grinding at 40m/min for 5 minutes, tabletting and forming, calcining at 1350 ℃ for 4.5 hours, and repeating the processes until the color of the product becomes light green to obtain tricalcium aluminate;
(2) Mixing sodium dodecyl sulfate and deionized water according to a mass ratio of 1:16.4, adding a sodium hydroxide solution until the pH value of the solution is 11, adding tricalcium aluminate with the mass of 0.25 times that of the sodium dodecyl sulfate, sealing in a nitrogen atmosphere, placing in a water bath at 25 ℃, performing ultrasonic treatment at 450W for 11 hours, placing in a water bath at 65 ℃, and aging for 24 hours to obtain a calcium aluminum layered double hydroxide solution; adding toluene with the mass of 8.5 times of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1h, adding hydrochloric acid with the mass fraction of 36% and the mass fraction of 1.9 times of sodium dodecyl sulfate into the mixture, continuing to carry out ultrasonic treatment for 1h, transferring the mixture into a water bath kettle with the temperature of 90 ℃ to react for 24h, cooling to room temperature, washing with ethanol for 3 times, carrying out suction filtration, washing with deionized water for 3 times, carrying out suction filtration, and drying at the temperature of 65 ℃ for 10h to obtain a pretreated lamellar substance;
(3) Mixing methanol, 2-amino-4-hydroxy-1, 4-succinic acid, triethylamine and a pretreated lamellar material according to the mass ratio of 12:0.5:1:0.4, stirring for 30min at 150rpm, reacting at room temperature for 60min, cooling to 13 ℃, adding sodium borohydride with the mass of 0.1 times of the pretreated lamellar material, reacting at room temperature for 60min, adding deionized water with the mass of 80 times of the pretreated lamellar material, continuously stirring for 10min, washing for 3 times with dichloromethane, suction filtering, and drying at 60 ℃ for 10h to obtain an intermediate A;
(4) Mixing an intermediate A, acetone, 2- (7-aza-benzotriazol) -N, N, N ', N' -tetramethyl urea hexafluorophosphate, triethylamine and 2, 4-dihydroxyphenethylamine according to the mass ratio of 1:31:1.1:2.2:1.6, stirring for 16h at 90rpm, filtering, adding ethyl acetate which is 199 times of the mass of the intermediate A, performing ultrasonic treatment for 20min at 450W, washing for 4 times by using hydrochloric acid with the mass fraction of 5%, washing for 1 time by using deionized water, washing for 3 times by using saturated sodium bicarbonate, washing for 2 times by using deionized water, and drying for 10h at 60 ℃ to obtain an amidated lamellar compound;
(5) Mixing the amidated lamellar compound and ethyl acetate according to the mass ratio of 1:18, heating to 55 ℃, filtering while the mixture is hot, adding methanesulfonic acid with the mass of 0.3 times that of the amidated lamellar compound, reacting for 1.5h, and drying at 80 ℃ for 24h to obtain a modified lamellar compound;
(6) Mixing the modified lamellar matter, formaldehyde, deionized water and anhydrous sodium carbonate according to the mass ratio of 1:0.5:0.9:0.00125, stirring at 150rpm for 30min, and standing in a water bath at 85 ℃ for 5d to obtain self-made hydrogel; placing the self-made hydrogel in ethanol with the mass 2.5 times of that of the self-made hydrogel, standing for 3d, and replacing the ethanol once a day to obtain wet gel;
(7) Mixing fly ash, blast furnace slag powder, silica fume and grinding aid according to the mass ratio of 40:25:32.5:0.14, grinding until the volume average diameter D (4, 3) of particles is 150nm, wherein the mass ratio of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water in the grinding aid is 14:8:8:5:65, and preparing the superfine mineral admixture; mixing the superfine mineral admixture, the recycled aggregate and the wet gel according to the mass ratio of 15:10.5:30, uniformly stirring, pressurizing to 4MPa, ultrasonically stirring for 30min at 450W, adding the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid high-efficiency water reducer according to the mass ratio of 35:41:22.5:12:2, uniformly mixing the fine aggregate and the superfine mineral admixture according to the mass ratio of 35:15, and obtaining the self-compacting high-performance concrete of the superfine mineral admixture.
Example 3
(1) Mixing calcium oxide and aluminum hydroxide according to a mass ratio of 1:0.93, uniformly stirring, tabletting and forming, calcining at 1350 ℃ for 5 hours, grinding at 50m/min for 5 minutes, tabletting and forming, calcining at 1350 ℃ for 5 hours, and repeating the above processes until the color of the product becomes light green to obtain tricalcium aluminate;
(2) Mixing sodium dodecyl sulfate and deionized water according to a mass ratio of 1:16.4, adding a sodium hydroxide solution until the pH value of the solution is 12, adding tricalcium aluminate with the mass of 0.3 times that of the sodium dodecyl sulfate, sealing in a nitrogen atmosphere, placing in a water bath at 30 ℃ for 12 hours by ultrasonic treatment at 500W, placing in a water bath at 65 ℃ for aging for 24 hours to obtain a calcium aluminum layered double hydroxide solution; adding toluene with 10 times of the mass of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1 hour, adding hydrochloric acid with the mass fraction of 36% and with the mass fraction of 0.03 times of the mass of sodium dodecyl sulfate and triethoxy silicon-based butyraldehyde with the mass fraction of 2.3 times of the mass of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1 hour, transferring into a water bath kettle with 90 ℃ to react for 26 hours, cooling to room temperature, washing with ethanol for 3 times, carrying out suction filtration, washing with deionized water for 3 times, carrying out suction filtration, and drying at 65 ℃ for 10 hours to obtain a pretreated lamellar product;
(3) Mixing methanol, 2-amino-4-hydroxy-1, 4-succinic acid, triethylamine and a pretreated lamellar material according to the mass ratio of 14:0.6:1:0.4, stirring for 30min at 200rpm, reacting at room temperature for 70min, cooling to 15 ℃, adding sodium borohydride with the mass of 0.1 times of the pretreated lamellar material, reacting at room temperature for 70min, adding deionized water with the mass of 80 times of the pretreated lamellar material, continuously stirring for 10min, washing for 3 times with dichloromethane, suction filtering, and drying at 60 ℃ for 10h to obtain an intermediate A;
(4) Mixing an intermediate A, acetone, 2- (7-aza-benzotriazol) -N, N, N ', N' -tetramethyl urea hexafluorophosphate, triethylamine and 2, 4-dihydroxyphenethylamine according to the mass ratio of 1:34:1.1:2.2:2, stirring for 18h at 100rpm, filtering, adding ethyl acetate which is 199 times of the mass of the intermediate A, performing ultrasonic treatment for 20min at 500W, washing for 4 times by using hydrochloric acid with the mass fraction of 5%, washing for 1 time by using deionized water, washing for 3 times by using saturated sodium bicarbonate, washing for 2 times by using deionized water, and drying for 10h at 60 ℃ to obtain an amidated lamellar compound;
(5) Mixing the amidated lamellar compound and ethyl acetate according to the mass ratio of 1:20, heating to 60 ℃, filtering while the mixture is hot, adding methanesulfonic acid with the mass of 0.4 times that of the amidated lamellar compound, reacting for 2 hours, and drying at 80 ℃ for 24 hours to obtain a modified lamellar compound;
(6) Mixing the modified lamellar matter, formaldehyde, deionized water and anhydrous sodium carbonate according to the mass ratio of 1:0.6:1.2:0.002, stirring at 200rpm for 30min, and standing in a water bath at 85 ℃ for 5d to obtain self-made hydrogel; placing the self-made hydrogel in ethanol with the mass 3 times of that of the self-made hydrogel, standing for 3d, and replacing the ethanol once a day to obtain wet gel;
(7) Mixing fly ash, blast furnace slag powder, silica fume and grinding aid according to the mass ratio of 45:30:35:0.2, grinding until the volume average diameter D (4, 3) of particles is 150nm, wherein the mass ratio of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water in the grinding aid is 16:10:10:7:70, so as to prepare an ultrafine mineral admixture; mixing the superfine mineral admixture, the recycled aggregate and the wet gel according to the mass ratio of 20:15:40, uniformly stirring, pressurizing to 5MPa, ultrasonically treating for 30min by 500W, adding the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid high-efficiency water reducer according to the mass ratio of 40:50:30:18:3, and uniformly mixing the fine aggregate and the superfine mineral admixture according to the mass ratio of 40:20 to obtain the self-compacting high-performance concrete of the superfine mineral admixture.
Comparative example 1
Comparative example 1 differs from example 2 in that there are no steps (1), (2), step (3) being changed to: mixing methanol, 2-amino-4-hydroxy-1, 4-succinic acid, triethylamine and triethoxysilyl butyraldehyde according to a mass ratio of 12:0.5:1:0.4, stirring for 30min at 150rpm, reacting at room temperature for 60min, cooling to 13 ℃, adding sodium borohydride with the mass of 0.1 times that of the triethoxysilyl butyraldehyde, reacting at room temperature for 60min, adding deionized water with the mass of 80 times that of the triethoxysilyl butyraldehyde, continuously stirring for 10min, washing for 3 times with dichloromethane, suction filtering, and drying at 60 ℃ for 10h to obtain an intermediate A. The rest of the procedure is the same as in example 2.
Comparative example 2
Comparative example 2 differs from example 2 in that steps (3), (4) are not present, and step (5) is changed to: mixing the pretreated lamellar material and ethyl acetate according to the mass ratio of 1:18, heating to 55 ℃, filtering while the mixture is hot, adding methanesulfonic acid with the mass of 0.3 times that of the pretreated lamellar material, reacting for 1.5h, and drying at 80 ℃ for 24h to obtain the modified lamellar material. The rest of the procedure is the same as in example 2.
Comparative example 3
Comparative example 3 differs from example 2 in that there is no step (5), step (6) is changed to: mixing the amidated lamellar compound, formaldehyde, deionized water and anhydrous sodium carbonate according to the mass ratio of 1:0.5:0.9:0.00125, stirring at 150rpm for 30min, and standing in a water bath at 85 ℃ for 5d to obtain self-made hydrogel; placing the self-made hydrogel in ethanol with the mass of 2.5 times of that of the self-made hydrogel, standing for 3d, and replacing the ethanol once a day to obtain wet gel. The rest of the procedure is the same as in example 2.
Comparative example 4
Comparative example 4 differs from example 2 in that step (7) was changed to: mixing fly ash, blast furnace slag powder, silica fume and grinding aid according to the mass ratio of 40:25:32.5:0.14, grinding until the volume average diameter D (4, 3) of particles is 150nm, wherein the mass ratio of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water in the grinding aid is 14:8:8:5:65, and preparing the superfine mineral admixture; and mixing the superfine mineral admixture, the recycled aggregate, the wet gel, the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid in a mass ratio of 15:10.5:30:35:41:22.5:12:2, and uniformly mixing to obtain the self-compacting high-performance concrete of the superfine mineral admixture. The rest of the procedure is the same as in example 2.
Comparative example 5
Comparative example 5 differs from example 2 in that step (7) was changed to: placing wet gel at room temperature for 1d,50 ℃ for 1d,110 ℃ for 12h, and performing aerogel; mixing fly ash, blast furnace slag powder, silica fume and grinding aid according to the mass ratio of 40:25:32.5:0.14, grinding until the volume average diameter D (4, 3) of particles is 150nm, wherein the mass ratio of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water in the grinding aid is 14:8:8:5:65, and preparing the superfine mineral admixture; and mixing the superfine mineral admixture, the recycled aggregate, the aerogel, the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid in a mass ratio of 15:10.5:30:35:41:22.5:12:2, and uniformly mixing to obtain the self-compacting high-performance concrete of the superfine mineral admixture. The rest of the procedure is the same as in example 2.
Effect example
The results of the performance analysis of the self-compacting high performance concrete using the ultra-fine mineral blends of examples 1 to 3 and comparative examples 1 to 5 of the present invention are given in table 1 below.
TABLE 1
As can be found from the comparison of experimental data of examples and comparative examples, the calcium-aluminum layered double hydroxide can be used as an aerogel supporting structure, triethoxysilyl butyraldehyde, 2-amino-4-hydroxy-1, 4-succinic acid and 2, 4-dihydroxyphenethylamine are used for grafting modification, and then the self-made hydrogel is prepared by crosslinking with formaldehyde, so that the viscosity of an aqueous phase system is increased, meanwhile, water molecules are tightly grasped, the water retention effect is achieved, meanwhile, carboxyl can be used for anchoring and attaching to cement particles, and the benzene ring structure at the tail end of a long chain is beneficial to improving the dispersion among cement particles, and the good slump retention effect is achieved; then pressurizing to promote the hydrogel to infiltrate and wrap the recycled aggregate and the mineral admixture, so that the pores among the materials are reduced, and the compact structure of the concrete is further improved; then in the curing process, the hydrogel slowly releases water, cracks formed by self shrinkage of the concrete are reduced, the compact structure of the concrete is further improved, the hydrogel, the recycled aggregate, the mineral admixture and the fly ash form aerogel with a three-dimensional network structure along with the reduction of the water, and in the process of transforming the aerogel by the hydrogel, a certain micro-expansion effect is generated, and micro-cracks generated by hardening are filled, so that the purpose of hole sealing is achieved; in addition, the calcium-aluminum layered double hydroxide can generate hydration reaction with calcium sulfate mixed in cement, so that the calcium-aluminum layered double hydroxide is effectively filled in the gaps of the concrete, and the concrete is further densified.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (4)

1. The preparation method of the self-compacting high-performance concrete by using the superfine mineral admixture is characterized by comprising the following preparation steps of:
(1) Mixing calcium oxide and aluminum hydroxide according to a mass ratio of 1:0.93, uniformly stirring, tabletting and forming, calcining at 1350 ℃ for 4-5 hours, grinding for 5 minutes at 30-50 m/min, tabletting and forming, calcining at 1350 ℃ for 4-5 hours, and repeating the above processes until the color of the product becomes light green, thus obtaining tricalcium aluminate; mixing sodium dodecyl sulfate and deionized water according to a mass ratio of 1:16.4, adding a sodium hydroxide solution until the pH value of the solution is 10-12, adding tricalcium aluminate with the mass of 0.2-0.3 times that of the sodium dodecyl sulfate, sealing in a nitrogen atmosphere, placing in a water bath with the temperature of 20-30 ℃, performing ultrasonic treatment for 10-12 hours at 400-500W, placing in a water bath with the temperature of 65 ℃, and aging for 24 hours to obtain a calcium aluminum layered double hydroxide solution;
(2) Pretreating the calcium-aluminum layered double hydroxide solution to obtain a pretreated layered product; mixing methanol, 2-amino-4-hydroxy-1, 4-succinic acid, triethylamine and a pretreated lamellar substance according to the mass ratio of 10:0.4:1:0.4-14:0.6:1:0.4, stirring for 30min at 100-200 rpm, reacting for 50-70 min at room temperature, cooling to 10-15 ℃, adding sodium borohydride with the mass of 0.1 times of the pretreated lamellar substance, reacting for 50-70 min at room temperature, adding deionized water with the mass of 80 times of the pretreated lamellar substance, continuously stirring for 10min, washing for 3 times by using dichloromethane, suction filtering, and drying for 10h at 60 ℃ to obtain an intermediate A; the preparation method of the pretreated lamellar substance comprises the following steps: adding toluene with 7-10 times of the mass of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1h, adding hydrochloric acid with the mass fraction of 0.01-0.03 times of the mass fraction of sodium dodecyl sulfate being 36% and triethoxysilyl butyraldehyde with the mass fraction of 1.5-2.3 times of the mass fraction of sodium dodecyl sulfate, continuing to carry out ultrasonic treatment for 1h, transferring into a water bath kettle with the temperature of 90 ℃, reacting for 22-26 h, cooling to room temperature, washing with ethanol for 3 times, carrying out suction filtration, washing with deionized water for 3 times, carrying out suction filtration, and drying at the temperature of 65 ℃ for 10h;
(3) Mixing an intermediate A, acetone, 2- (7-aza-benzotriazole) -N, N, N ', N' -tetramethyl urea hexafluorophosphate, triethylamine and 2, 4-dihydroxyphenethylamine according to a mass ratio of 1:28:1.1:2.2:1.2-1:34:1.1:2.2:2.0, stirring at 80-100 rpm for 14-18 h, filtering, adding ethyl acetate with 199 times of the mass of the intermediate A, performing ultrasonic treatment for 20min at 400-500W, washing, and drying at 60 ℃ for 10h to obtain an amidated lamellar substance;
(4) Mixing the amidated lamellar compound and ethyl acetate according to the mass ratio of 1:16-1:20, heating to 50-60 ℃, filtering while the mixture is hot, adding methanesulfonic acid with the mass of 0.2-0.4 times that of the amidated lamellar compound, reacting for 1-2 h, and drying at 80 ℃ for 24h to obtain a modified lamellar compound;
(5) Mixing the modified lamellar matter, formaldehyde, deionized water and anhydrous sodium carbonate, stirring at 100-200 rpm for 30min, and standing in a water bath at 85 ℃ for 5d to obtain self-made hydrogel; placing the self-made hydrogel in ethanol with the mass 2-3 times of that of the self-made hydrogel, standing for 3d, and replacing the ethanol once a day to obtain wet gel;
(6) Mixing the superfine mineral admixture, the recycled aggregate and the wet gel according to the mass ratio of 10:6:20-20:15:40, uniformly stirring, pressurizing to 3-5 MPa, performing 400-500W ultrasonic treatment for 30min, adding the fine aggregate, the coarse aggregate, the cement, the water and the polycarboxylic acid high-efficiency water reducer according to the mass ratio of 30:32:15:1-40:50:30:18:3, and uniformly mixing the fine aggregate and the superfine mineral admixture according to the mass ratio of 30:10-40:20 to obtain the self-compacting high-performance concrete of the superfine mineral admixture.
2. The method for preparing the self-compacting high-performance concrete by using the superfine mineral admixture according to claim 1, wherein the specific washing step in the step (3) is as follows: washing with 5% hydrochloric acid for 4 times, deionized water for 1 time, saturated sodium bicarbonate for 3 times, and deionized water for 2 times.
3. The method for preparing the self-compacting high-performance concrete by using the superfine mineral admixture according to claim 1, wherein the mass ratio of the modified layered product, formaldehyde, deionized water and anhydrous sodium carbonate in the step (5) is 1:0.4:0.6:0.0005-1:0.6:1.2:0.002.
4. The method for preparing the self-compacting high-performance concrete by using the superfine mineral admixture according to claim 1, wherein the preparation method of the superfine mineral admixture in the step (6) is as follows: mixing the fly ash, the blast furnace slag powder, the silica fume and the grinding aid according to the mass ratio of 35:20:30:0.08-45:30:35:0.2, grinding until the volume average diameter D (4, 3) of the particles is 150nm, and preparing the superfine mineral admixture by using the grinding aid with the mass ratio of 12:6:6:3:60-16:10:10:7:70 of diethanol monoisopropanolamine, glycerol, sodium tripolyphosphate, polyvinylpyrrolidone and deionized water.
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