CN115073075A - Super-long structure high-crack-resistance compensation shrinkage concrete and preparation method thereof - Google Patents
Super-long structure high-crack-resistance compensation shrinkage concrete and preparation method thereof Download PDFInfo
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- CN115073075A CN115073075A CN202210504221.7A CN202210504221A CN115073075A CN 115073075 A CN115073075 A CN 115073075A CN 202210504221 A CN202210504221 A CN 202210504221A CN 115073075 A CN115073075 A CN 115073075A
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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
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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
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
-
- 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
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The application relates to the technical field of concrete, and particularly discloses ultralong structure high anti-cracking compensation shrinkage concrete and a preparation method thereof, wherein the ultralong structure high anti-cracking compensation shrinkage concrete comprises the following components in parts by weight: 140 portions of cement and 180 portions of cement; 60-100 parts of fly ash; 70-100 parts of mineral powder; 800 portions of sand and 1000 portions of sand; 800 portions of gravel and 1000 portions of gravel; 20-50 parts of an expanding agent; 12-16 parts of a water reducing agent; 1-3 parts of a hydration heat inhibitor; 150 portions of water and 170 portions of water; 2-6 parts of modified phase-change microcapsules. The ultra-long structure high-crack-resistance compensation shrinkage concrete can be used for an ultra-long concrete structure, and the expanding agent can generate certain limited expansion to compensate the shrinkage of the concrete and improve the crack resistance of the concrete; the concrete has the advantage of reducing temperature-dependent cracks without reducing the compressive strength of the concrete.
Description
Technical Field
The invention relates to the technical field of concrete, in particular to super-long structure high crack resistance compensation shrinkage concrete and a preparation method thereof.
Background
Concrete is one of the most important civil engineering materials of the present generation. The artificial stone is prepared by a cementing material, granular aggregate (also called aggregate), water, an additive and an admixture which are added if necessary according to a certain proportion, and is formed by uniformly stirring, compacting, forming, curing and hardening. Along with the massive construction of super-long concrete structures such as large-scale terminal buildings in China, the engineering application of continuous non-seam-structure construction is increasing day by day.
The related technology discloses concrete which comprises the following raw materials in parts by weight: 140 portions of cement and 180 portions of cement; 60-100 parts of fly ash; 70-100 parts of mineral powder; 800 portions of sand and 1000 portions of sand; 800 portions of gravel and 1000 portions of gravel; 12-16 parts of a water reducing agent; 150 portions of water and 170 portions of water.
In view of the above-mentioned related art, the inventors believe that the above-mentioned concrete is likely to crack at an early stage due to the hydration heat of the concrete, and also cracks are generated due to the change in the environmental temperature after curing.
Disclosure of Invention
In order to reduce cracks of concrete caused by temperature change, the application provides the high-crack-resistance compensation shrinkage concrete with the ultralong structure and the preparation method thereof.
In a first aspect, the application provides a high crack resistance compensation shrinkage concrete with an ultralong structure, which adopts the following technical scheme:
the super-long structure high-crack-resistance compensation shrinkage concrete comprises the following raw materials in parts by weight:
140 portions of cement and 180 portions of cement;
60-100 parts of fly ash;
70-100 parts of mineral powder;
800 portions of sand and 1000 portions of sand;
800 portions of gravel and 1000 portions of gravel;
20-50 parts of an expanding agent;
12-16 parts of a water reducing agent;
1-3 parts of a hydration heat inhibitor;
150 portions of water and 170 portions of water;
2-6 parts of modified phase change microcapsules;
the preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, mixing paraffin and water, heating until the paraffin is completely melted, adding a compound emulsifier, uniformly mixing, and emulsifying to obtain a paraffin emulsion;
loading, namely uniformly mixing the paraffin emulsion and the zeolite, preserving heat, filtering and drying to obtain the paraffin-loaded zeolite;
preparing a graphene aqueous dispersion, dispersing graphene oxide in water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, adjusting the pH value to be alkalescent, uniformly mixing, adding ethylenediamine, mixing, performing heating reaction, washing, performing freeze drying to obtain modified graphene, mixing the modified graphene with a strong-acid aqueous solution, and performing ultrasonic treatment to obtain the graphene aqueous dispersion;
preparing a graphene phase-change microcapsule, adding zeolite loaded with paraffin into graphene aqueous dispersion, uniformly mixing, washing and drying to obtain the graphene phase-change microcapsule;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing melamine, a urea solution, a formaldehyde solution and water, adding triethanolamine, adjusting the pH value to be alkalescent, and heating for reaction to obtain the urea-formaldehyde resin prepolymer;
preparing a modified phase-change microcapsule, adding the graphene phase-change microcapsule into the urea resin prepolymer, uniformly mixing, heating for reaction, filtering, washing and drying to obtain the modified phase-change microcapsule.
By adopting the technical scheme, as the zeolite is adopted to load the paraffin, a part of the paraffin can enter the micropores in the zeolite, and a part of the paraffin is attached to the surface of the zeolite, the zeolite can improve the structural strength of the modified phase-change microcapsule and can also improve the heat conductivity coefficient of the modified phase-change microcapsule; when graphene is modified, ethylenediamine reduces graphene oxide to graft an amino group on the surface of graphene, the amino group is protonated with hydrogen ions under a strong acid condition, and the surface of graphene is positively charged, so that the graphene is beneficial to being coated on the surface of paraffin subsequently; because there is the space between graphite alkene lamella and the lamella, paraffin probably flows out from the gap in the melting process of being heated, leads to the phase transition enthalpy to reduce, this application adopts urea-formaldehyde resin to wrap up the surface at modified graphite alkene, has filled the gap between graphite alkene lamella, has improved the closely knit degree of modified phase transition microcapsule wall material, has reduced the gap of wall material, improves circulation stability, and urea-formaldehyde resin has certain negative effect to the coefficient of heat conductivity of modified phase transition microcapsule, but still satisfies the requirement of application. After the modified phase-change microcapsule is added into concrete, the compressive strength of the concrete is not reduced basically, the heating and cooling rates of the concrete are reduced, and cracks of the concrete caused by temperature change are reduced.
The expanding agent can generate certain limited expansion, compensate the shrinkage of concrete and improve the anti-cracking performance of the concrete.
Optionally, the mass ratio of the compound emulsifier to the paraffin is 1 (10-15), the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: (1-1.2).
By adopting the technical scheme, the compounded emulsifier can fully emulsify the paraffin to obtain stable paraffin emulsion, so that the surface of the stable paraffin emulsion has negative charges, and the formation of microcapsules is facilitated.
Optionally, the mass ratio of the paraffin to the zeolite is 1: (1.5-2).
By adopting the technical scheme, the paraffin is too little, and the heat storage capacity of the modified phase-change microcapsule is reduced; too much paraffin is added, the heat conductivity coefficient of the modified phase-change microcapsule is lower, and the structural strength is lower.
Optionally, the particle size of the zeolite is 250-350 nm.
By adopting the technical scheme, the zeolite with proper particle size is beneficial to loading paraffin and forming microcapsules.
Optionally, in the step of preparing the graphene aqueous dispersion, the graphene aqueous dispersion is heated to 70-75 ℃ and reacted for 10-12 h.
By adopting the technical scheme, the reduction of graphene oxide by ethylenediamine is facilitated, and amido is grafted on the surface of graphene.
Optionally, in the step of preparing the graphene phase change microcapsule, the mass ratio of the modified graphene to the paraffin is (0.5-0.8): 10.
by adopting the technical scheme, the modified graphene is too small in dosage, paraffin is difficult to completely wrap, and the heat conductivity coefficient is low; the modified graphene is used in a large amount, so that although the thermal conductivity is increased, the cost is greatly increased.
Optionally, in the step of preparing the urea-formaldehyde resin prepolymer, the pH is adjusted to 8-9.
Through adopting above-mentioned technical scheme, be favorable to urea-formaldehyde resin reaction and parcel graphite alkene.
Optionally, in the step of preparing the modified phase-change microcapsule, the phase-change microcapsule is uniformly mixed at 800rpm and 300 ℃.
By adopting the technical scheme, the rotating speed is too small, the wall material is not favorable for wrapping the graphene phase change microcapsules, and the rotating speed is too large, so that the size of the modified phase change microcapsules is reduced.
Optionally, the water in the ultra-long structure high crack resistance compensation shrinkage concrete raw material is micro-nano bubble water.
By adopting the technical scheme, the workability and durability of concrete can be improved by the micro-nano bubble water.
In a second aspect, the application provides a preparation method of the ultra-long structure high crack resistance compensation shrinkage concrete, which adopts the following technical scheme:
a preparation method of the ultra-long structure high crack resistance compensation shrinkage concrete comprises the following steps:
uniformly mixing cement, fly ash, mineral powder, a swelling agent and the modified phase-change microcapsules, adding part of water, and uniformly mixing to obtain a cementing material;
adding sand and gravel into the cementing material, and uniformly mixing to obtain an aggregate mixture;
step three, uniformly mixing the water reducing agent, the hydration heat inhibitor and the other part of water to obtain an additive mixture;
and step four, uniformly mixing the admixture mixture and the aggregate mixture to obtain the ultra-long structure high crack resistance compensation shrinkage concrete.
By adopting the technical scheme, after the modified phase-change microcapsule is added into concrete, the compressive strength of the concrete is not reduced basically, the heating and cooling rates of the concrete are reduced, and cracks of the concrete caused by temperature change are reduced.
In summary, the present application has the following beneficial effects:
1. because the modified phase-change microcapsules are added into the concrete, the cracks caused by hydration heat are reduced, the heating and cooling rates of the concrete are reduced, and the cracks caused by temperature change of the concrete are reduced.
2. In the application, the zeolite is adopted to load the paraffin, so that the zeolite can improve the structural strength of the modified phase-change microcapsule and can also improve the heat conductivity coefficient of the modified phase-change microcapsule; the urea-formaldehyde resin is wrapped on the surface of the modified graphene, so that gaps among graphene sheets are filled, the gaps of wall materials are reduced, and the circulation stability is improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of modified phase-Change microcapsule
Preparation example 1
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing 10kg of paraffin and 20L of water, heating until the paraffin is No. 60 paraffin and is completely melted, adding a compound emulsifier, wherein the mass ratio of the compound emulsifier to the paraffin is 1:10, the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: stirring at 1,1200 rpm for 2h, and emulsifying to obtain paraffin emulsion; loading, namely uniformly mixing the paraffin emulsion and zeolite, wherein the particle size of the zeolite is 250 nanometers, the mass ratio of the paraffin to the zeolite is 1:1.5, keeping the temperature at 60 ℃ for 2 hours, filtering and drying to obtain the paraffin-loaded zeolite;
preparing graphene aqueous dispersion, dispersing 0.3kg of graphene oxide in 300L of water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, dropwise adding ammonia water to adjust the pH value to 9, uniformly mixing, adding 180ml of ethylenediamine, uniformly mixing, heating to 70 ℃, reacting for 12 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, performing freeze drying for 48 hours to obtain modified graphene, mixing 0.5kg of modified graphene with deionized water with the pH value of 1, and performing ultrasonic treatment for 1 hour to obtain the graphene aqueous dispersion;
preparing a graphene phase-change microcapsule, adding zeolite loaded with paraffin into graphene water dispersion, stirring for 2 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, and drying to obtain the graphene phase-change microcapsule;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing 2kg of melamine, 4kg of urea solution with the mass concentration of 95%, 40kg of formaldehyde solution with the mass concentration of 37% and 20kg of water, adding triethanolamine, adjusting the pH value to 8, heating to 70 ℃, and reacting for 1h at 400rpm to obtain the urea-formaldehyde resin prepolymer;
preparing a modified phase-change microcapsule, adding the graphene phase-change microcapsule into the urea resin prepolymer, uniformly stirring at 300rpm, heating to 60 ℃, reacting for 1h, filtering, washing and drying to obtain the modified phase-change microcapsule.
Preparation example 2
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, mixing 10kg of paraffin wax and 20L of water, wherein the paraffin wax is No. 60 paraffin wax, heating until the paraffin wax is completely melted, adding a compound emulsifier, and the mass ratio of the compound emulsifier to the paraffin wax is 1:12, wherein the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: 1.1, stirring at 1200rpm for 2h, and emulsifying to obtain paraffin emulsion; loading, namely uniformly mixing the paraffin emulsion and zeolite, wherein the particle size of the zeolite is 300 nanometers, the mass ratio of the paraffin to the zeolite is 1:1.8, keeping the temperature at 60 ℃ for 2 hours, filtering and drying to obtain the paraffin-loaded zeolite;
preparing graphene aqueous dispersion, dispersing 0.3kg of graphene oxide in 300L of water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, dropwise adding ammonia water to adjust the pH value to 9.5, uniformly mixing, adding 180ml of ethylenediamine, uniformly mixing, heating to 72 ℃, reacting for 11 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, performing freeze drying for 48 hours to obtain modified graphene, mixing 0.5kg of modified graphene with deionized water with the pH value of 1, and performing ultrasonic treatment for 1 hour to obtain the graphene aqueous dispersion;
preparing graphene phase change microcapsules, adding zeolite loaded with paraffin into graphene aqueous dispersion, stirring for 2 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, and drying to obtain the graphene phase change microcapsules;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing 2kg of melamine, 4kg of urea solution with the mass concentration of 95%, 40kg of formaldehyde solution with the mass concentration of 37% and 20kg of water, adding triethanolamine, adjusting the pH to 8.5, heating to 70 ℃, and reacting for 1h at 400rpm to obtain the urea-formaldehyde resin prepolymer;
preparing a modified phase-change microcapsule, adding the graphene phase-change microcapsule into the urea resin prepolymer, uniformly stirring at 300rpm, heating to 60 ℃, reacting for 1h, filtering, washing and drying to obtain the modified phase-change microcapsule.
Preparation example 3
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing 10kg of paraffin and 20L of water, heating until the paraffin is No. 60 paraffin and is completely melted, adding a compound emulsifier, wherein the mass ratio of the compound emulsifier to the paraffin is 1:15, the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: 1.2, stirring at 1200rpm for 2h, and emulsifying to obtain paraffin emulsion; loading, namely uniformly mixing the paraffin emulsion and zeolite, wherein the particle size of the zeolite is 350 nanometers, the mass ratio of the paraffin to the zeolite is 1:2, keeping the temperature at 60 ℃ for 2 hours, filtering and drying to obtain the paraffin-loaded zeolite;
preparing graphene aqueous dispersion, dispersing 0.3kg of graphene oxide in 300L of water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, dropwise adding ammonia water to adjust the pH value to 10, uniformly mixing, adding 180ml of ethylenediamine, uniformly mixing, heating to 75 ℃ to react for 10 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, performing freeze drying for 48 hours to obtain modified graphene, mixing 0.5kg of modified graphene with deionized water with the pH value of 1, and performing ultrasonic treatment for 1 hour to obtain the graphene aqueous dispersion;
preparing graphene phase change microcapsules, adding zeolite loaded with paraffin into graphene aqueous dispersion, stirring for 2 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, and drying to obtain the graphene phase change microcapsules;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing 2kg of melamine, 4kg of urea solution with the mass concentration of 95%, 40kg of formaldehyde solution with the mass concentration of 37% and 20kg of water, adding triethanolamine, adjusting the pH value to 9, heating to 70 ℃, and reacting for 1h at 400rpm to obtain the urea-formaldehyde resin prepolymer;
preparing a modified phase-change microcapsule, adding the graphene phase-change microcapsule into the urea resin prepolymer, uniformly stirring at 300rpm, heating to 60 ℃, reacting for 1h, filtering, washing and drying to obtain the modified phase-change microcapsule.
Preparation example 4
The modified phase change microcapsule is different from preparation example 2 in that 0.6kg of modified graphene is mixed with deionized water having a pH of 1 in the step of preparing the graphene aqueous dispersion.
Preparation example 5
The modified phase change microcapsule is different from preparation example 2 in that 0.8kg of modified graphene is mixed with deionized water having a pH of 1 in the step of preparing the graphene aqueous dispersion.
Preparation example 6
The modified phase change microcapsule is different from preparation example 2 in that 0.1kg of modified graphene is mixed with deionized water having a pH of 1 in the step of preparing the graphene aqueous dispersion.
Preparation example 7
The modified phase change microcapsule is different from preparation example 2 in that, in the step of preparing the graphene aqueous dispersion, 1.5kg of modified graphene is mixed with deionized water having a pH of 1.
Preparation example 8
The modified phase-change microcapsule is different from preparation example 4 in that in the step of preparing the modified phase-change microcapsule, the phase-change microcapsule is uniformly mixed at 500 rpm.
Preparation example 9
The modified phase-change microcapsule is different from preparation example 4 in that in the step of preparing the modified phase-change microcapsule, the phase-change microcapsule is uniformly mixed at 800 rpm.
Preparation example 10
The modified phase-change microcapsule is different from preparation example 4 in that in the step of preparing the modified phase-change microcapsule, the phase-change microcapsule is uniformly mixed at 100 rpm.
Preparation example 11
The modified phase-change microcapsule is different from preparation example 4 in that in the step of preparing the modified phase-change microcapsule, the phase-change microcapsule is uniformly mixed at 1500 rpm.
Comparative preparation example 1
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing 10kg of paraffin and 20L of water, heating until the paraffin is No. 60 paraffin and is completely melted, adding a compound emulsifier, wherein the mass ratio of the compound emulsifier to the paraffin is 1:12, the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: 1.1, stirring at 1200rpm for 2h, and emulsifying to obtain paraffin emulsion;
preparing graphene aqueous dispersion, dispersing 0.3kg of graphene oxide in 300L of water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, dropwise adding ammonia water to adjust the pH value to 9.5, uniformly mixing, adding 180ml of ethylenediamine, uniformly mixing, heating to 72 ℃, reacting for 11 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, performing freeze drying for 48 hours to obtain modified graphene, mixing 0.5kg of modified graphene with deionized water with the pH value of 1, and performing ultrasonic treatment for 1 hour to obtain the graphene aqueous dispersion;
preparing the graphene phase change microcapsule, adding the paraffin emulsion into the graphene aqueous dispersion, stirring for 2 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, and drying to obtain the modified phase change microcapsule.
Comparative preparation example 2
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing 10kg of paraffin and 20L of water, heating until the paraffin is No. 60 paraffin and is completely melted, adding a compound emulsifier, wherein the mass ratio of the compound emulsifier to the paraffin is 1:12, the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: 1.1, stirring at 1200rpm for 2h, and emulsifying to obtain paraffin emulsion;
preparing graphene aqueous dispersion, dispersing 0.3kg of graphene oxide in 300L of water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, dropwise adding ammonia water to adjust the pH value to 9.5, uniformly mixing, adding 180ml of ethylenediamine, uniformly mixing, heating to 72 ℃, reacting for 11 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, performing freeze drying for 48 hours to obtain modified graphene, mixing 0.5kg of modified graphene with deionized water with the pH value of 1, and performing ultrasonic treatment for 1 hour to obtain the graphene aqueous dispersion;
preparing a graphene phase-change microcapsule, adding a paraffin emulsion into a graphene aqueous dispersion, stirring for 2 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, and drying to obtain the graphene phase-change microcapsule;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing 2kg of melamine, 4kg of urea solution with the mass concentration of 95%, 40kg of formaldehyde solution with the mass concentration of 37% and 20kg of water, adding triethanolamine, adjusting the pH to 8.5, heating to 70 ℃, and reacting for 1h at 400rpm to obtain the urea-formaldehyde resin prepolymer;
preparing a modified phase-change microcapsule, adding the graphene phase-change microcapsule into the urea resin prepolymer, uniformly stirring at 300rpm, heating to 60 ℃, reacting for 1h, filtering, washing and drying to obtain the modified phase-change microcapsule.
Comparative preparation example 3
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing 10kg of paraffin and 20L of water, heating until the paraffin is No. 60 paraffin and is completely melted, adding a compound emulsifier, wherein the mass ratio of the compound emulsifier to the paraffin is 1:12, the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: 1.1, stirring at 1200rpm for 2h, and emulsifying to obtain paraffin emulsion; loading, namely uniformly mixing the paraffin emulsion and zeolite, wherein the particle size of the zeolite is 300 nanometers, the mass ratio of the paraffin to the zeolite is 1:1.8, keeping the temperature at 60 ℃ for 2 hours, filtering and drying to obtain the paraffin-loaded zeolite;
preparing graphene aqueous dispersion, dispersing 0.3kg of graphene oxide in 300L of water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, dropwise adding ammonia water to adjust the pH value to 9.5, uniformly mixing, adding 180ml of ethylenediamine, uniformly mixing, heating to 72 ℃, reacting for 11 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, performing freeze drying for 48 hours to obtain modified graphene, mixing 0.5kg of modified graphene with deionized water with the pH value of 1, and performing ultrasonic treatment for 1 hour to obtain the graphene aqueous dispersion;
preparing the graphene phase change microcapsule, adding zeolite loaded with paraffin into graphene water dispersion, stirring for 2 hours, washing with absolute ethyl alcohol for three times, washing with deionized water for three times, and drying to obtain the modified phase change microcapsule.
Comparative preparation example 4
The preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing 10kg of paraffin and 20L of water, wherein the paraffin is No. 60 paraffin, heating until the paraffin is completely melted, adding an emulsifier span-80, stirring at 1200rpm for 2h, and emulsifying to obtain a paraffin emulsion;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing 2kg of melamine, 4kg of urea solution with the mass concentration of 95%, 40kg of formaldehyde solution with the mass concentration of 37% and 20kg of water, adding triethanolamine, adjusting the pH to 8.5, heating to 70 ℃, and reacting for 1h at 400rpm to obtain the urea-formaldehyde resin prepolymer;
preparing modified phase-change microcapsules, dropwise adding the paraffin emulsion into the urea-formaldehyde resin prepolymer, uniformly stirring at 300rpm, heating to 60 ℃, reacting for 1h, filtering, washing and drying to obtain the modified phase-change microcapsules.
Examples
Example 1
The super-long structure high-crack-resistance compensation shrinkage concrete comprises the following raw materials in parts by weight:
140kg of cement;
100kg of fly ash;
70kg of mineral powder;
800kg of sand;
1000kg of crushed stone;
20kg of expanding agent;
12kg of water reducing agent, wherein the water reducing agent is a polycarboxylic acid water reducing agent;
1kg of hydration heat inhibitor, wherein the hydration heat inhibitor is dextrin organic polymer additive produced by Jiangsu Subot new materials GmbH;
150kg of water, wherein the water is micro-nano bubble water;
2kg of modified phase change microcapsule, the modified phase change microcapsule is prepared by the preparation example 1;
the preparation method of the ultra-long structure high crack resistance compensation shrinkage concrete comprises the following steps:
uniformly mixing cement, fly ash, mineral powder, a swelling agent and the modified phase-change microcapsules, adding part of water, and uniformly mixing to obtain a cementing material;
adding sand and gravel into the cementing material, and uniformly mixing to obtain an aggregate mixture;
step three, uniformly mixing the water reducing agent, the hydration heat inhibitor and the other part of water to obtain an additive mixture;
and step four, uniformly mixing the admixture mixture and the aggregate mixture to obtain the ultra-long structure high crack resistance compensation shrinkage concrete.
Examples 2 to 11
The difference between the ultralong structure high crack resistance compensation shrinkage concrete and the embodiment 1 is that modified phase change microcapsules are prepared in preparation examples 2-11 in sequence.
Example 12
Compared with the embodiment 2, the ultra-long structure high crack resistance compensation shrinkage concrete is characterized by comprising the following components in parts by weight:
150kg of cement;
80kg of fly ash;
85kg of mineral powder;
900kg of sand;
crushing 900kg of stones;
35kg of expanding agent;
14kg of water reducing agent;
2kg of hydration heat inhibitor;
160kg of water;
2kg of modified phase change microcapsules.
Example 13
Compared with the embodiment 2, the ultra-long structure high crack resistance compensation shrinkage concrete is characterized by comprising the following components in parts by weight:
180kg of cement;
60kg of fly ash;
100kg of mineral powder;
1000kg of sand;
800kg of crushed stone;
50kg of expanding agent;
16kg of water reducing agent;
3kg of hydration heat inhibitor;
170kg of water;
2kg of modified phase change microcapsules.
Example 14
The difference between the ultralong structure high crack resistance compensating shrinkage concrete and the concrete in the embodiment 12 is that the mass of the modified phase change microcapsule is 4 kg.
Example 15
The difference between the ultralong structure high crack resistance compensating shrinkage concrete and the concrete in the embodiment 12 is that the mass of the modified phase change microcapsule is 6 kg.
Comparative example
Comparative examples 1 to 4
The difference between the ultralong structure high crack resistance compensation shrinkage concrete and the concrete in the embodiment 2 is that modified phase change microcapsules are prepared in sequence from comparative preparation examples 1-4.
Blank control group
The difference between the super-long structure high crack resistance compensation shrinkage concrete and the concrete in the embodiment 2 is that modified phase change microcapsules are not added into the raw materials.
Performance test
Detection method
(1) The concrete of example 2, comparative example 4 and blank control was tested for 7d restricted expansion in water and 21d restricted expansion in air, and the results are shown in table 1.
(2) The modified phase-change microcapsules prepared in preparation examples 1 to 11 and preparation examples 1 to 4 were used as samples, and the results of measuring the thermal conductivity are shown in table 2.
(3) The modified phase-change microcapsules prepared in preparation examples 1 to 11 and preparation examples 1 to 4 were tested by a differential scanning calorimeter under the following test conditions: the temperature rise rate is 5 ℃/min, the temperature rise range is-20 ℃ to 80 ℃, the temperature drop rate is 5 ℃/min, the temperature drop range is 80 ℃ to-20 ℃, the cycle frequency is 500 times, and the percentage of reduction of the phase change enthalpy is recorded, and the result is shown in table 2.
(4) Preparing a standard test block according to a GB-T50081-2019 concrete physical and mechanical property test method, and testing the compression strength of the concrete in examples 1-7, examples 12-15, comparative examples 1-4 and a blank control group; and measuring the total cracking area per unit area after pouring the concrete for 24 hours. The results are shown in Table 3.
TABLE 1 test results of concrete shrinkage Properties
TABLE 2 detection results of percentage reduction of heat conductivity and phase change enthalpy
| Preparation example No | Thermal conductivity W/(m.K) | Percent reduction of enthalpy of phase change/%) |
| Preparation example 1 | 0.332 | 1.85 |
| Preparation example 2 | 0.335 | 1.80 |
| Preparation example 3 | 0.329 | 1.83 |
| Preparation example 4 | 0.426 | 1.72 |
| Preparation example 5 | 0.603 | 1.66 |
| Preparation example 6 | 0.237 | 1.98 |
| Preparation example 7 | 0.956 | 1.51 |
| Preparation example 8 | 0.428 | 1.78 |
| Preparation example 9 | 0.427 | 1.76 |
| Preparation example 10 | 0.425 | 1.88 |
| Preparation example 11 | 0.428 | 1.86 |
| Comparative preparation example 1 | 0.308 | 6.89 |
| Comparative preparation example 2 | 0.287 | 2.31 |
| Comparative preparation example 3 | 0.411 | 5.85 |
| Comparative preparation example 4 | 0.178 | 5.13 |
TABLE 3 Total cracking area and compressive Strength test results in Unit area
The combination of example 2, comparative example 4 and the blank control group and the combination of table 1 shows that the limited expansion rate of comparative example 4 is higher than that of the blank control group, which shows that the modified phase-change microcapsule prepared by wrapping paraffin with urea resin can improve the limited expansion rate and improve the performance of concrete shrinkage compensation, and the limited expansion rate of example 2 is higher than that of comparative example 4, which shows that the modified phase-change microcapsule prepared by the method of the present application can further improve the performance of concrete shrinkage compensation.
It can be seen from the combination of the preparation examples 1 to 11 and the comparative preparation examples 1 to 4 and the combination of the table 2 that the thermal conductivity of the paraffin wax is low in the comparative preparation example 4 only by coating the paraffin wax with the urea resin, and the percentage of decrease in phase change enthalpy after 500 cycles is high, which indicates that the modified phase change microcapsule obtained in the comparative preparation example 4 has low thermal conductivity and poor cycle stability. The thermal conductivity and the reduction percentage of the phase change enthalpy of the paraffin coated by the modified graphene in the comparative preparation example 1 are higher than those in the comparative preparation example 4, which shows that the modified graphene serving as the capsule wall can improve the thermal conductivity of the modified phase change microcapsule, but the cycle stability of the modified phase change microcapsule is deteriorated; the urea-formaldehyde resin is coated on the surface of the graphene in the comparative preparation example 2, the heat conductivity coefficient is lower than that in the comparative preparation example 1 and higher than that in the comparative preparation example 4, and the reduction percentage of the phase change enthalpy is far lower than that in the comparative preparation example 1, which shows that the urea-formaldehyde resin can improve the cycle stability of the modified phase change microcapsule; in comparative preparation example 3, zeolite is added to the core material, and compared with comparative preparation example 1, the thermal conductivity is greatly improved, but the percentage of phase change enthalpy reduction is further improved, which indicates that both zeolite and modified graphene can improve the thermal conductivity of the modified phase change microcapsule, but the cycle stability of the modified phase change microcapsule is deteriorated, and the possible reason is that holes or gaps exist when the graphene wraps paraffin droplets; compared with the comparative preparation example 3, the preparation example 2 has the advantages that the urea-formaldehyde resin is coated on the surface of the graphene, the heat conductivity coefficient is reduced to a certain extent, but the reduction percentage of the phase change enthalpy is greatly reduced, which indicates that the modified phase change microcapsule has better comprehensive performance when zeolite and the urea-formaldehyde resin are introduced into the microcapsule. In the preparation examples 4 to 5, the thermal conductivity is gradually increased when the amount of the modified graphene is increased, the thermal conductivity is greatly reduced when a small amount of the modified graphene is used in the preparation example 6, and the cost is relatively high although the thermal conductivity is improved when a large amount of the modified graphene is used in the preparation example 7, and therefore, the mass ratio of the modified graphene to the paraffin is preferably (0.5 to 0.8): 10; preparation examples 8-11 in the step of preparing modified phase-change microcapsules, the stirring speed was changed, the thermal conductivity was not greatly changed, and the percentage of decrease in phase-change enthalpy was increased when the stirring speed was too slow or too fast, and therefore, the stirring speed was preferably 300-800 rpm.
When the blank control group is taken as reference, the total cracking area per unit area is reduced and the compressive strength is reduced when the paraffin coated by the urea-formaldehyde resin is added in the comparative example 4, which can be seen by combining the examples 1-7, 12-15, 1-4 and the blank control group and combining the table 3, the modified phase-change microcapsules can reduce the cracks generated by the concrete and reduce the compressive strength of the concrete; the modified phase-change microcapsules of comparative preparation examples 1 to 3 are added in comparative examples 1 to 3, so that the total cracking area per unit area is reduced, and the compressive strength is reduced, while the modified phase-change microcapsules prepared in preparation example 2 are added in example 2, the total cracking area per unit area is reduced, and the compressive strength is not reduced, which indicates that after the zeolite is added in the core material, the structural strength of the modified phase-change microcapsules can be improved, and the influence on the compressive strength of concrete is reduced; example 14 increases the amount of the modified phase-change microcapsule, further decreases the total area of the crack in the unit area, slightly decreases the compressive strength, but still greater than 40MPa, example 15 continues to increase the amount of the modified phase-change microcapsule, further decreases the total area of the crack in the unit area, slightly decreases the compressive strength, but still greater than 40MPa, and considering all together, the amount of the modified phase-change microcapsule is preferably 2 to 6 parts.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The super-long structure high anti-cracking compensation shrinkage concrete is characterized in that: the raw materials comprise the following components in parts by weight:
140 portions of cement and 180 portions of cement;
60-100 parts of fly ash;
70-100 parts of mineral powder;
800 portions of sand and 1000 portions of sand;
800 portions of gravel and 1000 portions of gravel;
20-50 parts of an expanding agent;
12-16 parts of a water reducing agent;
1-3 parts of a hydration heat inhibitor;
150 portions of water and 170 portions of water;
2-6 parts of modified phase change microcapsules;
the preparation method of the modified phase-change microcapsule comprises the following steps:
emulsifying, namely mixing paraffin and water, heating until the paraffin is completely melted, adding a compound emulsifier, uniformly mixing, and emulsifying to obtain a paraffin emulsion;
loading, namely uniformly mixing the paraffin emulsion and the zeolite, preserving heat, filtering and drying to obtain the paraffin-loaded zeolite;
preparing a graphene aqueous dispersion, dispersing graphene oxide in water, performing ultrasonic treatment to obtain the graphene aqueous dispersion, adjusting the pH value to be alkalescent, uniformly mixing, adding ethylenediamine, mixing, performing heating reaction, washing, performing freeze drying to obtain modified graphene, mixing the modified graphene with a strong-acid aqueous solution, and performing ultrasonic treatment to obtain the graphene aqueous dispersion;
preparing a graphene phase-change microcapsule, adding zeolite loaded with paraffin into graphene aqueous dispersion, uniformly mixing, washing and drying to obtain the graphene phase-change microcapsule;
preparing a urea-formaldehyde resin prepolymer, uniformly mixing melamine, a urea solution, a formaldehyde solution and water, adding triethanolamine, adjusting the pH value to be alkalescent, and heating for reaction to obtain the urea-formaldehyde resin prepolymer;
preparing a modified phase-change microcapsule, adding the graphene phase-change microcapsule into the urea resin prepolymer, uniformly mixing, heating for reaction, filtering, washing and drying to obtain the modified phase-change microcapsule.
2. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 1, characterized in that: the mass ratio of the compound emulsifier to the paraffin is 1 (10-15), the compound emulsifier comprises sodium dodecyl benzene sulfonate and span-80, and the mass ratio of the sodium dodecyl benzene sulfonate to the span-80 is 1: (1-1.2).
3. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 2, characterized in that: the mass ratio of the paraffin to the zeolite is 1: (1.5-2).
4. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 2, characterized in that: the particle size of the zeolite is 250-350 nm.
5. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 1, characterized in that: in the step of preparing the graphene aqueous dispersion, the graphene aqueous dispersion is heated to 70-75 ℃ and reacts for 10-12 h.
6. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 1, characterized in that: in the step of preparing the graphene phase change microcapsule, the mass ratio of the modified graphene to the paraffin is (0.5-0.8): 10.
7. the ultra-long structure high crack resistance compensation shrinkage concrete according to claim 1, characterized in that: in the step of preparing the urea-formaldehyde resin prepolymer, the pH value is adjusted to 8-9.
8. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 1, characterized in that: in the step of preparing the modified phase-change microcapsule, the phase-change microcapsule is uniformly mixed at the speed of 300-800 rpm.
9. The ultra-long structure high crack resistance compensation shrinkage concrete according to claim 1, characterized in that: the water in the ultra-long structure high crack resistance compensation shrinkage concrete raw material is micro-nano bubble water.
10. The method for preparing the ultra-long structure high crack resistance compensation shrinkage concrete according to any one of claims 1 to 9, characterized in that: the method comprises the following steps:
uniformly mixing cement, fly ash, mineral powder, a swelling agent and the modified phase-change microcapsules, adding part of water, and uniformly mixing to obtain a cementing material;
adding sand and gravel into the cementing material, and uniformly mixing to obtain an aggregate mixture;
step three, uniformly mixing the water reducing agent, the hydration heat inhibitor and the other part of water to obtain an additive mixture;
and step four, uniformly mixing the admixture mixture and the aggregate mixture to obtain the ultra-long structure high crack resistance compensation shrinkage concrete.
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