CN115028413A - Wear-resistant high-strength cement and preparation method thereof - Google Patents
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
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- 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
- C04B2201/52—High compression strength concretes, i.e. with a compression strength higher than about 55 N/mm2, e.g. reactive powder concrete [RPC]
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Abstract
The invention discloses wear-resistant high-strength cement and a preparation method thereof, and relates to the technical field of building materials. During the preparation of the wear-resistant high-strength cement, bagasse is carbonized and oxidized into carbon oxide fibers, ammonia and methyl acrylate react to prepare semi-substituted polyamide, the carbon oxide fibers react with tri (2-aminoethyl) amine, the semi-substituted polyamide and trans-1, 4-diamino-2-butene to prepare modified carbon fibers, allyl alcohol glycidyl ether and triethoxysilane react to prepare epoxy silane, 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane react to prepare an organic silicon polymer, the organic silicon polymer and azo polyethylene glycol monomethyl ether react to prepare the modified organic silicon polymer, and the cement, the modified carbon fibers, the modified organic silicon polymer and an alkaline activator are mixed to prepare the wear-resistant high-strength cement. The wear-resistant high-strength cement prepared by the invention has excellent compression resistance and early strength.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to wear-resistant high-strength cement and a preparation method thereof.
Background
The cement is a powdered hydraulic inorganic cementitious material. Water is added and stirred to form slurry which can be hardened in air or water and can firmly bond sand, stone and other materials together. The early lime and pozzolan mixtures are similar to modern lime and pozzolan cements, and concrete made by cementing crushed stone with them not only has higher strength after hardening, but also resists erosion by fresh water or salt-containing water. As an important cementing material, the high-performance cement is widely applied to engineering such as civil construction, water conservancy, national defense and the like for a long time.
Along with the development of society, the construction of roads and buildings needs to use a large amount of cement, the concrete formed by the cement is inevitably damaged in the long-term use process, the ordinary cement is repaired, the maintenance time is long, and the cement is inconvenient, so that the cement which can be rapidly repaired and used and has higher compressive strength needs to be developed.
Disclosure of Invention
The invention aims to provide wear-resistant high-strength cement and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the wear-resistant high-strength cement is characterized in that the wear-resistant high-strength cement is prepared by mixing cement, modified carbon fibers, a modified organic silicon polymer and an alkaline activator.
Preferably, the modified carbon fiber is prepared by carbonizing and oxidizing bagasse into oxidized carbon fiber, and reacting the oxidized carbon fiber with tri (2-aminoethyl) amine, semi-substituted polyamide and trans-1, 4-diamino-2-butene in sequence.
Preferably, the semi-substituted polyamide is prepared by reacting ammonia and methyl acrylate.
Preferably, the modified organic silicon polymer is prepared by reacting allyl alcohol glycidyl ether with triethoxysilane to prepare epoxy silane, reacting 2, 3-dihydroxy-1-butene, vinyl triethoxysilane with epoxy silane to prepare an organic silicon polymer, and reacting the organic silicon polymer with azo polyethylene glycol monomethyl ether.
As optimization, the preparation method of the wear-resistant high-strength cement comprises the following preparation steps:
(1) oxidation treatment: immersing carbon fibers in concentrated nitric acid, stirring and reacting for 2-3 h at 70-80 ℃ and 800-1000 r/min, taking out, placing in pure water, soaking for 8-10 min, filtering, washing for 3-5 times by using absolute ethyl alcohol, and drying for 3-4 h at 60-70 ℃ to obtain oxidized carbon fibers;
(2) modification of oxidized carbon fibers: mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to a mass ratio of 2: 1: 0.3: 50-3: 1: 0.5: 70, uniformly mixing, carrying out ultrasonic reaction for 2-3 h at 60-70 ℃ at 30-40 kHz, filtering, washing for 3-5 times by pure water, drying for 3-4 h at 60-70 ℃, then placing in a methanol solution with the mass of 20-25 times that of oxidized carbon fibers, adding semi-substituted polyamide with the mass of 2-4 times that of the oxidized carbon fibers, stirring and reacting for 20-24 h at 20-30 ℃ at 800-1000 r/min, filtering, washing for 3-5 times by pure water and absolute ethyl alcohol respectively, drying for 4-6 h at 60-70, and mixing with trans-1, 4-diamino-2-butene and methanol according to the mass ratio of 1: 3: 30-1: 5: 40, uniformly mixing, stirring and reacting for 20-24 hours at 20-30 ℃ at 800-1000 r/min, filtering, washing for 3-5 times by using pure water and absolute ethyl alcohol respectively, and drying for 4-6 hours at 60-70 ℃ to obtain modified carbon fibers;
(3) preparation of the silicone polymer: 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane are mixed according to the mass ratio of 2: 1: 1-4: 2: 3, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.01-0.02 time of that of 2, 3-dihydroxy-1-butene, stirring at 90-100 ℃ for 20-30 min at 300-500 r/min, heating to 150-160 ℃, continuing stirring for 6-8 h, cooling to room temperature, standing at 50-60 ℃ for 30-40 min at 1-2 kPa to obtain an organic silicon polymer;
(4) modification of the silicone polymer: the preparation method comprises the following steps of (1) mixing an organic silicon polymer, azo polyethylene glycol monomethyl ether, N-dimethylformamide and ammonia water with the mass fraction of 10-15% in a mass ratio of 2: 1: 8: 10-3: 1: 10: 12, uniformly mixing, stirring and reacting for 6-8 h at 10-20 ℃ at 800-1000 r/min, and drying for 20-24 h at 10-20 ℃ under 40-80 Pa to prepare a modified organic silicon polymer;
(5) mixing materials: sodium hydroxide and sodium silicate are mixed according to the mass ratio of 1: 1-1: 2, uniformly mixing the raw materials to prepare an alkaline activator, and mixing cement, modified carbon fibers, a modified organic silicon polymer and the alkaline activator according to a mass ratio of 60: 20: 10: 3-70: 28: 15: 5, uniformly mixing to prepare the wear-resistant high-strength cement.
As optimization, the preparation method of the carbon fiber in the step (1) comprises the following steps: immersing bagasse in a sodium hypochlorite solution with the mass fraction of 3-5% at normal temperature and normal pressure, standing for 10-12 h, filtering, washing for 3-5 times with pure water, soaking in a urea solution with the mass fraction of 30-40% for 2-3 h, filtering, placing in a vacuum tube furnace, standing for 20-30 min at 100-120 ℃ in a nitrogen atmosphere, standing for 40-50 min at 300-400 ℃, standing for 20-30 min at 1000-1200 ℃, cooling to room temperature, and taking out to prepare the bagasse.
As optimization, the preparation method of the semi-substituted polyamide in the step (2) comprises the following steps: mixing 8-12% of ammonia methanol solution and methyl acrylate according to a mass ratio of 1: 3-1: 5, uniformly mixing, stirring and reacting for 20-24 hours at 20-30 ℃ at 800-1000 r/min, and standing for 60-80 minutes at 40-50 ℃ under 1-2 kPa to prepare the water-based paint.
Preferably, the preparation method of the epoxy silane in the step (3) comprises the following steps: allyl alcohol glycidyl ether, triethoxysilane and n-hexane are mixed according to the mass ratio of 1: 1: 8-1: 1: 10, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.03-0.05 time that of allyl alcohol glycidyl ether, stirring and refluxing for 4-6 hours at 70-80 ℃ and 500-800 r/min, and standing for 3-4 hours at 20-30 ℃ and 1-2 kPa to prepare the allyl alcohol glycidyl ether.
As optimization, the preparation method of the azo-based polyethylene glycol monomethyl ether in the step (4) comprises the following steps: succinic anhydride and polyethylene glycol monomethyl ether are mixed according to the mass ratio of 1: 4-1: 6, uniformly mixing, stirring for 3-4 hours at 70-80 ℃ at 800-1000 r/min, adding into thionyl chloride with the mass of 8-10 times of that of polyethylene glycol monomethyl ether, adding tetrahydrofuran with the mass of 0.04-0.08 time of that of polyethylene glycol monomethyl ether, stirring and reacting for 2-3 hours at 40-50 ℃ at 300-500 r/min, heating to 60-70 ℃, continuing stirring and reacting for 2-3 hours, and drying for 30-40 minutes at 10-30 ℃ under 40-80 Pa to obtain acyl chloride-based polyethylene glycol monomethyl ether; mixing acyl chloride polyethylene glycol monomethyl ether, p-diaminoazobenzene, dichloromethane and triethylamine according to a mass ratio of 1: 0.8: 10: 0.4-1: 1: 12: 1, uniformly mixing, stirring for 2-3 hours at 0-5 ℃ at 300-500 r/min, and standing for 6-8 hours at 10-20 ℃ under 1-2 kPa.
Preferably, the cement in the step (5) is ordinary portland cement.
Compared with the prior art, the invention has the following beneficial effects:
the invention is prepared by mixing cement, modified carbon fiber, modified organic silicon polymer and alkali activator.
Firstly, bagasse is carbonized and oxidized into oxidized carbon fibers, ammonia and methyl acrylate react to prepare semi-substituted polyamide, the oxidized carbon fibers react with tri (2-aminoethyl) amine, the semi-substituted polyamide and trans-1, 4-diamino-2-butene in sequence to prepare modified carbon fibers, the tri (2-aminoethyl) amine, the semi-substituted polyamide and the trans-1, 4-diamino-2-butene grow on the oxidized carbon fibers according to surface branching, so that the prepared modified carbon fibers have higher branching degree and the number of amino groups and imino groups, nitrogen atoms can easily form covalent bonds with metal ions to perform complex reaction, the dissolution rate of tricalcium silicate and tetracalcium aluminoferrite in cement is improved, the compactness of portland cement is also improved, and the supersaturation degree of calcium hydroxide generated by adding water and stirring the cement is improved due to the formation of the complex, thereby effectively preventing the cement from generating loose crystalline phase structure by early hydration, improving the compactness of the portland cement and further improving the early strength;
secondly, allyl alcohol glycidyl ether and triethoxysilane react to prepare epoxy silane, 2, 3-dihydroxy-1-butylene, vinyl triethoxysilane and epoxy silane react to prepare an organic silicon polymer, the organic silicon polymer and azo polyethylene glycol monomethyl ether react to prepare a modified organic silicon polymer, one hydrophilic end and one hydrophobic end of the modified organic silicon polymer can reduce surface tension, so that the wetting capacity of water on cement particles is enhanced, the hydration active points of the cement particles are increased, the cement is solidified and combined more tightly, meanwhile, in the cement hydration maintenance process, the organic silicon polymer is hydrolyzed in outdoor sun and alkaline environments to form silane with silicon hydroxyl and double bonds, the modified carbon fibers and inorganic particles in the cement are connected with each other at the interface, and azo bonds on the modified organic silicon polymer are hydrated, the curing process is broken to form free radicals to initiate the polymerization of double bonds, thereby improving the compressive strength.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to illustrate the method for testing each index of the abrasion-resistant high-strength cement manufactured in the following examples as follows:
compression resistance: the wear-resistant high-strength cement obtained in each example and the comparative example material are cured for 28 days in the same outdoor environment, shaped into solid blocks with the same size and shape, and tested for compressive strength according to GB/T50081-2002.
Early strength performance: the wear-resistant high-strength cement obtained in each example and the comparative example material are cured in the same outdoor environment for 3 days to form solid blocks with the same size and shape, and the compressive strength is tested according to GB/T50081-2002 to obtain the early strength.
Example 1
(1) Oxidation treatment: immersing bagasse in a sodium hypochlorite solution with the mass fraction of 3% at normal temperature and normal pressure, standing for 12h, filtering, washing for 3 times by using pure water, soaking in a urea solution with the mass fraction of 30% for 3h, filtering, placing in a vacuum tube furnace, standing for 30min at 100 ℃ in a nitrogen atmosphere, standing for 50min at 300 ℃, standing for 30min at 1000 ℃, cooling to room temperature, and taking out to obtain carbon fiber; immersing carbon fibers in concentrated nitric acid, stirring and reacting at 70 ℃ at 800r/min for 3h, taking out, placing in pure water, soaking for 8min, filtering, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ for 4h to obtain oxidized carbon fibers;
(2) modification of oxidized carbon fibers: mixing 8 mass percent of ammonia methanol solution and methyl acrylate according to a mass ratio of 1: 3, uniformly mixing, stirring and reacting at 20 ℃ at 800r/min for 24h, and standing at 40 ℃ under 1kPa for 80min to obtain semi-generation polyamide; mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to a mass ratio of 2: 1: 0.3: 50, uniformly mixing, carrying out ultrasonic reaction for 3h at 60 ℃ and 30kHz, filtering, washing for 3 times by pure water, drying for 4h at 60 ℃, then placing in a methanol solution with the mass of 20 times that of the oxidized carbon fiber, adding semi-substituted polyamide with the mass of 2 times that of the oxidized carbon fiber, stirring and reacting for 24h at 20 ℃ and 800r/min, filtering, washing for 3 times by pure water and absolute ethyl alcohol respectively, drying for 6h at 60, and mixing with trans-1, 4-diamino-2-butene and methanol according to the mass ratio of 1: 3: 30, uniformly mixing, stirring and reacting for 20 hours at 20 ℃ at 1000r/min, filtering, washing 3 times by using pure water and absolute ethyl alcohol respectively, and drying for 6 hours at 60 ℃ to obtain modified carbon fibers;
(3) preparation of the silicone polymer: mixing allyl alcohol glycidyl ether, triethoxysilane and n-hexane in a mass ratio of 1: 1: 8, uniformly mixing, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.03 time that of allyl alcohol glycidyl ether, stirring and refluxing for 6 hours at 70 ℃ and 500r/min, and standing for 4 hours at 20 ℃ and 1kPa to prepare epoxy silane; 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane are mixed according to the mass ratio of 2: 1: 1, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.01 time of that of 2, 3-dihydroxy-1-butene, stirring at 90 ℃ and 300r/min for 30min, heating to 150 ℃, continuing stirring for 8h, cooling to room temperature, and standing at 50 ℃ and 1kPa for 40min to obtain an organic silicon polymer;
(4) modification of the silicone polymer: succinic anhydride and polyethylene glycol monomethyl ether are mixed according to the mass ratio of 1: 4, uniformly mixing, stirring at 70 ℃ and 800r/min for 4h, adding into thionyl chloride with the mass of 8 times that of polyethylene glycol monomethyl ether, adding tetrahydrofuran with the mass of 0.04 time that of the polyethylene glycol monomethyl ether, stirring and reacting at 40 ℃ and 300r/min for 3h, heating to 60 ℃, continuing stirring and reacting for 3h, and drying at 10 ℃ and 40Pa for 40min to obtain acyl chloride-based polyethylene glycol monomethyl ether; mixing acyl chloride polyethylene glycol monomethyl ether, p-diaminoazobenzene, dichloromethane and triethylamine according to a mass ratio of 1: 0.8: 10: 0.4, uniformly mixing, stirring at 0 ℃ and 300r/min for 3h, and standing at 10 ℃ and 1kPa for 8h to obtain azo-polyethylene glycol monomethyl ether; mixing an organic silicon polymer, azo polyethylene glycol monomethyl ether, N-dimethylformamide and ammonia water with the mass fraction of 10% according to the mass ratio of 2: 1: 8: 10, uniformly mixing, stirring and reacting for 8 hours at 10 ℃ and 800r/min, and drying for 24 hours at 10 ℃ and 40Pa to prepare a modified organic silicon polymer;
(5) mixing materials: sodium hydroxide and sodium silicate are mixed according to the mass ratio of 1: 1, uniformly mixing to prepare an alkaline activator, and mixing PO42.5 cement, modified carbon fibers, a modified organic silicon polymer and the alkaline activator according to a mass ratio of 60: 20: 10: 3, uniformly mixing to prepare the wear-resistant high-strength cement.
Example 2
(1) Oxidation treatment: immersing bagasse in a sodium hypochlorite solution with the mass fraction of 4% at normal temperature and normal pressure, standing for 11h, filtering, washing with pure water for 4 times, soaking in a urea solution with the mass fraction of 35% for 2.5h, filtering, placing in a vacuum tube furnace, standing for 25min at 110 ℃ in a nitrogen atmosphere, standing for 45min at 350 ℃, standing for 25min at 1100 ℃, cooling to room temperature, and taking out to obtain carbon fibers; immersing carbon fibers in concentrated nitric acid, stirring and reacting at 75 ℃ and 900r/min for 2.5h, taking out, placing in pure water, soaking for 9min, filtering, washing for 4 times by using absolute ethyl alcohol, and drying at 65 ℃ for 3.5h to obtain oxidized carbon fibers;
(2) modification of oxidized carbon fibers: mixing ammonia methanol solution with the mass fraction of 10% and methyl acrylate according to the mass ratio of 1: 4, uniformly mixing, stirring and reacting at 25 ℃ and 900r/min for 22h, and standing at 45 ℃ and 1.5kPa for 70min to obtain semi-generation polyamide; mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to a mass ratio of 2.5: 1: 0.4: 60, uniformly mixing, carrying out ultrasonic reaction for 2.5h at 65 ℃ and 35kHz, filtering, washing for 4 times by pure water, drying for 3.5h at 65 ℃, then placing in a methanol solution with 22 times of the mass of the oxidized carbon fiber, adding half-substituted polyamide with 3 times of the mass of the oxidized carbon fiber, stirring and reacting for 22h at 25 ℃ and 900r/min, filtering, washing for 4 times by pure water and absolute ethyl alcohol respectively, drying for 5h at 65, and mixing with trans-1, 4-diamino-2-butene and methanol according to the mass ratio of 1: 3: 35, uniformly mixing, stirring and reacting at 25 ℃ and 900r/min for 22 hours, filtering, washing with pure water and absolute ethyl alcohol for 4 times respectively, and drying at 65 ℃ for 5 hours to obtain modified carbon fibers;
(3) preparation of the silicone polymer: mixing allyl alcohol glycidyl ether, triethoxysilane and n-hexane in a mass ratio of 1: 1: 9, uniformly mixing, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.04 times that of allyl alcohol glycidyl ether, stirring and refluxing for 5 hours at the temperature of 75 ℃ and the speed of 600r/min, and standing for 3.5 hours at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare epoxy silane; 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane are mixed according to the mass ratio of 3: 1.5: 2, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.015 time of that of the 2, 3-dihydroxy-1-butene, stirring at 95 ℃ and 400r/min for 25min, heating to 155 ℃, continuing stirring for 7h, cooling to room temperature, and standing at 55 ℃ and 1.5kPa for 35min to obtain an organic silicon polymer;
(4) modification of the silicone polymer: succinic anhydride and polyethylene glycol monomethyl ether are mixed according to the mass ratio of 1: 5, uniformly mixing, stirring at 75 ℃ and 900r/min for 3.5h, adding into thionyl chloride with the mass 9 times that of polyethylene glycol monomethyl ether, adding tetrahydrofuran with the mass 0.06 time that of polyethylene glycol monomethyl ether, stirring at 45 ℃ and 400r/min for reaction for 2.5h, heating to 65 ℃, continuing stirring for reaction for 2.5h, drying at 20 ℃ and 60Pa for 35min, and obtaining acyl chloride-based polyethylene glycol monomethyl ether; the preparation method comprises the following steps of (1) mixing acyl chloride polyethylene glycol monomethyl ether, p-diamino azobenzene, dichloromethane and triethylamine in a mass ratio of 1: 0.8: 10: 0.4, stirring the mixture evenly for 2.5 hours at the temperature of 3 ℃ and at the speed of 400r/min, and standing the mixture for 7 hours at the temperature of 15 ℃ and at the pressure of 1.5kPa to prepare azo-polyethylene glycol monomethyl ether; the preparation method comprises the following steps of (1) mixing an organic silicon polymer, azo polyethylene glycol monomethyl ether, N-dimethylformamide and 12% ammonia water in mass percentage of 2.5: 1: 9: 11, uniformly mixing, stirring and reacting for 7 hours at 15 ℃ and 900r/min, and drying for 22 hours at 15 ℃ and 6Pa to obtain a modified organic silicon polymer;
(5) mixing materials: sodium hydroxide and sodium silicate are mixed according to the mass ratio of 1: 1.5, uniformly mixing to prepare an alkaline activator, and mixing PO42.5 cement, modified carbon fibers, a modified organic silicon polymer and the alkaline activator according to a mass ratio of 65: 24: 12: 4, uniformly mixing to prepare the wear-resistant high-strength cement.
Example 3
(1) Oxidation treatment: immersing bagasse in a sodium hypochlorite solution with the mass fraction of 5% at normal temperature and normal pressure, standing for 10h, filtering, washing for 5 times by using pure water, soaking in a urea solution with the mass fraction of 40% for 2h, filtering, placing in a vacuum tube furnace, standing for 20min at 120 ℃ in a nitrogen atmosphere in sequence, standing for 40min at 400 ℃, standing for 20min at 1200 ℃, cooling to room temperature, and taking out to obtain carbon fibers; immersing carbon fibers in concentrated nitric acid, stirring and reacting at 80 ℃ and 1000r/min for 2h, taking out, placing in pure water, soaking for 10min, filtering, washing for 5 times by using absolute ethyl alcohol, and drying at 70 ℃ for 3h to obtain oxidized carbon fibers;
(2) modification of oxidized carbon fibers: mixing ammonia methanol solution with the mass fraction of 12% and methyl acrylate according to the mass ratio of 1: 3, uniformly mixing, stirring and reacting at 30 ℃ for 20 hours at 1000r/min, and standing at 50 ℃ for 60 minutes under 2kPa to obtain semi-polyamide; mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to the mass ratio of 3: 1: 0.5: 70, uniformly mixing, carrying out ultrasonic reaction for 2 hours at 70 ℃ and 40kHz, filtering, washing for 5 times by pure water, drying for 3 hours at 70 ℃, then placing in a methanol solution with the mass of 25 times that of the oxidized carbon fiber, adding half-substituted polyamide with the mass of 4 times that of the oxidized carbon fiber, stirring and reacting for 20 hours at 30 ℃ and 1000r/min, filtering, washing for 5 times by pure water and absolute ethyl alcohol respectively, drying for 4 hours at 70, and then mixing with trans-1, 4-diamino-2-butene and methanol according to the mass ratio of 1: 5: 40, uniformly mixing, stirring and reacting for 20 hours at 30 ℃ and 1000r/min, filtering, washing for 5 times by using pure water and absolute ethyl alcohol respectively, and drying for 4 hours at 70 ℃ to obtain modified carbon fibers;
(3) preparation of the silicone polymer: mixing allyl alcohol glycidyl ether, triethoxysilane and n-hexane in a mass ratio of 1: 1: 10, uniformly mixing, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.05 time that of allyl alcohol glycidyl ether, stirring and refluxing for 4 hours at 80 ℃ and 800r/min, and standing for 3 hours at 30 ℃ and 2kPa to prepare epoxy silane; mixing 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane in a mass ratio of 4: 2: 3, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.02 time of that of the 2, 3-dihydroxy-1-butene, stirring at 100 ℃ and 500r/min for 20min, heating to 160 ℃, continuing stirring for 6h, cooling to room temperature, and standing at 60 ℃ and 2kPa for 30min to obtain an organic silicon polymer;
(4) modification of the silicone polymer: succinic anhydride and polyethylene glycol monomethyl ether are mixed according to the mass ratio of 1: 4, uniformly mixing, stirring at 70 ℃ and 800r/min for 4h, adding into thionyl chloride with the mass of 8 times that of polyethylene glycol monomethyl ether, adding tetrahydrofuran with the mass of 0.04 time that of the polyethylene glycol monomethyl ether, stirring and reacting at 40 ℃ and 300r/min for 3h, heating to 60 ℃, continuing stirring and reacting for 3h, and drying at 10 ℃ and 40Pa for 40min to obtain acyl chloride-based polyethylene glycol monomethyl ether; mixing acyl chloride polyethylene glycol monomethyl ether, p-diaminoazobenzene, dichloromethane and triethylamine according to a mass ratio of 1: 1: 12: 1, uniformly mixing, stirring for 2 hours at 5 ℃ and 500r/min, and standing for 6 hours at 20 ℃ and 2kPa to obtain azo-polyethylene glycol monomethyl ether; the preparation method comprises the following steps of (1) mixing an organic silicon polymer, azo polyethylene glycol monomethyl ether, N-dimethylformamide and ammonia water with the mass fraction of 10-15% in a mass ratio of 3: 1: 10: 12, uniformly mixing, stirring and reacting for 6 hours at 20 ℃ at 1000r/min, and drying for 20 hours at 20 ℃ under 80Pa to prepare a modified organic silicon polymer;
(5) mixing materials: sodium hydroxide and sodium silicate are mixed according to the mass ratio of 1: 2, uniformly mixing the materials to prepare an alkaline activator, and mixing PO42.5 cement, modified carbon fibers, a modified organic silicon polymer and the alkaline activator according to a mass ratio of 65: 24: 12: 4, uniformly mixing to prepare the wear-resistant high-strength cement.
Comparative example 1
The preparation method of the wear-resistant high-strength cement of comparative example 1 is different from that of example 2 only in the difference of step (2), and the step (2) is modified as follows: modification of oxidized carbon fibers: mixing ammonia methanol solution with the mass fraction of 10% and methyl acrylate according to the mass ratio of 1: 4, uniformly mixing, stirring and reacting at 25 ℃ and 900r/min for 22h, and standing at 45 ℃ and 1.5kPa for 70min to obtain semi-polyamide; mixing oxidized carbon fiber, ethylenediamine, sodium hydroxide and pure water according to a mass ratio of 2.5: 1: 0.4: 60, uniformly mixing, carrying out ultrasonic reaction for 2.5h at 65 ℃ and 35kHz, filtering, washing for 4 times by pure water, drying for 3.5h at 65 ℃, then placing in a methanol solution with 22 times of the mass of the oxidized carbon fiber, adding half-substituted polyamide with 3 times of the mass of the oxidized carbon fiber, stirring and reacting for 22h at 25 ℃ and 900r/min, filtering, washing for 4 times by pure water and absolute ethyl alcohol respectively, drying for 5h at 65, and mixing with trans-1, 4-diamino-2-butene and methanol according to the mass ratio of 1: 3: 35, uniformly mixing, stirring and reacting for 22 hours at 25 ℃ and 900r/min, filtering, washing for 4 times by using pure water and absolute ethyl alcohol respectively, and drying for 5 hours at 65 ℃ to obtain the modified carbon fiber. The remaining steps were performed in the same manner as in example 2.
Comparative example 2
The preparation method of the wear-resistant high-strength cement of comparative example 2 is different from that of example 2 only in the difference of step (2), and step (1) is modified as follows: (2) modification of oxidized carbon fibers: mixing ammonia methanol solution with the mass fraction of 10% and methyl acrylate according to the mass ratio of 1: 4, uniformly mixing, stirring and reacting at 25 ℃ and 900r/min for 22h, and standing at 45 ℃ and 1.5kPa for 70min to obtain semi-polyamide; mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to a mass ratio of 2.5: 1: 0.4: 60, uniformly mixing, carrying out ultrasonic reaction for 2.5h at 65 ℃ and 35kHz, filtering, washing for 4 times by pure water, drying for 3.5h at 65 ℃, then placing in a methanol solution with 22 times of the mass of the oxidized carbon fiber, adding a half-substituted polyamide with 3 times of the mass of the oxidized carbon fiber, stirring and reacting for 22h at 25 ℃ and 900r/min, filtering, washing for 4 times by pure water and absolute ethyl alcohol respectively, and drying for 5h at 65 ℃ to obtain the modified carbon fiber. The remaining steps were performed in the same manner as in example 2.
Comparative example 3
(1) Oxidation treatment: immersing bagasse in a sodium hypochlorite solution with the mass fraction of 4% at normal temperature and normal pressure, standing for 11h, filtering, washing with pure water for 4 times, soaking in a urea solution with the mass fraction of 35% for 2.5h, filtering, placing in a vacuum tube furnace, standing for 25min at 110 ℃ in a nitrogen atmosphere, standing for 45min at 350 ℃, standing for 25min at 1100 ℃, cooling to room temperature, and taking out to obtain carbon fibers; immersing carbon fibers in concentrated nitric acid, stirring and reacting at 75 ℃ and 900r/min for 2.5h, taking out, placing in pure water, soaking for 9min, filtering, washing for 4 times by using absolute ethyl alcohol, and drying at 65 ℃ for 3.5h to obtain oxidized carbon fibers;
(2) modification of oxidized carbon fibers: mixing ammonia methanol solution with the mass fraction of 10% and methyl acrylate according to the mass ratio of 1: 4, uniformly mixing, stirring and reacting at 25 ℃ and 900r/min for 22h, and standing at 45 ℃ and 1.5kPa for 70min to obtain semi-polyamide; mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to a mass ratio of 2.5: 1: 0.4: 60, uniformly mixing, carrying out ultrasonic reaction for 2.5h at 65 ℃ and 35kHz, filtering, washing for 4 times by pure water, drying for 3.5h at 65 ℃, then placing in a methanol solution with 22 times of the mass of the oxidized carbon fiber, adding a semi-substituted polyamide with 3 times of the mass of the oxidized carbon fiber, stirring and reacting for 22h at 25 ℃ and 900r/min, filtering, washing for 4 times by pure water and absolute ethyl alcohol respectively, drying for 5h at 65, and mixing with trans-1, 4-diamino-2-butene and methanol according to a mass ratio of 1: 3: 35, uniformly mixing, stirring and reacting at 25 ℃ and 900r/min for 22 hours, filtering, washing with pure water and absolute ethyl alcohol for 4 times respectively, and drying at 65 ℃ for 5 hours to obtain modified carbon fibers;
(3) preparation of epoxy silane: mixing allyl alcohol glycidyl ether, triethoxysilane and n-hexane in a mass ratio of 1: 1: 9, uniformly mixing, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.04 times that of allyl alcohol glycidyl ether, stirring and refluxing for 5 hours at 75 ℃ and 600r/min, and standing for 3.5 hours at 25 ℃ and 1.5kPa to prepare epoxy silane;
(4) modification: succinic anhydride and polyethylene glycol monomethyl ether are mixed according to the mass ratio of 1: 5, uniformly mixing, stirring at 75 ℃ and 900r/min for 3.5h, adding into thionyl chloride with the mass of 9 times that of polyethylene glycol monomethyl ether, adding tetrahydrofuran with the mass of 0.06 time that of polyethylene glycol monomethyl ether, stirring and reacting at 45 ℃ and 400r/min for 2.5h, heating to 65 ℃, continuing stirring and reacting for 2.5h, and drying at 20 ℃ and 60Pa for 35min to obtain acyl chloride-based polyethylene glycol monomethyl ether; mixing acyl chloride polyethylene glycol monomethyl ether, p-diaminoazobenzene, dichloromethane and triethylamine according to a mass ratio of 1: 0.8: 10: 0.4, stirring the mixture evenly for 2.5 hours at the temperature of 3 ℃ and at the speed of 400r/min, and standing the mixture for 7 hours at the temperature of 15 ℃ and at the pressure of 1.5kPa to prepare azo-polyethylene glycol monomethyl ether; epoxy silane, azo polyethylene glycol monomethyl ether, N-dimethylformamide and 12% ammonia water in mass percentage are mixed according to the mass ratio of 2.5: 1: 9: 11, uniformly mixing, stirring and reacting for 7 hours at 15 ℃ and 900r/min, and drying for 22 hours at 15 ℃ under 6Pa to obtain modified silane;
(5) mixing materials: sodium hydroxide and sodium silicate are mixed according to the mass ratio of 1: 1.5, uniformly mixing to prepare an alkaline activator, and mixing PO42.5 cement, modified carbon fibers, modified silane and the alkaline activator according to a mass ratio of 65: 24: 12: 4, uniformly mixing to prepare the wear-resistant high-strength cement.
Comparative example 4
The preparation method of the wear-resistant high-strength cement of comparative example 4 is different from that of example 2 only in that step (4) is not performed, and step (5) is modified as follows: PO42.5 cement, modified carbon fiber, organic silicon polymer and an alkaline activator are mixed according to the mass ratio of 65: 24: 12: 4, uniformly mixing to prepare the wear-resistant high-strength cement. The remaining steps were performed in the same manner as in example 2.
Comparative example 5
(1) Immersing bagasse in a sodium hypochlorite solution with the mass fraction of 4% at normal temperature and normal pressure, standing for 11h, filtering, washing with pure water for 4 times, soaking in a urea solution with the mass fraction of 35% for 2.5h, filtering, placing in a vacuum tube furnace, standing for 25min at 110 ℃ in a nitrogen atmosphere, standing for 45min at 350 ℃, standing for 25min at 1100 ℃, cooling to room temperature, and taking out to obtain carbon fibers;
(2) preparation of the silicone polymer: mixing allyl alcohol glycidyl ether, triethoxysilane and n-hexane in a mass ratio of 1: 1: 9, uniformly mixing, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.04 times that of allyl alcohol glycidyl ether, stirring and refluxing for 5 hours at the temperature of 75 ℃ and the speed of 600r/min, and standing for 3.5 hours at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare epoxy silane; 2, 3-dihydroxy-1-butene, vinyltriethoxysilane and epoxy silane are mixed according to the mass ratio of 3: 1.5: 2, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.015 time of that of the 2, 3-dihydroxy-1-butene, stirring at 95 ℃ and 400r/min for 25min, heating to 155 ℃, continuing stirring for 7h, cooling to room temperature, and standing at 55 ℃ and 1.5kPa for 35min to obtain an organic silicon polymer;
(3) mixing materials: PO42.5 cement, carbon fiber, organic silicon polymer and an alkaline activator are mixed according to the mass ratio of 65: 24: 12: 4, uniformly mixing to prepare the wear-resistant high-strength cement.
Examples of effects
The following table 1 shows performance analysis results of the compressive properties and the early strength properties of the wear-resistant high-strength cements prepared in examples 1 to 3 and comparative examples 1 to 5 of the present invention.
TABLE 1
| Compressive strength | Early strength | Compressive strength | Early strength | ||
| Example 1 | 61.7MPa | 53.0MPa | Comparative example 2 | 52.7MPa | 35.9MPa |
| Example 2 | 62.2MPa | 53.3MPa | Comparative example 3 | 49.6MPa | 39.9MPa |
| Example 3 | 62.1MPa | 52.9MPa | Comparative example 4 | 50.4MPa | 40.4MPa |
| Comparative example 1 | 60.4MPa | 40.2MPa | Comparative example 5 | 47.8MPa | 31.7MPa |
As can be seen from the comparison of the experimental data of examples 1-3 and comparative examples 1-5 in Table 1, the wear-resistant high-strength cement prepared by the invention has good compression resistance and early strength.
The comparison of the experimental data of examples 1, 2 and 3 and comparative example 1 shows that the early strength of examples 1, 2 and 3 is higher than that of comparative example 1, which indicates that in the modification process of the oxidized carbon fiber, tris (2-aminoethyl) amine is used to perform branching growth on the surface of the oxidized carbon fiber compared with ethylenediamine, so that the prepared modified carbon fiber has higher branching degree and the number of amino groups and imino groups, nitrogen atoms can easily form covalent bonds with metal ions to perform a complexing reaction, so that the dissolution rates of tricalcium silicate and tetracalcium aluminoferrite in cement are improved, the compactness of portland cement is also improved, the supersaturation degree of calcium hydroxide generated by stirring cement with water is improved due to the formation of the complex, a loose crystalline phase structure generated by early hydration of cement is effectively prevented, and the compactness of portland cement is also improved, thereby improving the early strength of the wear-resistant high-strength cement; from the comparison of the experimental data of examples 1, 2 and 3 and comparative example 2, it can be found that the compressive strength and the early strength of examples 1, 2 and 3 are higher than those of comparative example 2, which shows that in the modification process of the oxidized carbon fiber, the final reaction with trans-1, 4-diamino-2-butene improves the number of surface amino groups and improves the effect of the complex reaction, thereby improving the early strength of the wear-resistant high-strength cement; secondly, carbon-carbon double bonds in the trans-1, 4-diamino-2-butene can participate in free radical polymerization reaction initiated by azo bond breakage, so that the compressive strength of the wear-resistant high-strength cement is improved; from a comparison of the experimental data of examples 1, 2,3 and comparative example 3, it can be seen that the high compressive strength of examples 1, 2,3 and comparative example 3 illustrates that the reaction of 2, 3-dihydroxy-1-butene, vinyltriethoxysilane and epoxysilane to form a silicone polymer results in improved structural stability of the silane, meanwhile, the water repellent agent reacts with azo-polyethylene glycol monomethyl ether, and hydrophilic groups are introduced, so that the surface tension is reduced, the wetting capacity of water on cement particles is enhanced, the hydration active points of the cement particles are increased, the cement is solidified and combined more tightly, and in the cement hydration maintenance process, in outdoor sun and alkaline environment, the organic silicon polymer is hydrolyzed into silane with silicon hydroxyl and double bond, the modified carbon fibers and the inorganic particles in the cement are connected by an interface, so that the compressive strength of the wear-resistant high-strength cement is improved; from the comparison of the experimental data of examples 1, 2 and 3 and comparative example 4, it can be seen that the compressive strength of examples 1, 2 and 3 is higher than that of comparative example 4, which illustrates that the reaction of the organosilicon polymer and the azo-polyethylene glycol monomethyl ether increases the hydrophilic effect, reduces the surface tension, enhances the wetting ability of water to cement particles, and simultaneously the azo bond can initiate the polymerization of double bonds, thereby improving the compressive strength of the wear-resistant high-strength cement.
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 attributes 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 (10)
1. The preparation method of the wear-resistant high-strength cement is characterized in that the wear-resistant high-strength cement is prepared by mixing cement, modified carbon fibers, a modified organic silicon polymer and an alkaline activator.
2. The method for preparing wear-resistant high-strength cement according to claim 1, wherein the modified carbon fiber is prepared by carbonizing and oxidizing bagasse into oxidized carbon fiber, and reacting the oxidized carbon fiber with tris (2-aminoethyl) amine, semi-substituted polyamide and trans-1, 4-diamino-2-butene in sequence.
3. The method as claimed in claim 2, wherein the semi-substituted polyamide is prepared by reacting ammonia and methyl acrylate.
4. The method for preparing the wear-resistant high-strength cement as claimed in claim 1, wherein the modified organosilicon polymer is prepared by reacting allyl alcohol glycidyl ether with triethoxysilane to prepare epoxy silane, reacting 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane to prepare organosilicon polymer, and reacting the organosilicon polymer with azo polyethylene glycol monomethyl ether.
5. The method for preparing the wear-resistant high-strength cement as claimed in claim 1, wherein the method for preparing the wear-resistant high-strength cement comprises the following steps:
(1) oxidation treatment: immersing carbon fibers in concentrated nitric acid, stirring and reacting for 2-3 h at 70-80 ℃ and 800-1000 r/min, taking out, placing in pure water, soaking for 8-10 min, filtering, washing for 3-5 times by using absolute ethyl alcohol, and drying for 3-4 h at 60-70 ℃ to obtain oxidized carbon fibers;
(2) modification of oxidized carbon fibers: mixing oxidized carbon fiber, tri (2-aminoethyl) amine, sodium hydroxide and pure water according to a mass ratio of 2: 1: 0.3: 50-3: 1: 0.5: 70, uniformly mixing, carrying out ultrasonic reaction for 2-3 h at 60-70 ℃ and 30-40 kHz, filtering, washing for 3-5 times by pure water, drying for 3-4 h at 60-70 ℃, then placing in a methanol solution with the mass of 20-25 times that of the oxidized carbon fiber, adding semi-substituted polyamide with the mass of 2-4 times that of the oxidized carbon fiber, stirring and reacting for 20-24 h at 20-30 ℃ and 800-1000 r/min, filtering, washing for 3-5 times by pure water and absolute ethyl alcohol respectively, drying for 4-6 h at 60-70, and mixing with trans-1, 4-diamino-2-butene and methanol according to the mass ratio of 1: 3: 30-1: 5: 40, uniformly mixing, stirring and reacting for 20-24 hours at 20-30 ℃ at 800-1000 r/min, filtering, washing for 3-5 times by using pure water and absolute ethyl alcohol respectively, and drying for 4-6 hours at 60-70 ℃ to obtain modified carbon fibers;
(3) preparation of the silicone polymer: 2, 3-dihydroxy-1-butene, vinyl triethoxysilane and epoxy silane are mixed according to the mass ratio of 2: 1: 1-4: 2: 3, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.01-0.02 time of that of 2, 3-dihydroxy-1-butene, stirring at 90-100 ℃ for 20-30 min at 300-500 r/min, heating to 150-160 ℃, continuing stirring for 6-8 h, cooling to room temperature, standing at 50-60 ℃ for 30-40 min at 1-2 kPa to obtain an organic silicon polymer;
(4) modification of the silicone polymer: the preparation method comprises the following steps of (1) mixing an organic silicon polymer, azo polyethylene glycol monomethyl ether, N-dimethylformamide and ammonia water with the mass fraction of 10-15% in a mass ratio of 2: 1: 8: 10-3: 1: 10: 12, uniformly mixing, stirring and reacting for 6-8 h at 10-20 ℃ at 800-1000 r/min, and drying for 20-24 h at 10-20 ℃ under 40-80 Pa to prepare a modified organic silicon polymer;
(5) mixing materials: sodium hydroxide and sodium silicate are mixed according to the mass ratio of 1: 1-1: 2, uniformly mixing the raw materials to prepare an alkaline activator, and mixing cement, modified carbon fibers, a modified organic silicon polymer and the alkaline activator according to a mass ratio of 60: 20: 10: 3-70: 28: 15: 5, uniformly mixing to prepare the wear-resistant high-strength cement.
6. The method for preparing the wear-resistant high-strength cement as claimed in claim 5, wherein the carbon fiber in the step (1) is prepared by: immersing bagasse in a sodium hypochlorite solution with the mass fraction of 3-5% at normal temperature and normal pressure, standing for 10-12 h, filtering, washing for 3-5 times with pure water, soaking in a urea solution with the mass fraction of 30-40% for 2-3 h, filtering, placing in a vacuum tube furnace, standing for 20-30 min at 100-120 ℃ in a nitrogen atmosphere, standing for 40-50 min at 300-400 ℃, standing for 20-30 min at 1000-1200 ℃, cooling to room temperature, and taking out to prepare the bagasse.
7. The method for preparing wear-resistant high-strength cement according to claim 5, wherein the semi-substituted polyamide in the step (2) is prepared by: mixing 8-12% of ammonia methanol solution and methyl acrylate according to a mass ratio of 1: 3-1: 5, uniformly mixing, stirring and reacting for 20-24 hours at 20-30 ℃ at 800-1000 r/min, and standing for 60-80 minutes at 40-50 ℃ under 1-2 kPa to prepare the water-based paint.
8. The method for preparing the wear-resistant high-strength cement as claimed in claim 5, wherein the epoxy silane in the step (3) is prepared by: mixing allyl alcohol glycidyl ether, triethoxysilane and n-hexane in a mass ratio of 1: 1: 8-1: 1: 10, adding divinyl tetramethyl disiloxane platinum salt with the mass of 0.03-0.05 time that of allyl alcohol glycidyl ether, stirring and refluxing for 4-6 hours at 70-80 ℃ and 500-800 r/min, and standing for 3-4 hours at 20-30 ℃ and 1-2 kPa to prepare the allyl alcohol glycidyl ether.
9. The method for preparing the wear-resistant high-strength cement as claimed in claim 5, wherein the azo-based polyethylene glycol monomethyl ether prepared in step (4) is prepared by: succinic anhydride and polyethylene glycol monomethyl ether are mixed according to the mass ratio of 1: 4-1: 6, uniformly mixing, stirring for 3-4 hours at 70-80 ℃ at 800-1000 r/min, adding into thionyl chloride with the mass of 8-10 times of that of polyethylene glycol monomethyl ether, adding tetrahydrofuran with the mass of 0.04-0.08 time of that of polyethylene glycol monomethyl ether, stirring and reacting for 2-3 hours at 40-50 ℃ at 300-500 r/min, heating to 60-70 ℃, continuing stirring and reacting for 2-3 hours, and drying for 30-40 minutes at 10-30 ℃ under 40-80 Pa to obtain acyl chloride-based polyethylene glycol monomethyl ether; mixing acyl chloride polyethylene glycol monomethyl ether, p-diaminoazobenzene, dichloromethane and triethylamine according to a mass ratio of 1: 0.8: 10: 0.4-1: 1: 12: 1, uniformly mixing, stirring at 0-5 ℃ for 2-3 h at 300-500 r/min, and standing at 10-20 ℃ for 6-8 h under 1-2 kPa to prepare the water-based paint.
10. The method for preparing the wear-resistant high-strength cement as claimed in claim 5, wherein the cement in the step (5) is ordinary portland cement.
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