CN115819039A - High-strength environment-friendly artistic micro-cement and preparation method thereof - Google Patents
High-strength environment-friendly artistic micro-cement and preparation method thereof Download PDFInfo
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- CN115819039A CN115819039A CN202211485504.8A CN202211485504A CN115819039A CN 115819039 A CN115819039 A CN 115819039A CN 202211485504 A CN202211485504 A CN 202211485504A CN 115819039 A CN115819039 A CN 115819039A
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- 239000004568 cement Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 40
- 239000011347 resin Substances 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000011398 Portland cement Substances 0.000 claims abstract description 7
- 229920003086 cellulose ether Polymers 0.000 claims abstract description 7
- 239000010881 fly ash Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 63
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 48
- 238000002156 mixing Methods 0.000 claims description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000758 substrate Substances 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 239000006004 Quartz sand Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 25
- 239000000706 filtrate Substances 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 24
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 24
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 22
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 22
- -1 polydimethylsiloxane Polymers 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000003822 epoxy resin Substances 0.000 claims description 14
- 229920000647 polyepoxide Polymers 0.000 claims description 14
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 12
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 12
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 12
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 11
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 11
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 11
- ASOKPJOREAFHNY-UHFFFAOYSA-N 1-Hydroxybenzotriazole Chemical compound C1=CC=C2N(O)N=NC2=C1 ASOKPJOREAFHNY-UHFFFAOYSA-N 0.000 claims description 10
- 239000004593 Epoxy Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 6
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 125000003700 epoxy group Chemical group 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 5
- 238000005034 decoration Methods 0.000 description 5
- 239000003973 paint Substances 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical group ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- 238000006845 Michael addition reaction Methods 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses high-strength environment-friendly artistic micro-cement and a preparation method thereof, wherein the modified cement comprises a component A and a component B, and the component A comprises the following raw materials in parts by weight: 80-100 parts of portland cement, 10-30 parts of fly ash, 30-35 parts of modified resin, 120-150 parts of reinforcing filler and 5-10 parts of cellulose ether MKX15000PP20; the component B is a curing agent; after the component A and the component B are blended, the curing agent reacts with an epoxy group on the modified resin, so that the modified resin is crosslinked and cured, a large number of organic silicon resin chain segments are endowed to the modified resin, the waterproof performance of the micro cement is improved, the micro cement is irradiated by ultraviolet light when not cured, the sulfydryl on the surface of the reinforcing filler irradiated by the ultraviolet light can be grafted with double bonds in molecules of the modified resin, and the curing strength of the micro cement is improved.
Description
Technical Field
The invention relates to the technical field of micro-cement preparation, in particular to high-strength environment-friendly artistic micro-cement and a preparation method thereof.
Background
The wall surface decoration material is a material which is used for building wall surfaces to play a role in decoration and enables the building wall surfaces to be attractive and tidy, and can be generally divided into a painting class, a facing material class and a novel wall material class. The paint wall decoration material represented by the latex paint has the advantages of light weight, bright color, convenient construction and maintenance and the like, has the largest market share, but also has the problems of fixed texture, poor durability, easy color loss and fading and the like. With the continuous promotion of the requirements of people on the architectural decoration style, the traditional wall decoration material is difficult to meet the requirements. The micro-cement is novel surface decorative cement which is started in recent years, can realize integral seamless construction of wall surfaces, ground surfaces and top surfaces, and realizes space extension to the maximum extent, so that the micro-cement is required to have the characteristics of high strength, strong wear resistance, excellent water resistance, smoothness, pollution resistance, lower content of organic volatile matters than paint and the like.
Disclosure of Invention
The invention aims to provide high-strength environment-friendly artistic micro-cement and a preparation method thereof, and solves the problem of low mechanical strength of the artistic micro-cement at the present stage.
The purpose of the invention can be realized by the following technical scheme:
the high-strength environment-friendly artistic micro-cement comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 80-100 parts of Portland cement, 30-35 parts of modified resin, 120-150 parts of reinforcing filler and 5-10 parts of cellulose ether MKX15000PP20; the component B is a curing agent.
The mass ratio of the component A to the component B is 2-3:1.
The high-strength environment-friendly artistic micro-cement is prepared by the following steps:
weighing the raw materials in parts by weight, uniformly mixing the component A raw material with water, then adding the component B raw material, and uniformly mixing to obtain the high-strength environment-friendly artistic micro-cement.
Further, the modified resin is prepared by the following steps:
step A1: uniformly mixing KH550, concentrated hydrochloric acid and methanol, stirring for 6-8 days at the rotation speed of 200-300r/min and the temperature of 60-70 ℃, filtering to remove filtrate, dispersing a substrate in ethanol, adding acrylic acid, and reacting for 2-3 hours at the rotation speed of 150-200r/min and the temperature of 20-25 ℃ to obtain cage-type silsesquioxane;
step A2: uniformly mixing epoxy resin EP-20, dibenzoyl peroxide and tetrahydrofuran to obtain a resin solution, uniformly mixing cage-type silsesquioxane, methyl methacrylate, methoxy polyethylene glycol acrylate and tetrahydrofuran, stirring at the rotation speed of 150-200r/min and the temperature of 80-85 ℃ for 15-30min, heating to 120-130 ℃, adding the resin solution, reacting for 3-4h, and distilling to remove tetrahydrofuran to obtain the modified resin.
Further, the volume ratio of the KH550 to the concentrated hydrochloric acid in the step A1 is 30, the mass fraction of the concentrated hydrochloric acid is 36%, and the mass ratio of the substrate to the acrylic acid is 1:3.
Further, the dosage ratio of the epoxy resin EP-20, dibenzoyl peroxide and tetrahydrofuran in the step A2 is 15g.
Further, the curing agent is prepared by the following steps:
uniformly mixing dihydroxy polydimethylsiloxane, a sodium hydroxide solution and epichlorohydrin, reacting for 6-8h at the rotation speed of 300-500r/min and the temperature of 30-40 ℃ to obtain epoxy polydimethylsiloxane, mixing the epoxy polydimethylsiloxane and ethylenediamine, and stirring and reacting for 5-7h at the rotation speed of 150-200r/min and the temperature of 50-60 ℃ to obtain the curing agent.
Further, the molar ratio of hydroxyl groups on the dihydroxy polydimethylsiloxane, sodium hydroxide and epichlorohydrin is 1.
Further, the reinforcing filler is prepared by the following steps:
step B1: dispersing quartz sand in ethanol, adding KH550 and deionized water, stirring for 3-5h at the rotation speed of 200-300r/min and the temperature of 60-70 ℃, filtering to remove filtrate, uniformly mixing a substrate, carboxymethyl cellulose, 1-hydroxybenzotriazole and deionized water, reacting for 6-8h at the rotation speed of 150-200r/min and the temperature of 25-30 ℃, filtering to remove filtrate, and preparing pretreated quartz sand;
and step B2: dispersing pretreated quartz sand in a sodium hydroxide solution, carrying out heat preservation treatment for 1-1.5h at the temperature of 20-25 ℃, filtering to remove filtrate, uniformly mixing a substrate, glycidyl methacrylate and dioxane, and reacting for 7-9h at the rotation speed of 200-300r/min and the temperature of 60-80 ℃ to obtain the modified quartz sand.
And step B3: dispersing the modified quartz sand in tetrahydrofuran, introducing excessive hydrogen sulfide gas, stirring and reacting for 30-40h at the rotation speed of 150-200r/min and the temperature of 45-50 ℃, filtering to remove filtrate, washing a substrate with ethanol, and drying to obtain the reinforcing filler.
Further, the dosage of KH550 in the step B1 is 5-8% of the mass of the quartz sand, and the mass ratio of the substrate, the carboxymethyl cellulose and the 1-hydroxybenzotriazole is 3.
Further, the mass fraction of the sodium hydroxide solution in the step B2 is 15%, and the mass ratio of the substrate to the glycidyl methacrylate is 1:5.
The invention has the beneficial effects that: the invention discloses a high-strength environment-friendly artistic micro-cement, which comprises a component A and a component B, wherein the component A comprises: portland cement, modified resin, a reinforcing filler and cellulose ether MKX15000PP20; the component B is a curing agent; KH500 is used as a raw material for polymerization, amino is converted into ammonium chloride group under the action of hydrochloric acid, and then reacts with acrylic acid, so that the amino chloride group reacts with carboxyl to prepare cage-type silsesquioxane, under the action of dibenzoyl peroxide, alpha-H on the carbon adjacent to the ether bond in the epoxy resin EP-20 forms free radicals which can perform graft reaction with carbon-carbon double bonds, methyl methacrylate, methoxy polyethylene glycol acrylate and partial double bonds on the cage-type silsesquioxane are polymerized to form polyacrylic acid taking the cage-type silsesquioxane as a core and are grafted on the molecular chain of the epoxy resin EP-20 to prepare the modified resin, and a curing agent takes dihydroxy polydimethylsiloxane and epoxy chloropropane as raw materials for reaction, so that hydroxyl at two ends of the dihydroxy polydimethylsiloxane reacts with chlorine atom sites on the epoxy chloropropane, and then reacts with ethylenediamine to form amino end capping, preparing a curing agent, taking quartz sand and KH550 as raw materials as a reinforcing filler, grafting active amino groups on the surface of the quartz sand, adding carboxymethyl cellulose, dehydrating and condensing carboxyl groups on the carboxymethyl cellulose and the surface amino groups to form pretreated quartz sand of the quartz sand coated with cellulose, treating the pretreated quartz sand with a sodium hydroxide solution to react hydroxyl groups in the surface cellulose with sodium hydroxide, reacting with glycidyl methacrylate, alkalifying and ring-opening glycidyl methacrylate, introducing double bonds on the surface, treating with hydrogen sulfide gas, converting the double bonds into sulfydryl groups through a Michael addition reaction to prepare the reinforcing filler, blending the component A and the component B, reacting the curing agent with epoxy groups on modified resin to crosslink and cure the modified resin, and endowing the modified resin with a large number of organic silicon resin chain segments, the waterproof performance of the micro cement is improved, the micro cement is not cured and is irradiated by ultraviolet light, the sulfydryl on the surface of the reinforcing filler irradiated by the ultraviolet light can be grafted with double bonds in modified resin molecules, so that the curing strength of the micro cement is improved, meanwhile, the hyperbranched structure of the modified resin and the core-shell structure of the modified quartz sand are improved, the mechanical strength of the micro cement is greatly improved, and the environmental protection of the micro cement is guaranteed without adding other organic solvents.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, 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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-strength environment-friendly artistic micro-cement comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 80 parts of portland cement, 30 parts of modified resin, 10 parts of fly ash, 120 parts of reinforcing filler and 5 parts of cellulose ether MKX15000PP20; the component B is a curing agent.
The mass ratio of component A to component B was 2:1.
The high-strength environment-friendly artistic micro-cement is prepared by the following steps:
weighing the raw materials in parts by weight, uniformly mixing the component A raw material with water, then adding the component B raw material, and uniformly mixing to obtain the high-strength environment-friendly artistic micro-cement.
The amount of water used is 40% by mass of component A.
The modified resin is prepared by the following steps:
step A1: uniformly mixing KH550, concentrated hydrochloric acid and methanol, stirring for 6 days at the rotation speed of 200r/min and the temperature of 60 ℃, filtering to remove filtrate, dispersing a substrate in ethanol, adding acrylic acid, and reacting for 2 hours at the rotation speed of 150r/min and the temperature of 20 ℃ to obtain cage-type silsesquioxane;
step A2: uniformly mixing epoxy resin EP-20, dibenzoyl peroxide and tetrahydrofuran to obtain a resin solution, uniformly mixing cage-type silsesquioxane, methyl methacrylate, methoxy polyethylene glycol acrylate and tetrahydrofuran, stirring at the rotation speed of 150r/min and the temperature of 80 ℃ for 15min, heating to 120 ℃, adding the resin solution, reacting for 3h, and distilling to remove tetrahydrofuran to obtain the modified resin.
The volume ratio of KH550 to concentrated hydrochloric acid in the step A1 is 30, the mass fraction of the concentrated hydrochloric acid is 36%, and the mass ratio of the substrate to the acrylic acid is 1:3.
The dosage ratio of the epoxy resin EP-20, the dibenzoyl peroxide and the tetrahydrofuran in the step A2 is 15g.
The curing agent is prepared by the following steps:
uniformly mixing dihydroxy polydimethylsiloxane, a sodium hydroxide solution and epoxy chloropropane, reacting for 6 hours at the rotation speed of 300r/min and the temperature of 30 ℃ to prepare epoxy polydimethylsiloxane, mixing the epoxy polydimethylsiloxane and ethylenediamine, and stirring and reacting for 5 hours at the rotation speed of 150r/min and the temperature of 50 ℃ to prepare the curing agent.
The molar ratio of hydroxyl groups on the dihydroxy polydimethylsiloxane, sodium hydroxide and epichlorohydrin is 1.
The reinforcing filler is prepared by the following steps:
step B1: dispersing quartz sand in ethanol, adding KH550 and deionized water, stirring for 3h at the rotation speed of 200r/min and the temperature of 60 ℃, filtering to remove filtrate, uniformly mixing a substrate, carboxymethyl cellulose, 1-hydroxybenzotriazole and deionized water, reacting for 6h at the rotation speed of 150r/min and the temperature of 25 ℃, and filtering to remove the filtrate to obtain pretreated quartz sand;
and step B2: dispersing pretreated quartz sand in a sodium hydroxide solution, carrying out heat preservation treatment for 1h at the temperature of 20 ℃, filtering to remove filtrate, uniformly mixing a substrate, glycidyl methacrylate and dioxane, and reacting for 7h at the rotation speed of 200r/min and the temperature of 60 ℃ to obtain the modified quartz sand.
And step B3: dispersing the modified quartz sand in tetrahydrofuran, introducing excessive hydrogen sulfide gas, stirring and reacting for 30 hours at the rotation speed of 150r/min and the temperature of 45 ℃, filtering to remove filtrate, washing a substrate with ethanol, and drying to obtain the reinforcing filler.
The dosage of KH550 in the step B1 is 5% of the mass of the quartz sand, and the mass ratio of the substrate, the carboxymethyl cellulose and the 1-hydroxybenzotriazole is 3.
The mass fraction of the sodium hydroxide solution in the step B2 is 15 percent, and the mass ratio of the substrate to the glycidyl methacrylate is 1:5.
Example 2
The high-strength environment-friendly artistic micro-cement comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 90 parts of portland cement, 20 parts of fly ash, 33 parts of modified resin, 150 parts of reinforcing filler and 8 parts of cellulose ether MKX15000PP20; the component B is a curing agent.
The mass ratio of the component A to the component B is 2.5.
The high-strength environment-friendly artistic micro-cement is prepared by the following steps:
weighing the raw materials in parts by weight, uniformly mixing the component A raw material with water, then adding the component B raw material, and uniformly mixing to obtain the high-strength environment-friendly artistic micro-cement.
The amount of water used is 40% by mass of component A.
The modified resin is prepared by the following steps:
step A1: uniformly mixing KH550, concentrated hydrochloric acid and methanol, stirring for 7 days at the rotation speed of 200r/min and the temperature of 65 ℃, filtering to remove filtrate, dispersing a substrate in ethanol, adding acrylic acid, and reacting for 2.5 hours at the rotation speed of 150r/min and the temperature of 20 ℃ to obtain cage-type silsesquioxane;
step A2: uniformly mixing epoxy resin EP-20, dibenzoyl peroxide and tetrahydrofuran to obtain a resin solution, uniformly mixing cage-type silsesquioxane, methyl methacrylate, methoxy polyethylene glycol acrylate and tetrahydrofuran, stirring at the rotation speed of 150r/min and the temperature of 85 ℃ for 20min, heating to 125 ℃, adding the resin solution, reacting for 3.5h, and distilling to remove tetrahydrofuran to obtain the modified resin.
The volume ratio of KH550 to concentrated hydrochloric acid in the step A1 is 30, the mass fraction of the concentrated hydrochloric acid is 36%, and the mass ratio of the substrate to the acrylic acid is 1:3.
The dosage ratio of the epoxy resin EP-20, the dibenzoyl peroxide and the tetrahydrofuran in the step A2 is 15g.
The curing agent is prepared by the following steps:
uniformly mixing dihydroxy polydimethylsiloxane, a sodium hydroxide solution and epoxy chloropropane, reacting for 7 hours at the rotation speed of 300r/min and the temperature of 35 ℃ to prepare epoxy polydimethylsiloxane, mixing the epoxy polydimethylsiloxane and ethylenediamine, and stirring and reacting for 6 hours at the rotation speed of 150r/min and the temperature of 55 ℃ to prepare the curing agent.
The molar ratio of hydroxyl groups on the dihydroxy polydimethylsiloxane, sodium hydroxide and epichlorohydrin is 1.
The reinforcing filler is prepared by the following steps:
step B1: dispersing quartz sand in ethanol, adding KH550 and deionized water, stirring for 4h at the rotation speed of 300r/min and the temperature of 65 ℃, filtering to remove filtrate, uniformly mixing a substrate, carboxymethyl cellulose, 1-hydroxybenzotriazole and deionized water, reacting for 7h at the rotation speed of 150r/min and the temperature of 28 ℃, and filtering to remove the filtrate to obtain pretreated quartz sand;
and step B2: dispersing pretreated quartz sand in a sodium hydroxide solution, carrying out heat preservation treatment for 1h at the temperature of 25 ℃, filtering to remove filtrate, uniformly mixing a substrate, glycidyl methacrylate and dioxane, and reacting for 8h at the rotation speed of 200r/min and the temperature of 70 ℃ to obtain the modified quartz sand.
And step B3: dispersing the modified quartz sand in tetrahydrofuran, introducing excessive hydrogen sulfide gas, stirring and reacting for 35 hours at the rotation speed of 150r/min and the temperature of 50 ℃, filtering to remove filtrate, washing a substrate with ethanol, and drying to obtain the reinforcing filler.
The dosage of KH550 in the step B1 is 6% of the mass of the quartz sand, and the mass ratio of the substrate, the carboxymethyl cellulose and the 1-hydroxybenzotriazole is 3.
The mass fraction of the sodium hydroxide solution in the step B2 is 15 percent, and the mass ratio of the substrate to the glycidyl methacrylate is 1:5.
Example 3
The high-strength environment-friendly artistic micro-cement comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of portland cement, 30 parts of fly ash, 35 parts of modified resin, 150 parts of reinforcing filler and 10 parts of cellulose ether MKX15000PP20; the component B is a curing agent.
The mass ratio of component A to component B was 3:1.
The high-strength environment-friendly artistic micro-cement is prepared by the following steps:
weighing the raw materials in parts by weight, uniformly mixing the component A raw material with water, then adding the component B raw material, and uniformly mixing to obtain the high-strength environment-friendly artistic micro-cement.
The amount of water used is 40% by mass of component A.
The modified resin is prepared by the following steps:
step A1: uniformly mixing KH550, concentrated hydrochloric acid and methanol, stirring for 8 days at the rotation speed of 300r/min and the temperature of 70 ℃, filtering to remove filtrate, dispersing a substrate in ethanol, adding acrylic acid, and reacting for 3 hours at the rotation speed of 200r/min and the temperature of 25 ℃ to obtain cage-type silsesquioxane;
step A2: uniformly mixing epoxy resin EP-20, dibenzoyl peroxide and tetrahydrofuran to obtain a resin solution, uniformly mixing cage-type silsesquioxane, methyl methacrylate, methoxy polyethylene glycol acrylate and tetrahydrofuran, stirring at the rotation speed of 200r/min and the temperature of 85 ℃ for 30min, heating to 130 ℃, adding the resin solution, reacting for 4h, and distilling to remove tetrahydrofuran to obtain the modified resin.
The volume ratio of KH550 to concentrated hydrochloric acid in the step A1 is 30, the mass fraction of the concentrated hydrochloric acid is 36%, and the mass ratio of the substrate to the acrylic acid is 1:3.
The dosage ratio of the epoxy resin EP-20, the dibenzoyl peroxide and the tetrahydrofuran in the step A2 is 15g.
The curing agent is prepared by the following steps:
uniformly mixing dihydroxy polydimethylsiloxane, a sodium hydroxide solution and epoxy chloropropane, reacting for 8 hours at the rotation speed of 500r/min and the temperature of 40 ℃ to prepare epoxy polydimethylsiloxane, mixing the epoxy polydimethylsiloxane and ethylenediamine, and stirring and reacting for 7 hours at the rotation speed of 200r/min and the temperature of 60 ℃ to prepare the curing agent.
The molar ratio of hydroxyl groups on the dihydroxy polydimethylsiloxane, sodium hydroxide and epichlorohydrin is 1.
The reinforcing filler is prepared by the following steps:
step B1: dispersing quartz sand in ethanol, adding KH550 and deionized water, stirring for 5h at the rotation speed of 300r/min and the temperature of 70 ℃, filtering to remove filtrate, uniformly mixing a substrate, carboxymethyl cellulose, 1-hydroxybenzotriazole and deionized water, reacting for 8h at the rotation speed of 200r/min and the temperature of 30 ℃, and filtering to remove the filtrate to obtain pretreated quartz sand;
and step B2: dispersing pretreated quartz sand in a sodium hydroxide solution, carrying out heat preservation treatment for 1.5h at the temperature of 25 ℃, filtering to remove filtrate, uniformly mixing a substrate, glycidyl methacrylate and dioxane, and reacting for 9h at the rotation speed of 300r/min and the temperature of 80 ℃ to obtain the modified quartz sand.
And step B3: dispersing the modified quartz sand in tetrahydrofuran, introducing excessive hydrogen sulfide gas, stirring and reacting for 40h at the rotation speed of 200r/min and the temperature of 50 ℃, filtering to remove filtrate, washing a substrate with ethanol, and drying to obtain the reinforcing filler.
The dosage of KH550 in the step B1 is 5-8% of the mass of the quartz sand, and the mass ratio of the substrate, the carboxymethyl cellulose and the 1-hydroxybenzotriazole is 3.
The mass fraction of the sodium hydroxide solution in the step B2 is 15 percent, and the mass ratio of the substrate to the glycidyl methacrylate is 1:5.
Comparative example 1
In this comparative example, silica sand was used in place of the reinforcing filler in comparison with example 1, and the rest of the procedure was the same.
Comparative example 2
This comparative example compared with example 1, the epoxy resin EP-20 was used in place of the modified resin, and the procedure was the same.
Comparative example 3
This comparative example compared with example 1, in which the reinforcing filler was replaced by an epoxy resin EP-20 and by quartz sand, the rest of the procedure was the same.
The micro cements prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for compressive strength and flexural strength according to the standard of GB/T17671-1999, and the results are shown in the following table;
from the above table, it can be seen that the micro cement prepared in examples 1-3 has good compressive and flexural strength, and ensures the wear-resistant effect of the micro cement.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (9)
1. The high-strength environment-friendly artistic micro-cement is characterized in that: the composite material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 80-100 parts of portland cement, 10-30 parts of fly ash, 30-35 parts of modified resin, 120-150 parts of reinforcing filler and 5-10 parts of cellulose ether MKX15000PP20; the component B is a curing agent;
the modified resin is prepared by the following steps:
step A1: mixing KH550, concentrated hydrochloric acid and methanol, stirring, filtering to remove filtrate, dispersing a substrate in ethanol, adding acrylic acid, and reacting to obtain cage-type silsesquioxane;
step A2: uniformly mixing epoxy resin EP-20, dibenzoyl peroxide and tetrahydrofuran to obtain a resin solution, mixing and stirring cage-type silsesquioxane, methyl methacrylate, methoxy polyethylene glycol acrylate and tetrahydrofuran, heating, adding the resin solution, and reacting to obtain the modified resin.
2. The high-strength environment-friendly artistic micro-cement as claimed in claim 1, wherein: the volume ratio of KH550 to concentrated hydrochloric acid in the step A1 is 30, and the mass ratio of the substrate to acrylic acid is 1:3.
3. The high-strength environment-friendly artistic micro-cement as claimed in claim 1, wherein: the dosage ratio of the epoxy resin EP-20, the dibenzoyl peroxide and the tetrahydrofuran in the step A2 is 15g.
4. The high-strength environment-friendly artistic micro-cement as claimed in claim 1, wherein: the curing agent is prepared by the following steps:
mixing dihydroxy polydimethylsiloxane, a sodium hydroxide solution and epichlorohydrin for reaction to prepare epoxy polydimethylsiloxane, mixing the epoxy polydimethylsiloxane and ethylenediamine, and stirring for reaction to prepare the curing agent.
5. The high-strength environment-friendly artistic micro-cement as claimed in claim 4, wherein: the molar ratio of hydroxyl groups on the dihydroxy polydimethylsiloxane, sodium hydroxide and epichlorohydrin is 1.
6. The high-strength environment-friendly artistic micro-cement as claimed in claim 1, wherein: the reinforcing filler is prepared by the following steps:
step B1: dispersing quartz sand in ethanol, adding KH550 and deionized water, stirring, filtering to remove filtrate, and mixing and reacting a substrate, carboxymethyl cellulose, 1-hydroxybenzotriazole and deionized water to obtain pretreated quartz sand;
and step B2: dispersing the pretreated quartz sand in a sodium hydroxide solution, carrying out heat preservation treatment, filtering to remove filtrate, and mixing and reacting a substrate, glycidyl methacrylate and dioxane to obtain the modified quartz sand.
And step B3: dispersing the modified quartz sand in tetrahydrofuran, introducing excessive hydrogen sulfide gas, stirring for reaction, filtering to remove filtrate, washing a substrate with ethanol, and drying to obtain the reinforcing filler.
7. The high-strength environment-friendly artistic micro-cement as claimed in claim 6, wherein: the dosage of the KH550 in the step B1 is 5-8% of the mass of the quartz sand, and the mass ratio of the substrate, the carboxymethyl cellulose and the 1-hydroxybenzotriazole is 3.
8. The high-strength environment-friendly artistic micro-cement as claimed in claim 6, wherein: the mass ratio of the substrate and the glycidyl methacrylate in step B2 is 1:5.
9. The preparation method of the high-strength environment-friendly artistic micro-cement as claimed in claim 1, wherein the preparation method comprises the following steps: the method specifically comprises the following steps:
weighing the raw materials in parts by weight, uniformly mixing the component A raw material with water, then adding the component B raw material, and uniformly mixing to obtain the high-strength environment-friendly artistic micro-cement.
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