A kind of thermal insulation dry-mixed mortar with Yellow River sand for interior walls and its preparation process
By spray-coating and wrapping the vitrified microbeads with acrylic acid-urea-formaldehyde resin blended emulsion and coating and modifying the water-quenched manganese slag with a styrene-propane-silicon emulsion, the problem of easy breakage of the vitrified microbeads and low cross-linking density of the coating modifier during the stirring process is solved, and the effect of improving the compressive strength and performance of the thermal insulation dry powder mortar is achieved.
Patent Information
- Application Number
- CN202311424928.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-31
- Publication Date
- 2025-06-20
- Estimated Expiration
- 2043-10-31
AI Technical Summary
Existing vitrified microbeads are prone to break during stirring, resulting in poor insulation performance. The cross-linking density of commonly used coating modifiers is low, the compressive strength is not greatly improved, and the increase in pores leads to a decrease in compressive strength.
The vitrified microbeads were sprayed and wrapped with acrylic-urea-formaldehyde resin blend emulsion to form a three-dimensional mesh film with high cross-linking density, and the water-quenched manganese slag was coated and modified by styrene-propane-silicon emulsion to reduce the opening area of the holes and improve the compressive strength.
The compressive strength of vitrified microbeads is improved, the increase in pores is reduced, and the overall performance of thermally insulated dry powder mortar is enhanced.
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Figure CN117342848B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to dry-mixed mortar, and particularly to a thermal insulation dry-mixed mortar for interior walls using Yellow River sand and its preparation process. Background Art
[0002] To reduce the hidden dangers brought by the large accumulation of Yellow River sediment to water conservancy projects and at the same time realize the resource utilization of Yellow River sediment, Yellow River sand has gradually developed into a new type of building material and is widely used in the preparation of dry-mixed mortar. The vitrified microbead thermal insulation dry-mixed mortar is an inorganic thermal insulation material commonly used for interior wall insulation. Expanded vitrified microbeads are an inorganic glassy mineral material, showing irregular spherical particles with a porous cavity structure inside, having characteristics such as light weight, high porosity, and low thermal conductivity. However, vitrified microbeads are brittle and are extremely easy to break during the stirring process, resulting in a deterioration of the thermal insulation performance. Usually, organic high-molecular compounds such as phenolic resin are used to coat and modify the vitrified microbeads to improve the density and cylinder compressive strength, increasing the number of effective thermal insulation glass beads.
[0003] After coating and modification, a thin film will be formed on the surface of the vitrified microbeads to protect the glass beads from collisions during the stirring process. However, the cross-linking density of the thin film formed by the commonly used coating modifiers is relatively low, and the improvement of the compressive strength of the vitrified microbeads is not significant. At the same time, due to the large amount of glass beads doped in the thermal insulation mortar, the interfacial area between the vitrified microbeads and the cement paste matrix increases, resulting in an increase in pores, and the pores are easily connected to each other to form cracks or defects, causing the compressive strength of the mortar to decrease and affecting the use of the thermal insulation dry-mixed mortar. Therefore, a thermal insulation dry-mixed mortar for interior walls using Yellow River sand and its preparation process are needed to solve the above problems. Summary of the Invention
[0004] In view of the above deficiencies of the prior art, the purpose of the present invention is to provide a thermal insulation dry-mixed mortar for interior walls using Yellow River sand and its preparation process.
[0005] A thermal insulation dry-mixed mortar for interior walls using Yellow River sand and its preparation process specifically include the following steps:
[0006] S1: Surface modification pretreatment of Yellow River sand
[0007] The Yellow River sand is hydroxylated with a hydroxylation reagent, washed with water, dried, silicon coupling agent and toluene are added for silicon coupling reaction, the product is washed with toluene, dried, an initiator and toluene are added, acrylic acid is dropped for reaction, and the product is washed with toluene and dried to obtain surface-modified Yellow River sand;
[0008] S2: Preparation of acrylic-urea formaldehyde resin blend emulsion
[0009] The core pre-emulsion and the shell pre-emulsion are subjected to polymerization reaction to obtain an acrylic emulsion. A urea formaldehyde resin solution is prepared with deionized water, and the acrylic emulsion and the urea formaldehyde resin solution are stirred and mixed to obtain a blend emulsion;
[0010] S3: Spraying and coating of the vitrified microspheres with the blended emulsion
[0011] Mix 3 - 4 parts by mass of the blended emulsion and 6 - 7 parts by mass of water evenly, transfer to a sprayer to obtain an emulsion spray. Take 9 - 11 parts by mass of vitrified microspheres, spray the vitrified microspheres with the emulsion spray, continuously stir during the spraying process, and place the sprayed vitrified microspheres in an oven at 95 - 105 °C for drying for 35 - 45 h to obtain vitrified microspheres with an outer latex layer coating;
[0012] S4: Coating and modification of water - quenched manganese slag with styrene - acrylic - silicone emulsion
[0013] Mix ultrapure water, polyether - modified trisiloxane, and acrylate - modified silicone oil, add glacial acetic acid, stir and mix to obtain a silicone emulsion. Mix the styrene - acrylic emulsion, the silicone emulsion, and water, adjust the pH, disperse ultrasonically, transfer to a sprayer, spray the water - quenched manganese slag, and dry to obtain modified manganese slag;
[0014] S5: Reinforcement and modification of polypropylene fibers
[0015] Prepare a fiber - reinforcing agent emulsion with starch as the raw material, dilute with water, add polypropylene fibers, stir and disperse, let stand, and vacuum filter to obtain reinforced polypropylene fibers;
[0016] S6: Preparation of thermal insulation dry - mortar
[0017] Mix portland cement, fly ash, and surface - modified Yellow River sand in a mass ratio of 5 - 7:2 - 4:2 - 4 to obtain a gel material. Add the gel material, vitrified microspheres with an outer latex layer coating, modified water - quenched manganese slag, redispersible latex powder, hydroxypropyl methylcellulose ether, and reinforced polypropylene fibers to a mixing pan in a mass ratio of 40 - 60:50 - 70:40 - 60:2 - 4:0.5 - 0.8:0.3 - 0.5, dry - mix at 100 - 140 r / min for 2 - 5 min, and discharge to obtain thermal insulation dry - mortar.
[0018] Furthermore, the surface modification pretreatment of the Yellow River sand in step S1 specifically includes the following steps:
[0019] S1.1: Mix 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 4 - 5:1 to obtain a hydroxylation reagent. Take 100 - 120 volume parts of the hydroxylation reagent and mix with 10 - 15 parts by mass of Yellow River sand, stir and react for 3 - 4 h, wash with distilled water, and vacuum - dry at 50 - 60 °C to obtain hydroxylated Yellow River sand;
[0020] S1.2: Mix 10 - 15 parts by mass of hydroxylated Yellow River sand, 7 - 10 parts by volume of silane coupling agent and 50 - 70 parts by volume of toluene, stir and react at 70 - 80 °C for 15 - 20 h, wash the product with toluene, and dry it under vacuum at 50 - 60 °C to obtain silane - coupled Yellow River sand;
[0021] S1.3: Mix 10 - 15 parts by mass of silane - coupled Yellow River sand, 0.5 - 0.7 parts by mass of initiator and 120 - 150 parts by volume of toluene, drop - wise add 5 - 7 parts by volume of acrylic acid, react at 70 - 80 °C for 15 - 18 h, wash the product with toluene, and dry it under vacuum at 50 - 60 °C to obtain surface - modified Yellow River sand.
[0022] Further, step S2 for preparing the acrylic - urea formaldehyde resin blend emulsion specifically includes the following steps:
[0023] S2.1: Mix 0.4 - 0.8 parts by mass of nonylphenol polyoxyethylene ether, 0.3 - 0.6 parts by mass of dodecyl phenyl ether disulfonate, 10 - 20 parts by mass of methyl methacrylate, 10 - 20 parts by mass of butyl acrylate, 0.1 - 0.3 parts by mass of 1 - allyloxy - 2 - hydroxypropane sulfonate, 15 - 30 parts by mass of water and 0.1 - 0.3 parts by mass of ammonium persulfate to obtain a core pre - emulsion. Mix 0.3 - 0.6 parts by mass of nonylphenol polyoxyethylene ether, 0.2 - 0.4 parts by mass of dodecyl phenyl ether disulfonate, 2 - 5 parts by mass of glycidyl methacrylate, 7 - 15 parts by mass of 2 - ethylhexyl acrylate, 5 - 10 parts by mass of buffer solution, 10 - 20 parts by mass of water and 0.1 - 0.3 parts by mass of ammonium persulfate to obtain a shell pre - emulsion;
[0024] S2.2: Add 10 - 15 parts by mass of water into an emulsifying bottle, heat up to 50 - 60 °C, introduce nitrogen, drop - wise add the core pre - emulsion under stirring at 150 - 200 r / min, finish dropping within 30 - 40 min, add 0.05 - 0.08 parts by mass of sodium bisulfite, react at a constant temperature for 50 - 60 min, slowly drop - wise add the shell pre - emulsion, finish dropping within 50 - 60 min, add 0.03 - 0.06 parts by mass of sodium bisulfite, react at a constant temperature for 60 - 70 min, cool down, and filter to obtain an acrylic emulsion;
[0025] S2.3: Mix the aqueous urea formaldehyde resin with deionized water to prepare a urea formaldehyde resin solution with a mass fraction of 10 - 15%, and stir - mix the urea formaldehyde resin solution and the acrylic emulsion according to a mass ratio of 1:4 - 5 to obtain a blend emulsion.
[0026] Further, step S4 for coating and modifying water - quenched manganese slag with styrene - acrylic - organosilicon emulsion specifically includes the following steps:
[0027] S4.1: Pass the water - quenched manganese slag particles through a 4 - 20 - mesh sieve, wash them with distilled water, and dry them to obtain water - quenched manganese slag;
[0028] S4.2: Mix 4 - 8 parts by volume of ultrapure water, 0.75 - 1.5 parts by volume of polyether - modified trisiloxane, and 15 - 30 parts by volume of acrylate - modified silicone oil. Stir in 1 - 3 parts by volume of glacial acetic acid and stir for 5 - 10 min to obtain a silicone emulsion.
[0029] S4.3: Mix styrene - acrylic emulsion, silicone emulsion, and water in a mass ratio of 1:1 - 3:60 - 80 and mix evenly. Adjust the pH to 7 - 8 with sodium bicarbonate. Ultrasonicate at 50 - 70 W for 10 - 15 min in an ultrasonic disintegrator, transfer to a sprayer, spray the water - quenched manganese slag, and then put the sprayed water - quenched manganese slag into a drying oven and dry at 55 - 65 °C to obtain modified manganese slag.
[0030] Further, the enhancement modification of polypropylene fibers in step S5 specifically includes the following steps:
[0031] S5.1: Mix 10 - 15 parts by mass of starch, 100 - 200 parts by mass of water, 0.5 - 1 part by mass of sodium bisulfite, and 0.01 - 0.03 part by mass of ferrous sulfate. Stir and heat up to 88 - 95 °C, keep stirring at a constant temperature for 40 - 50 min to obtain gelatinized starch. Cool down to 75 - 80 °C, dropwise add 10 - 13 parts by mass of styrene, 5 - 8 parts by mass of butyl acrylate, and 2 - 4 parts by mass of 30% hydrogen peroxide. Finish dropping within 1 - 2 h and react at 75 - 80 °C for 80 - 90 min to obtain a fiber - reinforcing agent emulsion.
[0032] S5.2: Take 100 - 120 parts by volume of the fiber - reinforcing agent emulsion and mix it with 50 - 100 parts by volume of water. Shake well, add 10 - 15 parts by mass of polypropylene fibers, stir and disperse evenly, let it stand, and then vacuum filter to obtain reinforced polypropylene fibers, which are put into an oven to dry for standby.
[0033] Further, the silane coupling agent in step S1.2 is γ - (methacryloyloxy) propyltrimethoxysilane, and the initiator in step S1.3 is azobisisobutyronitrile.
[0034] Further, the buffer solution in step S2.1 is a mixed solution of sodium dihydrogen phosphate and disodium hydrogen phosphate with a pH of 7 - 7.8.
[0035] Further, the starch in step S5.1 is thermoplastic starch.
[0036] Further, the redispersible latex powder in step S6 is polyvinyl acetate - vinyl carboxylate copolymer or polyethylene - vinyl acetate copolymer. Beneficial effects
[0037] 1. The present invention uses an acrylic-urea formaldehyde resin blend emulsion to spray-wrap vitrified microspheres, which can form a three-dimensional network film with a high crosslinking density on the vitrified microspheres, thereby enhancing the compressive strength of the vitrified microspheres. The styrene-acrylic-silicone emulsion is used to coat and modify the water-quenched manganese slag, which can form a water-resistant film on the surface of the water-quenched manganese slag to reduce the opening area of the pores. The modified water-quenched manganese slag is incorporated into the thermal insulation mortar, occupying part of the space of the vitrified microspheres, reducing the interfacial area between the vitrified microspheres and the cement paste matrix, and avoiding the increase of pores, thereby improving the compressive strength of the thermal insulation dry powder mortar.
[0038] 2. The present invention prepares an acrylic emulsion by the seed emulsion polymerization method and introduces urea formaldehyde resin into the acrylic emulsion, which can improve the tensile strength and impermeability of the emulsion film after film formation. The molecular chain of the polymer in the acrylic emulsion contains a functional group epoxy group, and the acrylic molecular chains crosslink through the epoxy group to form a three-dimensional network structure. After adding urea formaldehyde resin, the epoxy group undergoes intermolecular crosslinking with the active hydroxymethyl and amino groups of the urea formaldehyde resin, thereby increasing the crosslinking point density of the polymer molecular chains, making the intermolecular arrangement more compact, making it difficult for small molecules to penetrate into the polymer film, reducing the water absorption rate of the vitrified microspheres, and at the same time increasing the tensile strength.
[0039] 3. The present invention can improve the dispersion performance of Yellow River sand in mortar by triple surface modification of Yellow River sand. First, hydroxylation is carried out on the Yellow River sand to introduce hydroxyl groups, then a coupling reaction is carried out to connect the silane coupling agent with the Yellow River sand by chemical bonds, and finally acrylic acid is grafted onto the surface of the Yellow River sand, so that high molecular compounds are polymerized on the surface of the Yellow River sand, generating a steric hindrance effect to avoid agglomeration between particles. At the same time, the high molecule contains functional groups such as hydroxyl groups and carboxyl groups, which can generate an electrostatic repulsion effect in an aqueous solution to promote the dispersion effect, and further improve the workability of the Yellow River sand in cement, which is more conducive to the performance of the dry powder mortar.
[0040] 4. The present invention uses starch as a raw material to prepare a fiber reinforcing agent and conducts surface strengthening modification on polypropylene fibers, which can improve the impact resistance and toughness of polypropylene fibers. Utilizing the film-forming property and adhesiveness of starch, it is graft copolymerized with styrene, butyl acrylate, hydrogen peroxide, etc. The synthesized reinforcing agent is adsorbed on the surface of the fiber, forming a film to increase the toughness and strength of the fiber, thereby improving the impact resistance of the dry powder mortar.
[0041] 5. The present invention adopts the method of ultrasonic dispersion, which can improve the uniformity of the styrene-acrylic-silicone mixed emulsion and the stability of shear dispersion, enhance the composite effect between latex particles, contribute to the surface coating modification of the water-quenched manganese slag, and is beneficial to improving the performance of the thermal insulation mortar. Description of the Drawings
[0042] Figure 1Process flow chart for preparing heat-insulating dry mortar with Yellow River sand for interior walls adopted in the embodiments of the present invention. Specific embodiments
[0043] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.
[0044] Example 1: A preparation process for heat-insulating dry mortar with Yellow River sand for interior walls, as Figure 1 shown, specifically includes the following steps:
[0045] S1: Surface modification pretreatment of Yellow River sand
[0046] Mix 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 5:1 to obtain a hydroxylation reagent. During the mixing process, use a glass rod to drain, let the hydrogen peroxide solution slowly flow along the inner wall of the beaker into the concentrated sulfuric acid, and carry out the process in a fume hood. Take 100 volume parts of the hydroxylation reagent and mix it with 12 mass parts of Yellow River sand, stir and react for 3 h. Wash the reacted solid matter with distilled water and vacuum dry it at 55 °C to obtain hydroxylated Yellow River sand;
[0047] Mix 11 mass parts of hydroxylated Yellow River sand, 7 volume parts of γ-(methacryloyloxy)propyltrimethoxysilane and 50 volume parts of toluene, stir and react at 75 °C for 17 h. Wash the reacted product with toluene and vacuum dry it at 55 °C to obtain silane-coupled Yellow River sand;
[0048] Mix 10 mass parts of silane-coupled Yellow River sand, 0.6 mass part of azobisisobutyronitrile and 130 volume parts of toluene, dropwise add 5 volume parts of acrylic acid, react at 75 °C for 16 h. Wash the reaction product with toluene and vacuum dry it at 55 °C to obtain surface-modified Yellow River sand;
[0049] S2: Prepare acrylic-urea formaldehyde resin blend emulsion
[0050] Mix 0.5 parts by mass of nonylphenol polyoxyethylene ether, 0.4 parts by mass of sodium dodecyl benzene ether disulfonate, 15 parts by mass of methyl methacrylate, 15 parts by mass of butyl acrylate, 0.2 parts by mass of sodium 1 - allyloxy - 2 - hydroxypropane sulfonate, 24 parts by mass of water and 0.2 parts by mass of ammonium persulfate to obtain a core pre - emulsion. Mix 0.5 parts by mass of nonylphenol polyoxyethylene ether, 0.3 parts by mass of sodium dodecyl benzene ether disulfonate, 4 parts by mass of glycidyl methacrylate, 10 parts by mass of 2 - ethylhexyl acrylate, 8 parts by mass of a mixed solution of sodium dihydrogen phosphate and disodium hydrogen phosphate with a pH of 7.3, 15 parts by mass of water and 0.2 parts by mass of ammonium persulfate to obtain a shell pre - emulsion;
[0051] Add 15 parts by mass of water to an emulsifying bottle, heat up to 55 °C, introduce nitrogen, and dropwise add the core pre - emulsion under stirring at 170 r / min. A constant - pressure dropping funnel can be used for feeding, and it is added dropwise within 35 min. Add 0.06 parts by mass of sodium bisulfite, react at a constant temperature for 55 min, slowly dropwise add the shell pre - emulsion, and finish adding it within 60 min. Add 0.05 parts by mass of sodium bisulfite, react at a constant temperature for 65 min, cool, and filter to obtain an acrylic emulsion;
[0052] Mix the aqueous urea - formaldehyde resin with deionized water to form a brown transparent liquid, and prepare a urea - formaldehyde resin solution with a mass fraction of 12% according to the calculated mass. Stir - mix the urea - formaldehyde resin solution and the acrylic emulsion at a mass ratio of 1:5 to obtain a blend emulsion;
[0053] S3: Spraying and coating of the blend emulsion on vitrified microspheres
[0054] Mix 4 parts by mass of the blend emulsion and 7 parts by mass of water evenly, transfer it to a sprayer to obtain an emulsion spray. Take 11 parts by mass of vitrified microspheres, spray the vitrified microspheres with the emulsion spray, continuously stir during the spraying process, and place the sprayed vitrified microspheres in an oven at 105 °C for drying for 40 h to obtain vitrified microspheres with an outer - coated latex layer;
[0055] S4: Coating and modification of water - quenched manganese slag with styrene - acrylic - silicone emulsion
[0056] Pass the water - quenched manganese slag particles through a 10 - mesh sieve, wash them with distilled water, remove the moisture and dry them to obtain water - quenched manganese slag;
[0057] Mix 6 parts by volume of ultrapure water, 1.2 parts by volume of polyether - modified trisiloxane and 20 parts by volume of acrylate - modified silicone oil, stir - add 2 parts by volume of glacial acetic acid, and stir for 8 min to obtain a silicone emulsion;
[0058] Mix styrene-acrylic emulsion, silicone emulsion and water evenly according to the mass ratio of 1:2:70, adjust the pH to 7 with sodium bicarbonate, put it into an ultrasonic disintegrator, set the ultrasonic rate to 60W, and ultrasonicate for 12 minutes. Then pour the mixed solution into a sprayer and spray it on the surface of water-quenched manganese slag. Put the sprayed water-quenched manganese slag into an oven and dry it at 60°C to obtain modified manganese slag;
[0059] S5: Reinforcement modification of polypropylene fiber
[0060] Mix 12 parts by mass of thermoplastic starch, 150 parts by mass of water, 0.7 part by mass of sodium bisulfite and 0.02 part by mass of ferrous sulfate, stir and heat up to 92°C, and stir at a constant temperature for 45 minutes to obtain gelatinized starch. Cool down to 75°C, and dropwise add 12 parts by mass of styrene, 7 parts by mass of butyl acrylate and 3 parts by mass of 30% hydrogen peroxide. Finish dropping in 1.5 hours and react at 75°C for 85 minutes to obtain fiber reinforcing agent emulsion;
[0061] Take 110 parts by volume of fiber reinforcing agent emulsion and mix it with 80 parts by volume of water, shake well, add 12 parts by mass of polypropylene fiber, and continuously stir to make the fiber reinforcing agent emulsion evenly distributed on the surface of the polypropylene fiber. Let it stand for 10 hours, filter it under vacuum at -0.1 MPa, and put it into an oven to dry at 150°C to obtain reinforced polypropylene fiber;
[0062] S6: Preparation of thermal insulation dry-mixed mortar
[0063] Mix portland cement, fly ash and surface-modified Yellow River sand according to the mass ratio of 6:3:3 to obtain gel material. Add the gel material, vitrified microspheres with an outer latex layer, modified water-quenched manganese slag, redispersible latex powder, hydroxypropyl methyl cellulose ether, and reinforced polypropylene fiber into a mixing pot according to the mass ratio of 50:60:50:3:0.6:0.4, and dry mix at 120 r / min for 3 minutes, then discharge to obtain thermal insulation dry-mixed mortar. The redispersible latex powder can be polyvinyl acetate-vinyl carboxylate copolymer or polyethylene-vinyl acetate copolymer.
[0064] Example 2: A preparation process of thermal insulation dry-mixed mortar for interior walls with Yellow River sand, as Figure 1 shown, specifically including the following steps:
[0065] S1: Surface modification pretreatment of Yellow River sand
[0066] Mix 98% concentrated sulfuric acid and 30% hydrogen peroxide according to the volume ratio of 4:1 to obtain a hydroxylation reagent. During the mixing process, use a glass rod to drain, let the hydrogen peroxide solution slowly flow along the inner wall of the beaker into the concentrated sulfuric acid, and carry out the operation in a fume hood. Take 120 parts by volume of the hydroxylation reagent and mix it with 15 parts by mass of Yellow River sand, stir and react for 3 hours, wash it with distilled water, and dry it under vacuum at 55°C to obtain hydroxylated Yellow River sand;
[0067] Mix 13 parts by mass of hydroxylated Yellow River sand, 8 parts by volume of γ-(methacryloyloxy)propyltrimethoxysilane and 60 parts by volume of toluene, stir and react at 75 °C for 17 h, wash the reaction product with toluene, and dry it under vacuum at 55 °C to obtain silane-coupled Yellow River sand;
[0068] Mix 12 parts by mass of silane-coupled Yellow River sand, 0.7 part by mass of azobisisobutyronitrile and 150 parts by volume of toluene, dropwise add 7 parts by volume of acrylic acid, react at 75 °C for 16 h, wash the reaction product with toluene, and dry it under vacuum at 55 °C to obtain surface-modified Yellow River sand;
[0069] S2: Prepare acrylic-urea formaldehyde resin blend emulsion
[0070] Mix 0.7 part by mass of nonylphenol polyoxyethylene ether, 0.5 part by mass of sodium dodecyl benzene ether disulfonate, 18 parts by mass of methyl methacrylate, 17 parts by mass of butyl acrylate, 0.3 part by mass of 1-allyloxy-2-hydroxypropane sulfonate, 28 parts by volume of water and 0.3 part by mass of ammonium persulfate to obtain a core pre-emulsion. Mix 0.6 part by mass of nonylphenol polyoxyethylene ether, 0.4 part by mass of sodium dodecyl benzene ether disulfonate, 5 parts by mass of glycidyl methacrylate, 12 parts by mass of 2-ethylhexyl acrylate, 10 parts by volume of a mixed solution of sodium dihydrogen phosphate and disodium hydrogen phosphate with a pH of 7.5, 18 parts by volume of water and 0.3 part by mass of ammonium persulfate to obtain a shell pre-emulsion;
[0071] Add 12 parts by volume of water to an emulsifying flask, heat up to 55 °C, introduce nitrogen, and dropwise add the core pre-emulsion under stirring at 170 r / min. A constant-pressure dropping funnel can be used for feeding, and finish dropping within 35 min. Add 0.08 part by mass of sodium bisulfite, react at a constant temperature for 55 min, slowly dropwise add the shell pre-emulsion, finish dropping within 60 min, add 0.06 part by mass of sodium bisulfite, react at a constant temperature for 65 min, cool, and filter to obtain an acrylic emulsion;
[0072] Mix the aqueous urea formaldehyde resin with deionized water to form a brown transparent liquid, prepare a 15% urea formaldehyde resin solution according to the calculated mass, and stir and mix the urea formaldehyde resin solution and the acrylic emulsion at a mass ratio of 1:4 to obtain a blend emulsion;
[0073] S3: Spraying and coating of the blend emulsion on expanded glass beads
[0074] Mix 3 parts by mass of the blend emulsion and 6 parts by volume of water evenly, transfer to a sprayer to obtain an emulsion spray. Take 9 parts by mass of expanded glass beads, spray the expanded glass beads with the emulsion spray, stir continuously during the spraying process, and place the sprayed expanded glass beads in an oven at 105 °C and dry for 40 h to obtain expanded glass beads with an outer latex layer coating;
[0075] S4: Coating and modification of water-quenched manganese slag with styrene-acrylic-silicone emulsion
[0076] Pass the water-quenched manganese slag particles through a 10-mesh sieve, wash them with distilled water, remove the moisture, and dry them to obtain water-quenched manganese slag;
[0077] Mix 8 parts by volume of ultrapure water, 1.5 parts by volume of polyether-modified trisiloxane, and 25 parts by volume of acrylate-modified silicone oil, stir in 3 parts by volume of glacial acetic acid, and stir for 8 min to obtain an organosilicon emulsion;
[0078] Mix the styrene-acrylic emulsion, the organosilicon emulsion, and water evenly according to a mass ratio of 1:3:80, adjust the pH to 7.5 with sodium bicarbonate, perform ultrasonic treatment at 60 W for 12 min in an ultrasonic disintegrator, put it into the ultrasonic disintegrator, set the ultrasonic rate to 60 W, and perform ultrasonic treatment for 12 min. Load the mixed solution into a sprayer and spray it on the surface of the water-quenched manganese slag. Put the sprayed water-quenched manganese slag into a drying oven and dry it at 60 °C to obtain modified manganese slag;
[0079] S5: Reinforcement modification of polypropylene fiber
[0080] Mix 15 parts by mass of thermoplastic starch, 180 parts by mass of water, 0.9 part by mass of sodium bisulfite, and 0.03 part by mass of ferrous sulfate, stir and heat up to 92 °C, keep stirring at a constant temperature for 45 min to obtain gelatinized starch, cool down to 75 °C, and dropwise add 13 parts by mass of styrene, 8 parts by mass of butyl acrylate, and 4 parts by mass of 30% hydrogen peroxide. The dropping is completed in 1.5 h, and react at 75 °C for 85 min to obtain a fiber reinforcing agent emulsion;
[0081] Take 120 parts by volume of the fiber reinforcing agent emulsion and mix it with 90 parts by volume of water, shake well, add 15 parts by mass of polypropylene fiber, continuously stir to make the fiber reinforcing agent emulsion evenly distributed on the surface of the polypropylene fiber, let it stand for 10 h, perform vacuum filtration at -0.1 MPa, and put it into an oven to dry at 150 °C to obtain reinforced polypropylene fiber;
[0082] S6: Preparation of thermal insulation dry-mixed mortar
[0083] Mix portland cement, fly ash, and surface-modified Yellow River sand according to a mass ratio of 7:4:4 to obtain a gel material. Add the gel material, outer-coated latex layer expanded perlite, modified water-quenched manganese slag, redispersible latex powder, hydroxypropyl methyl cellulose ether, and reinforced polypropylene fiber to a mixing pan according to a mass ratio of 55:65:55:4:0.6:0.7, and perform dry mixing at 120 r / min for 3 min, then discharge to obtain thermal insulation dry-mixed mortar. The redispersible latex powder can be polyvinyl acetate-vinyl carboxylate copolymer or polyethylene-vinyl acetate copolymer.
[0084] Example 3: A preparation process of thermal insulation dry-mixed mortar for interior walls with Yellow River sand, as Figure 1 shown, specifically including the following steps:
[0085] S1: Surface modification pretreatment of Yellow River sand
[0086] Mix 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 5:1 to obtain a hydroxylation reagent. During the mixing process, use a glass rod to guide the flow, slowly pour the hydrogen peroxide solution along the inner wall of the beaker into the concentrated sulfuric acid, and carry out the operation in a fume hood. Take 100 volume parts of the hydroxylation reagent and mix it with 12 mass parts of Yellow River sand, stir and react for 3.5 h. Wash the reacted solid with distilled water and vacuum dry it at 60 °C to obtain hydroxylated Yellow River sand;
[0087] Mix 11 mass parts of hydroxylated Yellow River sand, 7 volume parts of γ-(methacryloyloxy)propyltrimethoxysilane and 50 mL of toluene, stir and react at 80 °C for 15 h. Wash the product with toluene and vacuum dry it at 60 °C to obtain silane-coupled Yellow River sand;
[0088] Mix 10 mass parts of silane-coupled Yellow River sand, 0.6 mass part of azobisisobutyronitrile and 130 volume parts of toluene, dropwise add 5 volume parts of acrylic acid, react at 70 °C for 18 h. Wash the product with toluene and vacuum dry it at 60 °C to obtain surface-modified Yellow River sand;
[0089] S2: Preparation of acrylic-urea formaldehyde resin blend emulsion
[0090] Mix 0.5 mass part of nonylphenol polyoxyethylene ether, 0.4 mass part of dodecyl benzene ether disulfonate, 15 mass parts of methyl methacrylate, 15 mass parts of butyl acrylate, 0.2 mass part of 1-allyloxy-2-hydroxypropane sulfonate, 24 mass parts of water and 0.2 mass part of ammonium persulfate to obtain a core pre-emulsion. Mix 0.5 mass part of nonylphenol polyoxyethylene ether, 0.3 mass part of dodecyl benzene ether disulfonate, 4 mass parts of glycidyl methacrylate, 10 mass parts of 2-ethylhexyl acrylate, 8 mass parts of a mixed solution of sodium dihydrogen phosphate and disodium hydrogen phosphate with a pH of 7.3, 15 mass parts of water and 0.2 mass part of ammonium persulfate to obtain a shell pre-emulsion;
[0091] Add 15 mass parts of water to an emulsifying bottle, heat up to 60 °C, introduce nitrogen, and dropwise add the core pre-emulsion under stirring at 200 r / min. A constant-pressure dropping funnel can be used for feeding, and finish dropping within 40 min. Add 0.06 mass part of sodium bisulfite, react at a constant temperature for 60 min, slowly dropwise add the shell pre-emulsion, finish dropping within 50 min, add 0.05 mass part of sodium bisulfite, react at a constant temperature for 70 min, cool down, and filter to obtain an acrylic emulsion;
[0092] Mix the aqueous urea formaldehyde resin with deionized water to form a brown transparent liquid, and prepare a 12% urea formaldehyde resin solution according to the calculated mass. Stir and mix the urea formaldehyde resin solution and the acrylic emulsion in a mass ratio of 1:5 to obtain a blend emulsion;
[0093] S3: Spraying and coating of the vitrified microspheres with the blended emulsion
[0094] Mix 4 parts by mass of the blended emulsion and 7 parts by mass of water evenly, transfer to a sprayer to obtain an emulsion spray. Take 11 parts by mass of vitrified microspheres and spray them with the emulsion spray. Stir continuously during the spraying process. Place the sprayed vitrified microspheres in an oven at 100 °C and dry for 38 h to obtain vitrified microspheres with an outer latex layer coating;
[0095] S4: Coating and modification of water-quenched manganese slag with styrene-acrylic-silicone emulsion
[0096] Pass the water-quenched manganese slag particles through a 15-mesh sieve, wash them with distilled water, remove the moisture and dry them to obtain water-quenched manganese slag;
[0097] Mix 6 parts by volume of ultrapure water, 1.2 parts by volume of polyether-modified trisiloxane and 20 parts by volume of acrylate-modified silicone oil, stir and add 2 parts by volume of glacial acetic acid, and stir for 10 min to obtain a silicone emulsion;
[0098] Mix the styrene-acrylic emulsion, the silicone emulsion and water evenly according to a mass ratio of 1:2:70, adjust the pH to 7 with sodium bicarbonate, carry out ultrasonic treatment at 70 W for 10 min in an ultrasonic crusher, put it into the ultrasonic crusher, set the ultrasonic rate to 60 W, and carry out ultrasonic treatment for 12 min. Load the mixed solution into a sprayer and spray it on the surface of the water-quenched manganese slag. Place the sprayed water-quenched manganese slag in a drying oven and dry it at 65 °C to obtain modified manganese slag;
[0099] S5: Reinforcement and modification of polypropylene fibers
[0100] Mix 12 parts by mass of thermoplastic starch, 150 parts by mass of water, 0.7 part by mass of sodium bisulfite and 0.02 part by mass of ferrous sulfate, stir and heat up to 95 °C, keep stirring at a constant temperature for 40 min to obtain gelatinized starch. Cool down to 80 °C, dropwise add 12 parts by mass of styrene, 7 parts by mass of butyl acrylate and 3 parts by mass of 30% hydrogen peroxide. Finish dropping in 2 h and react at 80 °C for 80 min to obtain a fiber reinforcing agent emulsion;
[0101] Take 110 parts by volume of the fiber reinforcing agent emulsion and mix it with 80 parts by volume of water, shake well, add 12 parts by mass of polypropylene fibers, continuously stir to make the fiber reinforcing agent emulsion evenly distributed on the surface of the polypropylene fibers, let it stand for 15 h, carry out vacuum filtration at -0.2 MPa, and put it into an oven to dry at 130 °C to obtain reinforced polypropylene fibers;
[0102] S6: Preparation of thermal insulation dry-mixed mortar
[0103] Mix portland cement, fly ash, and surface-modified Yellow River sand in a mass ratio of 6:3:3 to obtain a gel material. Add the gel material, vitrified microspheres with an outer latex layer, modified water-quenched manganese slag, redispersible latex powder, hydroxypropyl methyl cellulose ether, and reinforced polypropylene fiber to a mixing pot in a mass ratio of 50:60:50:3:0.6:0.4, dry mix at 140 r / min for 5 min, and discharge to obtain the thermal insulation dry-mixed mortar. The redispersible latex powder can be polyvinyl acetate-ethylene copolymer or polyethylene-vinyl acetate copolymer.
[0104] The above embodiments are only illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Any person familiar with this technology can modify or change the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical ideas disclosed by the present invention should still be covered by the claims of the present invention.
Claims
1. A preparation process of a heat-insulating dry powder mortar with Yellow River sand for interior walls, characterized in that, Specifically, it includes the following steps: S1: Surface modification pretreatment of Yellow River sand Hydroxylate Yellow River sand with concentrated sulfuric acid and hydrogen peroxide, wash with water, dry, add silane coupling agent and toluene, carry out silane coupling reaction, wash the product with toluene, dry, add initiator and toluene, dropwise add acrylic acid for reaction, wash the product with toluene, dry to obtain surface-modified Yellow River sand; S2: Prepare acrylic-urea formaldehyde resin blend emulsion Mix nonylphenol polyoxyethylene ether, sodium dodecyl benzene ether disulfonate, methyl methacrylate, butyl acrylate, sodium 1-acryloxy-2-hydroxypropane sulfonate, water and ammonium persulfate to obtain a core pre-emulsion. Mix nonylphenol polyoxyethylene ether, sodium dodecyl benzene ether disulfonate, glycidyl methacrylate, 2-ethylhexyl acrylate, buffer solution, water and ammonium persulfate to obtain a shell pre-emulsion. Polymerize the core pre-emulsion and the shell pre-emulsion to obtain an acrylic emulsion. Prepare a urea formaldehyde resin solution with deionized water, and stir and mix the acrylic emulsion and the urea formaldehyde resin solution to obtain a blend emulsion; S3: Spraying and coating of the blend emulsion on vitrified microspheres Mix 3-4 parts by mass of the blend emulsion and 6-7 parts by mass of water evenly, transfer to a sprayer to obtain an emulsion spray. Take 9-11 parts by mass of vitrified microspheres, spray the vitrified microspheres with the emulsion spray, continuously stir during the spraying process, and place the sprayed vitrified microspheres in an oven at 95-105 °C for drying for 35-45 h to obtain vitrified microspheres with an outer latex layer; S4: Coating and modification of water-quenched manganese slag with styrene-acrylic-silicone emulsion Mix ultrapure water, polyether-modified trisiloxane and acrylate-modified silicone oil, add glacial acetic acid, stir and mix to obtain a silicone emulsion. Mix styrene-acrylic emulsion, silicone emulsion and water, adjust the pH, disperse ultrasonically, transfer to a sprayer, spray on water-quenched manganese slag, and dry to obtain modified manganese slag; S5: Reinforcement modification of polypropylene fiber Mix starch, water, sodium bisulfite and ferrous sulfate, stir to obtain gelatinized starch, cool down, dropwise add styrene, butyl acrylate and 30% hydrogen peroxide, react to obtain a fiber reinforcing agent emulsion, dilute with water, add polypropylene fiber, stir and disperse, let stand, vacuum filter to obtain reinforced polypropylene fiber; S6: Preparation of thermal insulation dry-mixed mortar Mix portland cement, fly ash and surface-modified Yellow River sand in a mass ratio of 5-7:2-4:2-4 to obtain a gel material. Add the gel material, vitrified microspheres with an outer latex layer, modified water-quenched manganese slag, redispersible latex powder, hydroxypropyl methyl cellulose ether, and reinforced polypropylene fiber to a mixing pot in a mass ratio of 40-60:50-70:40-60:2-4:0.5-0.8:0.3-0.5, and dry mix at 100-140 r / min for 2-5 min, then discharge to obtain thermal insulation dry-mixed mortar.
2. The preparation process of a heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 1, characterized in that, Step S1: Surface modification pretreatment of Yellow River sand, specifically includes the following steps: S1.1: Mix 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 4 - 5:1 to obtain a hydroxylation reagent. Take 100 - 120 volume parts of the hydroxylation reagent and mix it with 10 - 15 mass parts of Yellow River sand, stir and react for 3 - 4 h, wash with distilled water, and vacuum dry at 50 - 60 °C to obtain hydroxylated Yellow River sand; S1.2: Mix 10 - 15 mass parts of hydroxylated Yellow River sand, 7 - 10 volume parts of silane coupling agent, and 50 - 70 volume parts of toluene, stir and react at 70 - 80 °C for 15 - 20 h, wash the product with toluene, and vacuum dry at 50 - 60 °C to obtain silane-coupled Yellow River sand; S1.3: Mix 10 - 15 mass parts of silane-coupled Yellow River sand, 0.5 - 0.7 mass parts of initiator, and 120 - 150 volume parts of toluene, dropwise add 5 - 7 volume parts of acrylic acid, react at 70 - 80 °C for 15 - 18 h, wash the product with toluene, and vacuum dry at 50 - 60 °C to obtain surface-modified Yellow River sand.
3. The preparation process of a heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 1, characterized in that, Step S2: Prepare an acrylic-urea formaldehyde resin blend emulsion, specifically including the following steps: S2.1: Mix 0.4 - 0.8 mass parts of nonylphenol polyoxyethylene ether, 0.3 - 0.6 mass parts of dodecyl benzene ether disulfonate, 10 - 20 mass parts of methyl methacrylate, 10 - 20 mass parts of butyl acrylate, 0.1 - 0.3 mass parts of 1-acryloxy-2-hydroxypropane sulfonate, 15 - 30 mass parts of water, and 0.1 - 0.3 mass parts of ammonium persulfate to obtain a core pre-emulsion. Mix 0.3 - 0.6 mass parts of nonylphenol polyoxyethylene ether, 0.2 - 0.4 mass parts of dodecyl benzene ether disulfonate, 2 - 5 mass parts of glycidyl methacrylate, 7 - 15 mass parts of 2-ethylhexyl acrylate, 5 - 10 mass parts of buffer solution, 10 - 20 mass parts of water, and 0.1 - 0.3 mass parts of ammonium persulfate to obtain a shell pre-emulsion; S2.2: Add 10 - 15 mass parts of water to an emulsifying bottle, heat up to 50 - 60 °C, introduce nitrogen, dropwise add the core pre-emulsion under stirring at 150 - 200 r / min, finish dropping within 30 - 40 min, add 0.05 - 0.08 mass parts of sodium bisulfite, react at a constant temperature for 50 - 60 min, slowly dropwise add the shell pre-emulsion, finish dropping within 50 - 60 min, add 0.03 - 0.06 mass parts of sodium bisulfite, react at a constant temperature for 60 - 70 min, cool, and filter to obtain an acrylic emulsion; S2.3: Mix aqueous urea formaldehyde resin and deionized water to prepare a urea formaldehyde resin solution with a mass fraction of 10 - 15%, and stir and mix the urea formaldehyde resin solution and the acrylic emulsion in a mass ratio of 1:4 - 5 to obtain a blend emulsion.
4. The preparation process of a heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 1, characterized in that, Step S4: Coating and modifying water-quenched manganese slag with a styrene-acrylic-silicone emulsion, specifically including the following steps: S4.1: Pass the water-quenched manganese slag particles through a 4 - 20 mesh sieve, wash with distilled water, and dry to obtain water-quenched manganese slag; S4.2: Mix 4 - 8 volume parts of ultrapure water, 0.75 - 1.5 volume parts of polyether-modified trisiloxane, and 15 - 30 volume parts of acrylate-modified silicone oil, stir and add 1 - 3 volume parts of glacial acetic acid, and stir for 5 - 10 min to obtain a silicone emulsion; S4.3: Mix styrene-acrylic emulsion, silicone emulsion and water evenly according to the mass ratio of 1:1 - 3:60 - 80, adjust the pH to 7 - 8 with sodium bicarbonate, carry out ultrasonic treatment at 50 - 70 W for 10 - 15 min in an ultrasonic crusher, transfer it to a sprayer, spray the water-quenched manganese slag, and put the sprayed water-quenched manganese slag into an oven to dry at 55 - 65 °C to obtain the modified manganese slag.
5. The preparation process of a heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 1, characterized in that, Step S5: The enhancement modification of polypropylene fiber specifically includes the following steps: S5.1: Mix 10 - 15 parts by mass of starch, 100 - 200 parts by mass of water, 0.5 - 1 part by mass of sodium bisulfite and 0.01 - 0.03 part by mass of ferrous sulfate, stir and heat up to 88 - 95 °C, keep stirring at a constant temperature for 40 - 50 min to obtain gelatinized starch, cool down to 75 - 80 °C, dropwise add 10 - 13 parts by mass of styrene, 5 - 8 parts by mass of butyl acrylate and 2 - 4 parts by mass of 30% hydrogen peroxide, finish dropping in 1 - 2 h, and react at 75 - 80 °C for 80 - 90 min to obtain the fiber reinforcing agent emulsion; S5.2: Take 100 - 120 parts by volume of the fiber reinforcing agent emulsion and mix it with 50 - 100 parts by volume of water, shake well, add 10 - 15 parts by mass of polypropylene fiber, stir and disperse evenly, let it stand, carry out vacuum filtration to obtain the reinforced polypropylene fiber, and put it into an oven to dry for standby.
6. The preparation process of a heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 2, characterized in that, The silane coupling agent in step S1.2 is γ-(methacryloyloxy)propyltrimethoxysilane, and the initiator in step S1.3 is azobisisobutyronitrile.
7. The preparation process of a kind of heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 3, characterized in that, The buffer solution in step S2.1 is a mixed solution of sodium dihydrogen phosphate and disodium hydrogen phosphate with a pH of 7 - 7.
8.
8. The preparation process of a kind of heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 5, characterized in that, The starch in step S5.1 is thermoplastic starch.
9. The preparation process of a kind of heat-insulating dry powder mortar with Yellow River sand for interior walls according to claim 1, characterized in that, The redispersible latex powder in step S6 is polyvinyl acetate - vinyl carboxylate copolymer or polyethylene - vinyl acetate copolymer.
10. A kind of heat-insulating dry powder mortar with Yellow River sand for interior walls, characterized in that, It is prepared by the preparation process of the interior wall heat-insulating dry mortar with Yellow River sand described in any one of the above claims 1 - 9.
Citation Information
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