CN117003507B - High-efficiency waterproof polysilicone permeable crystallization type waterproof coating - Google Patents

High-efficiency waterproof polysilicone permeable crystallization type waterproof coating Download PDF

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CN117003507B
CN117003507B CN202310984135.5A CN202310984135A CN117003507B CN 117003507 B CN117003507 B CN 117003507B CN 202310984135 A CN202310984135 A CN 202310984135A CN 117003507 B CN117003507 B CN 117003507B
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CN117003507A (en
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杨军
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Guizhou Yuqi Shengda Industrial Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/02Treatment
    • C04B20/023Chemical treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10Coating or impregnating
    • C04B20/1055Coating or impregnating with inorganic materials
    • C04B20/107Acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/60Agents for protection against chemical, physical or biological attack
    • C04B2103/65Water proofers or repellants
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention relates to the technical field of waterproof paint, in particular to a high-efficiency waterproof polysilicone permeable crystallization type waterproof paint, which comprises the following raw materials in parts by weight: 30-70 parts of silicate cement, 20-28 parts of quartz sand, 10-15 parts of filler, 1-3 parts of complex catalyst, 4-8 parts of sodium carbonate, 2-6 parts of calcium chloride, 3-7 parts of electropositive modified multi-sheet particles, 8-13 parts of microencapsulated electronegative modified nano-sheets, 0.5-1.5 parts of polycarboxylic acid water reducer, 1-3 parts of film forming additive and 0.2-0.6 part of methyl cellulose. The polysilicone permeable crystallization type waterproof coating can be hydrated to generate insoluble crystals, compact base concrete and block water seepage channels, can form a continuous phase compact lamellar structure to block external moisture from seeping, can form a multi-layer lamellar structure partition layer in the pores of the concrete, can limit the generated insoluble crystals and prevent the insoluble crystals from separating from the pores of the concrete, and thus has a durable waterproof and impervious effect.

Description

High-efficiency waterproof polysilicone permeable crystallization type waterproof coating
Technical Field
The invention relates to the technical field of waterproof coatings, in particular to a high-efficiency waterproof polysilicone permeable crystallization type waterproof coating.
Background
Concrete is a heterogeneous, porous, high permeability material with a microcrack structure, a rough surface, which can adsorb water through capillaries, a process often accompanied by the adsorption of harmful substances. In the case of water, the water can cause frost and thawing of materials, if the materials are corroded by moisture in the air for a long time, the base material is subjected to high stress of dry-wet alternation, surface cracking is caused, and harmful substances are invaded by the generation and development of cracks; substances dissolved in water, especially chloride ions, can damage the passivation layer on the surface of the steel bar, causing catastrophic corrosion; the water can entrain pollutants and dust, so that the structure is polluted; the water also allows salt migration from the interior of the material to the exterior, thereby weathering the structure surface and creating salt frost. Combining the various degradation mechanisms of concrete structures, it is known that almost all chemical and physical processes affecting the durability of concrete structures involve two major factors, namely water and its migration in the concrete pores and cracks. Therefore, the concrete structure adopts the surface to prevent water from entering the external environment, and is very important to improve the durability of the concrete and ensure the clean appearance of the concrete.
For example, the invention patent with publication number CN102464476a discloses a cement-based permeable crystalline waterproof coating, which comprises, by weight, 50-65% of Portland cement, 5-15% of sodium carbonate and calcium chloride active materials, 2-5% of citric acid, 2-7% of a regulator, 20-40% of silica sand and 1% of fluorosilicic acid.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide the high-efficiency waterproof polysilicone permeable crystallization type waterproof coating.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the high-efficiency waterproof polysilicone permeable crystallization type waterproof coating comprises the following raw materials in parts by weight: 30-70 parts of silicate cement, 20-28 parts of quartz sand, 10-15 parts of filler, 1-3 parts of complex catalyst, 4-8 parts of sodium carbonate, 2-6 parts of calcium chloride, 3-7 parts of electropositive modified multi-sheet particles, 8-13 parts of microencapsulated electronegative modified nano-sheets, 0.5-1.5 parts of polycarboxylic acid water reducer, 1-3 parts of film forming additive and 0.2-0.6 part of methyl cellulose.
As a further preferable scheme of the invention, the complex catalyst is prepared from zeolite powder, lithium silicate, gluconate and isobutyl triethoxysilane according to the mass ratio of (70-100): (5-10): (8-12): (3-6) mixing;
the filler is at least one of fly ash and silica fume;
the film forming auxiliary agent is at least one of propylene glycol butyl ether and propylene glycol methyl ether acetate.
As a further preferable mode of the invention, the preparation method of the electropositive modified multi-lamellar particles comprises the following steps:
1) Dissolving 0.1-0.3mol of 1-bromobehenyl and 1-3mol of N, N' -tetramethyl-1, 6-hexamethylenediamine in 1000-2000mL of mixture, heating for 10-15h at 70-75 ℃, cooling to room temperature, filtering the product, washing with diethyl ether, dissolving 0.1-0.2mol of the product and 0.2-0.4mol of 1-bromohexane in 300-500mL of acetonitrile, refluxing for 10-15h, cooling to room temperature, filtering the product, repeatedly washing with diethyl ether, and drying for later use;
2) Mixing the standby product with tetraethyl silicate, aluminum sulfate, sodium hydroxide, sulfuric acid and deionized water according to the molar ratio (30-40): 1: (100-120): (10-16): (18-23): (4000-6000), fully mixing, heating in a homogeneous reactor for 5-8d, cooling to room temperature after the reaction is finished, repeatedly washing with deionized water, drying, and calcining for 4-6h in an air atmosphere to obtain multi-layered particles;
3) Adding the multi-layered particles into deionized water, dispersing uniformly to obtain a dispersion liquid, mixing with ethylenediamine-hydrochloric acid solution for 30-50s, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, stirring and mixing for 15-20min, dialyzing for 24-30h, changing ultrapure water every 2-3h, and drying to obtain the electropositive modified multi-layered particles.
As a further preferred embodiment of the present invention, the mixture consists of acetonitrile and toluene;
the reflux temperature is 70-75 ℃.
As a further preferred embodiment of the invention, the heating in the homogeneous reactor is carried out at 150-160 ℃;
the calcination temperature is 550-580 ℃.
As a further preferable scheme of the invention, the dosage proportion of the multi-layered particles, deionized water, ethylenediamine-hydrochloric acid solution and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is (5-10) g: (300-500) mL: (80-120) mL: (0.8-1.3) g;
the concentration of the ethylenediamine-hydrochloric acid solution is 0.5-0.8mol/L.
As a further preferable scheme of the invention, the preparation method of the microencapsulated electronegative modified nanosheets comprises the following steps:
1) Dissolving diboron trioxide in methanol at room temperature, rapidly stirring and dissolving, adding urea, fully stirring, and placing on a porcelain boat, wherein the volume ratio of nitrogen to hydrogen is (0.05-0.08): 1, heating to 1000-1100 ℃ at 8-10 ℃/min and calcining for 4-6 hours in the mixed gas atmosphere to obtain the nano-sheet;
2) Adding sodium dodecyl alcohol polyoxyethylene ether sulfate into deionized water at room temperature, fully stirring, sequentially adding sodium chloride, dodecyl dimethyl betaine and nanosheets, fully stirring for 1-2h, performing centrifugal separation, dialyzing for 20-26h, changing ultrapure water every 1-2h, and drying to obtain electronegative modified nanosheets;
3) Adding the electronegative modified nano-sheet into a sodium alginate solution, uniformly mixing, dripping into a calcium chloride solution, solidifying and shaping for 30-50min, filtering and washing, transferring into a chitosan solution, stirring and mixing for 30-50min, and filtering, washing and drying to obtain the microencapsulated electronegative modified nano-sheet.
As a further preferable scheme of the invention, the dosage proportion of the diboron trioxide, the methanol and the urea is (0.5-1.0) g: (10-20) mL: (2.4-3.2) g;
the dosage proportion of the dodecyl alcohol polyoxyethylene ether sodium sulfate, deionized water, sodium chloride, dodecyl dimethyl betaine and the nano-sheet is (4-6) g: (100-120) mL: (5-8) g: (0.1-0.3) g: (0.3-0.7) g.
As a further preferable scheme of the invention, the dosage proportion of the electronegative modified nano-sheet, the sodium alginate solution, the calcium chloride solution and the chitosan solution is (1-3) g: (10-20) mL: (30-50) mL: (120-160) mL.
As a further preferable scheme of the invention, the concentration of the sodium alginate solution is 2-5wt%;
the concentration of the calcium chloride solution is 2-3wt%;
the concentration of the chitosan solution is 1-3wt%.
Compared with the prior art, the invention has the beneficial effects that:
in the invention, after the polysilicone permeable crystallization type waterproof paint is mixed with water, cement, a complex catalyst, sodium carbonate, calcium chloride, and the like are rapidly dissolved in the water, C3AF, C4A, C S and the like in the cement begin to hydrate at first, and Ca is released 2+ Plasma, liquid phase is in strong alkalinity, and the complexing catalyst starts complexing Ca 2+ True solutions, so-called calcilytic complexes, the active material assumes a non-tacky, colloid-like morphology in the coating system; when the waterproof paint is coated on the surface of the fully wetted concrete, as water in the coating permeates into the base layer, the complex catalyst in the coating and the colloid active material permeate into the capillary holes of the base layer, and the complex catalyst combines Ca in part of the capillary holes in the permeation process 2+ Thereby avoiding Ca 2+ With trace SiO remaining in capillary holes 3 2- Premature reaction, blocking capillary holes; the active material which is permeated into the capillary holes is hydrated in a strong alkaline environment and combines Ca 2+ The complex catalyst of (2) utilizes the coordination space center and the electronic effect to reduce the hydration active material and Ca 2+ The activation energy of the reaction promotes the generation of insoluble crystals; secondly, the hydration active material can generate self polycondensation reaction to generate hydrophobic white crystal substances, and in addition, the complex catalyst stimulates the cement clinker such as C2S and the like with unhydrated capillary pore walls to continuously hydrate to generate hydrated CaSiO 3 And insoluble crystals are generated, so that the base layer concrete is compacted, and the seepage passage is blocked, and the base layer concrete shows excellent waterproof and seepage-resistant performances.
In order to further improve the waterproof and impervious effects, the invention is characterized in that 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is added after the synthesized multi-layered particles are mixed with ethylenediamine-hydrochloric acid solution to perform stirring reaction to obtain the positively modified multi-layered particles, the synthesized nano-sheets are modified by an anionic viscoelastic surfactant to serve as core materials, and the core materials are subjected to coating treatment by adopting sodium alginate and chitosan, so that the microencapsulated negatively modified nano-sheets are obtained, after the coating treatment, the positively modified multi-layered particles and the negatively modified nano-sheets are separated from each other, agglomeration of the capsule walls is avoided under the action of static electricity, so that the polysilicone osmotic crystalline waterproof paint has qualified stability, and when the polysilicone osmotic crystalline waterproof paint is mixed with water for use, the capsule walls of the microencapsulated negatively modified nano-sheets are broken under the action of external force, the embedded negatively modified nano-sheets are subjected to release treatment, and are subjected to electrostatic adsorption with the positively modified multi-layered particles under the action of static electricity, so that the negatively modified nano-sheets can be embedded into the positively modified nano-sheets, and can be prevented from penetrating into the porous layers of the porous concrete, and the porous structure can be prevented from being formed, and the porous structure can be continuously separated from the porous layers of the porous concrete.
The polysilicone permeable crystallization type waterproof coating can be hydrated to generate insoluble crystals, can compact base layer concrete to block a seepage passage, can form a continuous phase compact lamellar structure, can effectively play a role in blocking outside moisture seepage, can form a multi-layer lamellar structure partition layer in a pore of the concrete, can play a role in limiting solidification of the generated insoluble crystals and prevent the insoluble crystals from separating from the pore of the concrete, and thus can have a durable waterproof and anti-seepage effect.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the embodiment of the invention, the complex catalyst is prepared from zeolite powder, lithium silicate, gluconate and isobutyl triethoxysilane according to the mass ratio of 70:5:8:3, mixing; silica fume is selected as filler; the film forming auxiliary agent is propylene glycol butyl ether.
Example 1
The high-efficiency waterproof polysilicone permeable crystallization type waterproof coating comprises the following raw materials in parts by weight: 30 parts of silicate cement, 20 parts of quartz sand, 10 parts of filler, 1 part of complex catalyst, 4 parts of sodium carbonate, 2 parts of calcium chloride, 3 parts of positively-modified multi-lamellar particles, 8 parts of microencapsulated negatively-modified nano-sheets, 0.5 part of polycarboxylic acid water reducer, 1 part of film forming additive and 0.2 part of methyl cellulose.
The preparation method of the electropositive modified multi-lamellar particles comprises the following steps:
1) Dissolving 0.1mol of 1-bromobehenyl and 1mol of N, N' -tetramethyl-1, 6-hexamethylenediamine in 1000mL of a mixture composed of acetonitrile and toluene by mass, heating at 70 ℃ for 10h, cooling to room temperature, filtering the product, washing with diethyl ether, dissolving 0.1mol of the product and 0.2mol of 1-bromohexane in 300mL of acetonitrile, refluxing at 70 ℃ for 10h, cooling to room temperature, filtering the product, repeatedly washing with diethyl ether, and drying for later use;
2) Mixing the standby product with tetraethyl silicate, aluminum sulfate, sodium hydroxide, sulfuric acid and deionized water according to a molar ratio of 30:1:100:10:18:4000, fully mixing, placing in a homogeneous reactor, heating at 150 ℃ for 5d, cooling to room temperature after the reaction is finished, repeatedly washing with deionized water, drying, and calcining at 550 ℃ for 4h in air atmosphere to obtain multi-layered particles;
3) Adding 5g of multi-lamellar particles into 300mL of deionized water, dispersing uniformly to obtain a dispersion liquid, mixing with 80mL of ethylenediamine-hydrochloric acid solution with the concentration of 0.5mol/L for 30s, adding 0.8g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, stirring and mixing for 15min at 800r/min, dialyzing for 24h, changing ultrapure water every 2h, and drying to obtain the electropositive modified multi-lamellar particles.
The preparation method of the microencapsulated electronegative modified nano-sheet comprises the following steps:
1) 0.5g of diboron trioxide is dissolved in 10mL of methanol at room temperature, after rapid stirring and dissolution, 2.4g of urea is added, and after full stirring, the mixture is put on a porcelain boat, and the volume ratio of nitrogen to hydrogen is 0.05:1, heating to 1000 ℃ at 8 ℃/min under the atmosphere of the mixed gas composed of the components, and calcining for 4 hours to obtain the nano-sheet;
2) Adding 4g of sodium dodecyl alcohol polyoxyethylene ether sulfate into 100mL of deionized water at room temperature, fully stirring, sequentially adding 5g of sodium chloride, 0.1g of dodecyl dimethyl betaine and 0.3g of nanosheets, fully stirring for 1h, performing centrifugal separation, dialyzing for 20h, changing ultrapure water every 1h, and drying to obtain electronegative modified nanosheets;
3) Adding 1g of electronegative modified nano-sheet into 10mL of sodium alginate solution with the concentration of 2wt%, uniformly mixing, dripping into 30mL of calcium chloride solution with the concentration of 2wt%, solidifying and shaping for 30min, filtering and washing, transferring into 120mL of chitosan solution with the concentration of 1wt%, stirring and mixing for 30min, filtering, washing and drying to obtain the microencapsulated electronegative modified nano-sheet.
Example 2
The high-efficiency waterproof polysilicone permeable crystallization type waterproof coating comprises the following raw materials in parts by weight: 60 parts of silicate cement, 23 parts of quartz sand, 12 parts of filler, 2 parts of complex catalyst, 6 parts of sodium carbonate, 4 parts of calcium chloride, 5 parts of positively-charged modified multi-lamellar particles, 10 parts of microencapsulated negatively-charged modified nano-sheets, 1 part of polycarboxylic acid water reducer, 2 parts of film forming additive and 0.5 part of methyl cellulose.
The preparation method of the electropositive modified multi-lamellar particles comprises the following steps:
1) Dissolving 0.2mol of 1-bromobehenyl and 2mol of N, N' -tetramethyl-1, 6-hexamethylenediamine in 1500mL of a mixture consisting of acetonitrile, toluene and the like by mass, heating the mixture at 72 ℃ for 12h, cooling the mixture to room temperature, filtering the product, washing the product with diethyl ether, dissolving 0.2mol of the product and 0.3mol of 1-bromohexane in 400mL of acetonitrile, refluxing the mixture at 72 ℃ for 13h, cooling the mixture to room temperature, filtering the product, repeatedly washing the product with diethyl ether, and drying the product for later use;
2) Mixing the standby product with tetraethyl silicate, aluminum sulfate, sodium hydroxide, sulfuric acid and deionized water according to a mole ratio of 35:1:110:14:20:5000, fully mixing, placing in a homogeneous reactor, heating at 155 ℃ for 7d, cooling to room temperature after the reaction is finished, repeatedly washing with deionized water, drying, and calcining at 560 ℃ for 5h in an air atmosphere to obtain multi-layered particles;
3) Adding 7g of multi-lamellar particles into 400mL of deionized water, dispersing uniformly to obtain a dispersion liquid, mixing with 100mL of ethylenediamine-hydrochloric acid solution with the concentration of 0.7mol/L for 40s, adding 1.2g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, stirring and mixing for 18min at 850r/min, dialyzing for 27h, changing ultrapure water every 3h, and drying to obtain the electropositive modified multi-lamellar particles.
The preparation method of the microencapsulated electronegative modified nano-sheet comprises the following steps:
1) 0.8g of diboron trioxide is dissolved in 15mL of methanol at room temperature, after rapid stirring and dissolution, 2.8g of urea is added, and after full stirring, the mixture is put on a porcelain boat, and after nitrogen and hydrogen are mixed according to the volume ratio of 0.07:1, heating to 1050 ℃ at 9 ℃/min under the atmosphere of the mixed gas composed of the components, and calcining for 5 hours to obtain the nano-sheet;
2) Adding 5g of sodium dodecyl alcohol polyoxyethylene ether sulfate into 110mL of deionized water at room temperature, fully stirring, sequentially adding 7g of sodium chloride, 0.2g of dodecyl dimethyl betaine and 0.5g of nanosheets, fully stirring for 1h, performing centrifugal separation, dialyzing for 25h, changing ultrapure water every 1h, and drying to obtain electronegative modified nanosheets;
3) Adding 2g of electronegative modified nano-sheets into 15mL of sodium alginate solution with the concentration of 3wt%, uniformly mixing, dripping into 40mL of calcium chloride solution with the concentration of 2.5wt%, solidifying and shaping for 40min, filtering and washing, transferring into 150mL of chitosan solution with the concentration of 2wt%, stirring and mixing for 40min, filtering, washing and drying to obtain the microencapsulated electronegative modified nano-sheets.
Example 3
The high-efficiency waterproof polysilicone permeable crystallization type waterproof coating comprises the following raw materials in parts by weight: 70 parts of silicate cement, 28 parts of quartz sand, 15 parts of filler, 3 parts of complex catalyst, 8 parts of sodium carbonate, 6 parts of calcium chloride, 7 parts of positively-modified multi-layered particles, 13 parts of microencapsulated negatively-modified nano-sheets, 1.5 parts of polycarboxylic acid water reducer, 3 parts of film forming additive and 0.6 part of methyl cellulose.
The preparation method of the electropositive modified multi-lamellar particles comprises the following steps:
1) Dissolving 0.3mol of 1-bromobehenyl and 3mol of N, N' -tetramethyl-1, 6-hexamethylenediamine in 2000mL of a mixture composed of acetonitrile, toluene and the like by mass, heating the mixture at 75 ℃ for 15h, cooling the mixture to room temperature, filtering the product, washing the product with diethyl ether, dissolving 0.2mol of the product and 0.4mol of 1-bromohexane in 500mL of acetonitrile, refluxing the mixture at 75 ℃ for 15h, cooling the mixture to room temperature, filtering the product, repeatedly washing the product with diethyl ether, and drying the product for later use;
2) Mixing the standby product with tetraethyl silicate, aluminum sulfate, sodium hydroxide, sulfuric acid and deionized water according to a molar ratio of 40:1:120:16:23:6000, fully mixing, placing in a homogeneous reactor, heating at 160 ℃ for 8d, cooling to room temperature after the reaction is finished, repeatedly washing with deionized water, drying, and calcining at 580 ℃ for 6h in air atmosphere to obtain multi-layered particles;
3) Adding 10g of multi-lamellar particles into 500mL of deionized water, dispersing uniformly to obtain a dispersion liquid, mixing with 120mL of ethylenediamine-hydrochloric acid solution with the concentration of 0.8mol/L for 50s, adding 1.3g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, stirring and mixing for 20min at 900r/min, dialyzing for 30h, changing ultrapure water every 3h, and drying to obtain the electropositive modified multi-lamellar particles.
The preparation method of the microencapsulated electronegative modified nano-sheet comprises the following steps:
1) 1g of diboron trioxide is dissolved in 20mL of methanol at room temperature, after rapid stirring and dissolution, 3.2g of urea is added, and after full stirring, the mixture is put on a porcelain boat, and after nitrogen and hydrogen are mixed according to the volume ratio of 0.08:1, heating to 1100 ℃ at 10 ℃/min under the atmosphere of the mixed gas composed of the components, and calcining for 6 hours to obtain the nano-sheet;
2) Adding 6g of sodium dodecyl alcohol polyoxyethylene ether sulfate into 120mL of deionized water at room temperature, fully stirring, sequentially adding 8g of sodium chloride, 0.3g of dodecyl dimethyl betaine and 0.7g of nanosheets, fully stirring for 2 hours, centrifuging, dialyzing for 26 hours, changing ultrapure water every 2 hours, and drying to obtain electronegativity modified nanosheets;
3) Adding 3g of electronegative modified nano-sheets into 20mL of sodium alginate solution with the concentration of 5wt%, uniformly mixing, dripping into 50mL of calcium chloride solution with the concentration of 3wt%, solidifying and shaping for 50min, filtering and washing, transferring into 160mL of chitosan solution with the concentration of 3wt%, stirring and mixing for 50min, filtering, washing and drying to obtain the microencapsulated electronegative modified nano-sheets.
Comparative example 1: this comparative example is essentially the same as example 1, except that the electropositive modified multi-lamellar particles are absent.
Comparative example 2: this comparative example is essentially the same as example 1, except that multi-lamellar particles are used instead of electropositively modified multi-lamellar particles.
Comparative example 3: this comparative example is essentially the same as example 1, except that microencapsulated electronegative modified nanoplatelets are not contained.
Comparative example 4: this comparative example is essentially the same as example 1, except that nanoplatelets are used instead of microencapsulated electronegative modified nanoplatelets.
Comparative example 5: this comparative example is substantially the same as example 1 except that instead of microencapsulated electronegative modified nanoplatelets, electronegative modified nanoplatelets are used.
Test experiment:
s1 test standard:
and carrying out a water penetration resistance test and an anti-seepage pressure ratio test of the concrete according to GB18455-2012 Cement-based penetration crystalline waterproof material.
S2, preparing concrete:
200 parts of cement, 70 parts of mineral powder, 50 parts of fly ash, 165 parts of water, 950 parts of sand, 960 parts of stone, 8.8 parts of water reducer, 12 parts of polysilicone permeable crystallization type waterproof paint and 0.18 part of nano alumina; dividing water into two parts, wherein one part is used for dissolving a water reducing agent, and the other part is used for mixing with nano alumina and polysilicone permeable crystalline waterproof coating; according to the proportion of the components, a certain amount of cement, mineral powder, fly ash, sand and stone are weighed and poured into a concrete mixer to be dry-mixed for 5min, then a water reducing agent is weighed and added with water to be dissolved, after being uniformly stirred, the mixture is poured into the mixer, and is stirred again until the concrete is fully fluidized, then a mixture which is obtained by uniformly mixing the polysilicone permeable crystallization type waterproof paint, nano alumina and water in advance is added, the mixture is stirred until the mixture is uniformly distributed in the concrete, and finally the stirred concrete is molded and maintained according to the test standard of the corresponding performance, thus obtaining a concrete sample; among them, polysilicone penetrating crystalline type waterproof coating materials are provided by examples 1 to 3 and comparative examples 1 to 5, respectively.
S3, performance test:
the concrete samples were taken for the concrete water penetration resistance test measurement, and the concrete results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the polysilicone permeable crystallization type waterproof coating of the invention can be applied to concrete to remarkably improve the waterproof and impermeable properties, so that the waterproof and impermeable coating has high impermeable pressure and high impermeable pressure ratio.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.

Claims (8)

1. The high-efficiency waterproof polysilicone permeable crystallization type waterproof coating is characterized by comprising the following raw materials in parts by weight: 30-70 parts of silicate cement, 20-28 parts of quartz sand, 10-15 parts of filler, 1-3 parts of complex catalyst, 4-8 parts of sodium carbonate, 2-6 parts of calcium chloride, 3-7 parts of electropositive modified multi-lamellar particles, 8-13 parts of microencapsulated electronegative modified nano-sheets, 0.5-1.5 parts of polycarboxylic acid water reducer, 1-3 parts of film forming additive and 0.2-0.6 part of methyl cellulose;
the complex catalyst is prepared from zeolite powder, lithium silicate, gluconate and isobutyl triethoxysilane according to the mass ratio of (70-100): (5-10): (8-12): (3-6) mixing;
the preparation method of the electropositive modified multi-lamellar particles comprises the following steps:
1) Dissolving 0.1-0.3mol of 1-bromobehenyl and 1-3mol of N, N' -tetramethyl-1, 6-hexamethylenediamine in 1000-2000mL of mixture, heating for 10-15h at 70-75 ℃, cooling to room temperature, filtering the product, washing with diethyl ether, dissolving 0.1-0.2mol of the product and 0.2-0.4mol of 1-bromohexane in 300-500mL of acetonitrile, refluxing for 10-15h, cooling to room temperature, filtering the product, repeatedly washing with diethyl ether, and drying for later use; the mixture consists of acetonitrile, toluene and the like;
2) Mixing the standby product with tetraethyl silicate, aluminum sulfate, sodium hydroxide, sulfuric acid and deionized water according to the molar ratio (30-40): 1: (100-120): (10-16): (18-23): (4000-6000), fully mixing, heating in a homogeneous reactor for 5-8d, cooling to room temperature after the reaction is finished, repeatedly washing with deionized water, drying, and calcining for 4-6h in an air atmosphere to obtain multi-layered particles;
3) Adding the multi-layered particles into deionized water, dispersing uniformly to obtain a dispersion liquid, mixing with ethylenediamine-hydrochloric acid solution for 30-50s, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, stirring and mixing for 15-20min, dialyzing for 24-30h, changing ultrapure water every 2-3h, and drying to obtain positively modified multi-layered particles;
the preparation method of the microencapsulated electronegative modified nano-sheet comprises the following steps:
1) Dissolving diboron trioxide in methanol at room temperature, rapidly stirring and dissolving, adding urea, fully stirring, and placing on a porcelain boat, wherein the volume ratio of nitrogen to hydrogen is (0.05-0.08): 1, heating to 1000-1100 ℃ at 8-10 ℃/min and calcining for 4-6 hours in the mixed gas atmosphere to obtain the nano-sheet;
2) Adding sodium dodecyl alcohol polyoxyethylene ether sulfate into deionized water at room temperature, fully stirring, sequentially adding sodium chloride, dodecyl dimethyl betaine and nanosheets, fully stirring for 1-2h, performing centrifugal separation, dialyzing for 20-26h, changing ultrapure water every 1-2h, and drying to obtain electronegative modified nanosheets;
3) Adding the electronegative modified nano-sheet into a sodium alginate solution, uniformly mixing, dripping into a calcium chloride solution, solidifying and shaping for 30-50min, filtering and washing, transferring into a chitosan solution, stirring and mixing for 30-50min, and filtering, washing and drying to obtain the microencapsulated electronegative modified nano-sheet.
2. A highly effective waterproof polysilicone permeable crystalline waterproof coating according to claim 1, wherein,
the filler is at least one of fly ash and silica fume;
the film forming auxiliary agent is at least one of propylene glycol butyl ether and propylene glycol methyl ether acetate.
3. A highly effective water-resistant polysilicone permeable crystalline water resistant paint according to claim 1, wherein the reflow temperature is 70-75 ℃.
4. A highly effective water-resistant polysilicone permeable crystalline water resistant paint according to claim 1, wherein the heating in the homogeneous phase reactor is carried out at 150-160 ℃;
the calcination temperature is 550-580 ℃.
5. The high-efficiency waterproof polysilicone permeable crystalline waterproof coating according to claim 1, wherein the dosage ratio of the multi-layered particles, deionized water, ethylenediamine-hydrochloric acid solution, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is (5-10) g: (300-500) mL: (80-120) mL: (0.8-1.3) g;
the concentration of the ethylenediamine-hydrochloric acid solution is 0.5-0.8mol/L.
6. The high-efficiency waterproof polysilicone permeable crystallization type waterproof coating according to claim 1, wherein the dosage proportion of the diboron trioxide, the methanol and the urea is (0.5-1.0) g: (10-20) mL: (2.4-3.2) g;
the dosage proportion of the dodecyl alcohol polyoxyethylene ether sodium sulfate, deionized water, sodium chloride, dodecyl dimethyl betaine and the nano-sheet is (4-6) g: (100-120) mL: (5-8) g: (0.1-0.3) g: (0.3-0.7) g.
7. The high-efficiency waterproof polysilicone permeable crystallization type waterproof coating according to claim 1, wherein the dosage proportion of electronegative modification nano sheet, sodium alginate solution, calcium chloride solution and chitosan solution is (1-3) g: (10-20) mL: (30-50) mL: (120-160) mL.
8. The high-efficiency waterproof polysilicone permeable crystalline waterproof coating according to claim 1, wherein the concentration of the sodium alginate solution is 2-5wt%;
the concentration of the calcium chloride solution is 2-3wt%;
the concentration of the chitosan solution is 1-3wt%.
CN202310984135.5A 2023-08-07 2023-08-07 High-efficiency waterproof polysilicone permeable crystallization type waterproof coating Active CN117003507B (en)

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CN106747081A (en) * 2016-12-09 2017-05-31 金华市欣生沸石开发有限公司 Cementitious capillary waterproofing material
CN108996973A (en) * 2018-09-30 2018-12-14 中国十七冶集团有限公司 A kind of penetration crystallization type water proofing paint
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