CN113956016A - Nano-permeation crystallization self-healing inorganic waterproof material on back water surface and preparation method thereof - Google Patents

Nano-permeation crystallization self-healing inorganic waterproof material on back water surface and preparation method thereof Download PDF

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CN113956016A
CN113956016A CN202111429317.3A CN202111429317A CN113956016A CN 113956016 A CN113956016 A CN 113956016A CN 202111429317 A CN202111429317 A CN 202111429317A CN 113956016 A CN113956016 A CN 113956016A
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朱耀台
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Zhu Yaotai
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Zhu Yaotai
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • C04B28/26—Silicates of the alkali metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5076—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with masses bonded by inorganic cements
    • C04B41/5089—Silica sols, alkyl, ammonium or alkali metal silicate cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
    • C04B41/61—Coating or impregnation
    • C04B41/65—Coating or impregnation with inorganic materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00482—Coating or impregnation materials
    • C04B2111/00508—Cement paints
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention discloses a nano-permeable crystallization self-healing inorganic waterproof material on a back surface and a preparation method thereof, wherein the nano-permeable crystallization inorganic waterproof powder material comprises sodium carbonate, silica fume, rubber powder and quartz sand, and further comprises the following components: sequestering agent, fiber agent, water reducing agent, talcum powder, defoaming agent, paraffin and porous hollow SiO2/Al2O3Composite nanospheres, a permeable crystallization material, zinc phthalate and a wax water repellent. The invention is suitable for the technical field of building waterproofing, has higher apparent density or tap density, is beneficial to the final sample product to obtain excellent comprehensive physical properties such as surface strength and the like, and is beneficial to stronger precipitation-complexation reaction between the waterproof material and alkaline substances in cement concreteSo as to form a more compact compound hydrated substance and improve the performances of the cement concrete such as compressive strength, impermeability pressure ratio and the like.

Description

Nano-permeation crystallization self-healing inorganic waterproof material on back water surface and preparation method thereof
Technical Field
The invention belongs to the technical field of building waterproofing, and particularly relates to a nano-permeable crystallization self-healing inorganic waterproof material on a back water surface and a preparation method thereof.
Background
The cement concrete is essentially attributed to a heterogeneous structure, micro cracks and pores existing inside the cement concrete are basic properties of the cement concrete, and are difficult to completely eliminate, and the defects of the micro cracks, the pores and the like existing on the surface of the cement concrete can accelerate the deterioration of the permeability of the cement concrete, so that the anti-permeability performance (waterproof performance) of the cement concrete is sharply reduced. In order to avoid the generation of harmful-level microcracks or pores and control the size of the microcracks or the pores to be in an harmless level (the pores are less than 20nm), a great deal of research is carried out by a plurality of researchers at home and abroad from the aspects of material formula composition, preparation process and the like aiming at the permeation resistance of cement concrete, wherein the research and development of a high-performance cement-based permeable crystalline waterproof material is one of the currently effective technical schemes. The cement-based capillary crystalline waterproof material (CCCW) is a rigid waterproof material which is prepared by taking portland cement or ordinary portland cement, fine quartz sand or silica sand and the like as base materials and doping active chemical substances (catalysts) and other auxiliary materials. Under the action of water, active chemical substances contained in the cement-based permeable crystalline waterproof material are brought into pores in the surface layer of the structure through the erosion of surface water to the inside of the structure, and are subjected to an interactive hydration reaction with components such as free calcium oxide in concrete. The crystals absorb water and swell in the structural pores from sparse to dense, so that a compact anti-permeability area is gradually formed on the surface layer of the concrete structure towards depth, and the integral anti-permeability capability of the structure is further improved;
the traditional waterproof material has the defects of poor self toughness, low expansion coefficient matching degree with a cement concrete matrix, poor interface compatibility and the like, and induces the waterproof material to crack, hole and the like in the service process, so that the surface strength and the anti-permeability of the cement concrete are deteriorated, the protection capability of the cement concrete is finally failed in advance, and the service life cycle of the cement concrete is shortened. Furthermore, literature studies have shown that: microspheric SiO2/Al2O3The powder has the advantages of large bulk density, high volume specific capacity, good fluidity, excellent dispersibility and processability and the like. Microspheric SiO2/Al2O3Compared with the traditional irregular flaky or granular powder, the powder has higher apparent density or tap density, and is beneficial to obtaining excellent comprehensive physical properties such as surface strength of the final sample product.
Disclosure of Invention
The invention aims to solve the problems in the background technology and provides a nano-permeable crystallized self-healing inorganic waterproof material on a back water surface and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
the nano-permeable crystallized self-healing inorganic waterproof powder material on the back surface comprises sodium carbonate, silica fume, rubber powder and quartz sand, and further comprises the following components: sequestering agent, fiber agent, water reducing agent, talcum powder, defoaming agent, paraffin and porous hollow SiO2/Al2O3Composite nanospheres, a permeable crystallization material, zinc phthalate and a wax water repellent.
Preferably, the rubber powder is redispersible latex powder, and the particle size of the quartz sand is 0.3mm-0.5 mm.
Preferably, the fiber agent comprises an expanding agent, fibers and a dispersing agent, the defoaming agent comprises a chloroplatinic acid-isopropanol solution, hexachloro-p-xylene, a cosolvent, polyether modified polysiloxane, an alkaline catalyst and a dehydrogenation catalyst, and the penetrating crystal material comprises sodium silicate, redispersible latex powder and ordinary silicate cement.
Preferably, the porous hollow SiO2/Al2O3The hollow nanospheres of the composite nanospheres have the size of 150 nm-200 nm and the pore size of 50 nm-60 nm.
The preparation method of the nano-permeable crystallized self-healing inorganic waterproof material on the back surface comprises the following steps:
the method comprises the following steps: grinding treatment of bed material
Grinding sodium carbonate raw material by using a grinding device, drying the ground sodium carbonate, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to a ratio of 1: 1, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, di-zinc phthalate and wax water repellent into the base material obtained in the step one, fully mixing and stirring the materials uniformly, continuing to heat the mixture by superheated steam at the temperature of 115-145 ℃ for about 30-45 min, heating while stirring, and cooling to obtain corresponding primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing at the stirring temperature of 40-50 ℃, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of the polymerization environment at 0.01-0.03 MPa, simultaneously adding a cosolvent, keeping the polymerization temperature at 80-100 ℃, keeping the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide to prepare an expanding agent, mixing glass fiber and polyester fiber to prepare composite fiber, wherein the dispersing agent is glyceryl tristearate preferentially, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing, adding absolute ethyl alcohol in a ratio of 1: 5 with the dispersing agent, transferring the mixture into a reaction kettle to be fully stirred and mixed, keeping the reaction temperature at 60-70 ℃ and the reaction time at 2 hours, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement to obtain a mixture, blending the mixture with redispersible latex powder to form a mixed material, and secondly, compounding the mixed material with the primary waterproof powder obtained in the second step to obtain composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres with the permeable crystallization material composite powder obtained in the fifth step, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, and pressurizing and heatingTreating, namely increasing the pressure in the reaction kettle to 10-35 MPa, adjusting the hydrothermal temperature to 40-50 ℃, and continuously reacting for 6-12 h to obtain porous hollow SiO2/Al2O3Composite nanosphere modified permeable crystalline material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nano-sphere modified permeable crystalline material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 40-60 ℃, adding absolute ethyl alcohol with the mass ratio of 1: 2 to the mixture, simultaneously adding the high-hydrophilic defoaming agent prepared in the third step into the mixed solution for continuous stirring, keeping the rotating speed of a stirring rod at 100-200 r/min, then carrying out evaporation crystallization on the mixed solution, and crushing and grinding the evaporated crystal to obtain the final SiO crystal2/Al2O3Composite nanosphere modified permeable crystalline inorganic waterproof powder material
Preferably, the particle size of the sodium carbonate ground in the first step is 0.1mm-0.3mm, the drying temperature in the first step is 30-50 ℃, the mass ratio of the talcum powder to the paraffin in the second step is 2: 3-2: 5, and the mass ratio of the talcum powder to the base material is 1: 2-1: 4.5.
Preferably, the mass ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene in the step III is 1: 5 to 1: 9, and the mass ratio of the polyether modified polysiloxane to the alkali catalyst is 3: 1 to 5: 1.
Preferably, the mass ratio of the sodium bicarbonate to the calcium oxide in the step four is 1: 1 to 1: 3, and the mass ratio of the glass fiber to the polyester fiber is 1: 2 to 1: 5.
Preferably, in the fifth step, the mass ratio of the sodium silicate to the ordinary portland cement is 1: 3 to 1: 7, and the mass ratio of the mixed material to the redispersible latex powder is 1: 0.3 to 1: 0.8.
Preferably, the porous hollow SiO in the sixth step2/Al2O3And D, the mass ratio of the composite nanospheres to the permeable crystallization material composite powder obtained in the step five is 1: 6 to 1: 2.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. in the present invention, microspheric SiO2/Al2O3The powder has the advantages of large bulk density, high volume specific capacity, good fluidity, excellent dispersibility, processability and the like, has higher apparent density or tap density, and is beneficial to obtaining excellent comprehensive physical properties such as surface strength and the like of a final sample product.
2. In the present invention, porous hollow SiO2/Al2O3The composite nanosphere modified permeable crystallization inorganic waterproof material is beneficial to the waterproof material and the alkaline substance (Ca) in the cement concrete2+、SiO3 2-Etc.) to form more compact composite hydrated substance (Ca)5Si6(OH)4H20-Al(OH)3) The compression strength (28d) and the impervious pressure ratio (28d) of the cement concrete are improved.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
sodium carbonate, silica fume, absolute ethyl alcohol, rubber powder, quartz sand, a polyvalent chelating agent, a fiber agent, a water reducing agent, a permeable crystallization material and porous hollow SiO2/Al2O3The compound nanospheres are used as raw material formula, and porous hollow SiO is prepared by optimization2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof material. The method comprises the following specific steps:
the method comprises the following steps: grinding treatment of bed material
Grinding a sodium carbonate raw material by using a grinding device, wherein the particle size of the ground sodium carbonate is 0.1mm, drying the ground material at the temperature of 30 ℃, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to the ratio of 1: 1, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, zinc phthalate and a wax water repellent into the base material obtained in the first step, wherein the ratio of the talcum powder to the paraffin is 2: 3, and the ratio of the talcum powder to the base material is 1: 2, fully mixing and uniformly stirring the materials, continuing to heat the materials by superheated steam at 115 ℃ for about 30min, keeping stirring the materials while heating, and then cooling the materials to obtain primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing, stirring at 40 ℃, keeping the ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene at 1: 5, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of a polymerization environment at 0.01MPa, keeping the ratio of the polyether modified polysiloxane to the alkaline catalyst at 3: 1, simultaneously adding a cosolvent, keeping the polymerization temperature at 80 ℃, keeping the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide at a ratio of 1: 1 to prepare an expanding agent, mixing glass fiber and polyester fiber at a ratio of 1: 2 to prepare composite fiber, preferentially using glyceryl tristearate as a dispersing agent, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing, adding absolute ethyl alcohol at a ratio of 1: 5 to the dispersing agent, transferring the absolute ethyl alcohol into a reaction kettle, fully stirring and mixing, keeping the reaction temperature at 60 ℃, reacting for 2 hours, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement according to the mass ratio of 1: 3, and blending the obtained mixture and the redispersible latex powder according to the mass ratio of 1: 0.3 to form a mixed material; secondly, compounding the composite powder with the primary waterproof powder in the second step to obtain corresponding composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres and the permeable crystallization material composite powder obtained in the fifth step according to the mass ratio of 1: 6, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, carrying out pressurization and heating treatment, increasing the pressure in the reaction kettle to 10MPa, adjusting the temperature to 40 ℃ to obtain SiO2/Al2O3Composite nanosphere modified permeable crystalline material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nano-sphere modified permeable crystallization material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 40 ℃, adding absolute ethyl alcohol with the mass ratio of the mixture to the absolute ethyl alcohol of 1: 2, adding a defoaming agent into the mixed solution, stirring at the stirring speed of 100r/min, evaporating and crystallizing the mixed solution, crushing and grinding crystals to finally obtain SiO2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material.
Example 2:
sodium carbonate, silica fume, orWater ethanol, rubber powder, quartz sand, sequestering agent, fiber agent, water reducing agent, permeable crystallization material and porous hollow SiO2/Al2O3The composite nanospheres are used as raw materials to prepare corresponding porous hollow SiO2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof material. The method comprises the following specific steps:
the method comprises the following steps: grinding treatment of bed material
Grinding a sodium carbonate raw material by using a grinding device, wherein the particle size of the ground sodium carbonate is 0.3mm, drying the ground material at the temperature of 50 ℃, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to the ratio of 1: 4, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, zinc phthalate and a wax water repellent into the base material obtained in the first step, wherein the ratio of the talcum powder to the paraffin is 2: 5, and the ratio of the talcum powder to the base material is 1: 4.5, fully mixing and uniformly stirring, then continuing to heat by using superheated steam at 145 ℃ for about 45min, keeping stirring the raw materials while heating, and then cooling to obtain primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing, stirring at 50 ℃, keeping the ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene at 1: 9, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of a polymerization environment at 0.03MPa, keeping the ratio of the polyether modified polysiloxane to the alkaline catalyst at 5: 1, simultaneously adding a cosolvent, keeping the polymerization temperature at 100 ℃, keeping the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide according to a mass ratio of 1: 3 to prepare an expanding agent, mixing glass fiber and polyester fiber according to a mass ratio of 1: 5 to prepare composite fiber, preferentially adopting glyceryl tristearate as a dispersing agent, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing is completed, adding absolute ethyl alcohol according to a ratio of 1: 5 to the dispersing agent, transferring the mixture into a reaction kettle, fully stirring and mixing, simultaneously keeping the reaction temperature at 70 ℃, and keeping the reaction time at 2h, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement according to the mass ratio of 1: 7, and blending the obtained mixture and redispersible latex powder according to the mass ratio of 1: 0.8 to form a mixed material; secondly, compounding the composite powder with the primary waterproof powder in the second step to obtain corresponding composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres and the permeable crystallization material composite powder obtained in the fifth step according to the mass ratio of 3: 6, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, carrying out pressurization and heating treatment, increasing the pressure in the reaction kettle to 35MPa, adjusting the temperature to 50 ℃ to obtain SiO2/Al2O3Composite nanosphere modified permeable crystalline material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nanometer ball modified permeable crystallization material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 60 ℃, adding into the mixtureAdding the defoaming agent into the mixed solution while stirring at the stirring speed of 200r/min, then carrying out evaporative crystallization on the mixed solution, and crushing and grinding crystals to finally obtain SiO2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material.
Example 3:
the coating is prepared from sodium carbonate, silica fume, absolute ethyl alcohol, rubber powder, quartz sand and the following components: sequestering agent, fibrous agent, water reducing agent, osmotic crystalline material, and porous hollow SiO2/Al2O3The compound nanospheres are used as raw material formula, and the corresponding porous hollow SiO is prepared by regulating and controlling the formula process2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof material. The method comprises the following specific steps:
the method comprises the following steps: grinding treatment of bed material
Grinding a sodium carbonate raw material by using a grinding device, wherein the particle size of the ground sodium carbonate is 0.15mm, drying the ground material at the temperature of 40 ℃, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to the ratio of 1: 3, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, zinc phthalate and a wax water repellent into the base material obtained in the first step, wherein the ratio of the talcum powder to the paraffin is 2: 4, and the ratio of the talcum powder to the base material is 1: 3, fully mixing and uniformly stirring the materials, continuing to heat the materials by superheated steam at 120 ℃ for about 35min, keeping stirring the materials while heating, and then cooling the materials to obtain primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing, stirring at 45 ℃, keeping the ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene at 1: 7, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of the polymerization environment at 0.02MPa, keeping the ratio of the polyether modified polysiloxane to the alkaline catalyst at 4: 1, simultaneously adding a cosolvent, keeping the polymerization temperature between 90 ℃ and the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide at a mass ratio of 1: 2 to prepare an expanding agent, mixing glass fiber and polyester fiber at a mass ratio of 1: 3 to prepare composite fiber, preferentially adopting glyceryl tristearate as a dispersing agent, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing is completed, adding absolute ethyl alcohol at a ratio of 1: 5 to the dispersing agent, transferring the absolute ethyl alcohol into a reaction kettle, fully stirring and mixing, simultaneously keeping the reaction temperature at 65 ℃, and reacting for 2 hours, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement according to the mass ratio of 1: 5, and blending the obtained mixture and the redispersible latex powder according to the mass ratio of 1: 0.6 to form a mixed material; secondly, compounding the composite powder with the primary waterproof powder in the second step to obtain corresponding composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres and the permeable crystallization material composite powder obtained in the fifth step according to the mass ratio of 2.5: 6, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, carrying out pressurization and heating treatment, enhancing the pressure in the kettle to be 30MPa, adjusting the temperature to be 45 ℃ to obtain SiO2/Al2O3Composite nanosphere modified permeable crystalline material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nano-sphere modified permeable crystallization material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 55 ℃, adding absolute ethyl alcohol with the mass ratio of the mixture to the absolute ethyl alcohol of 1: 2, adding a defoaming agent into the mixed solution, stirring at the stirring speed of 150r/min, evaporating and crystallizing the mixed solution, crushing and grinding crystals to finally obtain SiO2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material.
Example 4:
the coating is prepared from sodium carbonate, silica fume, absolute ethyl alcohol, rubber powder, quartz sand and the following components: sequestering agent, fibrous agent, water reducing agent, osmotic crystalline material, and porous hollow SiO2/Al2O3The compound nanospheres are used as raw material formula, and the corresponding porous hollow SiO is prepared by regulating and controlling the formula process2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material. The method comprises the following specific steps:
the method comprises the following steps: grinding treatment of bed material
Grinding a sodium carbonate raw material by using a grinding device, wherein the particle size of the ground sodium carbonate is 0.18m, drying the ground material at the temperature of 37 ℃, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to the ratio of 1: 2.5, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, zinc phthalate and a wax water repellent into the base material obtained in the first step, wherein the ratio of the talcum powder to the paraffin is 2: 3.5, and the ratio of the talcum powder to the base material is 1: 3.5, fully mixing and uniformly stirring, then continuing to heat by superheated steam at 128 ℃ for about 38min, keeping stirring the raw materials while heating, and then cooling to obtain primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing, stirring at 46 ℃, keeping the ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene at 1: 7, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of a polymerization environment at 0.015MPa, and the ratio of the polyether modified polysiloxane to the alkaline catalyst at 3.5: 1, simultaneously adding a cosolvent, keeping the polymerization temperature at 85 ℃, keeping the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide according to a mass ratio of 1: 1.5 to prepare an expanding agent, mixing glass fiber and polyester fiber according to a mass ratio of 1: 3.5 to prepare composite fiber, preferentially using glyceryl tristearate as a dispersing agent, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing, adding absolute ethyl alcohol according to a ratio of 1: 5 to the dispersing agent, transferring the mixture into a reaction kettle, fully stirring and mixing, keeping the reaction temperature at 64 ℃ and the reaction time at 2h, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement according to the mass ratio of 1: 5.5, and blending the obtained mixture and redispersible latex powder according to the mass ratio of 1: 0.7 to form a mixed material; secondly, compounding the composite powder with the primary waterproof powder in the second step to obtain corresponding composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres and the permeable crystallization material composite powder obtained in the fifth step according to the mass ratio of 1.7: 6, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, carrying out pressurization and heating treatment, emphasizing the pressure in the kettle to be 18MPa, adjusting the temperature to be 48 ℃ to obtain SiO2/Al2O3Composite nanosphere modified permeable crystalline material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nano-sphere modified permeable crystallization material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 57 ℃, adding absolute ethyl alcohol with the mass ratio of the mixture to the absolute ethyl alcohol of 1: 2, adding a defoaming agent into the mixed solution, stirring at the stirring speed of 180r/min, evaporating and crystallizing the mixed solution, crushing and grinding crystals to finally obtain SiO2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material.
Example 5:
the coating is prepared from sodium carbonate, silica fume, absolute ethyl alcohol, rubber powder, quartz sand and the following components: the traditional permeable crystallization inorganic waterproof material is prepared by taking a polyvalent chelating agent, a fiber agent, a water reducing agent and a permeable crystallization material as raw materials. The method comprises the following specific steps:
the method comprises the following steps: grinding treatment of bed material
Grinding a sodium carbonate raw material by using a grinding device, wherein the particle size of the ground sodium carbonate is 0.28m, drying the ground material at the temperature of 48 ℃, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to the ratio of 1: 3.8, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, zinc phthalate and a wax water repellent into the base material obtained in the first step, wherein the ratio of the talcum powder to the paraffin is 2: 4.7, and the ratio of the talcum powder to the base material is 1: 3.8, fully mixing and uniformly stirring, then continuing to heat by superheated steam at 135 ℃ for 42min, keeping stirring the raw materials while heating, and then cooling to obtain primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing, stirring at 46 ℃, keeping the ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene at 1: 5.8, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of a polymerization environment at 0.025MPa, and the ratio of the polyether modified polysiloxane to the alkaline catalyst at 4.8: 1, simultaneously adding a cosolvent, keeping the polymerization temperature between 95 ℃, keeping the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide according to a mass ratio of 1: 2.8 to prepare an expanding agent, mixing glass fiber and polyester fiber according to a mass ratio of 1: 3.2 to prepare composite fiber, preferentially using glyceryl tristearate as a dispersing agent, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing, adding absolute ethyl alcohol according to a ratio of 1: 5 to the dispersing agent, transferring the mixture into a reaction kettle, fully stirring and mixing, keeping the reaction temperature at 68 ℃, reacting for 2 hours, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement according to the mass ratio of 1: 6.2, and blending the obtained mixture and redispersible latex powder according to the mass ratio of 1: 0.6 to form a mixed material; secondly, compounding the composite powder with the primary waterproof powder in the second step to obtain corresponding composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres and the permeable crystallization material composite powder obtained in the fifth step according to the mass ratio of 1.5: 6, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, carrying out pressurization and heating treatment, emphasizing the pressure in the kettle to be 16MPa, adjusting the temperature to be 52 ℃ to obtain SiO2/Al2O3Composite nanosphere modified permeable crystalline material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nano-sphere modified permeable crystallization material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 52 ℃, adding absolute ethyl alcohol with the mass ratio of the mixture to 1: 2, adding a defoaming agent into the mixed solution, stirring at the stirring speed of 185r/min, evaporating and crystallizing the mixed solution, crushing and grinding crystals to obtain SiO final product2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material.
The traditional permeable crystallization inorganic waterproof powder material prepared in the embodiment is taken as a research object, and is prepared into corresponding waterproof paint with a solvent-deionized water according to a certain proportion, and the prepared waterproof paint is uniformly coated on the surface of cement concrete for performance comparison tests such as surface wettability, compressive strength (28d), impermeability pressure ratio (28d) and the like.
The analysis shows that: compared with the unmodified traditional cement concrete (example 5, comparison group), the nano permeable crystallization inorganic waterproof material, namely SiO, designed and developed by the invention2/Al2O3After the composite nanosphere modified permeable crystalline inorganic waterproof powder material is applied to cement concrete, the surface interface wettability between the waterproof material and the cement concrete can be effectively reduced, the permeability is increased, the performances of the cement concrete such as the compressive strength (28d), the impermeability pressure ratio (28d) and the like are improved, and an excellent waterproof effect is shown.
Figure BDA0003379538560000161
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. The nano-permeable crystallization self-healing inorganic waterproof material on the back water surface is characterized in that: the nano-penetration crystallization inorganic waterproof powder material comprises sodium carbonate, silica fume, rubber powder and quartz sand, and also comprises the following components: sequestering agent, fiber agent, water reducing agent, talcum powder, defoaming agent, paraffin and porous hollow SiO2/Al2O3Composite nanospheres, a permeable crystallization material, zinc phthalate and a wax water repellent.
2. The backside nano-penetration crystallization self-healing inorganic waterproof material according to claim 1, wherein: the rubber powder is redispersible latex powder, and the particle size of the quartz sand is 0.3mm-0.5 mm.
3. The backside nano-penetration crystallization self-healing inorganic waterproof material according to claim 1, wherein: the fiber agent comprises an expanding agent, fibers and a dispersing agent, the defoaming agent comprises a chloroplatinic acid-isopropanol solution, hexachloro-p-xylene, a cosolvent, polyether modified polysiloxane, an alkaline catalyst and a dehydrogenation catalyst, and the penetrating crystal comprises sodium silicate, redispersible latex powder and ordinary silicate cement.
4. The backside nano-penetration crystallization self-healing inorganic waterproof material according to claim 1, wherein: the porous hollow SiO2/Al2O3The hollow nanospheres of the composite nanospheres have the size of 150 nm-200 nm and the pore size of 50 nm-60 nm.
5. The method for preparing the self-healing inorganic waterproof material with nano-permeation crystallization on the back surface according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
the method comprises the following steps: grinding treatment of bed material
Grinding sodium carbonate raw material by using a grinding device, drying the ground sodium carbonate, adding quartz sand and rubber powder, mixing and stirring, adding a sequestering agent prepared by mixing sodium hexametaphosphate and disodium ethylene diamine tetraacetate according to a ratio of 1: 1, and finally preparing a corresponding base material;
step two: preparation of primary water-proof powder
Adding talcum powder, paraffin, di-zinc phthalate and wax water repellent into the base material obtained in the step one, fully mixing and stirring the materials uniformly, continuing to heat the mixture by superheated steam at the temperature of 115-145 ℃ for about 30-45 min, heating while stirring, and cooling to obtain corresponding primary waterproof powder;
step three: preparation of high hydrophilic defoaming agent
Adding chloroplatinic acid-isopropanol solution and hexachloro-p-xylene into a reaction kettle, mixing at the stirring temperature of 40-50 ℃, keeping the reaction time for 30min, then carrying out vacuum polymerization on the mixed solution, polyether modified polysiloxane and an alkaline catalyst, controlling the ratio of the polyether modified polysiloxane to the mixed solution at 1: 2, controlling the vacuum degree of the polymerization environment at 0.01-0.03 MPa, simultaneously adding a cosolvent, keeping the polymerization temperature at 80-100 ℃, keeping the polymerization time at 1h, and cooling to obtain the high-hydrophilicity type defoaming agent;
step four: preparation of crack resistant fiber agent
Mixing sodium bicarbonate and calcium oxide to prepare an expanding agent, mixing glass fiber and polyester fiber to prepare composite fiber, wherein the dispersing agent is glyceryl tristearate preferentially, then mixing the expanding agent and the composite fiber at normal temperature, adding the dispersing agent after mixing, adding absolute ethyl alcohol in a ratio of 1: 5 with the dispersing agent, transferring the mixture into a reaction kettle to be fully stirred and mixed, keeping the reaction temperature at 60-70 ℃ and the reaction time at 2 hours, and drying and grinding the obtained reaction product to obtain the crack-resistant fiber agent with excellent performance;
step five: preparation of infiltration crystallization material composite powder
Firstly, mixing sodium silicate and ordinary portland cement to obtain a mixture, blending the mixture with redispersible latex powder to form a mixed material, and secondly, compounding the mixed material with the primary waterproof powder obtained in the second step to obtain composite powder of the permeable crystallization material;
step six: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystalline material composite powder
Mixing porous hollow SiO2/Al2O3Mixing the composite nanospheres with the permeable crystallization material composite powder obtained in the fifth step, keeping the external environment temperature to be higher than 5 ℃ during mixing, transferring the material into a reaction kettle after mixing is finished, carrying out pressurization and heating treatment, increasing the pressure in the reaction kettle to 10-35 MPa, adjusting the hydrothermal temperature to 40-50 ℃, and continuously reacting for 6-12 h to obtain porous hollow SiO2/Al2O3 composite nanosphere modified permeable crystallization material composite powder;
step seven: SiO22/Al2O3Preparation of composite nanosphere modified permeable crystallization inorganic waterproof powder material
The crack-resistant fiber agent prepared in the fourth step and the porous hollow SiO prepared in the sixth step2/Al2O3Mixing composite nano-sphere modified permeable crystallization material composite powder according to the mass ratio of 1: 8, keeping the mixing temperature at 40-60 ℃, adding absolute ethyl alcohol with the mass ratio of the mixture of 1: 2, simultaneously adding the high-hydrophilic defoaming agent prepared in the third step into the mixed solution for continuous stirring, and keeping the mixed solutionKeeping the rotation speed of the stirring rod at 100r/min-200r/min, then evaporating and crystallizing the mixed liquid, and grinding the evaporated crystal to obtain the final SiO2/Al2O3The composite nanometer ball modified permeable crystallized inorganic waterproof powder material.
6. The method for preparing the self-healing inorganic waterproof material with nano-penetration crystallization on the back surface as claimed in claim 5, wherein the method comprises the following steps: the particle size of the ground sodium carbonate in the first step is 0.1mm-0.3mm, the drying temperature in the first step is 30-50 ℃, the mass ratio of the talcum powder to the paraffin in the second step is 2: 3-2: 5, and the mass ratio of the talcum powder to the base material is 1: 2-1: 4.5.
7. The method for preparing the self-healing inorganic waterproof material with nano-penetration crystallization on the back surface as claimed in claim 5, wherein the method comprises the following steps: the mass ratio of the chloroplatinic acid-isopropanol solution to the hexachloro-p-xylene in the step III is 1: 5 to 1: 9, and the mass ratio of the polyether modified polysiloxane to the alkali catalyst is 3: 1 to 5: 1.
8. The method for preparing the self-healing inorganic waterproof material with nano-penetration crystallization on the back surface as claimed in claim 5, wherein the method comprises the following steps: the mass ratio of the sodium bicarbonate to the calcium oxide in the step four is 1: 1 to 1: 3, and the mass ratio of the glass fiber to the polyester fiber is 1: 2 to 1: 5.
9. The method for preparing the self-healing inorganic waterproof material with nano-penetration crystallization on the back surface as claimed in claim 5, wherein the method comprises the following steps: in the fifth step, the mass ratio of the sodium silicate to the ordinary portland cement is 1: 3 to 1: 7, and the mass ratio of the mixed material to the redispersible latex powder is 1: 0.3 to 1: 0.8.
10. The method for preparing the self-healing inorganic waterproof material with nano-penetration crystallization on the back surface as claimed in claim 5, wherein the method comprises the following steps: in the sixth step, porous hollow SiO is adopted2/Al2O3Composite nanosphere and step fiveThe mass ratio of the permeable crystallization material composite powder is 1: 6 to 1: 2.
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