CN112029408A - Environment-friendly waterproof coating and preparation method thereof - Google Patents
Environment-friendly waterproof coating and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses an environment-friendly waterproof coating which is characterized by being prepared from the following components in parts by weight: 30-40 parts of natural asphalt modified vinyl polyurethane, 20-30 parts of vinyl modified hyperbranched polysulfonamide, 10-15 parts of epoxy group POSS, 3-5 parts of hyperbranched polyborate, 0.5-1.5 parts of initiator, 1-3 parts of dispersant, 0.5-1.5 parts of film-forming assistant and 5-10 parts of nano filler. The invention also provides a preparation method of the environment-friendly waterproof coating. The environment-friendly waterproof coating disclosed by the invention is good in environment-friendly performance, remarkable in waterproof effect, good in mechanical property, weather resistance, corrosion resistance, flame retardance and high and low temperature resistance, and large in adhesive force with a base material.
Description
Technical Field
The invention relates to the technical field of coatings, and particularly relates to an environment-friendly waterproof coating and a preparation method thereof.
Background
In recent years, with the continuous development and refinement of the domestic coating industry, the market has more and more outstanding requirements on the coating with special functions, and the waterproof coating is one of the special functional coatings with larger use amount and market demand, and is widely applied to waterproof engineering in the building industry due to excellent waterproof performance and easy construction performance.
The waterproof coating is coated on the surface of a building, a layer of film is formed through volatilization of a solvent or moisture or a chemical reaction of two components, so that the surface of the building is isolated from water, the effects of permeation resistance and water resistance are achieved, and the damage of an external environment and a base layer movable gap is prevented by using the strength and elasticity of the film. However, the traditional waterproof coating is easy to cause phenomena such as aging, drying crack, deformation, fracture, delamination and the like in the using process, and the waterproof property and the weather resistance of the formed paint film are required to be further improved, so that the service life is short. The existing waterproof coating has the technical formula that firstly, the main materials are mostly polymer emulsion emulsified by surfactant, and secondly, plasticizer, dispersant and various surfactants are added to meet the requirements of elasticity, leveling property, viscosity, stability, coating hand feeling and other 'construction performances' of the product. The addition of these adjuvants is harmful to the environment and human body.
The Chinese invention patent with application publication number CN 102079918A discloses a building waterproof paint, which comprises the following components in percentage by weight: 30-50 parts of polyvinyl acetate, 20-30 parts of ethylene-vinyl acetate polymer, 6-10 parts of kaolin, 0.5-2.5 parts of film-forming additive, 6-10 parts of coarse whiting, 0.1-3 parts of dispersing agent, 0.3-0.8 part of defoaming agent, 3-8 parts of silica sol and the balance of deionized water. The building waterproof coating provided by the invention has the advantages of convenient construction, low cost and good leakage-proof effect, and has the defects of poor high and low temperature resistance, poor chemical corrosion resistance and poor mechanical property.
Therefore, the development of the environment-friendly waterproof coating which has good environmental protection performance, obvious waterproof effect, good mechanical property, weather resistance, corrosion resistance and high and low temperature resistance, has large adhesive force with the base material, meets the market demand, has wide market value and application prospect, and has very important significance for promoting the development of waterproof material industry.
Disclosure of Invention
In view of the above, the invention aims to provide an environment-friendly waterproof coating and a preparation method thereof, wherein the preparation method is simple, convenient to construct, low in preparation cost, small in dependence on reaction equipment and suitable for industrial production; the environment-friendly waterproof coating prepared by the preparation method has the advantages of good environment-friendly performance, obvious waterproof effect, good mechanical property, weather resistance, corrosion resistance, flame retardance, high and low temperature resistance and large adhesive force with a base material.
In order to achieve the purpose, the invention adopts the technical scheme that:
the environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 30-40 parts of natural asphalt modified vinyl polyurethane, 20-30 parts of vinyl modified hyperbranched polysulfonamide, 10-15 parts of epoxy group POSS, 3-5 parts of hyperbranched polyborate, 0.5-1.5 parts of initiator, 1-3 parts of dispersant, 0.5-1.5 parts of film-forming assistant and 5-10 parts of nano filler.
Preferably, the nano filler is at least one of nano titanium dioxide, nano boron fiber and nano silicon dioxide.
Preferably, the film forming auxiliary agent is at least one of propylene glycol, methyl ether, propylene glycol butyl ether, alcohol ester twelve and diethylene glycol butyl ether; the dispersing agent is sodium hexametaphosphate and/or sodium polycarboxylate.
Preferably, the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile.
Preferably, the preparation method of the hyperbranched polyborate is described in Chinese patent application No. 200710017753.3, example 1.
Preferably, the preparation method of the epoxy POSS is described in Chinese patent application No. 201710325757, namely example 7.
Preferably, the preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 3-5 hours at 70-80 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 3-6 times, and then performing rotary evaporation to remove residual diethyl ether to obtain the vinyl modified hyperbranched polysulfone amine.
Preferably, the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is (3-5):1, (0.4-0.7):0.2, (25-35).
Preferably, the alkaline catalyst is at least one of sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate; the polymerization inhibitor is at least one of 1, 4-naphthoquinone and chloranil; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the preparation method of the hyperbranched polysulfone amine is disclosed in example 1 of application publication No. CN 108440958A.
Preferably, the preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding the natural asphalt, the vinyl polyurethane and the catalyst into N-methyl pyrrolidone, heating to 100-130 ℃ at the speed of 3-8 ℃/min under the atmosphere of nitrogen or inert gas, and stirring for 4-6 hours under heat preservation to obtain the natural asphalt modified vinyl polyurethane.
Preferably, the mass ratio of the natural asphalt to the vinyl polyurethane to the catalyst to the N-methyl pyrrolidone is (0.5-1.5): (3-5): (0.8-1.2): (20-30).
Preferably, the catalyst is selected from at least one of phosphoric acid, boric acid and p-toluenesulfonic acid; the inert gas is any one of helium, neon and argon.
Preferably, the preparation method of the vinyl polyurethane is as follows: xuanmei Hemerocallis, mechanical Properties of vinyl polyurethane research [ J ] thermosetting resin, 1992,000(004):26, which is VPU-10.
The invention also aims to provide a preparation method of the environment-friendly waterproof coating, which is characterized by comprising the following steps: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at the temperature of 130-150 ℃, cooling, crushing, performing cyclone separation, uniformly mixing the mixture with the initiator, and curing for 2-5 days.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly waterproof coating provided by the invention is simple, convenient to construct, low in preparation cost, small in dependence on reaction equipment and suitable for industrial production.
(2) The environment-friendly waterproof coating provided by the invention overcomes the defects that the traditional waterproof coating is easy to cause aging, cracking, deformation, breaking, layering and the like in the using process, the water resistance and the weather resistance of a formed paint film are required to be further improved, and the service life is short, and also overcomes the problems that the environmental protection property and the water resistance of the existing waterproof coating are required to be further improved.
(3) According to the environment-friendly waterproof coating provided by the invention, the natural asphalt modified vinyl polyurethane is added, the excellent performances of the natural asphalt and the polyurethane are combined, the waterproof performance is better, the comprehensive performance is more excellent, substances with a toxic polyaromatic ring structure in the asphalt are fixed in the coating layer through a cationic polycondensation reaction under the catalysis of acid with vinyl on the vinyl polyurethane through modification, the effects of enhancing the mechanical performance and the weather resistance are achieved, the substances are not easy to overflow and cause harm to the environment and human health, the environmental harm is reduced while the excellent performances such as low price, excellent waterproof performance and the like are utilized, and the economic benefit, the social benefit and the ecological benefit are higher.
(4) According to the environment-friendly waterproof coating provided by the invention, the natural asphalt modified vinyl polyurethane and the residual vinyl on the vinyl modified hyperbranched polysulfone amine are subjected to copolymerization reaction under the action of an initiator, and the hydroxyl on the hyperbranched polyborate and the amino on the vinyl modified hyperbranched polysulfone amine can be subjected to chemical reaction with the epoxy group on the epoxy group POSS, so that a three-dimensional network structure is formed, the comprehensive performance is effectively improved, and particularly, the weather resistance and the waterproofness can be effectively improved by introducing the groups of hydrophobic structures such as sulfone group and borate group.
(5) According to the environment-friendly waterproof coating provided by the invention, the coating is a powder coating, no solvent or water is added, and air is used as a dispersion medium, so that the pollution of a volatile organic solvent to the environment is reduced, the cost is reduced, the defects of slow drying, poor comprehensive performances such as waterproofness and the like of a water-based coating can be avoided, and the aims of good comprehensive performances, short drying time, low cost and excellent environment-friendliness are fulfilled.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
In the embodiment of the invention, the raw materials are all purchased commercially; the preparation method of the hyperbranched polyborate is disclosed in Chinese patent application No. 200710017753.3, namely example 1; the preparation method of the epoxy POSS is described in Chinese patent application No. 201710325757, namely example 7; the preparation method of the hyperbranched polysulfone amine is disclosed in example 1 of application publication No. CN 108440958A; see the preparation method of the vinyl polyurethane: xuanmei Hemerocallis, mechanical Properties of vinyl polyurethane research [ J ] thermosetting resin, 1992,000(004):26, which is VPU-10.
Example 1
The environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 30 parts of natural asphalt modified vinyl polyurethane, 20 parts of vinyl modified hyperbranched polysulfone amine, 10 parts of epoxy group POSS, 3 parts of hyperbranched polyborate, 0.5 part of initiator, 1 part of dispersant, 0.5 part of film-forming assistant and 5 parts of nano filler; the nano filler is nano titanium dioxide; the film-forming assistant is propylene glycol; the dispersant is sodium hexametaphosphate; the initiator is azobisisobutyronitrile.
The preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 3 hours at 70 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 3 times, and then removing residual diethyl ether by rotary evaporation to obtain vinyl modified hyperbranched polysulfone amine; the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is 3:1:0.4:0.2: 25; the alkaline catalyst is sodium hydroxide; the polymerization inhibitor is 1, 4-naphthoquinone; the high boiling point solvent is dimethyl sulfoxide.
The preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding natural asphalt, vinyl polyurethane and a catalyst into N-methyl pyrrolidone, heating to 100 ℃ at the speed of 3 ℃/min under the nitrogen atmosphere, and stirring for 4 hours under heat preservation to obtain natural asphalt modified vinyl polyurethane; the mass ratio of the natural asphalt to the vinyl polyurethane to the catalyst to the N-methyl pyrrolidone is 0.5:3:0.8: 20; the catalyst is selected from phosphoric acid.
The preparation method of the environment-friendly waterproof coating is characterized by comprising the following steps of: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at 130 ℃, cooling, crushing, performing cyclone separation, uniformly mixing with the initiator, and curing for 2 days.
Example 2
The environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 33 parts of natural asphalt modified vinyl polyurethane, 23 parts of vinyl modified hyperbranched polysulfone amine, 12 parts of epoxy group POSS, 3.5 parts of hyperbranched polyborate, 0.9 part of initiator, 1.5 parts of dispersant, 0.8 part of film-forming assistant and 6 parts of nano filler; the nano filler is nano boron fiber; the film-forming auxiliary agent is methyl ether; the dispersant is sodium polycarboxylate; the initiator is azobisisoheptonitrile.
The preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 3.5 hours at 72 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 4 times, and then performing rotary evaporation to remove residual diethyl ether to obtain vinyl modified hyperbranched polysulfone amine; the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is 3.5:1:0.5:0.2: 27; the alkaline catalyst is sodium carbonate; the polymerization inhibitor is 1, 4-naphthoquinone; the high boiling point solvent is N, N-dimethylformamide.
The preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding natural asphalt, vinyl polyurethane and a catalyst into N-methyl pyrrolidone, heating to 110 ℃ at the speed of 5 ℃/min under the atmosphere of helium, and stirring for 4.5 hours under heat preservation to obtain natural asphalt modified vinyl polyurethane; the mass ratio of the natural asphalt to the vinyl polyurethane to the catalyst to the N-methyl pyrrolidone is 0.8:3.5:0.9: 22; the catalyst is boric acid.
The preparation method of the environment-friendly waterproof coating is characterized by comprising the following steps of: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at 135 ℃, cooling, crushing, performing cyclone separation, uniformly mixing with the initiator, and curing for 3 days.
Example 3
The environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 35 parts of natural asphalt modified vinyl polyurethane, 25 parts of vinyl modified hyperbranched polysulfone amine, 13 parts of epoxy group POSS, 4 parts of hyperbranched polyborate, 1 part of initiator, 2 parts of dispersant, 1 part of film-forming assistant and 8 parts of nano filler; the nano filler is nano silicon dioxide; the film-forming auxiliary agent is propylene glycol butyl ether; the dispersant is sodium hexametaphosphate; the initiator is azobisisobutyronitrile.
The preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 4 hours at 75 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 4 times, and then removing residual diethyl ether by rotary evaporation to obtain vinyl modified hyperbranched polysulfone amine; the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is 4:1:0.55:0.2: 30; the alkaline catalyst is potassium hydroxide; the polymerization inhibitor is tetrachlorobenzoquinone; the high boiling point solvent is N, N-dimethylacetamide.
The preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding natural asphalt, vinyl polyurethane and a catalyst into N-methyl pyrrolidone, heating to 115 ℃ at the speed of 6 ℃/min under the atmosphere of neon, and stirring for 5 hours under heat preservation to obtain natural asphalt modified vinyl polyurethane; the mass ratio of the natural asphalt to the vinyl polyurethane to the catalyst to the N-methyl pyrrolidone is 1:4:1: 25; the catalyst is p-toluenesulfonic acid.
The preparation method of the environment-friendly waterproof coating is characterized by comprising the following steps of: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at 140 ℃, then cooling, crushing, performing cyclone separation, uniformly mixing with the initiator, and curing for 3.5 days.
Example 4
The environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 38 parts of natural asphalt modified vinyl polyurethane, 28 parts of vinyl modified hyperbranched polysulfone amine, 14 parts of epoxy group POSS, 4.5 parts of hyperbranched polyborate, 1.4 parts of initiator, 2.5 parts of dispersant, 1.4 parts of film-forming assistant and 9 parts of nano filler; the nano filler is formed by mixing nano titanium dioxide, nano boron fiber and nano silicon dioxide according to the mass ratio of 1:2: 3; the film-forming auxiliary agent is formed by mixing propylene glycol, methyl ether, propylene glycol butyl ether, alcohol ester twelve and diethylene glycol butyl ether according to the mass ratio of 1:1:2:3: 2; the dispersing agent is formed by mixing sodium hexametaphosphate and sodium polycarboxylate according to the mass ratio of 3: 5; the initiator is formed by mixing azodiisobutyronitrile and azodiisoheptonitrile according to the mass ratio of 2: 3.
The preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 4.5 hours at 78 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 6 times, and then performing rotary evaporation to remove residual diethyl ether to obtain vinyl modified hyperbranched polysulfone amine; the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is 4.5:1:0.65:0.2: 33; the alkaline catalyst is prepared by mixing sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate according to the mass ratio of 1:2: 4; the polymerization inhibitor is formed by mixing 1, 4-naphthoquinone and chloranil in a mass ratio of 3: 5; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:3:2: 3.
The preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding natural asphalt, vinyl polyurethane and a catalyst into N-methyl pyrrolidone, heating to 125 ℃ at the speed of 7 ℃/min under the argon atmosphere, and stirring for 5.5 hours under heat preservation to obtain natural asphalt modified vinyl polyurethane; the mass ratio of the natural asphalt to the vinyl polyurethane to the catalyst to the N-methyl pyrrolidone is 1.4:4.5:1.1: 28; the catalyst is prepared by mixing phosphoric acid, boric acid and p-toluenesulfonic acid according to the mass ratio of 1:3: 5.
The preparation method of the environment-friendly waterproof coating is characterized by comprising the following steps of: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at 145 ℃, cooling, crushing, performing cyclone separation, uniformly mixing with the initiator, and curing for 4.5 days.
Example 5
The environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 40 parts of natural asphalt modified vinyl polyurethane, 30 parts of vinyl modified hyperbranched polysulfone amine, 15 parts of epoxy group POSS, 5 parts of hyperbranched polyborate, 1.5 parts of initiator, 3 parts of dispersant, 1.5 parts of film-forming assistant and 10 parts of nano filler; the nano filler is nano titanium dioxide; the film-forming auxiliary agent is diethylene glycol butyl ether; the dispersant is sodium hexametaphosphate; the initiator is azobisisobutyronitrile.
The preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 5 hours at 80 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 6 times, and then removing residual diethyl ether by rotary evaporation to obtain vinyl modified hyperbranched polysulfone amine; the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is 5:1:0.7:0.2: 35; the alkaline catalyst is potassium carbonate; the polymerization inhibitor is tetrachlorobenzoquinone; the high boiling point solvent is N-methyl pyrrolidone.
The preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding natural asphalt, vinyl polyurethane and a catalyst into N-methyl pyrrolidone, heating to 130 ℃ at the speed of 8 ℃/min under the nitrogen atmosphere, and stirring for 6 hours under heat preservation to obtain natural asphalt modified vinyl polyurethane; the mass ratio of the natural asphalt to the vinyl polyurethane to the catalyst to the N-methyl pyrrolidone is 1.5:5:1.2: 30; the catalyst is selected from phosphoric acid.
The preparation method of the environment-friendly waterproof coating is characterized by comprising the following steps of: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at 150 ℃, cooling, crushing, performing cyclone separation, uniformly mixing with the initiator, and curing for 5 days.
Comparative example 1
This example provides an environmentally friendly waterproof coating having the same formulation and preparation method as example 1, except that no hyperbranched polyborate ester is added.
Comparative example 2
This example provides an environmentally friendly waterproof coating having the same formulation and preparation method as example 1, except that no epoxy based POSS is added.
Comparative example 3
This example provides an environmentally friendly waterproof coating, which is prepared according to the same formulation and preparation method as in example 1, except that the vinyl polyurethane is modified by using vinyl polyurethane instead of natural asphalt.
Comparative example 4
The present example provides an environmental protection waterproof coating, the formulation and preparation method are the same as example 1, except that no vinyl modified hyperbranched polysulfonamide is added.
The environmental waterproof coatings obtained in the above examples 1 to 5 and comparative examples 1 to 4 were subjected to performance tests, the test results are shown in table 1, and the test method was performed according to G BT21776-2008 and the corresponding national standard.
TABLE 1 environmental protection waterproof coating Properties
| Test items | Adhesion force | Salt spray resistance for 24h | Contact angle | Impermeability (0.3MPa, 30min) |
| Unit of | Stage | — | ° | — |
| Example 1 | 4B | No bubble and no drop | 123 | Is impervious to water |
| Example 2 | 4B | No bubble and no drop | 126 | Is impervious to water |
| Example 3 | 5B | No bubble and no drop | 130 | Is impervious to water |
| Example 4 | 5B | No bubble and no drop | 132 | Is impervious to water |
| Example 5 | 5B | No bubble and no drop | 133 | Is impervious to water |
| Comparative example 1 | 3B | Without slight drop of bubbles | 110 | Is impervious to water |
| Comparison ofExample 2 | 3B | Without slight drop of bubbles | 112 | Is impervious to water |
| Comparative example 3 | 3B | Without slight drop of bubbles | 107 | Is impervious to water |
| Comparative example 4 | 3B | Without slight drop of bubbles | 115 | Is impervious to water |
As can be seen from Table 1, the environmentally-friendly waterproof coating disclosed by the embodiment of the invention has more excellent mechanical waterproofness and corrosion resistance and larger adhesion, which is the result of the synergistic effect of the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The environment-friendly waterproof coating is characterized by being prepared from the following components in parts by weight: 30-40 parts of natural asphalt modified vinyl polyurethane, 20-30 parts of vinyl modified hyperbranched polysulfonamide, 10-15 parts of epoxy group POSS, 3-5 parts of hyperbranched polyborate, 0.5-1.5 parts of initiator, 1-3 parts of dispersant, 0.5-1.5 parts of film-forming assistant and 5-10 parts of nano filler.
2. The environment-friendly waterproof paint as claimed in claim 1, wherein the nano filler is at least one of nano titanium dioxide, nano boron fiber and nano silica.
3. The environment-friendly waterproof paint as claimed in claim 1, wherein the film forming aid is at least one of propylene glycol, methyl ether, propylene glycol butyl ether, alcohol ester dodeca and diethylene glycol butyl ether; the dispersing agent is sodium hexametaphosphate and/or sodium polycarboxylate.
4. The environment-friendly waterproof coating material as claimed in claim 1, wherein the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile.
5. The environment-friendly waterproof coating material as claimed in claim 1, wherein the preparation method of the vinyl modified hyperbranched polysulfone amine comprises the following steps: adding hyperbranched polysulfone amine, 3, 4-epoxy cyclohexyl methyl methacrylate, a basic catalyst and a polymerization inhibitor into a high boiling point solvent, stirring and reacting for 3-5 hours at 70-80 ℃, then precipitating in water, washing the precipitated polymer with diethyl ether for 3-6 times, and then performing rotary evaporation to remove residual diethyl ether to obtain the vinyl modified hyperbranched polysulfone amine.
6. The environment-friendly waterproof coating material as claimed in claim 5, wherein the mass ratio of the hyperbranched polysulfone amine to the 3, 4-epoxy cyclohexyl methyl methacrylate to the basic catalyst to the polymerization inhibitor to the high boiling point solvent is (3-5):1, (0.4-0.7):0.2, (25-35).
7. The environment-friendly waterproof paint as claimed in claim 5, wherein the alkaline catalyst is at least one of sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate; the polymerization inhibitor is at least one of 1, 4-naphthoquinone and chloranil; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
8. The environment-friendly waterproof coating material as claimed in claim 1, wherein the preparation method of the natural asphalt modified vinyl polyurethane comprises the following steps: adding the natural asphalt, the vinyl polyurethane and the catalyst into N-methyl pyrrolidone, heating to 100-130 ℃ at the speed of 3-8 ℃/min under the atmosphere of nitrogen or inert gas, and stirring for 4-6 hours under heat preservation to obtain the natural asphalt modified vinyl polyurethane.
9. The environment-friendly waterproof coating as claimed in claim 8, wherein the mass ratio of the natural asphalt, the vinyl polyurethane, the catalyst and the N-methyl pyrrolidone is (0.5-1.5): (3-5): (0.8-1.2): (20-30); the catalyst is selected from at least one of phosphoric acid, boric acid and p-toluenesulfonic acid; the inert gas is any one of helium, neon and argon.
10. The environment-friendly waterproof coating material as claimed in any one of claims 1 to 9, wherein the preparation method of the environment-friendly waterproof coating material comprises the following steps: firstly, uniformly mixing the components except the initiator according to the parts by weight to obtain a mixture, then adding the mixture into a double-screw extruder, extruding at the temperature of 130-150 ℃, cooling, crushing, performing cyclone separation, uniformly mixing the mixture with the initiator, and curing for 2-5 days.
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| CN112500731A (en) * | 2020-12-22 | 2021-03-16 | 张可新 | Anti-cracking putty powder and preparation method thereof |
| CN115198259A (en) * | 2022-07-21 | 2022-10-18 | 深圳市钝化技术有限公司 | Passivating solution for stainless steel and preparation method thereof |
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| CN102492116A (en) * | 2011-11-27 | 2012-06-13 | 吉林大学 | Epoxy resin and polyhedral silsesquioxane nano hybrid material and its preparation method |
| CN104403556A (en) * | 2014-12-07 | 2015-03-11 | 李永志 | Water-proof car powder coating with good adhesion |
| CN107190515A (en) * | 2017-05-10 | 2017-09-22 | 上海工程技术大学 | The preparation method and application of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants |
| CN111234691A (en) * | 2020-04-03 | 2020-06-05 | 朱生寿 | Antibacterial and mildew-proof coating with good weather resistance |
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| CN101041718A (en) * | 2007-04-27 | 2007-09-26 | 西安交通大学 | Preparation method for hyper branched boric acid ester |
| CN102492116A (en) * | 2011-11-27 | 2012-06-13 | 吉林大学 | Epoxy resin and polyhedral silsesquioxane nano hybrid material and its preparation method |
| CN104403556A (en) * | 2014-12-07 | 2015-03-11 | 李永志 | Water-proof car powder coating with good adhesion |
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| CN111234691A (en) * | 2020-04-03 | 2020-06-05 | 朱生寿 | Antibacterial and mildew-proof coating with good weather resistance |
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| CN112500731A (en) * | 2020-12-22 | 2021-03-16 | 张可新 | Anti-cracking putty powder and preparation method thereof |
| CN115198259A (en) * | 2022-07-21 | 2022-10-18 | 深圳市钝化技术有限公司 | Passivating solution for stainless steel and preparation method thereof |
| CN115198259B (en) * | 2022-07-21 | 2023-09-15 | 深圳市钝化技术有限公司 | Passivation solution for stainless steel and preparation method thereof |
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