CN110862741A - Preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof coating - Google Patents
Preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof coating Download PDFInfo
- Publication number
- CN110862741A CN110862741A CN201911173000.0A CN201911173000A CN110862741A CN 110862741 A CN110862741 A CN 110862741A CN 201911173000 A CN201911173000 A CN 201911173000A CN 110862741 A CN110862741 A CN 110862741A
- Authority
- CN
- China
- Prior art keywords
- parts
- weight
- temperature
- added
- polyurethane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
-
- 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
- C09D175/08—Polyurethanes from polyethers
-
- 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
- C09D5/08—Anti-corrosive paints
-
- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention belongs to the technical field of waterproof coatings, and particularly relates to a preparation method of a high-temperature-resistant polyurea elastic flame-retardant waterproof coating. The reaction activity of the amino-terminated compound and the isocyanate component is extremely high, and no catalyst is needed, so that the high-temperature resistance of the coating is further improved, and the coating has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of waterproof coatings, and particularly relates to a preparation method of a high-temperature-resistant polyurea elastic flame-retardant waterproof coating.
Background
The polyurea elastic waterproof material is a polyurea elastomer material which is composed of main raw materials such as isocyanate semi-prepolymer, aromatic amine chain extender, polyether, pigment, auxiliary agent and the like. The novel spraying technology is a green and environment-friendly novel spraying technology which is formed by adopting novel equipment and novel process field spraying, and is one of the international excellent spraying technologies at present. The overweight anticorrosive material is mainly used for corrosion prevention and water prevention of concrete storage tanks and accessory facilities in various industries such as sewage treatment pools, drainage ditches, pickling tanks, plating baths, neutralization pools, evaporation pools, petroleum, chemical engineering, oil fields and the like. The anticorrosive paint can be applied in a relatively harsh corrosive environment compared with the conventional anticorrosive paint, and has a longer protection period than the conventional anticorrosive paint. The heavy anti-corrosion coating is mainly different from the conventional anti-corrosion coating in the technical content and the technical difficulty, relates to technical progress and product development in many aspects, does not depend on knowledge and experience of the coating excessively, but depends on knowledge and intersection of multiple subjects such as electronics, physics, ecology, machinery, instruments, management and the like, synthesis of high-corrosion-resistant resin, application of efficient dispersing agent and rheological additive, development of novel anti-corrosion and anti-permeability pigment and filler, application of advanced construction tool, construction maintenance technology, field detection technology and the like, and all need to be applied to the heavy anti-corrosion coating and coating comprehensively. The heavy anti-corrosion paint is mainly different from the conventional anti-corrosion paint in that the heavy anti-corrosion paint has high technical content and great technical difficulty, the related technical progress and product research and development do not depend too much on the knowledge and experience of the paint, the heavy anti-corrosion paint depends on the knowledge and intersection of multiple subjects such as electronics, physics, ecology, machinery, instruments, management and the like, the technology of the heavy anti-corrosion paint is derived from the synthesis of high-resistant resin, the application of high-efficiency dispersing agents and rheological additives, the development of novel anti-corrosion and anti-permeability pigments and fillers, advanced and special test equipment and other supporting measures. The main drawbacks of poly-urea elastomer coatings are: the curing speed is too fast, the interlayer adhesion is poor, and the high temperature resistance and corrosion resistance are poor, so that a preparation method of the high temperature resistant polyurea elastic flame-retardant waterproof coating is urgently needed to be developed by the technical personnel in the field.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-temperature-resistant polyurea elastic flame-retardant waterproof coating aiming at the defects in the prior art, and a paint film can be formed on the surface of concrete. The film has strong compactness, uniform distribution and strong binding capacity, and has low cost, and the obvious defects of water resistance, easy pollution and the like of the concrete surface are overcome.
The invention is realized by the following technical scheme:
the technical scheme adopted by the invention for solving the problems is as follows:
a preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof paint comprises the following steps:
firstly, preparing a grafting solution:
weighing 25-35 parts by weight of at least one of 2-hydroxyethyl methacrylate, methacrylic acid, vinyl acetate or isooctyl acrylate and 1.5-3.0 parts by weight of an organic siloxane coupling agent, dissolving in 85-95 parts by weight of a solvent to obtain a graft solution, wherein the organic siloxane coupling agent is one of β - (3, 4-epoxycyclohexyl) ethyl trimethoxy silane or gamma-isocyanate propyl trimethoxy silane, and the solvent is one of tetrahydrofuran, toluene, dichloromethane or trichloromethane;
secondly, preparing a polyurethane emulsion solution:
after 25-33 parts of hydroxyl-terminated polybutadiene liquid rubber with the number average molecular weight of 2500-5000 are subjected to vacuum dehydration, 24-26 parts of lysine triisocyanate and 42-53 parts of butanone are added and uniformly mixed, the mixture reacts for 1-3 hours at the temperature of 80-85 ℃, the temperature is reduced to room temperature, 0.5-1 part of dimorpholinyl diethyl ether diluted by 5-7 parts of butanone is dropwise added, the dropwise adding speed is controlled, after dropwise adding for 10-20 minutes, the temperature is kept for 10-20 minutes, the temperature is increased to 80-90 ℃, 2-4 parts of epoxy chloropropane is added for end capping, stirring is carried out for 20 minutes, the temperature is reduced to 40 ℃, glacial acetic acid is added to adjust the pH value to 6.5-7, the temperature is kept for 20 minutes, deionized water is added for high-speed dispersion at 600 revolutions per minute, 1.3-2.5 parts of kieselguhr is added;
thirdly, preparing modified polyurethane:
weighing 0.1-1.5 parts by weight of an initiator, adding the initiator into the polyurethane emulsion solution obtained in the second step, adding the grafting solution added with the initiator into the polyurethane emulsion solution added with the initiator under inert gas, heating to 85-95 ℃ to react for 0.5-1 h, cooling to room temperature after the reaction is finished, discharging, washing and drying the obtained product to obtain modified polyurethane;
the initiator is one of potassium persulfate and ammonium persulfate.
Fourthly, synthesis of the modified vinyl ester resin:
putting 2-12 parts by weight of vinyl ester resin into a container with a stirrer, adding 0.5-10 parts by weight of gamma-aminopropyltriethoxysilane, stirring at normal temperature, and reacting for 1-5 hours to obtain modified vinyl ester resin;
fifthly: preparing a polyurethane prepolymer:
28-42 parts of pentaerythritol polyether tetrol; 14-16 parts of triphenylmethane triisocyanate; 3-6 parts of cordierite powder; 3-7 parts of sericite powder, 0.5-1 part of an organosilane coupling agent, 10-12 parts of tetrabromophthalate diol and 4-6 parts of dibromo neopentyl glycol; wherein the hydroxyl value of the polyester polyol is 20-90 mgKOH/g, the viscosity of the polyester polyol is 3000-8000 mPas, the viscosity of the isocyanate is 1000-3000 mPas, and the polyester polyol is added into a reaction kettle and then is subjected to prepolymerization reaction for 1-3 hours at 60-80 ℃ under the protection of nitrogen to obtain a polyurethane prepolymer;
sixthly, the method comprises the following steps: chain extension of polyurethane prepolymer:
after the prepolymerization reaction, adding 0.6-2.5 parts by weight of dimethyl triphenylmethane tetraisocyanate and 1-5 parts by weight of diethyl toluene diamine chain extender into a reaction kettle, and carrying out chain extension reaction for 0.5-2 hours at 60-80 ℃ under the protection of nitrogen;
seventhly, the method comprises the following steps: modification of polyurethane prepolymer:
after chain extension reaction, adding the modified vinyl ester resin obtained in the fourth step and the polyurethane prepolymer at 60-80 ℃ and uniformly stirring, adding the modified polyurethane obtained in the third step and stirring for 0.5-1 hour;
eighthly: preparing high-temperature resistant polyurea elastic flame-retardant waterproof paint:
and cooling the reaction kettle to room temperature, adding 1-2.5 parts by weight of dimethyl-thio-toluenediamine into the reaction kettle, stirring and aging for 0.5-1 h, and adding 10-20 parts by weight of propylene carbonate into the reaction kettle at a constant speed under the stirring condition to obtain the high-temperature-resistant polyurea elastic flame-retardant waterproof coating.
Further, in the first step, the weight ratio of at least one of 2-hydroxyethyl methacrylate, methacrylic acid, vinyl acetate or isooctyl acrylate to the organosiloxane coupling agent is 23-25: 1.
Further, in the third step, at least one of ethanol, butyl acetate, acetone or methanol is adopted in the washing process.
The invention has the beneficial effects that:
the preparation method of the high-temperature-resistant polyurea elastic flame-retardant waterproof coating disclosed by the invention comprises hydroxyl-terminated polybutadiene liquid rubber and a hydroxyl-terminated chain extender, adopts vinyl ester resin modified polyurea coating, and does not contain any hydroxyl component and catalyst. Because the reaction activity of the amino-terminated compound and the isocyanate component is extremely high, the reaction can be instantly completed at room temperature or low temperature without any catalyst, thereby effectively overcoming the fatal defects that the polyurethane elastomer foams and the material performance is rapidly reduced due to the influence of the environmental temperature and humidity in the construction process.
Compared with the prior art, the invention has the following advantages:
the solid content is 100 percent, volatile organic matters are not generated, and the environmental protection requirement is met; the coating does not contain a catalyst, is quickly cured, and can be sprayed and molded on various curved surfaces without sagging; the paint is insensitive to temperature and moisture, and is slightly influenced by the ambient humidity and the temperature during construction; the one-time construction thickness can be from 1 millimeter to several centimeters, the defects of the previous construction for multiple times are overcome, and the construction period is shortened;
excellent physical properties such as tensile strength, tear strength, elongation, abrasion resistance, puncture resistance, and the like. Particularly, the high elongation rate ensures that the concrete has good crack following performance and can effectively protect the concrete base material with cracks; excellent corrosion resistance, can resist long-term soaking of most of corrosive media such as acid, alkali, salt, seawater and the like; the whole structure has no seam, the coating is compact, and the waterproof effect is excellent; the adhesive force to various substrates is high and durable, and the adhesive does not crack or fall off. The coating does not contain a catalyst, is rapid, can be sprayed and formed on any curved surface inclined plane and vertical plane, does not generate a sagging phenomenon, is not sensitive to moisture and humidity, and is not influenced by the ambient temperature and the moisture during construction. 100 percent of solid content, no volatile organic compound and environmental protection. The urea spraying waterproof coating can be sprayed or poured according to the volume ratio of 1:1, the thickness range of one-time construction can be from hundreds of micrometers to several centimeters, the defects of multiple previous constructions are overcome (the recommended thickness is excellent physicochemical properties such as tensile strength, secondary growth rate, flexibility, wear resistance, chemical resistance, corrosion resistance and the like, the coating has good thermal stability, can be used for a long time at 120 ℃, and can bear short-time thermal shock at 150 ℃, the prototype has good reproducibility, the coating is continuous, compact, seamless and pinhole-free, the complete equipment is convenient to use and construct, the efficiency is extremely high, and the urea spraying waterproof coating fundamentally and effectively prevents the reaction of isocyanate, moisture and moisture due to the introduction of an amino-terminated compound in a resin component, a foam elastomer cannot be formed, and the mechanical properties of the material are greatly improved.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
A preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof paint comprises the following steps:
firstly, preparing a grafting solution:
weighing 25 parts by weight of isooctyl acrylate and 1.5 parts by weight of an organic siloxane coupling agent, dissolving in 85 parts by weight of a solvent to obtain a grafting solution, wherein the organic siloxane coupling agent is β - (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, and the solvent is trichloromethane;
secondly, preparing a polyurethane emulsion solution:
vacuum dehydrating 25 parts of hydroxyl-terminated polybutadiene liquid rubber with the number average molecular weight of 2500, adding 24 parts of lysine triisocyanate and 42 parts of butanone, uniformly mixing, reacting at the temperature of 80 ℃ for 1h, cooling to room temperature, dropwise adding 0.5 part of dimorpholinyl diethyl ether diluted by 7 parts of butanone, controlling the dropwise adding speed, after finishing dropwise adding for 10min, keeping the temperature for 10min, heating to 80 ℃, adding 2 parts of epoxy chloropropane for end sealing, stirring for 20min, cooling to 40 ℃, adding glacial acetic acid for adjusting the pH value to 6.5, keeping the temperature for 20min, adding deionized water for high-speed dispersion at 600 revolutions per minute, adding 1.3 parts of kieselguhr, and removing butanone in vacuum to obtain a polyurethane emulsion solution;
thirdly, preparing modified polyurethane:
weighing 0.1 part by weight of initiator, adding the initiator into the polyurethane emulsion solution obtained in the second step, adding the grafting solution added with the initiator into the polyurethane emulsion solution added with the initiator under inert gas, heating to 85 ℃ to perform reaction for 0.5h, cooling to room temperature after the reaction is finished, discharging, washing and drying the obtained product to obtain the modified polyurethane;
the initiator is one of potassium persulfate and ammonium persulfate.
Fourthly, synthesis of the modified vinyl ester resin:
putting 2 parts by weight of vinyl ester resin into a container with a stirrer, adding 0.5 part by weight of gamma-aminopropyltriethoxysilane, and stirring at normal temperature for reaction for 1 hour to obtain modified vinyl ester resin;
fifthly: preparing a polyurethane prepolymer:
42 parts of pentaerythritol polyether tetrol; 14 parts by weight of triphenylmethane triisocyanate; 3 parts of cordierite powder; 3 parts of sericite powder, 0.5 part of organosilane coupling agent, 10 parts of tetrabromophthalate glycol and 4 parts of dibromo neopentyl glycol; wherein the hydroxyl value of the polyester polyol is 20mgKOH/g, the viscosity of the polyester polyol is 3000mPas, the viscosity of the isocyanate is 1000mPas, and the polyester polyol is added into a reaction kettle and then is subjected to prepolymerization reaction for 1 hour at 60 ℃ under the protection of nitrogen to obtain a polyurethane prepolymer;
sixthly, the method comprises the following steps: chain extension of polyurethane prepolymer:
after the prepolymerization reaction, adding 0.6 weight part of dimethyltriphenylmethane tetraisocyanate and 1 weight part of diethyltoluenediamine chain extender into a reaction kettle, and carrying out chain extension reaction for 0.5 hour at 60 ℃ under the protection of nitrogen;
seventhly, the method comprises the following steps: modification of polyurethane prepolymer:
after chain extension reaction, adding the modified vinyl ester resin obtained in the step four and the polyurethane prepolymer at 60 ℃ and stirring uniformly, and then adding the modified polyurethane obtained in the step three and stirring for 0.5 hour;
eighthly: preparing high-temperature resistant polyurea elastic flame-retardant waterproof paint:
and cooling the reaction kettle to room temperature, adding 1 part by weight of dimethyl-sulfur-based toluenediamine into the reaction kettle, stirring and aging for 1h, and adding 20 parts by weight of propylene carbonate into the reaction kettle at a constant speed under the stirring condition to obtain the high-temperature-resistant polyurea elastic flame-retardant waterproof coating.
Further, in the first step, the weight ratio of the isooctyl acrylate to the organosiloxane coupling agent is 23: 1.
Further, ethanol is adopted in the washing process in the third step.
Example 2
A preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof paint comprises the following steps:
firstly, preparing a grafting solution:
weighing 35 parts by weight of methacrylic acid-2-hydroxyethyl ester and 3.0 parts by weight of organic siloxane coupling agent, and dissolving in 95 parts of solvent to obtain a grafting solution; the organic siloxane coupling agent is gamma-isocyanate propyl trimethoxy silane, and the solvent is tetrahydrofuran;
secondly, preparing a polyurethane emulsion solution:
vacuum dehydrating 33 parts of hydroxyl-terminated polybutadiene liquid rubber with the number average molecular weight of 5000, adding 26 parts of lysine triisocyanate and 53 parts of butanone, uniformly mixing, reacting at the temperature of 85 ℃ for 3 hours, cooling to room temperature, dropwise adding 1 part of dimorpholinyl diethyl ether diluted by 7 parts of butanone, controlling the dropwise adding speed, after finishing dropwise adding for 20 minutes, preserving heat for 20 minutes, heating to 90 ℃, adding 4 parts of epoxy chloropropane for end capping, stirring for 20 minutes, cooling to 40 ℃, adding glacial acetic acid for adjusting the pH value to 7, preserving heat for 20 minutes, adding deionized water for high-speed dispersion at 600 revolutions per minute, adding 2.5 parts of diatomite, and removing the butanone in vacuum to obtain a polyurethane emulsion solution;
thirdly, preparing modified polyurethane:
weighing 1.5 parts by weight of initiator, adding the initiator into the polyurethane emulsion solution obtained in the second step, adding the grafting solution added with the initiator into the polyurethane emulsion solution added with the initiator under inert gas, heating to 95 ℃ to perform reaction for 1h, cooling to room temperature after the reaction is finished, discharging, washing and drying the obtained product to obtain the modified polyurethane;
the initiator is one of potassium persulfate and ammonium persulfate.
Fourthly, synthesis of the modified vinyl ester resin:
putting 12 parts by weight of vinyl ester resin into a container with a stirrer, adding 10 parts by weight of gamma-aminopropyltriethoxysilane, and stirring at normal temperature for reaction for 5 hours to obtain modified vinyl ester resin;
fifthly: preparing a polyurethane prepolymer:
42 parts of pentaerythritol polyether tetrol; 16 parts by weight of triphenylmethane triisocyanate; 6 parts of cordierite powder; 7 parts of sericite powder, 1 part of organosilane coupling agent, 12 parts of tetrabromophthalate glycol and 6 parts of dibromo neopentyl glycol; wherein the hydroxyl value of the polyester polyol is 90mgKOH/g, the viscosity of the polyester polyol is 8000mPas, the viscosity of the isocyanate is 3000mPas, and the polyester polyol is added into a reaction kettle and then is subjected to prepolymerization reaction for 3 hours at 80 ℃ under the protection of nitrogen to obtain a polyurethane prepolymer;
sixthly, the method comprises the following steps: chain extension of polyurethane prepolymer:
after the prepolymerization reaction, adding 2.5 parts by weight of dimethyl triphenylmethane tetraisocyanate and 5 parts by weight of diethyl toluene diamine chain extender into a reaction kettle, and carrying out chain extension reaction for 2 hours at 80 ℃ under the protection of nitrogen;
seventhly, the method comprises the following steps: modification of polyurethane prepolymer:
after chain extension reaction, adding the modified vinyl ester resin obtained in the step four and the polyurethane prepolymer at 80 ℃, uniformly stirring, adding the modified polyurethane obtained in the step three, and stirring for 1 hour;
eighthly: preparing high-temperature resistant polyurea elastic flame-retardant waterproof paint:
and cooling the reaction kettle to room temperature, adding 2.5 parts by weight of dimethyl-thio-toluenediamine into the reaction kettle, stirring and aging for 1h, and adding 20 parts by weight of propylene carbonate into the reaction kettle at a constant speed under the stirring condition to obtain the high-temperature-resistant polyurea elastic flame-retardant waterproof coating.
Further, in the first step, the weight ratio of the 2-hydroxyethyl methacrylate to the organosiloxane coupling agent is 25: 1.
Further, acetone is adopted in the washing process in the third step.
TABLE 1 Performance test results of the high temperature resistant polyurea elastic flame retardant waterproof coating of each example and comparative example
Note: low temperature bendability was tested as 10.2.2 in GB/T16777-1997; the water impermeability is tested according to 11.2.2 in GB/T16777-1997, and the tensile strength and the elongation at break are tested according to 6.9 in GB/T19250-2013; the tearing strength is tested according to 6.10 in GB/T19250-2013; the low-temperature flexibility is tested according to GB/T1677 chapter 14; the wet base bond strength was tested in GB/T16777-2008, Chapter 8; the bonding strength with concrete is tested according to the method A of 7.1 in GB/T16777-2008; the water absorption rate is tested according to 6.15 in GB/T19250-2013; alkali resistance was tested according to GB/T9265-2009; the peel strength with concrete was tested according to GB/T2790-1995; the combustion performance is tested according to GB/T8626-2007, and the standard value can be referred to by using a vertical combustion test method (the technical principle of the polyurea elastomer waterproof coating and the application of the polyurea elastomer waterproof coating on a bridge, Touchuan, 2009, 45 th year, page 229 of urban construction).
As can be seen from Table 1, the flame-retardant waterproof coating in each example has good adhesion, corrosion resistance, flexibility and impact resistance, and has very good corrosion resistance.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (4)
1. A preparation method of the high-temperature-resistant polyurea elastic flame-retardant waterproof coating is characterized by comprising the following steps:
firstly, preparing a grafting solution:
weighing 25-35 parts by weight of at least one of 2-hydroxyethyl methacrylate, methacrylic acid, vinyl acetate or isooctyl acrylate and 1.5-3.0 parts by weight of an organic siloxane coupling agent, dissolving in 85-95 parts by weight of a solvent to obtain a graft solution, wherein the organic siloxane coupling agent is one of β - (3, 4-epoxycyclohexyl) ethyl trimethoxy silane or gamma-isocyanate propyl trimethoxy silane, and the solvent is one of tetrahydrofuran, toluene, dichloromethane or trichloromethane;
secondly, preparing a polyurethane emulsion solution:
after 25-33 parts of hydroxyl-terminated polybutadiene liquid rubber with the number average molecular weight of 2500-5000 are subjected to vacuum dehydration, 24-26 parts of lysine triisocyanate and 42-53 parts of butanone are added and uniformly mixed, the mixture reacts for 1-3 hours at the temperature of 80-85 ℃, the temperature is reduced to room temperature, 0.5-1 part of dimorpholinyl diethyl ether diluted by 5-7 parts of butanone is dropwise added, the dropwise adding speed is controlled, after dropwise adding for 10-20 minutes, the temperature is kept for 10-20 minutes, the temperature is increased to 80-90 ℃, 2-4 parts of epoxy chloropropane is added for end capping, stirring is carried out for 20 minutes, the temperature is reduced to 40 ℃, glacial acetic acid is added to adjust the pH value to 6.5-7, the temperature is kept for 20 minutes, deionized water is added for high-speed dispersion at 600 revolutions per minute, 1.3-2.5 parts of kieselguhr is added;
thirdly, preparing modified polyurethane:
weighing 0.1-1.5 parts by weight of an initiator, adding the initiator into the polyurethane emulsion solution obtained in the second step, adding the grafting solution added with the initiator into the polyurethane emulsion solution added with the initiator under inert gas, heating to 85-95 ℃ to react for 0.5-1 h, cooling to room temperature after the reaction is finished, discharging, washing and drying the obtained product to obtain modified polyurethane;
the initiator is one of potassium persulfate and ammonium persulfate;
fourthly, synthesis of the modified vinyl ester resin:
putting 2-12 parts by weight of vinyl ester resin into a container with a stirrer, adding 0.5-10 parts by weight of gamma-aminopropyltriethoxysilane, stirring at normal temperature, and reacting for 1-5 hours to obtain modified vinyl ester resin;
fifthly: preparing a polyurethane prepolymer:
28-42 parts of pentaerythritol polyether tetrol; 14-16 parts of triphenylmethane triisocyanate; 3-6 parts of cordierite powder; 3-7 parts of sericite powder, 0.5-1 part of an organosilane coupling agent, 10-12 parts of tetrabromophthalate diol and 4-6 parts of dibromo neopentyl glycol; wherein the hydroxyl value of the polyester polyol is 20-90 mgKOH/g, the viscosity of the polyester polyol is 3000-8000 mPas, the viscosity of the isocyanate is 1000-3000 mPas, and the polyester polyol is added into a reaction kettle and then is subjected to prepolymerization reaction for 1-3 hours at 60-80 ℃ under the protection of nitrogen to obtain a polyurethane prepolymer;
sixthly, the method comprises the following steps: chain extension of polyurethane prepolymer:
after the prepolymerization reaction, adding 0.6-2.5 parts by weight of dimethyl triphenylmethane tetraisocyanate and 1-5 parts by weight of diethyl toluene diamine chain extender into a reaction kettle, and carrying out chain extension reaction for 0.5-2 hours at 60-80 ℃ under the protection of nitrogen;
seventhly, the method comprises the following steps: modification of polyurethane prepolymer:
after chain extension reaction, adding the modified vinyl ester resin obtained in the fourth step and the polyurethane prepolymer at 60-80 ℃ and uniformly stirring, adding the modified polyurethane obtained in the third step and stirring for 0.5-1 hour;
eighthly: preparing high-temperature resistant polyurea elastic flame-retardant waterproof paint:
and cooling the reaction kettle to room temperature, adding 1-2.5 parts by weight of dimethyl-thio-toluenediamine into the reaction kettle, stirring and aging for 0.5-1 h, and adding 10-20 parts by weight of propylene carbonate into the reaction kettle at a constant speed under the stirring condition to obtain the high-temperature-resistant polyurea elastic flame-retardant waterproof coating.
2. The preparation method of the high temperature resistant polyurea elastic flame retardant waterproof coating material according to claim 1,
in the first step, 27.5-32 parts by weight of at least one of 2-hydroxyethyl methacrylate, methacrylic acid, vinyl acetate or isooctyl acrylate and 2.0-2.5 parts by weight of an organosiloxane coupling agent are added; in the third step, the initiator is 0.25-1.4 parts by weight, and the additive is 0.25-3 parts by weight.
3. The preparation method of the high-temperature-resistant polyurea elastic flame-retardant waterproof coating material according to claim 1, wherein in the first step, the weight ratio of at least one of 2-hydroxyethyl methacrylate, methacrylic acid, vinyl acetate or isooctyl acrylate to the organosiloxane coupling agent is 23-25: 1.
4. The method for preparing the high temperature resistant polyurea elastic flame retardant waterproof coating material according to claim 1, wherein at least one of ethanol, butyl acetate, acetone or methanol is adopted in the washing process in the step three.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911173000.0A CN110862741A (en) | 2019-11-26 | 2019-11-26 | Preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911173000.0A CN110862741A (en) | 2019-11-26 | 2019-11-26 | Preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110862741A true CN110862741A (en) | 2020-03-06 |
Family
ID=69655795
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911173000.0A Withdrawn CN110862741A (en) | 2019-11-26 | 2019-11-26 | Preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110862741A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122124A (en) * | 2021-04-06 | 2021-07-16 | 宋成镇 | Expansion type flame-retardant heat-insulating fireproof coating and preparation method thereof |
-
2019
- 2019-11-26 CN CN201911173000.0A patent/CN110862741A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122124A (en) * | 2021-04-06 | 2021-07-16 | 宋成镇 | Expansion type flame-retardant heat-insulating fireproof coating and preparation method thereof |
| CN113122124B (en) * | 2021-04-06 | 2022-04-22 | 宋成镇 | Expansion type flame-retardant heat-insulating fireproof coating and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108129637A (en) | Polyaspartic Polyurea elastomer and preparation method thereof | |
| CN107298930A (en) | A kind of preparation of organic silicon polyurea self stratifying coating and application method | |
| CN101864166B (en) | Method for preparing organic-silane-modified acrylic polyurethane ultraviolet curing prepolymer | |
| CN109851738B (en) | Preparation method of fluorine-silicon modified carbamido compound | |
| CN105505197A (en) | Ultraviolet curing coating and preparation method thereof | |
| KR101307351B1 (en) | Post-cure type polyurea composition and method for waterproof and anticorrosion of concrete structures using the same | |
| KR101901865B1 (en) | polyurea waterproofing materials and method for waterproofing using this | |
| KR101372812B1 (en) | Polyurea paint enable manual operation | |
| CN116656203A (en) | Coating composition with mildew-proof and antibacterial properties and preparation method thereof | |
| CN112409911A (en) | Polyurethane waterproof coating capable of being used on wet base surface and preparation method thereof | |
| CN110305508B (en) | Preparation method of polyborosiloxane modified polyurethane water-based paint | |
| CN103270122B (en) | Mono-fluid type paint composition for coating glass with excellent anti-lkalinity | |
| CN117106366B (en) | Single-component polyurea coating and preparation method and application thereof | |
| CN110862741A (en) | Preparation method of high-temperature-resistant polyurea elastic flame-retardant waterproof coating | |
| CN105461862A (en) | One-component water-based cationic polyurethane-fluorinated acrylate resin and preparation method thereof | |
| CN115386291B (en) | Single-component polyurethane waterproof coating and preparation method thereof | |
| CN115785850B (en) | Adhesion promoter, preparation method and application thereof, and waterproof adhesive single-component polyurethane sealant, and preparation method and application thereof | |
| CN115322674A (en) | High-adhesion glass finishing paint and preparation method thereof | |
| JPH0119344B2 (en) | ||
| CN115536783A (en) | Solvent-free, acrylic hybrid polyurethane resins, methods of making, compositions containing, and methods of making and using | |
| CN110776801A (en) | Preparation method of concrete corrosion-resistant waterproof coating | |
| CN114716901A (en) | Preparation method of ultralow-water-absorption double-component spray polyurea | |
| CN102382409A (en) | Aqueous resin composition, method for producing the same and metallic coating material | |
| CN117165158B (en) | Silane modified polyether waterproof paint and preparation method thereof | |
| CN115260228B (en) | Silicon-containing compound and preparation method thereof, and single-component polyurethane waterproof coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200306 |