CN111777887A - Flame-retardant heat-resistant waterborne polyurethane coating and preparation method thereof - Google Patents
Flame-retardant heat-resistant waterborne polyurethane coating and preparation method thereof Download PDFInfo
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- CN111777887A CN111777887A CN202010724224.2A CN202010724224A CN111777887A CN 111777887 A CN111777887 A CN 111777887A CN 202010724224 A CN202010724224 A CN 202010724224A CN 111777887 A CN111777887 A CN 111777887A
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Abstract
The invention discloses a flame-retardant heat-resistant waterborne polyurethane coating which is prepared from a prepolymer and a dispersing agent, wherein the mass ratio of the prepolymer to the dispersing agent is (3-5): 1-2; the prepolymer is prepared from the following raw materials; polytetrahydrofuran ether glycol, flame-retardant polyester ether polyol, diisocyanate, dimethyl silicone oil, a micromolecule chain extender, acetone, hollow glass beads and a filler; the dispersing agent comprises a hydrophilic chain extender, a defoaming agent, deionized water and ethylenediamine. The invention also discloses a preparation method of the waterborne polyurethane coating, wherein the flame-retardant polyester ether polyol and the filler are added into the raw materials, the flame-retardant polyester ether polyol contains benzene ring groups and phosphorus flame-retardant elements, so that the coating is endowed with excellent flame-retardant performance, the filler comprises tourmaline powder, talcum powder, kaolin and expanded perlite, and the filler has a strong specific surface area and a surface multi-medium open pore structure, so that the heat conductivity coefficient of the waterborne polyurethane coating is reduced, and the flame-retardant capability of the waterborne polyurethane coating is further improved.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a flame-retardant heat-resistant waterborne polyurethane coating and a preparation method thereof.
Background
Polyurethane coatings are the common coatings at present and can be divided into two-component polyurethane coatings and one-component polyurethane coatings. The paint has a plurality of varieties and wide application range, generally has good mechanical property, higher solid content and better performances in all aspects, is a paint variety with development prospect at present, and has main application directions of wood paints, automobile repair paints, anticorrosive paints, floor paints, electronic paints, special paints, polyurethane waterproof paints and the like. The disadvantages are that the construction process is complex, the requirement on the construction environment is high, and the paint film is easy to generate defects. The single-component polyurethane coating mainly comprises urethane oil coating, moisture-cured polyurethane coating, closed polyurethane coating and the like. The coating has a wider application range than a two-component coating, is mainly used for floor coatings, anticorrosive coatings, pre-roll coatings and the like, and has less overall performance than the two-component coating.
The waterborne polyurethane coating is the most ideal waterborne coating at present, but the comprehensive performances such as chemical resistance, water resistance, wear resistance, high temperature resistance and the like of the waterborne polyurethane coating are poorer in domestic research. In the prior art, the first three performances are mostly researched, and the research on the high temperature resistance is less. With the development of science and technology in recent years, people have increasingly increased demands for heat-resistant and flame-retardant water-based paint, and how to prepare flame-retardant and heat-resistant water-based paint becomes a technical problem to be solved at present.
Disclosure of Invention
The invention aims to provide a flame-retardant heat-resistant waterborne polyurethane coating and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
in the prior art, the water-based polyurethane coating has poor heat resistance, potential safety hazards exist when the water-based polyurethane coating is applied to the fields of building materials, textiles, leather and the like, the flame retardant property of the existing flame-retardant polyurethane coating is improved by introducing halogen groups, toxic and harmful substances are easy to generate, and the water-based flame-retardant polyurethane coating is single in property, poor in toughness and poor in wear resistance.
The purpose of the invention can be realized by the following technical scheme:
the flame-retardant heat-resistant waterborne polyurethane coating is prepared from a prepolymer and a dispersing agent, wherein the mass ratio of the prepolymer to the dispersing agent is (3-5): 1-2;
the prepolymer is prepared from the following raw materials: 20-25 parts of polytetrahydrofuran ether glycol, 25-30 parts of flame-retardant polyester ether polyol, 10-20 parts of diisocyanate, 2-5 parts of dimethyl silicone oil, 1-2 parts of small molecular chain extender, 60-80 parts of acetone, 2-4 parts of hollow glass beads and 3-8 parts of filler;
the dispersing agent is prepared from the following raw materials: 2-6 parts of hydrophilic chain extender, 0.1-0.8 part of defoaming agent, 25-35 parts of deionized water and 0.1-1.5 parts of ethylenediamine;
the preparation method of the flame-retardant heat-resistant waterborne polyurethane coating comprises the following steps:
firstly, putting 20-25 parts by weight of polytetrahydrofuran ether glycol and 25-30 parts by weight of flame-retardant polyester ether polyol into a reaction kettle, uniformly stirring, heating to 100-115 ℃, dehydrating in vacuum under the condition of-0.1 MPa until the water content is below 0.04%, putting 10-20 parts by weight of diisocyanate, heating to 85-95 ℃, carrying out heat preservation reaction for 1-3h, and cooling to 40 ℃ to obtain a mixture A;
secondly, adding 2-5 parts by weight of dimethyl silicone oil, 1-2 parts by weight of micromolecule chain extender and 60-80 parts by weight of acetone into the mixture A, heating to 50-55 ℃, uniformly stirring and mixing, then adding 2-4 parts by weight of hollow glass beads and 3-8 parts by weight of filler, and stirring for 3-5 hours to obtain a prepolymer;
thirdly, transferring the prepolymer into an emulsifier, adding 25-35 parts by weight of deionized water and 0.1-1.5 parts by weight of ethylenediamine into the prepolymer under the high-speed stirring of 1000-1500r/min, continuing to stir for 5min, then adjusting the rotating speed to 400-600r/min, adding 2-6 parts by weight of hydrophilic chain extender, and continuing to stir for 3-5h to obtain a mixture B;
and fourthly, removing acetone from the mixture B at the temperature of 40-45 ℃ and under the pressure of-0.09 MPa, adding 0.1-0.8 part by weight of defoaming agent, and uniformly stirring to obtain the flame-retardant heat-resistant waterborne polyurethane coating.
The diisocyanate is one or more of Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI) and Hexamethylene Diisocyanate (HDI) which are mixed in any proportion.
The preparation method of the flame-retardant polyester ether polyol comprises the following steps:
s1, mixing pyromellitic dianhydride, diethylene glycol and dibutyl tin oxide according to the mass ratio of 1-3: 2-5, 0.01-0.05, mixing and stirring under the protection of nitrogen, heating to 140 ℃ for reaction for 2-4h, wherein dibutyltin oxide is used as a catalyst, heating to 240 ℃ for reaction for 2-3h, then performing suction filtration for 2.5-3.5h, cooling to 65-80 ℃, and discharging to obtain a product, namely the pyromellitic acid polyester polyol;
s2, putting the pyromellitic acid polyester polyol and phosphorus oxychloride into a reactor according to the mass ratio of 1:3-5, controlling the temperature to be 60-80 ℃, reacting for 2-3h, finally heating to 100 ℃ and keeping the temperature at 120 ℃ for 3-4h, cooling, filtering, washing and drying to obtain pyromellitic acid flame-retardant polyester polyol;
s3, putting the pyromellitic acid flame-retardant polyester polyol and ethylenediamine into a reaction kettle according to the mass ratio of 1:0.05-0.1, taking the ethylenediamine as a catalyst, then putting propylene oxide which is 0.5-1 times of the mass of the pyromellitic acid polyester polyol into the reaction kettle, slowly heating to the temperature of 100-.
The micromolecule chain extender is one or a mixture of more than one of 1, 4-butanediol, glycol and diglycol in any proportion.
The filler comprises 3-5 parts by weight of tourmaline powder, 15-20 parts by weight of talcum powder, 10-15 parts by weight of kaolin and 5-10 parts by weight of expanded perlite.
The hydrophilic chain extender is one or a mixture of two of dimethylolpropionic acid, dimethylolbutyric acid and 1, 2-dihydroxy-3-sodium propane sulfonate.
The defoaming agent is prepared by the following method: mixing 1.5-3 parts by weight of dimethyl sulfoxide, 2-3 parts by weight of diphenyl azo carbohydrazide, 1-2 parts by weight of sodium tripolyphosphate, 3-7 parts by weight of sodium polynaphthalene formaldehyde sulfonate and 3-5 parts by weight of polyethylene glycol through a rubber mixing mill, and then extruding and granulating to obtain the polyethylene glycol.
The invention has the beneficial effects that:
1. the flame-retardant heat-resistant waterborne polyurethane coating disclosed by the invention has the advantages that the flame-retardant polyester ether polyol is added into the raw materials, and the flame-retardant polyester ether polyol contains benzene ring groups and phosphorus flame-retardant elements, so that the coating is endowed with excellent flame-retardant performance; and the dimethyl silicone oil is added into the system, and the formed polymer can gradually penetrate into polyurethane macromolecules to form a block or graft structure, so that the length of a molecular chain is increased, and the intermolecular force is improved.
2. The matching of the hollow glass microspheres, the tourmaline powder, the talcum powder, the kaolin and the expanded perlite in the coating greatly improves the consistency and the touch resistance of the coating, so that the coating has excellent strength, toughness, wear resistance and corrosion resistance during curing; tourmaline powder, talcum powder, kaolin and expanded perlite have strong specific surface area and a surface multi-medium open pore structure, so that the tourmaline powder has strong adsorption capacity, harmful dust in air is adsorbed after the tourmaline powder is solidified, negative ions are released by the tourmaline, the air is further purified, and the heat conductivity coefficient is reduced due to the internal porous structures of the tourmaline powder, the talcum powder, the kaolin and the expanded perlite, so that the flame retardant capacity of the tourmaline powder is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The flame-retardant heat-resistant waterborne polyurethane coating is prepared from a prepolymer and a dispersing agent, wherein the mass ratio of the prepolymer to the dispersing agent is 3: 1;
the prepolymer is prepared from the following raw materials: 20 parts of polytetrahydrofuran ether glycol, 25 parts of flame-retardant polyester ether polyol, 10 parts of diisocyanate, 2 parts of dimethyl silicone oil, 1 part of micromolecular chain extender, 60 parts of acetone, 2 parts of hollow glass beads and 3 parts of filler;
the dispersing agent is prepared from the following raw materials: 2 parts by weight of a hydrophilic chain extender, 0.1 part by weight of a defoaming agent, 25 parts by weight of deionized water and 0.1 part by weight of ethylenediamine;
the preparation method of the flame-retardant heat-resistant waterborne polyurethane coating comprises the following steps:
step one, putting 20 parts by weight of polytetrahydrofuran ether glycol and 25 parts by weight of flame-retardant polyester ether polyol into a reaction kettle, uniformly stirring, heating to 100 ℃, carrying out vacuum dehydration under the condition of-0.1 MPa until the water content is 0.03%, putting 10 parts by weight of diisocyanate, heating to 85 ℃, carrying out heat preservation reaction for 1 hour, and cooling to 40 ℃ to obtain a mixture A;
secondly, adding 2 parts by weight of dimethyl silicone oil, 1 part by weight of micromolecule chain extender and 60 parts by weight of acetone into the mixture A, heating to 50 ℃, uniformly stirring and mixing, then adding 2 parts by weight of hollow glass beads and 3 parts by weight of filler, and stirring for 3 hours to obtain a prepolymer;
thirdly, transferring the prepolymer into an emulsifier, adding 25 parts by weight of deionized water and 0.1 part by weight of ethylenediamine into the prepolymer under the high-speed stirring of 1000r/min, continuing to stir for 5min, then adjusting the rotation speed to 400r/min, adding 2 parts by weight of hydrophilic chain extender, and continuing to stir for 3h to obtain a mixture B;
and fourthly, removing acetone from the mixture B at the temperature of 40 ℃ and under the pressure of-0.09 MPa, adding 0.1 part by weight of defoaming agent, and uniformly stirring to obtain the flame-retardant heat-resistant waterborne polyurethane coating.
The diisocyanate is a mixture of Toluene Diisocyanate (TDI) and isophorone diisocyanate (IPDI) in any proportion.
The preparation method of the flame-retardant polyester ether polyol comprises the following steps:
s1, mixing pyromellitic dianhydride, diethylene glycol and dibutyl tin oxide according to the mass ratio of 1: 2:0.01, mixing and stirring under the protection of nitrogen, heating to 120 ℃, reacting for 2 hours, heating to 220 ℃, reacting for 2 hours, then performing suction filtration for 2.5 hours, cooling to 65 ℃, discharging, and obtaining a product, namely the pyromellitic polyester polyol;
s2, putting the pyromellitic acid polyester polyol and phosphorus oxychloride into a reactor according to the mass ratio of 1:3, controlling the temperature to be 60 ℃, reacting for 2 hours, finally heating to 100 ℃, preserving the temperature for 3 hours, cooling, filtering, washing and drying to obtain pyromellitic acid flame-retardant polyester polyol;
s3, putting the pyromellitic acid flame-retardant polyester polyol and ethylenediamine into a reaction kettle according to the mass ratio of 1:0.05, then putting epoxypropane with the mass of 0.5 time that of the pyromellitic acid polyester polyol into the reaction kettle, slowly heating to 100 ℃, keeping the pressure in the reaction kettle at 0.1MPa, reacting for 2 hours at the temperature and the pressure, vacuumizing, and carrying out filter pressing and discharging when the temperature is reduced to 80 ℃ to obtain the pyromellitic acid flame-retardant polyester ether polyol.
The micromolecular chain extender is 1, 4-butanediol.
The filler comprises 3 parts by weight of tourmaline powder, 15 parts by weight of talcum powder, 10 parts by weight of kaolin and 5 parts by weight of expanded perlite.
The hydrophilic chain extender is a mixture of dimethylolpropionic acid and dimethylolbutyric acid in any proportion.
The defoaming agent is prepared by the following method: mixing 1.5 parts by weight of dimethyl sulfoxide, 2 parts by weight of diphenyl azo carbohydrazide, 1 part by weight of sodium tripolyphosphate, 3 parts by weight of sodium polynaphthalenesulfonate and 3 parts by weight of polyethylene glycol through a rubber mixing mill, and then extruding and granulating to obtain the polyethylene glycol.
Example 2
The flame-retardant heat-resistant waterborne polyurethane coating comprises a prepolymer and a dispersing agent, wherein the mass ratio of the prepolymer to the dispersing agent is 4: 1;
the prepolymer comprises 23 parts by weight of polytetrahydrofuran ether glycol, 28 parts by weight of flame-retardant polyester ether polyol, 15 parts by weight of diisocyanate, 3 parts by weight of simethicone, 1.5 parts by weight of micromolecule chain extender, 70 parts by weight of acetone, 3 parts by weight of hollow glass beads and 5 parts by weight of filler;
the dispersing agent comprises 4 parts by weight of hydrophilic chain extender, 0.5 part by weight of defoaming agent, 30 parts by weight of deionized water and 1 part by weight of ethylenediamine;
the preparation method of the flame-retardant heat-resistant waterborne polyurethane coating comprises the following steps:
step one, putting 23 parts by weight of polytetrahydrofuran ether glycol and 28 parts by weight of flame-retardant polyester ether polyol into a reaction kettle, uniformly stirring, heating to 113 ℃, carrying out vacuum dehydration under the condition of-0.1 MPa until the water content is 0.02%, putting 15 parts by weight of diisocyanate, heating to 85-95 ℃, carrying out heat preservation reaction for 1.5h, and cooling to 40 ℃ to obtain a mixture A;
secondly, adding 3 parts by weight of simethicone, 1.5 parts by weight of micromolecule chain extender and 70 parts by weight of acetone into the mixture A, heating to 53 ℃, stirring and mixing uniformly, adding 3 parts by weight of hollow glass beads and 5 parts by weight of filler, and stirring for 4 hours to obtain a prepolymer;
thirdly, transferring the prepolymer into an emulsifier, adding 30 parts by weight of deionized water and 0.8 part by weight of ethylenediamine into the prepolymer under the high-speed stirring of 1200r/min, continuing to stir for 5min, then adjusting the rotation speed to 500r/min, adding 4 parts by weight of hydrophilic chain extender, and continuing to stir for 4h to obtain a mixture B;
and fourthly, removing acetone from the mixture B at the temperature of 43 ℃ and under the pressure of-0.09 MPa, adding 0.5 part by weight of defoaming agent, and uniformly stirring to obtain the flame-retardant heat-resistant waterborne polyurethane coating.
The diisocyanate is Toluene Diisocyanate (TDI).
The preparation method of the flame-retardant polyester ether polyol comprises the following steps:
s1, mixing pyromellitic dianhydride, diethylene glycol and dibutyl tin oxide according to the mass ratio of 2: 3:0.03, mixing and stirring under the protection of nitrogen, heating to 130 ℃, reacting for 3 hours, then heating to 230 ℃, reacting for 2.5 hours, then performing suction filtration for 3 hours, cooling to 70 ℃, discharging, and obtaining a product, namely the pyromellitic polyester polyol;
s2, putting the pyromellitic polyester polyol and phosphorus oxychloride into a reactor according to the mass ratio of 1:4, controlling the temperature to be 70 ℃, reacting for 2.5 hours, finally heating to 110 ℃, preserving the temperature for 3.5 hours, cooling, filtering, washing and drying to obtain pyromellitic flame-retardant polyester polyol;
s3, putting the pyromellitic acid flame-retardant polyester polyol and ethylenediamine into a reaction kettle according to the mass ratio of 1:0.05, then putting epoxypropane with the mass of 0.6 time that of the pyromellitic acid polyester polyol into the reaction kettle, slowly heating to 120 ℃, keeping the pressure in the reaction kettle at 0.15MPa, reacting for 3 hours at the temperature and the pressure, vacuumizing, and carrying out filter pressing and discharging when the temperature is reduced to 80 ℃ to obtain the pyromellitic acid flame-retardant polyester ether polyol.
The micromolecular chain extender is 1, 4-butanediol.
The filler comprises 4 parts by weight of tourmaline powder, 18 parts by weight of talcum powder, 12 parts by weight of kaolin and 7 parts by weight of expanded perlite.
The hydrophilic chain extender is a mixture of dimethylolpropionic acid and dimethylolbutyric acid in any proportion.
The defoaming agent is prepared by the following method: mixing 1.8 parts by weight of dimethyl sulfoxide, 3 parts by weight of diphenyl azo carbohydrazide, 2 parts by weight of sodium tripolyphosphate, 4 parts by weight of sodium polynaphthalenesulfonate and 4 parts by weight of polyethylene glycol through a rubber mixing mill, and then extruding and granulating to obtain the polyethylene glycol.
Example 3
The flame-retardant heat-resistant waterborne polyurethane coating comprises a prepolymer and a dispersing agent, wherein the mass ratio of the prepolymer to the dispersing agent is 5: 2;
the prepolymer comprises 25 parts by weight of polytetrahydrofuran ether glycol, 30 parts by weight of flame-retardant polyester ether polyol, 20 parts by weight of diisocyanate, 5 parts by weight of simethicone, 2 parts by weight of micromolecule chain extender, 80 parts by weight of acetone, 4 parts by weight of hollow glass beads and 8 parts by weight of filler;
the dispersing agent comprises 6 parts by weight of hydrophilic chain extender, 0.8 part by weight of defoaming agent, 35 parts by weight of deionized water and 1.5 parts by weight of ethylenediamine;
the preparation method of the flame-retardant heat-resistant waterborne polyurethane coating comprises the following steps:
firstly, putting 25 parts by weight of polytetrahydrofuran ether glycol and 30 parts by weight of flame-retardant polyester ether polyol into a reaction kettle, uniformly stirring, heating to 115 ℃, carrying out vacuum dehydration under the condition of-0.1 MPa until the water content is 0.03%, putting 20 parts by weight of diisocyanate, heating to 95 ℃, carrying out heat preservation reaction for 3 hours, and cooling to 40 ℃ to obtain a mixture A;
secondly, adding 5 parts by weight of dimethyl silicone oil, 2 parts by weight of micromolecular chain extender and 80 parts by weight of acetone into the mixture A, heating to 55 ℃, uniformly stirring and mixing, adding 4 parts by weight of hollow glass beads and 8 parts by weight of filler, and stirring for 5 hours to obtain a prepolymer;
thirdly, transferring the prepolymer into an emulsifier, adding 35 parts by weight of deionized water and 1.5 parts by weight of ethylenediamine into the prepolymer under the high-speed stirring of 1500r/min, continuing to stir for 5min, then adjusting the rotation speed to 600r/min, adding 6 parts by weight of hydrophilic chain extender, and continuing to stir for 5h to obtain a mixture B;
and fourthly, removing acetone from the mixture B at the temperature of 45 ℃ and under the pressure of-0.09 MPa, adding 0.8 part by weight of defoaming agent, and uniformly stirring to obtain the flame-retardant heat-resistant waterborne polyurethane coating.
The diisocyanate is Toluene Diisocyanate (TDI).
The preparation method of the flame-retardant polyester ether polyol comprises the following steps:
s1, mixing pyromellitic dianhydride, diethylene glycol and dibutyl tin oxide according to the mass ratio of 3: 0.05, mixing and stirring under the protection of nitrogen, heating to 140 ℃, reacting for 4 hours, heating to 240 ℃, reacting for 3 hours, then performing suction filtration for 3.5 hours, cooling to 80 ℃, discharging, and obtaining a product, namely the pyromellitic polyester polyol;
s2, putting the pyromellitic acid polyester polyol and phosphorus oxychloride into a reactor according to the mass ratio of 1:5, controlling the temperature to 80 ℃, reacting for 3 hours, finally heating to 120 ℃, preserving the heat for 4 hours, cooling, filtering, washing and drying to obtain pyromellitic acid flame-retardant polyester polyol;
s3, putting the pyromellitic acid flame-retardant polyester polyol and ethylenediamine into a reaction kettle according to the mass ratio of 1:0.1, then putting the same mass of propylene oxide of the pyromellitic acid polyester polyol into the reaction kettle, slowly heating to 130 ℃, keeping the pressure in the reaction kettle at 0.3MPa, reacting for 4 hours at the temperature and the pressure, vacuumizing, and carrying out filter pressing after the temperature is reduced to below 85 ℃, thus obtaining the pyromellitic acid flame-retardant polyester ether polyol.
The micromolecular chain extender is 1, 4-butanediol.
The hydrophilic chain extender is a mixture of dimethylolpropionic acid and dimethylolbutyric acid in any proportion.
The filler comprises 5 parts by weight of tourmaline powder, 20 parts by weight of talcum powder, 15 parts by weight of kaolin and 10 parts by weight of expanded perlite.
The defoaming agent is prepared by the following method: mixing 3 parts by weight of dimethyl sulfoxide, 3 parts by weight of diphenylazocarbohydrazide, 2 parts by weight of sodium tripolyphosphate, 7 parts by weight of sodium polynaphthalene formaldehyde sulfonate and 5 parts by weight of polyethylene glycol through a rubber mixing mill, and then extruding and granulating to obtain the polyethylene glycol.
Comparative example 1
The flame-retardant polyester ether polyol in example 1 was removed and the rest of the preparation process was unchanged.
Comparative example 2
The filler in example 2 was removed and the rest of the preparation was unchanged.
Comparative example 3
The flame retardant polyester ether polyol and filler of example 3 were removed and the remaining preparation was unchanged.
The flame retardant performance of the waterborne polyurethane coatings prepared in examples 1-3 and comparative examples 1-3 in the invention is detected, and the oxygen index is tested according to GB/T2406-1993; carrying out a vertical combustion performance test according to GB/T2408-1994; the test results are shown in the following table:
| test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Oxygen index/% | 35.7 | 33.4 | 37.6 | 25.3 | 26.1 | 27.4 |
| Total combustion time | 3s | 2s | 3s | 15s | 18s | 30s |
| Flame retardant rating | V-0 | V-0 | V-0 | V-1 | V-1 | V-2 |
The above table shows that the flame-retardant polyester ether polyol and the filler are added into the raw materials of the waterborne polyurethane coating prepared by the invention, the flame-retardant polyester ether polyol contains benzene ring groups and phosphorus flame-retardant elements, so that the coating is endowed with excellent flame-retardant performance, and the filler comprises tourmaline powder, talcum powder, kaolin and expanded perlite which have strong specific surface area and surface multi-medium open pore structure, so that the heat conductivity coefficient of the waterborne polyurethane coating is reduced, and the flame-retardant capability of the waterborne polyurethane coating is further improved.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions may be made in the specific embodiments described by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. The flame-retardant heat-resistant waterborne polyurethane coating is characterized by being prepared from a prepolymer and a dispersing agent, wherein the mass ratio of the prepolymer to the dispersing agent is (3-5): 1-2;
the prepolymer is prepared from the following raw materials: 20-25 parts of polytetrahydrofuran ether glycol, 25-30 parts of flame-retardant polyester ether polyol, 10-20 parts of diisocyanate, 2-5 parts of dimethyl silicone oil, 1-2 parts of small molecular chain extender, 60-80 parts of acetone, 2-4 parts of hollow glass beads and 3-8 parts of filler;
the dispersing agent is prepared from the following raw materials: 2-6 parts of hydrophilic chain extender, 0.1-0.8 part of defoaming agent, 25-35 parts of deionized water and 0.1-1.5 parts of ethylenediamine.
2. The flame-retardant heat-resistant aqueous polyurethane coating according to claim 1, wherein the diisocyanate is one or more of Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), and Hexamethylene Diisocyanate (HDI) mixed in an arbitrary ratio.
3. The flame-retardant heat-resistant waterborne polyurethane coating as claimed in claim 1, wherein the small-molecular chain extender is one or a mixture of 1, 4-butanediol, ethylene glycol and diethylene glycol in any proportion.
4. The flame-retardant heat-resistant waterborne polyurethane coating as claimed in claim 1, wherein the preparation method of the flame-retardant polyester ether polyol comprises the following steps:
s1, mixing pyromellitic dianhydride, diethylene glycol and dibutyl tin oxide according to the mass ratio of 1-3: 2-5, 0.01-0.05, mixing and stirring under the protection of nitrogen, heating to 140 ℃ for reaction for 2-4h, wherein dibutyltin oxide is used as a catalyst, heating to 240 ℃ for reaction for 2-3h, then performing suction filtration for 2.5-3.5h, cooling to 65-80 ℃, and discharging to obtain a product, namely the pyromellitic acid polyester polyol;
s2, putting the pyromellitic acid polyester polyol and phosphorus oxychloride into a reactor according to the mass ratio of 1:3-5, controlling the temperature to be 60-80 ℃, reacting for 2-3h, finally heating to 100 ℃ and keeping the temperature at 120 ℃ for 3-4h, cooling, filtering, washing and drying to obtain pyromellitic acid flame-retardant polyester polyol;
s3, putting the pyromellitic acid flame-retardant polyester polyol and ethylenediamine into a reaction kettle according to the mass ratio of 1:0.05-0.1, taking the ethylenediamine as a catalyst, then putting propylene oxide which is 0.5-1 times of the mass of the pyromellitic acid polyester polyol into the reaction kettle, slowly heating to the temperature of 100-.
5. The flame-retardant heat-resistant waterborne polyurethane coating as claimed in claim 1, wherein the filler comprises 3-5 parts by weight of tourmaline powder, 15-20 parts by weight of talcum powder, 10-15 parts by weight of kaolin and 5-10 parts by weight of expanded perlite.
6. The preparation method of the flame-retardant heat-resistant waterborne polyurethane coating as claimed in claim 1, wherein the method comprises the following steps:
firstly, putting 20-25 parts by weight of polytetrahydrofuran ether glycol and 25-30 parts by weight of flame-retardant polyester ether polyol into a reaction kettle, uniformly stirring, heating to 100-115 ℃, dehydrating in vacuum under the condition of-0.1 MPa until the water content is below 0.04%, putting 10-20 parts by weight of diisocyanate, heating to 85-95 ℃, keeping the temperature for reaction for 1-3h, and cooling to 40 ℃ to obtain a mixture A;
secondly, adding 2-5 parts by weight of simethicone, 1-2 parts by weight of micromolecule chain extender and 60-80 parts by weight of acetone into the mixture A, heating to 50-55 ℃, uniformly stirring and mixing, then adding 2-4 parts by weight of hollow glass beads and 3-8 parts by weight of filler, and stirring for 3-5 hours to obtain a prepolymer;
thirdly, transferring the prepolymer into an emulsifier, adding 25-35 parts by weight of deionized water and 0.1-1.5 parts by weight of ethylenediamine into the prepolymer under the high-speed stirring of 1000-1500r/min, continuing to stir for 5min, then adjusting the rotating speed to 400-600r/min, adding 2-6 parts by weight of hydrophilic chain extender, and continuing to stir for 3-5h to obtain a mixture B;
and fourthly, removing acetone from the mixture B at the temperature of 40-45 ℃ and under the pressure of-0.09 MPa, adding 0.1-0.8 part by weight of defoaming agent, and uniformly stirring to obtain the flame-retardant heat-resistant waterborne polyurethane coating.
7. The flame-retardant heat-resistant aqueous polyurethane coating according to claim 1, wherein the hydrophilic chain extender is one or a mixture of two of dimethylolpropionic acid, dimethylolbutyric acid and sodium 1, 2-dihydroxy-3-propanesulfonate.
8. The flame-retardant heat-resistant aqueous polyurethane coating according to claim 1, wherein the defoaming agent is prepared from 1.5 to 3 parts by weight of dimethyl sulfoxide, 2 to 3 parts by weight of diphenylazocarbohydrazide, 1 to 2 parts by weight of sodium tripolyphosphate, 3 to 7 parts by weight of sodium polynaphthalenesulfonate, and 3 to 5 parts by weight of polyethylene glycol.
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