CN112724824B - Environment-friendly fireproof coating and preparation method thereof - Google Patents
Environment-friendly fireproof 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
- C09D177/00—Coating compositions based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Coating compositions based on derivatives of such polymers
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- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- 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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Abstract
The invention discloses an environment-friendly fireproof coating which is characterized by comprising the following components in parts by weight: 40-60 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 5-7 parts of sulfonated polybenzimidazole, 6-8 parts of bisphenol A epoxy resin, 3-5 parts of boron phosphate hollow sphere foam, 1-2 parts of phosphorus pentoxide, 20-30 parts of filler, 1-3 parts of defoaming agent and 0.5-2.5 parts of dispersing agent. The invention also provides a preparation method of the environment-friendly fireproof coating. The environment-friendly fireproof coating provided by the invention has the advantages of good environment-friendly performance, good comprehensive performance and performance stability, obvious flame-retardant fireproof effect, excellent weather resistance, water resistance and high temperature resistance, and strong adhesion with a base material.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to an environment-friendly fireproof coating and a preparation method thereof.
Background
The coating can be coated on the surface of an object by different construction processes to form a continuous solid film with firm adhesion and certain strength. With the continuous progress of the human society, the requirements for coatings with different properties are increasing. The fireproof coating is widely applied in modern engineering, has the strongest adaptability and is most convenient to construct as a common functional coating, has a decorative effect, more importantly, has a fireproof and flame-retardant function, and plays a great role in ensuring the safety of buildings.
The fire-proof paint is a special paint which is used for the surface of a flammable base material, reduces the flammability of the surface of a coated material, retards the rapid spread of fire and is used for improving the fire endurance of the coated material. The fire-retardant coating in the prior art is usually prepared by adding a large amount of flame retardants containing halogen, nitrogen, phosphorus and the like into a formula of a common coating to realize a fire-retardant effect, the fire-retardant coating inevitably reduces the comprehensive performance of the coating along with the addition of a large amount of flame retardants, and the added flame retardants have unsatisfactory flame-retardant effect or generate toxic irritant gases during combustion and are easy to generate secondary pollution as wastes to hinder fire fighting and personnel evacuation and corrode instruments and equipment. In addition, the fireproof paint in the current market has the defects of poor water resistance and weather resistance, poor storage stability, short fire-resistant time, long drying time, poor decoration performance and the like.
For example, a chinese patent application No. 201810756048.3 discloses an environment-friendly fireproof coating, which comprises the following raw materials in parts by weight: 30-50 parts of acrylic emulsion, 5-10 parts of epoxy resin, 5-10 parts of aluminum hydroxide, 3-5 parts of zinc borate, 3-5 parts of kaolin, 2-3 parts of sepiolite, 1-2 parts of vitrified micro bubbles, 1-3 parts of graphene oxide, 1-3 parts of diaminodiphenyl sulfone, 1-2 parts of nonylphenol polyoxyethylene ether, 5-10 parts of pipewort flower inflorescence, 2-3 parts of adhesive and 30-50 parts of deionized water. The invention also discloses a preparation method of the environment-friendly fireproof coating. The paint prepared by the invention has good fireproof and flame-retardant performances under the combined action of various raw materials, can keep good stability in a high-temperature environment, and does not generate harmful gas in the using process. However, the coating has an excessively long drying time and the weather resistance is yet to be further improved.
The field still needs an environment-friendly fireproof coating with good environmental protection performance, good combination property and performance stability, obvious flame-retardant and fireproof effects and excellent weather resistance, water resistance and high temperature resistance.
Disclosure of Invention
In order to solve the problems described in the background art, the invention provides the environment-friendly fireproof coating which has the advantages of good environment-friendly performance, good comprehensive performance and performance stability, obvious flame-retardant and fireproof effects, excellent weather resistance, water resistance and high-temperature resistance and strong adhesion with a base material, and the preparation method thereof.
The invention adopts the technical scheme that the environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 40-60 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 5-7 parts of sulfonated polybenzimidazole, 6-8 parts of bisphenol A epoxy resin, 3-5 parts of boron phosphate hollow sphere foam, 1-2 parts of phosphorus pentoxide, 20-30 parts of filler, 1-3 parts of defoaming agent and 0.5-2.5 parts of dispersing agent.
In one embodiment of the invention, the dispersant is sodium hexametaphosphate and/or a sodium polycarboxylate salt.
In an embodiment of the present invention, the antifoaming agent is one or more of tributyl phosphate, antifoaming agent dele 3100, and antifoaming agent BYK 088.
In one embodiment of the invention, the filler is selected from attapulgite, sepiolite powder, calcium carbonate, titanium dioxide or a mixture of two or more thereof.
In one embodiment of the invention, the filler has a particle size of 800 to 1000 mesh.
In one embodiment of the present invention, the boron phosphate hollow sphere foam is a boron phosphate hollow sphere foam prepared according to the preparation method of chinese patent application No. 201910991534.8 (which is incorporated herein by reference as part of the present invention).
In one embodiment of the present invention, the bisphenol A type epoxy resin is selected from bisphenol A type epoxy resin E-12, bisphenol A type epoxy resin E-06, bisphenol A type epoxy resin E-03, or a mixture of two or more thereof in any ratio.
In one embodiment of the present invention, the sulfonated polybenzimidazole has a sulfonation degree of 80%, and is sulfonated polybenzimidazole obtained by exchanging sodium sulfonate polybenzimidazole prepared by the method of chinese patent application No. 20041001598.2 with dilute hydrochloric acid.
In one embodiment of the present invention, the method for preparing the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing the air in the kettle with inert gas, keeping the temperature in the high-pressure reaction kettle at 230-250 ℃ and the pressure at 1.0-2.0MPa, stirring for reaction for 3-5h, slowly exhausting gas and reducing the pressure to 0.7-1.2MPa within 1-2 h, simultaneously heating the temperature in the high-pressure reaction kettle to 265-280 ℃, stirring for reaction for 0.5-1 h, finally controlling the temperature to be 220-235 ℃ under a vacuum condition, stirring for reaction for 8-12h, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 3-6 times by using ethanol, finally taking out and blowing, placing in a drying box at 80-90 ℃ and drying to constant weight to obtain the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate.
In one embodiment of the invention, the molar ratio of the 2, 5-furandicarboxylic acid, the 2, 6-diaminopurine, the catalyst and the high-boiling solvent is 1.
In one embodiment of the invention, the catalyst is at least one of thiophosphonate, phosphorous acid, thiophosphoramide; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide; the inert gas is one of nitrogen, helium, neon and argon.
The invention also aims to provide a preparation method of the environment-friendly fireproof coating, which is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by using a powder sieve, the powder sieve is 50-100 meshes, and the product is cured for 3-5 days to obtain a finished product of the environment-friendly fireproof coating.
Detailed Description
The following detailed description of preferred embodiments of the invention will be made.
The raw materials in the examples of the invention are all purchased commercially.
The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 40-60 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 5-7 parts of sulfonated polybenzimidazole, 6-8 parts of bisphenol A epoxy resin, 3-5 parts of boron phosphate hollow sphere foam, 1-2 parts of phosphorus pentoxide, 20-30 parts of filler, 1-3 parts of defoaming agent and 0.5-2.5 parts of dispersing agent.
In one embodiment of the invention, the dispersant is sodium hexametaphosphate and/or a sodium polycarboxylate salt.
In an embodiment of the present invention, the antifoaming agent is one or more of tributyl phosphate, antifoaming agent dele 3100, and antifoaming agent BYK 088.
In one embodiment of the invention, the filler is selected from attapulgite, sepiolite powder, calcium carbonate, titanium dioxide or a mixture of two or more thereof.
In one embodiment of the invention, the filler has a particle size of 800 to 1000 mesh.
In one embodiment of the present invention, the boron phosphate hollow sphere foam is a boron phosphate hollow sphere foam prepared according to the preparation method of chinese patent application No. 201910991534.8 (which is incorporated herein by reference as part of the present invention).
In one embodiment of the present invention, the bisphenol A type epoxy resin is selected from bisphenol A type epoxy resin E-12, bisphenol A type epoxy resin E-06, bisphenol A type epoxy resin E-03, or a mixture of two or more thereof in any ratio.
In one embodiment of the present invention, the sulfonated polybenzimidazole has a sulfonation degree of 80%, and is sulfonated polybenzimidazole obtained by exchanging sodium sulfonate polybenzimidazole prepared by the method of chinese patent application No. 20041001598.2 with dilute hydrochloric acid.
In one embodiment of the present invention, the method for preparing the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing the air in the kettle with inert gas, keeping the temperature in the high-pressure reaction kettle at 230-250 ℃ and the pressure at 1.0-2.0MPa, stirring for reaction for 3-5h, slowly exhausting gas and reducing the pressure to 0.7-1.2MPa within 1-2 h, simultaneously heating the temperature in the high-pressure reaction kettle to 265-280 ℃, stirring for reaction for 0.5-1 h, finally controlling the temperature to be 220-235 ℃ under a vacuum condition, stirring for reaction for 8-12h, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 3-6 times by using ethanol, finally taking out and blowing, placing in a drying box at 80-90 ℃ and drying to constant weight to obtain the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate.
In one embodiment of the invention, the molar ratio of the 2, 5-furandicarboxylic acid, the 2, 6-diaminopurine, the catalyst and the high-boiling solvent is 1.
In one embodiment of the invention, the catalyst is at least one of thiophosphonate, phosphorous acid, thiophosphoramide; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide; the inert gas is one of nitrogen, helium, neon and argon.
The invention also aims to provide a preparation method of the environment-friendly fireproof coating, which is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, and after cooling, crushing and cyclone separation, a product is separated by using a powder sieve, the powder sieve is 80-180 meshes, and the product is cured for 3-5 days to obtain a finished product of the environment-friendly fireproof coating.
The beneficial effects of the invention are:
1. the preparation method is simple and easy to implement, does not need special process and special equipment, does not use solvent in the preparation process, has good labor environment, low labor intensity, convenient construction and high finished product qualification rate and preparation efficiency, and is suitable for continuous large-scale production.
2. Through the synergistic effect of the components, the defects that the conventional fireproof coating usually realizes the fireproof effect by adding a large amount of flame retardants containing halogen, nitrogen, phosphorus and the like into the formula of a common coating, the comprehensive performance of the coating is inevitably reduced along with the addition of a large amount of flame retardants, and the added flame retardants have unsatisfactory flame retardant effect or generate toxic irritant gas during combustion and are easy to generate secondary pollution as wastes, thus preventing fire fighting and personnel evacuation and simultaneously corroding instruments and equipment are overcome; the defects of poor water resistance and weather resistance, poor storage stability, short fire-resistant time, long drying time, poor decoration and the like of the fireproof coating on the current market are overcome, so that the prepared fireproof coating has the advantages of good environmental protection performance, good comprehensive performance and performance stability, remarkable flame-retardant and fireproof effects, excellent weather resistance, water resistance and high temperature resistance and strong adhesion with a substrate.
3. The added 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, sulfonated polybenzimidazole and bisphenol A epoxy resin are synergistic to form a film forming substance, sulfonic groups on the sulfonated polybenzimidazole form a catalyst for curing furan groups on the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, meanwhile, epoxy groups on the bisphenol A epoxy resin can perform an epoxy ring opening reaction with amino groups on purine groups of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, and in addition, the sulfonic groups on the sulfonated polybenzimidazole can also perform a crosslinking reaction with benzene rings on the bisphenol A epoxy resin under the catalysis of phosphorus pentoxide, so that a prepared coating film forms a three-dimensional network structure, and the comprehensive performance and the performance stability of the coating are effectively improved. So that the water resistance, high temperature resistance, weather resistance and aging resistance of the product are better.
4. The added 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate has a multi-nitrogen and conjugated structure and a steric effect on a purine structural molecular chain on a main chain, so that the flame retardant property of the coating is good, no hydroxyl group and other groups influencing the reaction yield exist on the molecular structure of a polycondensation monomer, the reaction selectivity is high, and the prepared polycondensate can provide reaction sites for coating curing due to the introduction of furan, and meanwhile, the compatibility among components of the coating can be enhanced, and the bonding property between the polycondensate and a base material is improved; the sulfonated polybenzimidazole not only can provide reaction sites and catalysts for cross-linking and curing of the coating, but also can improve the aging resistance, the high temperature resistance and the flame-retardant and fireproof performance of the coating when the self structure of the sulfonated polybenzimidazole enters a coating molecular chain; the bisphenol A epoxy resin can not only provide reaction sites for curing the coating, but also enhance the compatibility among all components of the coating and improve the bonding property with a substrate.
5. The added boron phosphate hollow sphere foam has a special structure and material, so that the flame-retardant and fireproof performance of the coating is obviously improved, and the heat-preservation, high-temperature-resistant and mechanical properties of the coating can be improved; the coating takes air as a dispersing agent, belongs to the field of powder coatings, does not add halogen and other components which are easy to generate toxic smoke, and has better environmental protection property.
Examples
The present invention will be described in further detail with reference to examples.
Example 1
The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 40 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 5 parts of sulfonated polybenzimidazole, 6 parts of bisphenol A epoxy resin, 3 parts of boron phosphate hollow sphere foam, 1 part of phosphorus pentoxide, 20 parts of filler, 1 part of defoaming agent and 0.5 part of dispersing agent.
The dispersant is sodium hexametaphosphate; the defoaming agent is tributyl phosphate; the filler is attapulgite; the particle size of the filler is 800 meshes; the bisphenol A type epoxy resin is bisphenol A type epoxy resin E-12.
The preparation method of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing air in the kettle with inert gas, keeping the temperature and the pressure in the high-pressure reaction kettle at 230 ℃ and 1.0MPa, stirring for reaction for 3 hours, slowly exhausting gas and reducing the pressure to 0.7MPa within 1 hour, simultaneously heating the temperature in the high-pressure reaction kettle to 265 ℃, stirring for reaction for 0.5 hour, finally controlling the temperature to be 220 ℃ under a vacuum condition, stirring for reaction for 8 hours, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 3 times, finally taking out and placing in a forced air drying oven to dry at 80 ℃ to constant weight to obtain a 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate; the molar ratio of the 2, 5-furandicarboxylic acid, the 2, 6-diaminopurine, the catalyst and the high-boiling solvent is 1; the catalyst is thiophosphonate; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by a powder sieve, the powder sieve is 80 meshes, and the product is cured for 3 days to obtain a finished product of the environment-friendly fireproof coating.
Example 2
The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 45 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 5.5 parts of sulfonated polybenzimidazole, 6.5 parts of bisphenol A epoxy resin, 3.5 parts of boron phosphate hollow sphere foam, 1.2 parts of phosphorus pentoxide, 22 parts of filler, 1.5 parts of defoaming agent and 1 part of dispersing agent.
The dispersant is sodium polycarboxylate; the antifoaming agent is antifoaming agent delete 3100; the filler is sepiolite powder; the particle size of the filler is 850 meshes; the bisphenol A type epoxy resin is bisphenol A type epoxy resin E-06.
The preparation method of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing the air in the kettle with inert gas, keeping the temperature in the high-pressure reaction kettle at 235 ℃ and the pressure at 1.3MPa, stirring for reaction for 3.5 hours, slowly exhausting and reducing the pressure to 0.8MPa within 1.2 hours, simultaneously heating the temperature in the high-pressure reaction kettle to 269 ℃, stirring for reaction for 0.6 hour, finally controlling the temperature to 225 ℃ under a vacuum condition, stirring for reaction for 9 hours, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 4 times with ethanol, finally taking out and placing in a blast drying box to dry to constant weight at 83 ℃ to obtain a 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate; the molar ratio of the 2, 5-furandicarboxylic acid to the 2, 6-diaminopurine to the catalyst to the high-boiling solvent is 1; the catalyst is phosphorous acid; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by a powder screen, the powder screen is 110 meshes, and the product is cured for 3.5 days to obtain a finished product of the environment-friendly fireproof coating.
Example 3
The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 50 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 6 parts of sulfonated polybenzimidazole, 7 parts of bisphenol A epoxy resin, 4 parts of boron phosphate hollow sphere foam, 1.5 parts of phosphorus pentoxide, 25 parts of filler, 2 parts of defoaming agent and 1.5 parts of dispersing agent.
The dispersant is sodium hexametaphosphate; the defoaming agent is a defoaming agent BYK088; the filler is double flying powder; the particle size of the filler is 900 meshes; the bisphenol A type epoxy resin is bisphenol A type epoxy resin E-03.
The preparation method of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing air in the kettle with inert gas, keeping the temperature and the pressure in the high-pressure reaction kettle at 240 ℃ and 1.5MPa, stirring for reaction for 4 hours, slowly exhausting gas and reducing the pressure to 0.9MPa within 1.5 hours, simultaneously heating the temperature in the high-pressure reaction kettle to 273 ℃, stirring for reaction for 0.8 hour, finally controlling the temperature to be 228 ℃ under a vacuum condition, stirring for reaction for 10 hours, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 5 times, finally taking out, placing in a blast drying box, and drying at 85 ℃ to constant weight to obtain a 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate; the molar ratio of the 2, 5-furandicarboxylic acid to the 2, 6-diaminopurine to the catalyst to the high-boiling solvent is 1; the catalyst is thiophosphoryl amide; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is neon.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by a powder screen, the powder screen is 130 meshes, and the product is cured for 4 days to obtain a finished product of the environment-friendly fireproof coating.
Example 4
The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 55 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 6.5 parts of sulfonated polybenzimidazole, 7.5 parts of bisphenol A epoxy resin, 4.5 parts of boron phosphate hollow sphere foam, 1.8 parts of phosphorus pentoxide, 29 parts of filler, 2.5 parts of defoaming agent and 2.3 parts of dispersing agent.
The dispersing agent is formed by mixing sodium hexametaphosphate and sodium polycarboxylate according to the mass ratio of 3; the defoaming agent is formed by mixing tributyl phosphate, a defoaming agent Demodex 3100 and a defoaming agent BYK088 according to a mass ratio of 1; the filler is prepared by mixing attapulgite, sepiolite powder, calcium carbonate powder and titanium dioxide according to a mass ratio of 2; the particle size of the filler is 950 meshes; the bisphenol A epoxy resin is prepared by mixing bisphenol A epoxy resin E-12, bisphenol A epoxy resin E-06 and bisphenol A epoxy resin E-03 according to a mass ratio of 2.
The preparation method of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing the air in the kettle with inert gas, keeping the temperature and the pressure in the high-pressure reaction kettle at 248 ℃ and 1.8MPa, stirring for reacting for 4.5 hours, slowly exhausting and reducing the pressure to 1.1MPa within 1.8 hours, simultaneously heating the temperature in the high-pressure reaction kettle to 277 ℃, stirring for reacting for 0.9 hour, finally controlling the temperature to be 233 ℃ under a vacuum condition, stirring for reacting for 11 hours, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 6 times with ethanol, finally taking out and placing in a blast drying box to dry at 88 ℃ to constant weight to obtain a 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate; the molar ratio of the 2, 5-furandicarboxylic acid to the 2, 6-diaminopurine to the catalyst to the high-boiling solvent is 1; the catalyst is prepared by mixing thiophosphonate, phosphorous acid and thiophosphoryl amide according to the mass ratio of 1; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide according to a mass ratio of 2; the inert gas is argon.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by a powder sieve, the powder sieve is 170 meshes, and the product is cured for 4.5 days to obtain a finished product of the environment-friendly fireproof coating.
Example 5
The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 60 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 7 parts of sulfonated polybenzimidazole, 8 parts of bisphenol A epoxy resin, 5 parts of boron phosphate hollow sphere foam, 2 parts of phosphorus pentoxide, 30 parts of filler, 3 parts of defoaming agent and 2.5 parts of dispersing agent.
The dispersant is sodium hexametaphosphate; the antifoaming agent is antifoaming agent modesty 3100; the filler is double flying powder; the particle size of the filler is 1000 meshes; the bisphenol A type epoxy resin is bisphenol A type epoxy resin E-06.
The preparation method of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high-boiling-point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing the air in the kettle with inert gas, keeping the temperature and the pressure in the high-pressure reaction kettle at 250 ℃ and 2.0MPa, stirring for reaction for 5 hours, slowly exhausting and reducing the pressure to 1.2MPa within 2 hours, simultaneously heating the temperature in the high-pressure reaction kettle to 280 ℃, stirring for reaction for 1 hour, finally controlling the temperature to be 235 ℃ under the vacuum condition, stirring for reaction for 12 hours, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 6 times, finally taking out and placing in a blast drying oven for drying at 90 ℃ to constant weight to obtain a 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate; the molar ratio of the 2, 5-furandicarboxylic acid to the 2, 6-diaminopurine to the catalyst to the high-boiling solvent is 1; the catalyst is phosphorous acid; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by a powder screen, the powder screen is 180 meshes, and the product is cured for 5 days to obtain a finished product of the environment-friendly fireproof coating.
Comparative example 1
An environmentally friendly fire retardant coating was prepared using substantially the same procedure and formulation as in example 1, except that no sulfonated polybenzimidazole was added.
Comparative example 2
An environmentally friendly fire retardant coating was prepared using substantially the same method and formulation as in example 1, except that no bisphenol a type epoxy resin was added.
Comparative example 3
An environmentally friendly fire retardant coating was prepared using substantially the same method and formulation as in example 1, except that no boron phosphate hollow sphere foam was added.
Comparative example 4
An eco-friendly fire retardant coating was prepared by substantially the same method and formulation as in example 1, except that a 2, 6-diaminopurine nucleoside/2, 5-furandicarboxylic acid polycondensate was used instead of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate; the preparation method of the 2,6-diaminopurine nucleoside/2,5-furandicarboxylic acid polycondensate is described in Chinese patent application example 1 of 202010217188.0.
The environmental-friendly fireproof coatings obtained in the examples 1 to 5 and the comparative examples 1 to 4 are tested according to corresponding national standards GB14907-2002, GB/T5210-2006, GB/T1733-93 and GB/T9756-2001 in China, and the test results are shown in Table 1.
TABLE 1 environmental protection fire-proof paint performance of examples and comparative examples
| Detecting items | Fire resistance (min) | Adhesion (Ma) | Water resistance (30 days soaking) | Scrub resistance (1000 times) |
| Example 1 | 57.4 | 10.9 | No abnormality | Non-leaking bottom material |
| Example 2 | 57.8 | 11.2 | No abnormality | Non-leaking bottom material |
| Example 3 | 58.3 | 11.5 | No abnormality | Non-leaking bottom material |
| Example 4 | 58.8 | 11.7 | No abnormality | Non-leaking bottom material |
| Example 5 | 59.1 | 11.9 | No abnormality | Non-leaking bottom material |
| Comparative example 1 | 47.6 | 9.2 | Falling off | Floor drain material |
| Comparative example 2 | 50.3 | 8.5 | Falling off | Floor drain material |
| Comparative example 3 | 45.8 | 10.4 | No abnormality | Non-leaking bottom material |
| Comparative example 4 | 53.2 | 11.2 | Falling off | Floor drain material |
As can be seen from Table 1, the environmental-friendly fireproof coating disclosed by the embodiment of the invention has better fire resistance, water resistance and scrubbing resistance, and has greater adhesion with a substrate, which is a result of the synergistic effect of the components.
The above-mentioned embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (9)
1. The environment-friendly fireproof coating is characterized by comprising the following components in parts by weight: 40-60 parts of 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate, 5-7 parts of sulfonated polybenzimidazole, 6-8 parts of bisphenol A epoxy resin, 3-5 parts of boron phosphate hollow sphere foam, 1-2 parts of phosphorus pentoxide, 20-30 parts of filler, 1-3 parts of defoaming agent and 0.5-2.5 parts of dispersing agent;
the preparation method of the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate comprises the following steps: adding 2, 5-furandicarboxylic acid, 2, 6-diaminopurine and a catalyst into a high boiling point solvent to form a solution, transferring the obtained solution into a high-pressure reaction kettle, replacing air in the kettle with inert gas, keeping the temperature in the high-pressure reaction kettle at 230-250 ℃ and the pressure at 1.0-2.0MPa, stirring for reaction for 3-5h, slowly exhausting gas within 1-2 h and reducing the pressure to 0.7-1.2MPa, simultaneously heating the temperature in the high-pressure reaction kettle to 265-280 ℃, stirring for reaction for 0.5-1 h, finally controlling the temperature to be 220-235 ℃ under vacuum conditions, stirring for reaction for 8-12h, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 3-6 times by using ethanol, finally taking out, blowing and drying at 80-90 ℃ in a drying box to constant weight to obtain the 2, 5-furandicarboxylic acid/2, 6-diaminopurine polycondensate.
2. The environment-friendly fireproof paint of claim 1, wherein the dispersant is sodium hexametaphosphate and/or sodium polycarboxylate.
3. The environment-friendly fireproof coating of claim 1, wherein the antifoaming agent is one or more of tributyl phosphate, antifoaming agent hume 3100, and antifoaming agent BYK 088.
4. The environment-friendly fireproof paint according to claim 1, wherein the filler is selected from attapulgite, sepiolite powder, calcium carbonate, titanium dioxide or a mixture of two or more of the above.
5. The environment-friendly fireproof coating of claim 1, wherein the filler has a particle size of 800-1000 mesh.
6. The environment-friendly fireproof paint according to claim 1, wherein the bisphenol A epoxy resin is selected from bisphenol A epoxy resin E-12, bisphenol A epoxy resin E-06, bisphenol A epoxy resin E-03 or a mixture of two or more thereof at any ratio.
7. The environment-friendly fireproof coating of claim 1, wherein the molar ratio of the 2, 5-furandicarboxylic acid to the 2, 6-diaminopurine to the catalyst to the high-boiling solvent is 1 (0.5-0.8) to (6-10).
8. The environment-friendly fireproof coating of claim 1, wherein the catalyst is at least one of thiophosphonate, phosphorous acid, thiophosphoramide; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide; the inert gas is one of nitrogen, helium, neon and argon.
9. A method for preparing the environment-friendly fireproof coating according to any one of claims 1 to 8, wherein the method comprises the following steps: the components are uniformly mixed according to the parts by weight to obtain a mixture, then the mixture is added into a double-screw extruder to be extruded, after cooling, crushing and cyclone separation, a product is separated by using a powder sieve, the powder sieve is 50-100 meshes, and the product is cured for 3-5 days to obtain a finished product of the environment-friendly fireproof coating.
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| CN1557860A (en) * | 2004-01-19 | 2004-12-29 | 上海交通大学 | Sulphonated polybenzimidazole and process for preparing the same |
| CN106497300A (en) * | 2016-10-17 | 2017-03-15 | 铜陵市肆得科技有限责任公司 | A kind of automobile leaf spring anti-flaming dope and preparation method thereof |
| CN110577227A (en) * | 2019-10-18 | 2019-12-17 | 福州大学 | Preparation method of boron phosphate hollow sphere foam |
| CN110746885A (en) * | 2019-11-27 | 2020-02-04 | 湖南辰砾新材料有限公司 | Sound-insulation weather-resistant waterproof coating and preparation method thereof |
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| CN1557860A (en) * | 2004-01-19 | 2004-12-29 | 上海交通大学 | Sulphonated polybenzimidazole and process for preparing the same |
| CN106497300A (en) * | 2016-10-17 | 2017-03-15 | 铜陵市肆得科技有限责任公司 | A kind of automobile leaf spring anti-flaming dope and preparation method thereof |
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