CN112680104A - Environment-friendly steel structure fireproof coating and preparation method thereof - Google Patents
Environment-friendly steel structure fireproof coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an environment-friendly steel structure fireproof coating which is characterized by being prepared from the following components in parts by weight: based on 20-30 parts of oxadiazolyl ionic film-forming polymer, 10-15 parts of carboxyl-terminated hyperbranched polyester, 8-10 parts of sulfonated phenoxycyclophosphazene, 3-5 parts of polyaryl oxadiazole fiber powder, 8-12 parts of white cement, 3-5 parts of attapulgite, 2-4 parts of phosphorus pentoxide, 1-2 parts of defoaming agent, 1-3 parts of flatting agent and 0.5-1.5 parts of dispersing agent. The invention also discloses a preparation method of the environment-friendly steel structure fireproof coating. The environment-friendly steel structure fireproof coating disclosed by the invention has the advantages of obvious flame-retardant and fireproof effects, good weather resistance and environment-friendly performance, strong adhesive force with a steel substrate and good humidity resistance.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to an environment-friendly steel structure fireproof coating and a preparation method thereof.
Background
In recent years, with rapid development of economy and society, building materials are continuously upgraded and updated. Various large buildings come along, and the main bearing components of the large buildings mostly depend on firm and light steel structures, and the steel structures endow the buildings with wide, light, concise and smooth styles without losing firmness, and are the main forms of the future large buildings. As a building type, the steel structure is widely adopted due to the advantages of light dead weight, high strength, good plasticity, short construction period, high flexibility and earthquake resistance level, energy conservation, environmental protection and the like, and particularly plays an irreplaceable role in large-span structures and high-rise buildings. However, the fire resistance of the steel structure is poor, the steel structure loses almost all the strength when the temperature reaches 600 ℃, and once a fire breaks out, the steel structure loses the bearing capacity, which seriously endangers the life and property safety of people. Therefore, fire protection of the steel structure is necessary.
The method for protecting the steel structure, which is widely used at present, is to coat the steel structure surface with steel structure fireproof paint. The fireproof paint for steel structure is one kind of special paint for reducing the surface flammability of steel structure, retarding the fire spreading and raising the fire resistance of steel structure. However, the existing steel structure fireproof coating only focuses on the fireproof performance index, and the environmental protection performance, the weather resistance and the like are insufficient. The fireproof coating for the steel structure on the market also has the defects of poor flame retardance, poor fire resistance, poor moisture resistance and poor weather resistance, the coating is easy to crack, remove powder and the like, the adhesion force with a steel substrate is poor, and the smoke safety problem exists.
Patent document CN1986715A discloses a tunnel steel structure fireproof paint, which is composed of acrylic emulsion, 582 resin, AEC expanded cement, refractory cement as binder, sepiolite, expanded perlite, fly ash, light calcium carbonate, and aluminum silicate fiber as inorganic heat insulation filler, vermiculite, ammonium dichromate, melamine, pentaerythritol, and ammonium polyphosphate as foaming material, and alumina, magnesium hydroxide, tin oxide, and ammonium borate as auxiliary agent.
Therefore, the environment-friendly steel structure fireproof coating which has the advantages of obvious flame-retardant fireproof effect, good weather resistance and environmental protection performance, strong adhesive force with a steel substrate and good humidity resistance is developed, meets the market demand, and has higher market value and popularization and application prospects.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the environment-friendly steel structure fireproof coating which has obvious flame-retardant fireproof effect, good weather resistance and environmental protection performance, strong adhesive force with a steel substrate and good humidity and heat resistance; meanwhile, the invention also provides a preparation method of the environment-friendly steel structure fireproof coating, and the preparation method is simple in process, convenient to construct, high in preparation efficiency and suitable for continuous large-scale production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 20-30 parts of oxadiazolyl ionic film-forming polymer, 10-15 parts of carboxyl-terminated hyperbranched polyester, 8-10 parts of sulfonated phenoxycyclophosphazene, 3-5 parts of polyaryl oxadiazole fiber powder, 8-12 parts of white cement, 3-5 parts of attapulgite, 2-4 parts of phosphorus pentoxide, 1-2 parts of defoaming agent, 1-3 parts of flatting agent and 0.5-1.5 parts of dispersing agent.
Preferably, the dispersant is sodium hexametaphosphate and/or sodium polycarboxylate.
Preferably, the antifoaming agent is one or more of tributyl phosphate, antifoaming agent dele 3100 and antifoaming agent BYK 088.
Preferably, the leveling agent is one or more of a polyacrylate leveling agent, a cellulose acetate butyrate leveling agent and a polyvinyl butyral leveling agent.
Preferably, the white cement is selected from the group consisting of those having the trade marks
White calcium aluminate cement of White, White portland cement of 625, White portland cement of 525.
Preferably, the particle size of the attapulgite is 1000-1200 meshes.
Preferably, the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter is 1-4 μm, and the length-diameter ratio is 25-45.
Preferably, the preparation method of the sulfonated phenoxyl cyclophosphazene comprises the following steps: 50% fuming sulfuric acid and phenoxy cyclophosphazene are placed into a three-necked bottle, a mechanical stirring device, a thermometer and a spherical condenser tube are arranged in the three-necked bottle, the three-necked bottle is heated to 110-120 ℃ under the stirring state, the temperature is reduced to 35-45 ℃ after the reaction for 6-8h, the reaction mixture is slowly poured into ice water, the ice water is neutralized to be neutral by sodium hydroxide solution, sodium chloride is added for salting out, a solid crude product is obtained, and then ethanol and water are used for recrystallization, so that the sulfonated phenoxy cyclophosphazene is obtained.
Preferably, the ratio of the fuming sulfuric acid to the phenoxyl cyclophosphazene is 40mL (1-3 g).
Preferably, the carboxyl-terminated hyperbranched polyester is selected from one or more of HyPer C10, HyPer C20, HyPer C30 or HyPer C40.
Preferably, the preparation method of the ionic film-forming polymer based on the oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 5-8 hours at 40-60 ℃, then performing rotary evaporation to remove the solvent, washing the product with diethyl ether for 3-6 times, performing rotary evaporation to remove residual diethyl ether, and finally placing the product in a vacuum drying oven at 85-95 ℃ for drying to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group.
Preferably, the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1 (6-10).
Preferably, the organic solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
The invention also aims to provide a preparation method of the environment-friendly steel structure 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 then products are separated by powder screening after cooling, crushing and cyclone separation in sequence, wherein the powder screening is 100 meshes and 200 meshes, and the products are cured for 1-3 days to obtain the environment-friendly steel structure fireproof coating.
Preferably, the extrusion temperature is 120-150 ℃.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly steel structure fireproof coating provided by the invention is simple in process, convenient to construct, high in preparation efficiency and suitable for continuous large-scale production.
(2) The environment-friendly steel structure fireproof coating provided by the invention overcomes the defects that the existing steel structure fireproof coating only focuses on fireproof performance indexes, and the environment-friendly performance, weather resistance and the like are insufficient; the fireproof coating for the steel structure on the market also has the defects of poor flame retardance, poor fire resistance, poor moisture resistance and poor weather resistance, the coating is easy to crack, remove powder and the like, the adhesion force with a steel substrate is poor, and the smoke safety problem exists; through the synergistic effect of the components, the prepared environment-friendly steel structure fireproof coating has the advantages of obvious flame-retardant and fireproof effects, good weather resistance and environmental protection performance, strong adhesive force with a steel substrate and good humidity and heat resistance.
(3) According to the environment-friendly steel structure fireproof coating provided by the invention, the ionic film-forming polymer based on the oxadiazole silane group is added, and the oxadiazole and silane structures are introduced into the main molecular chain and have synergistic effects, so that the prepared polymer has good film-forming property and good comprehensive performance and performance stability; the ionic structure introduced into the molecular chain can enhance the binding force between the ionic structure and steel, and provides reaction sites for subsequent crosslinking and curing, and meanwhile, the film forming materials of the structures have better flame-retardant and fireproof performances. The oxadiazole structure and the polyaryl oxadiazole fiber powder have similar structures, and compatibility between the oxadiazole structure and the polyaryl oxadiazole fiber powder is enhanced.
(4) According to the environment-friendly fireproof coating for the steel structure, the sulfonated phenoxy cyclophosphazene is added as a flame retardant component, and the synergistic effect is combined with the advantages of phosphorus-based, nitrogen-based and sulfonic organic flame retardants, so that the flame retardant and fireproof effects are better; the substance is not directly added like the traditional fireproof material, but is connected with quaternary ammonium salt cations in the film forming polymer through sulfonic groups in the molecular structure through ionic bonds, and meanwhile, the sulfonic groups can also perform cross-linking curing reaction with benzene rings on the molecular chain of the ionic film forming polymer based on the oxadiazolyl group and benzene rings on the polyaryl oxadiazole fiber powder under the catalytic action of phosphorus pentoxide, so that the cured coating has better comprehensive performance, better humidity and heat resistance, and more remarkable weather resistance, aging resistance, fireproof flame retardance and performance stability. Meanwhile, the carboxyl-terminated hyperbranched polyester can promote film formation, the carboxyl-terminated hyperbranched polyester can be connected with cations on the oxadiazole silyl-based ionic film-forming polymer through ionic bonds, free ions are reduced, and a coating film is formed on the surface of steel through a bridging effect, so that an anti-corrosion effect is achieved.
(5) According to the environment-friendly steel structure fireproof coating provided by the invention, the addition of the polyaryloxadiazole fiber powder can improve the mechanical property and the temperature resistance of a coating film, and can also improve the comprehensive performance of the coating film, and the white cement and the attapulgite are added in a matching manner, so that the adhesion performance of the coating and a base material can be enhanced. The coating takes air as a dispersion medium, does not contain volatile organic solvent, and is relatively environment-friendly.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
Example 1
An environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 20 parts of oxadiazolyl ionic film-forming polymer, 10 parts of carboxyl-terminated hyperbranched polyester, 8 parts of sulfonated phenoxy cyclophosphazene, 3 parts of polyaryl oxadiazole fiber powder, 8 parts of white cement, 3 parts of attapulgite, 2 parts of phosphorus pentoxide, 1 part of defoaming agent, 1 part of flatting agent and 0.5 part of dispersing agent; the dispersant is sodium hexametaphosphate; the defoaming agent is tributyl phosphate; the flatting agent is a polyacrylate flatting agent; the white cement is of the brand number
White calcium aluminate cement from White.
The particle size of the attapulgite is 1000 meshes; the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter is 1 μm, the length-diameter ratio is 25; the carboxyl-terminated hyperbranched polyester is HyPer C10.
The preparation method of the sulfonated phenoxyl cyclophosphazene comprises the following steps: putting 50% fuming sulfuric acid and phenoxyl cyclophosphazene into a three-necked bottle, wherein a mechanical stirring device, a thermometer and a spherical condenser pipe are arranged in the three-necked bottle, heating to 110 ℃ under the stirring state, reacting for 6 hours, cooling to 35 ℃, slowly pouring a reaction mixture into ice water, neutralizing to be neutral by using a sodium hydroxide solution, adding sodium chloride for salting out to obtain a solid crude product, and then recrystallizing by using ethanol and water to obtain the sulfonated phenoxyl cyclophosphazene; the ratio of the fuming sulfuric acid to the phenoxyl cyclophosphazene is 40mL:1 g.
The preparation method of the ionic film-forming polymer based on the oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 5 hours at 40 ℃, then performing rotary evaporation to remove the solvent, washing the product for 3 times by using diethyl ether, performing rotary evaporation to remove residual diethyl ether, and finally drying the product in a vacuum drying oven at 85 ℃ to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group; the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1: 6; the organic solvent is dimethyl sulfoxide.
The preparation method of the environment-friendly steel structure fireproof coating is characterized by comprising the following steps of: uniformly mixing the components in parts by weight to obtain a mixture, adding the mixture into a double-screw extruder for extrusion, sequentially cooling, crushing and performing cyclone separation, screening the product by using a powder screen, wherein the powder screen is 100 meshes, and curing for 1 day to obtain the environment-friendly steel structure fireproof coating; the extrusion temperature was 120 ℃.
Example 2
An environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 23 parts of oxadiazolyl ionic film-forming polymer, 11 parts of carboxyl-terminated hyperbranched polyester, 8.5 parts of sulfonated phenoxy cyclophosphazene, 3.5 parts of polyaryl oxadiazole fiber powder, 9 parts of white cement, 3.5 parts of attapulgite, 2.5 parts of phosphorus pentoxide, 1.2 parts of defoaming agent, 1.3 parts of flatting agent and 0.7 part of dispersing agent; the dispersant is sodium polycarboxylate; the antifoaming agent is antifoaming agent delete 3100; the leveling agent is cellulose acetate butyrate leveling agent; the white cement is white portland cement with the reference number of 625; the particle size of the attapulgite is 1050 meshes; the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter is 2 mu m, and the length-diameter ratio is 30; the carboxyl-terminated hyperbranched polyester is HyPer C20.
The preparation method of the sulfonated phenoxyl cyclophosphazene comprises the following steps: putting 50% fuming sulfuric acid and phenoxy cyclophosphazene into a three-necked bottle, wherein a mechanical stirring device, a thermometer and a spherical condenser pipe are arranged in the three-necked bottle, heating to 113 ℃ under the stirring state, reacting for 6.5 hours, cooling to 37 ℃, slowly pouring the reaction mixture into ice water, neutralizing to be neutral by using a sodium hydroxide solution, adding sodium chloride for salting out to obtain a solid crude product, and recrystallizing by using ethanol and water to obtain the sulfonated phenoxy cyclophosphazene; the ratio of the fuming sulfuric acid to the phenoxyl cyclophosphazene is 40mL to 1.5 g.
The preparation method of the ionic film-forming polymer based on the oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 6 hours at 45 ℃, then performing rotary evaporation to remove the solvent, washing the product for 3-6 times by using diethyl ether, performing rotary evaporation to remove residual diethyl ether, and finally drying at 88 ℃ in a vacuum drying oven to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group; the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1: 7; the organic solvent is N, N-dimethylformamide.
The preparation method of the environment-friendly steel structure fireproof coating is characterized by comprising the following steps of: uniformly mixing the components in parts by weight to obtain a mixture, adding the mixture into a double-screw extruder for extrusion, sequentially cooling, crushing and performing cyclone separation, screening the product by using a powder screen, wherein the powder screen is 130 meshes, and curing for 1.5 days to obtain the environment-friendly steel structure fireproof coating; the extrusion temperature was 130 ℃.
Example 3
An environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 25 parts of oxadiazolyl ionic film-forming polymer, 13 parts of carboxyl-terminated hyperbranched polyester, 9 parts of sulfonated phenoxy cyclophosphazene, 4 parts of polyaryl oxadiazole fiber powder, 10 parts of white cement, 4 parts of attapulgite, 3 parts of phosphorus pentoxide, 1.5 parts of defoaming agent, 2 parts of flatting agent and 1 part of dispersing agent; the dispersant is sodium hexametaphosphate; the defoaming agent is a defoaming agent BYK 088; the flatting agent is a polyvinyl butyral flatting agent; the white cement is white portland cement with the reference number of 525; the particle size of the attapulgite is 1100 meshes; the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter was 2.5 μm and the aspect ratio was 35.
The preparation method of the sulfonated phenoxyl cyclophosphazene comprises the following steps: putting 50% fuming sulfuric acid and phenoxyl cyclophosphazene into a three-necked bottle, wherein a mechanical stirring device, a thermometer and a spherical condenser pipe are arranged in the three-necked bottle, heating to 115 ℃ under the stirring state, reacting for 7 hours, cooling to 40 ℃, slowly pouring a reaction mixture into ice water, neutralizing to be neutral by using a sodium hydroxide solution, adding sodium chloride for salting out to obtain a solid crude product, and then recrystallizing by using ethanol and water to obtain the sulfonated phenoxyl cyclophosphazene; the ratio of the fuming sulfuric acid to the phenoxyl cyclophosphazene is 40mL:2 g; the carboxyl-terminated hyperbranched polyester is HyPer C30.
The preparation method of the ionic film-forming polymer based on the oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 6.5 hours at 50 ℃, then performing rotary evaporation to remove the solvent, washing the product for 5 times by using diethyl ether, performing rotary evaporation to remove residual diethyl ether, and finally drying the product in a vacuum drying oven at 90 ℃ to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group; the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1: 8; the organic solvent is N-methyl pyrrolidone.
The preparation method of the environment-friendly steel structure fireproof coating is characterized by comprising the following steps of: uniformly mixing the components in parts by weight to obtain a mixture, adding the mixture into a double-screw extruder for extrusion, sequentially cooling, crushing and performing cyclone separation, screening the product by using a powder screen, wherein the powder screen is 150 meshes, and curing for 2 days to obtain the environment-friendly steel structure fireproof coating; the extrusion temperature was 135 ℃.
Example 4
An environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 28 parts of oxadiazolyl ionic film-forming polymer, 14 parts of carboxyl-terminated hyperbranched polyester, 9.5 parts of sulfonated phenoxy cyclophosphazene, 4.5 parts of polyaryl oxadiazole fiber powder, 11 parts of white cement, 4.5 parts of attapulgite, 3.5 parts of phosphorus pentoxide, 1.9 parts of defoaming agent, 2.8 parts of flatting agent and 1.3 parts of dispersing agent; the dispersing agent is formed by mixing sodium hexametaphosphate and sodium polycarboxylate according to the mass ratio of 3: 5; the defoaming agent is formed by mixing tributyl phosphate, a defoaming agent Demodex 3100 and a defoaming agent BYK088 according to the mass ratio of 2:1: 3; the flatting agent is formed by mixing a polyacrylate flatting agent, a cellulose acetate butyrate flatting agent and a polyvinyl butyral flatting agent according to a mass ratio of 2:2: 3; the white cement is of the brand number
White calcium aluminate cement of White, White Portland cement with the reference numeral 625 and White Portland cement with the reference numeral 525 are mixed according to the mass ratio of 3:5: 1.
The particle size of the attapulgite is 1150 meshes; the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter was 3.5 μm and the aspect ratio was 42. The carboxyl-terminated hyperbranched polyester is prepared by mixing HyPer C10, HyPer C20, HyPer C30 and HyPer C40 in a mass ratio of 1:1:2: 3.
The preparation method of the sulfonated phenoxyl cyclophosphazene comprises the following steps: putting 50% fuming sulfuric acid and phenoxy cyclophosphazene into a three-necked bottle, wherein a mechanical stirring device, a thermometer and a spherical condenser pipe are arranged in the three-necked bottle, heating to 118 ℃ under the stirring state, reacting for 7.8h, cooling to 43 ℃, slowly pouring the reaction mixture into ice water, neutralizing to neutrality by using a sodium hydroxide solution, adding sodium chloride for salting out to obtain a solid crude product, and recrystallizing by using ethanol and water to obtain the sulfonated phenoxy cyclophosphazene; the ratio of the fuming sulfuric acid to the phenoxyl cyclophosphazene is 40mL to 2.7 g.
The preparation method of the ionic film-forming polymer based on the oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 7.5 hours at 58 ℃, then performing rotary evaporation to remove the solvent, washing the product for 3-6 times by using diethyl ether, performing rotary evaporation to remove residual diethyl ether, and finally drying at 93 ℃ in a vacuum drying oven to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group; the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1: 9.5; the organic solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone according to the mass ratio of 1:3: 5.
The preparation method of the environment-friendly steel structure fireproof coating is characterized by comprising the following steps of: uniformly mixing the components in parts by weight to obtain a mixture, adding the mixture into a double-screw extruder for extrusion, sequentially cooling, crushing and performing cyclone separation, screening the product by using a powder screen, wherein the powder screen is 180 meshes, and curing for 2.8 days to obtain the environment-friendly steel structure fireproof coating; the extrusion temperature was 145 ℃.
Example 5
An environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 30 parts of oxadiazolyl ionic film-forming polymer, 15 parts of carboxyl-terminated hyperbranched polyester, 10 parts of sulfonated phenoxy cyclophosphazene, 5 parts of polyaryl oxadiazole fiber powder, 12 parts of white cement, 5 parts of attapulgite, 4 parts of phosphorus pentoxide, 2 parts of defoaming agent, 3 parts of flatting agent and 1.5 parts of dispersing agent; the dispersant is sodium hexametaphosphate; the defoaming agent is a defoaming agent BYK 088; the flatting agent is a polyacrylate flatting agent; the white cement is white portland cement with the reference number of 525; the particle size of the attapulgite is 1200 meshes; the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter was 4 μm and the aspect ratio was 45. The carboxyl-terminated hyperbranched polyester is HyPer C40.
The preparation method of the sulfonated phenoxyl cyclophosphazene comprises the following steps: putting 50% fuming sulfuric acid and phenoxyl cyclophosphazene into a three-necked bottle, wherein a mechanical stirring device, a thermometer and a spherical condenser pipe are arranged in the three-necked bottle, heating to 120 ℃ under the stirring state, reacting for 8 hours, cooling to 45 ℃, slowly pouring a reaction mixture into ice water, neutralizing to be neutral by using a sodium hydroxide solution, adding sodium chloride for salting out to obtain a solid crude product, and then recrystallizing by using ethanol and water to obtain the sulfonated phenoxyl cyclophosphazene; the ratio of the fuming sulfuric acid to the phenoxyl cyclophosphazene is 40mL:3 g.
The preparation method of the ionic film-forming polymer based on the oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 8 hours at 60 ℃, then performing rotary evaporation to remove the solvent, washing the product for 6 times by using diethyl ether, performing rotary evaporation to remove residual diethyl ether, and finally drying the product in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group; the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1: 10; the organic solvent is dimethyl sulfoxide.
The preparation method of the environment-friendly steel structure fireproof coating is characterized by comprising the following steps of: uniformly mixing the components in parts by weight to obtain a mixture, adding the mixture into a double-screw extruder for extrusion, sequentially cooling, crushing and performing cyclone separation, screening the product by using a powder screen, wherein the powder screen is 200 meshes, and curing for 3 days to obtain the environment-friendly steel structure fireproof coating; the extrusion temperature was 150 ℃.
Comparative example 1
This example provides an environmentally friendly fire-retardant coating for steel structures, which is formulated and prepared substantially the same as in example 1, except that no ionic film-forming polymer based on oxadiazolyl groups is added.
Comparative example 2
The present example provides an environment-friendly fire-retardant coating for steel structures, which has a formulation and a preparation method substantially the same as those of example 1, except that no carboxyl-terminated hyperbranched polyester is added.
Comparative example 3
The present example provides an environmental protection fire retardant coating for steel structure, the formulation and preparation method is basically the same as example 1, except that sulfonated phenoxy cyclophosphazene is used to replace phenoxy cyclophosphazene.
Comparative example 4
This example provides an environmentally friendly fire retardant coating for steel structures, which is formulated and prepared in substantially the same manner as in example 1, except that no polyaryl oxadiazole fiber powder is added.
The environmental-friendly steel structure fireproof coatings obtained in the examples 1-5 and the comparative examples 1-4 are subjected to related performance tests, the test results are shown in the table 1, and the test methods are shown in GB 14907-2002.
TABLE 1 fire-retardant coating performance for environment-friendly steel structure of examples and comparative examples
As can be seen from Table 1, the environmental-friendly steel structure fireproof coating disclosed by the embodiment of the invention has better fire resistance, damp-heat resistance and salt-mist corrosion resistance than the comparative product, and has higher bonding strength and compressive strength, which are the result of the synergistic effect of the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An environment-friendly steel structure fireproof coating is characterized by being prepared from the following components in parts by weight: based on 20-30 parts of oxadiazolyl ionic film-forming polymer, 10-15 parts of carboxyl-terminated hyperbranched polyester, 8-10 parts of sulfonated phenoxycyclophosphazene, 3-5 parts of polyaryl oxadiazole fiber powder, 8-12 parts of white cement, 3-5 parts of attapulgite, 2-4 parts of phosphorus pentoxide, 1-2 parts of defoaming agent, 1-3 parts of flatting agent and 0.5-1.5 parts of dispersing agent.
2. The environment-friendly steel structure fireproof paint of claim 1, wherein the dispersant is sodium hexametaphosphate and/or sodium polycarboxylate; the antifoaming agent is one or more of tributyl phosphate, antifoaming agent Demodex 3100 and antifoaming agent BYK 088.
3. The environment-friendly steel structure fireproof paint as claimed in claim 1, wherein the leveling agent is one or more of polyacrylate leveling agent, cellulose acetate butyrate leveling agent and polyvinyl butyral leveling agent.
4. The environment-friendly fireproof coating for steel structures, as claimed in claim 1, wherein the white cement is selected from the group consisting of cement of the brand number
White calcium aluminate cement of White, White Portland cement of 625, at least one kind of White Portland cement of 525 of the reference number; the carboxyl-terminated hyperbranched polyester is selected from one or more of HyPer C10, HyPer C20, HyPer C30 or HyPer C40.
5. The environment-friendly steel structure fireproof coating as claimed in claim 1, wherein the particle size of the attapulgite is 1000-1200 mesh; the polyaryloxadiazole fiber powder is polyester staple fiber powder; the average diameter is 1-4 μm, and the length-diameter ratio is 25-45.
6. The environment-friendly fireproof coating for steel structures, as claimed in claim 1, wherein the preparation method of the sulfonated phenoxy cyclophosphazene comprises the following steps: 50% fuming sulfuric acid and phenoxy cyclophosphazene are placed into a three-necked bottle, a mechanical stirring device, a thermometer and a spherical condenser tube are arranged in the three-necked bottle, the three-necked bottle is heated to 110-120 ℃ under the stirring state, the temperature is reduced to 35-45 ℃ after the reaction for 6-8h, the reaction mixture is slowly poured into ice water, the ice water is neutralized to be neutral by sodium hydroxide solution, sodium chloride is added for salting out, a solid crude product is obtained, and then ethanol and water are used for recrystallization, so that the sulfonated phenoxy cyclophosphazene is obtained.
7. The environment-friendly steel structure fireproof coating of claim 6, wherein the ratio of fuming sulfuric acid to phenoxy cyclophosphazene is 40mL (1-3) g.
8. The environment-friendly fireproof coating for steel structures, according to claim 1, wherein the preparation method of the ionic film-forming polymer based on oxadiazolyl group comprises the following steps: adding 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole and bis-dichloromethyl dimethylsilane into an organic solvent, stirring and reacting for 5-8 hours at 40-60 ℃, then performing rotary evaporation to remove the solvent, washing the product with diethyl ether for 3-6 times, performing rotary evaporation to remove residual diethyl ether, and finally placing the product in a vacuum drying oven at 85-95 ℃ for drying to constant weight to obtain the ionic film-forming polymer based on the oxadiazolyl group.
9. The environment-friendly steel structure fireproof paint of claim 8, wherein the molar ratio of the 2, 5-bis (diethylamino) phenyl-1, 3, 4-diazole to the bis-dichloromethyl dimethylsilane to the organic solvent is 1:1 (6-10); the organic solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
10. The preparation method of the environment-friendly fireproof coating for the steel structure according to any one of claims 1 to 9, which is characterized by comprising the following steps: uniformly mixing the components in parts by weight to obtain a mixture, adding the mixture into a double-screw extruder for extrusion, sequentially cooling, crushing and performing cyclone separation, screening the product by using a powder screen, wherein the powder screen is 100 meshes and 200 meshes, and curing for 1-3 days to obtain the environment-friendly steel structure fireproof coating; the extrusion temperature is 120-150 ℃.
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