CN118165580A - Bio-based intumescent water-based flame retardant coating with strong adhesion performance and preparation method thereof - Google Patents
Bio-based intumescent water-based flame retardant coating with strong adhesion performance and preparation method thereof Download PDFInfo
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- CN118165580A CN118165580A CN202410221974.6A CN202410221974A CN118165580A CN 118165580 A CN118165580 A CN 118165580A CN 202410221974 A CN202410221974 A CN 202410221974A CN 118165580 A CN118165580 A CN 118165580A
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Abstract
The invention discloses a bio-based intumescent water-based flame retardant coating with strong adhesive property and a preparation method thereof, wherein the coating is prepared from the following raw materials in parts by weight: 100-300 parts of deionized water, 10-40 parts of gluconate, 10-30 parts of chitosan salt, 40-45 parts of phytic acid, 1-2 parts of an anti-aging agent and 0.3-0.4 part of an anti-freeze thawing auxiliary agent. The flame-retardant coating is suitable for various base materials, and solves the problem of short service life of the coating due to weak binding force between the coating and a matrix; the flame retardant coating has high flame retardant efficiency, the thickness of the coating is about 200 mu m, the polypropylene can be effectively flame-retarded by vertical combustion through UL-94V-0 level, the Limiting Oxygen Index (LOI) is 46.1%, the coating rapidly expands about 100 times after meeting fire, the inside of the carbon layer is honeycomb-shaped, the surface of the carbon layer is continuous and compact, and the condensed phase flame retardant effect is obvious; the preparation method of the coating is simple, the coating is highly transparent and smooth, and the coating has the advantages of convenient processing, energy conservation, emission reduction, wide application and the like.
Description
Technical Field
The invention relates to a transparent bio-based intumescent water-based flame retardant coating with strong adhesive property and a preparation method thereof, and application of the flame retardant coating on the surfaces of base materials such as plastics, wood, rigid polyurethane foam, wallpaper and the like, belonging to the technical field of preparation of environment-friendly water-based intumescent flame retardant coatings.
Background
Many combustible and flammable materials release a great deal of heat during the combustion process and produce dense smoke and toxic and harmful gases, and the fire caused by these materials poses serious threats to the safety of human lives and property every year. While conventional flame retardant technology has achieved some success, with increasing demands for flame retardant performance, such as high flame retardant efficiency, flame retardant durability, low heat release, low smoke, low toxic and harmful gas emissions, etc., flame retardant applications have met with increasing challenges because of the increased flame retardant performance affecting or even deteriorating the inherent properties of flammable materials.
The flame-retardant coating is a functional material, and generally a flame retardant is added into a film forming agent which does not have flame retardant property to realize flame retardant or fireproof functions, and is widely used for wood flame retardance and steel plate fireproof. The flame-retardant coating is simple in construction, can adopt various construction modes of roller coating, dip coating, brush coating and spray coating, can play a role in decorating and protecting a base material, and simultaneously reduces the influence of flame on the base material. The water-based paint is novel environment-friendly paint because the water-based paint does not contain an organic solvent, and the film forming agent is mainly water-based organic resin (water-based polyurethane, water-based acrylic ester, water-based epoxy resin and the like), and the water-based flame-retardant paint can be prepared after the flame retardant is added into the water-based organic resin. In recent years, bio-based materials have been attracting attention because of the advantages of green, environmental protection and reproducibility, so bio-based coatings become key to carbon reduction and emission reduction in the coating industry.
Chinese patent CN112662235A discloses a water-based bio-based flame-retardant luminous paint, a preparation method and application thereof, and the water-based bio-based flame-retardant luminous paint prepared by the method is applied to preparing flame-retardant wood, and the paint is directly brushed on the surface of the wood and dried for more than 12 hours at room temperature. However, the binding force between the coating and the matrix is not detailed, the coating has no light transmittance, and the coating is milky white under natural light after being dried and emits light in the dark, so that the coating is not suitable for certain materials which need to keep the characteristics of the coating. Chinese patent CN112175435A discloses a "flame-retardant antibacterial coating for aluminum alloy doors and windows and a preparation method thereof", the flame-retardant antibacterial coating prepared by the method is sprayed on the surface of the aluminum alloy doors and windows for 2-3 layers, and after the flame-retardant antibacterial coating is cured and formed on the surface of the aluminum alloy doors and windows, the flame-retardant antibacterial coating is formed; however, the flame-retardant antibacterial coating has various materials and complicated preparation steps. Chinese patent CN116239931A discloses a preparation method of a water-based epoxy intumescent fire-retardant coating with a phytic acid complexing copper ion h-BN base, wherein Melamine (MEL), pentaerythritol (PER) and ammonium polyphosphate (APP) are used in the preparation process of the coating, and the application of non-renewable resources is not eliminated; and the preparation steps of the coating are complicated, the coating is cured for 7 days at normal temperature after brushing, and is baked for 3 days at 40 ℃, so that the curing time is long, and the curing condition is harsh. Chinese patent CN202211697762.2 discloses a method for preparing bio-based intumescent flame retardant for interior wall coating, and the obtained bio-based intumescent flame retardant needs to be added with film forming agent for use.
The flame retardant coating is an additive flame retardant coating, the addition of the flame retardant can damage the continuity of a film forming phase, so that the adhesive force and mechanical property of the coating are reduced, the stability and long-acting property of the flame retardant coating are directly influenced, and the firmness of a carbon layer formed in flame is also influenced, so that the high adhesive force is one of the necessary performances of the flame retardant coating. In addition, additive-type flame retardant coatings are generally opaque, limiting their field of application. Therefore, the bio-based water-based flame-retardant coating which has the performances of flame retardance, strong adhesion, transparency, antibiosis and the like and is suitable for different base materials is developed, has great practical significance and application value, not only meets the environment-friendly concept, but also can widen the application range of the flame-retardant coating.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the bio-based intumescent water-based flame retardant coating with strong adhesion performance and the preparation method thereof, and the obtained coating has the performances of flame retardance, strong adhesion, transparency, antibiosis and the like, is suitable for different base materials, not only meets the environment-friendly concept, but also can widen the application range of the flame retardant coating.
The mechanism of the invention is described as follows: the invention reacts gluconate, phytic acid and chitosan salt at normal temperature to form the functional coating with flame retardance through a sol-gel method. The gluconate and chitosan salt have abundant hydroxyl groups in the structure, and form a chemical crosslinking structure under the strong chelation and dehydration of phytic acid. Meanwhile, the rest hydroxyl and amino form a network structure of physical and chemical crosslinking together due to the action of hydrogen bonds, and the flame-retardant system is a film-forming system at the same time, so that the coating does not need to be added with film-forming substances alone, has the characteristic of intrinsic flame retardance, and compared with the additive flame-retardant coating, the continuous phase of the coating is not damaged, the flame-retardant component is distributed more uniformly, and the flame-retardant efficiency is higher.
The ternary system consisting of gluconate, chitosan and phytic acid contains a large number of hydroxyl groups, and the formed coating has hydrogen bonding effect with active functional groups on the surface of a matrix, so that the coating has strong adhesiveness. In the ternary system, chitosan salt and gluconate can serve as a carbon source and a gas source in the flame-retardant coating, and phytic acid serves as an acid source, so that the intumescent flame-retardant requirement is completely met. Under the action of high temperature or flame, the flame-retardant coating coated on the protected substrate is expanded and carbonized severely to form a non-combustible honeycomb carbon layer which is tens times thicker than the original coating, and the honeycomb structure is filled with non-combustible gas, so that good heat insulation effect is generated, heat is effectively prevented from being transferred to the substrate, and the protected substrate can be kept at a lower temperature for a certain time; secondly, physical changes such as softening, melting, expanding and the like of the coating and chemical actions such as decomposition, crosslinking and carbonization of phytic acid, chitosan salt and gluconate in the coating can absorb a large amount of heat, so that the combustion temperature and flame propagation speed are reduced; third, metal ions can play a role in catalyzing and carbonizing and stabilizing the carbon layer, and further help the flame-retardant coating to obtain excellent flame-retardant performance.
The flame-retardant coating provided by the invention is highly transparent, and the light transmittance is more than 90%, so that the flame-retardant coating has the effects of decoration and attractive appearance, and the application range of the flame-retardant coating is widened. The chitosan salt, the metal ions and the phytic acid have antibacterial property, and the antibacterial property of the flame-retardant coating is endowed. In addition, the flame retardant coating is a water-based coating, the flame retardants are all biomass materials, the source is wide, the preparation method of the coating is simple, and the flame retardant coating is green and energy-saving.
The invention provides a bio-based intumescent water-based flame retardant coating with strong adhesive property, which is prepared from the following raw materials in parts by weight:
100-300 parts of deionized water
Gluconate 10-40 parts
10-30 Parts of chitosan salt
40-45 Parts of phytic acid
1-2 Parts of anti-aging agent
0.3-0.4 Part of freeze thawing resistant additive.
In the above embodiments, the gluconate salt includes, but is not limited to, one of calcium gluconate, sodium gluconate, magnesium gluconate, or a combination thereof (mixed in any ratio when combined).
In the scheme, the chitosan salt comprises one of chitosan quaternary ammonium salt, chitosan hydrochloride, chitosan lactate and chitosan nitrate or a combination thereof (mixed according to any proportion when in various combinations), and the substitution degree is more than or equal to 80 percent.
In the above embodiments, the phytic acid is 50-70wt.% phytic acid solution.
In the above scheme, the anti-aging agent is any one of UV-770, UV-531 and anti-aging agent 1010 to improve the anti-aging capability of the coating.
In the scheme, the freeze-thawing resistant auxiliary agent is a Coriolis environment-friendly scrubbing-resistant freeze-thawing resistant auxiliary agent Genapol 2070 so as to improve the freeze-thawing resistance of the coating.
The invention provides a preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property, which comprises the following steps:
(1) Adding deionized water and gluconate into a beaker, and stirring in a water bath kettle at 50-80 ℃ until the deionized water and the gluconate are completely dissolved;
(2) Cooling the solution to normal temperature, slowly adding chitosan salt, and stirring at the speed of 100-200 rmp at normal temperature for 1-1.5 h to uniformly disperse;
(3) Slowly adding phytic acid solution, and stirring at a speed of 100-200 rmp at normal temperature for 30-60 min;
(4) Adding an anti-aging agent and an anti-freeze thawing auxiliary agent, and stirring at a speed of 100 rmp for 20 min; and uniformly mixing to obtain the bio-based intumescent water-based flame retardant coating with strong adhesive property.
The invention provides application of the bio-based intumescent water-based flame retardant coating with strong adhesive property.
The application range of the bio-based intumescent water-based flame retardant coating with strong adhesive property provided by the invention comprises, but is not limited to, plastic, wood, wallpaper, rigid polyurethane foam, steel and other substrates.
The bio-based intumescent water-based flame retardant coating with strong adhesive property provided by the invention needs to carry out simple pretreatment on the surface of a matrix when being applied to plastics or other matrixes with low surface polarity, and the bio-based intumescent water-based flame retardant coating comprises any one of a flame burning method, a polishing method and an adhesive force treating agent treatment method.
The bio-based intumescent water-based flame retardant coating with strong adhesive property provided by the invention is applicable to the following paint coating modes: knife coating, brush coating, dip coating or roller coating. And (3) drying the coating at 15-35 ℃ for 18-24 hours, and suggesting multiple coating when the thickness of the dried coating exceeds 200 mu m.
When the bio-based intumescent water-based flame retardant coating with strong adhesive property provided by the invention is used as flame retardant coating for steel plate fireproof, any one of acrylic emulsion, organic silicon resin or wood wax oil is required to be coated on the surface of the steel plate in advance as primer, the thickness of the primer is about 50-150 mu m, after the primer is dried, the surface of the steel plate coated with the primer is coated with the flame retardant coating of the invention as finish paint, the thickness of the flame retardant coating is more than or equal to 1500 mu m, and the coating is carried out for 4-6 times.
The bio-based intumescent water-based flame retardant coating with strong adhesion property provided by the invention meets the requirement of an adhesive because of strong adhesion, and can also be used as a flame retardant adhesive for bonding various materials.
The invention has the beneficial effects that:
(1) The flame-retardant coating is suitable for various base materials, even for polyolefin materials with very low surface energy, a coating with firm interface bonding can be obtained by simply treating the surface of the polyolefin material (a flame burning method, a polishing method and an adhesive force treatment), the problem of low service life of the coating due to weak bonding force between the coating and a matrix is solved, and the application range of the coating is enlarged;
(2) The flame retardant coating disclosed by the invention has high flame retardant efficiency, the thickness of the coating is about 200 mu m, the flame retardant polypropylene can be effectively flame-retarded, the vertical combustion passes through UL-94V-0 level, the LOI is 46.1%, the coating rapidly expands by about 100 times after encountering fire, the inside of the carbon layer is honeycomb-shaped, the surface of the carbon layer is continuous and compact, and the condensed phase flame retardant effect is obvious;
(3) The flame-retardant coating disclosed by the invention is simple in preparation method, high in transparency and smoothness, and has the advantages of convenience in processing, energy conservation, emission reduction, wide application and the like;
(4) The flame-retardant coating is a water-based coating, adopts gluconate, chitosan salt and phytic acid as raw materials, belongs to biomass renewable resources, and has the advantages of environmental protection; and has good antibacterial property.
Drawings
FIG. 1 is cone calorimetric data for examples 1 and 2.
FIG. 2 is the back temperature data of the steel and polypropylene plates with flame retardant coating of example 3.
Fig. 3 is light transmittance data for the flame retardant coating of example 3.
FIG. 4 is coating adhesion comparison data for the flame retardant coating of example 3, a commercially available acrylic emulsion, and the flame retardant acrylic coating of comparative example 2.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
Example 1
The preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property comprises the following steps (in parts by weight):
(1) Adding 120 parts of deionized water and 28 parts of calcium gluconate into a beaker, and stirring in a water bath kettle at 60 ℃ until the mixture is completely dissolved;
(2) After the solution is cooled to normal temperature, 12 parts of chitosan quaternary ammonium salt is slowly added, and the solution is stirred at the normal temperature at the speed of 100 rmp for 1.5 h so as to be uniformly dispersed;
(3) Slowly adding 28 parts of 50 wt percent phytic acid solution, and stirring 40 min at the speed of 100 rmp at normal temperature;
(4) 1 part of an anti-aging agent 1010 and 0.3 part of Genapol 2070 were added and stirred at a speed of 100 rmp for 20 min. The bio-based intumescent water-based flame retardant coating with strong adhesive property is obtained after uniform mixing.
Application one: the flame retardant coating of example 1 was applied by knife coating to the surface of polypropylene treated with an adhesion treatment agent, and the coating was dried at 18℃for 20: 20 h to give flame retardant polypropylene having a one-sided thickness of 200 μm after drying out for Limiting Oxygen Index (LOI) and vertical burn test (UL-94).
And (2) application II: coating acrylic emulsion on the surface of a steel plate in a blade coating mode to serve as a primer, wherein the thickness of the primer is 50 mu m, coating the fire-retardant coating of the embodiment 1 on the surface of the steel plate coated with the primer to serve as a finish paint after the primer is dried, and after the coating is dried, coating the steel plate with the single side thickness of 1500 mu m for 5 times, and drying to obtain a fire-retardant steel plate for back temperature testing; the flame-retardant coating of the embodiment 1 is coated on the surface of the polypropylene burnt by flame in a knife coating mode, the coating is dried at 18 ℃ to 20 h, the thickness of one side of the dried coating is 1500 mu m, the coating is divided into 5 times, and the flame-retardant polypropylene obtained after drying is used for back temperature test.
Example 2
The preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property comprises the following steps (in parts by weight):
(1) Adding 140 parts of deionized water and 21 parts of sodium gluconate into a beaker, and stirring in a water bath kettle at 60 ℃ until the deionized water and the 21 parts of sodium gluconate are completely dissolved;
(2) After the solution is cooled to normal temperature, 18 parts of chitosan quaternary ammonium salt is slowly added, and the solution is stirred at the normal temperature at the speed of 100 rmp for 1.5 h so as to be uniformly dispersed;
(3) Slowly adding 26 parts of 50 wt% phytic acid solution, and stirring 40 min at the speed of 100 rmp at normal temperature;
(4) 1.5 parts of UV-770 and 0.3 part of Genapol 2070 are added and stirred at a speed of 100 rmp for 20: 20 min. The bio-based intumescent water-based flame retardant coating with strong adhesive property is obtained after uniform mixing.
Application one: the flame retardant coating of example 2 was applied by brushing to the surface of a polypropylene polished by a surface and the coating was dried at 25℃for 18 h to give a flame retardant polypropylene having a single side coating thickness of 200 μm after the coating was dried out for Limiting Oxygen Index (LOI) and vertical burning test (UL-94).
And (2) application II: coating acrylic emulsion on the surface of a steel plate in a brushing mode to serve as a primer, wherein the thickness is 80 mu m, coating the fire-retardant coating of the embodiment 2 on the surface of the steel plate coated with the primer to serve as a finish paint after the primer is dried, and dividing the coating into 4 times of coating after the coating is dried completely, so that a fireproof steel plate is obtained after the coating is dried and used for back temperature testing; the flame-retardant coating of the embodiment 2 is coated on the surface of the polypropylene burnt by flame in a brushing mode, the coating is dried at 25 ℃ to 18 h, the thickness of one side of the dried coating is 1500 mu m, the coating is divided into 4 times of coating, and the flame-retardant polypropylene obtained after drying is used for back temperature test.
Example 3
The preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property comprises the following steps (in parts by weight):
(1) 160 parts of deionized water and 18 parts of magnesium gluconate are added into a beaker, and the mixture is stirred in a water bath kettle at 70 ℃ until the mixture is completely dissolved;
(2) After the solution is cooled to normal temperature, 20 parts of chitosan lactate is slowly added, and the solution is stirred at the normal temperature at the speed of 200 rmp for 1h so as to be uniformly dispersed;
(3) Slowly adding 20 parts of 70 wt% phytic acid solution, and stirring at a speed of 200 rmp at normal temperature for 30min;
(4) 1.8 parts of UV-770 and 0.3 part of Genapol 2070 are added and stirred at a speed of 100 rmp for 20 min. The bio-based intumescent water-based flame retardant coating with strong adhesive property is obtained after uniform mixing.
Application one: the flame retardant coating of example 3 was applied to the surface of flame-burned polypropylene by knife coating, and the coating was dried at 28℃for 15 h to give flame retardant polypropylene, with a single side thickness of 200 μm after the coating was dried out, for Limiting Oxygen Index (LOI) and vertical burn test (UL-94).
And (2) application II: coating acrylic emulsion on the surface of a steel plate in a blade coating mode to serve as a primer, wherein the thickness is 100 mu m, coating the fire-retardant coating of the embodiment 3 on the surface of the steel plate coated with the primer to serve as a finish paint after the primer is dried, and after the coating is dried, coating the steel plate with the single side thickness of 1500 mu m for 4 times, and drying to obtain a fireproof steel plate for back temperature testing; the flame-retardant coating of the embodiment 3 is coated on the surface of the polypropylene burnt by flame in a knife coating mode, the coating is dried at 28 ℃ for 15 h, the thickness of one side of the dried coating is 1500 mu m, the coating is divided into 4 times of coating, and the flame-retardant polypropylene obtained after drying is used for back temperature test.
And (3) application III: the flame retardant coating of example 3 (coating thickness: about 200 μm) was uniformly applied to both ends of the polyurethane foam, and after leaving at room temperature 6h, the coating surfaces which had not been completely dried were bonded, and after leaving at room temperature 12: 12h, the polyurethane foam after bonding was obtained.
Example 4
The preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property comprises the following steps (in parts by weight):
(1) 180 parts of deionized water and 14 parts of sodium gluconate are added into a beaker, and the mixture is stirred in a water bath kettle at 80 ℃ until the mixture is completely dissolved;
(2) After the solution is cooled to normal temperature, 24 parts of chitosan hydrochloride is slowly added, and the solution is stirred at the speed of 150 rmp at the normal temperature for 1.2 h so as to be uniformly dispersed;
(3) Slowly adding 16 parts of 50 wt% phytic acid solution, and stirring 35min at a speed of 150 rmp at normal temperature;
(4) 2 parts of anti-UV-531 and 0.4 parts of Genapol 2070 were added and stirred at a speed of 100 rmp for 20: 20 min. The bio-based intumescent water-based flame retardant coating with strong adhesive property is obtained after uniform mixing.
Application one: the flame retardant coating of example 4 was applied by dip coating to the surface of polypropylene by flame ignition, and the coating was dried at 30℃for 12 h to give flame retardant polypropylene, with a one-sided thickness of 200 μm after the coating was dried out, for Limiting Oxygen Index (LOI) and vertical burn test (UL-94).
And (2) application II: coating acrylic emulsion on the surface of a steel plate in a dip-coating mode to serve as a primer, wherein the thickness is 70 mu m, coating the fire-retardant coating of the embodiment 4 on the surface of the steel plate coated with the primer to serve as a finish paint after the primer is dried, and dividing the steel plate into 4 times of coating after the coating is dried completely, wherein the fire-retardant steel plate is obtained after the coating is dried and used for back temperature testing; the flame-retardant coating of the embodiment 4 is coated on the surface of polypropylene burnt by flame in a dip-coating mode, the coating is dried at 30 ℃ to 12h, the thickness of one side of the dried coating is 1500 mu m, the coating is divided into 4 times of coating, and the flame-retardant polypropylene obtained after drying is used for back temperature test.
Example 5
The preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property comprises the following steps (in parts by weight):
(1) Adding 240 parts of deionized water and 14 parts of sodium gluconate into a beaker, and stirring in a water bath kettle at 50 ℃ until the deionized water and the 14 parts of sodium gluconate are completely dissolved;
(2) After the solution is cooled to normal temperature, 28 parts of chitosan hydrochloride is slowly added, and the solution is stirred at the normal temperature at the speed of 200 rmp for 1h so as to be uniformly dispersed;
(3) Slowly adding 14 parts of 70 wt% phytic acid solution, and stirring at a speed of 200 rmp at normal temperature for 20 min;
(4) 0.2 part of dimethylsiloxane, 2 parts of anti-aging agent 1010 and 0.4 part of Genapol 2070 were added and stirred at a speed of 100 rmp for 30 min. The bio-based intumescent water-based flame retardant coating with strong adhesive property is obtained after uniform mixing.
Application one: the flame retardant coating of example 5 was coated on the surface of polypropylene by flame firing by roll coating, and the coating was dried at 35℃for 10 h to obtain flame retardant polypropylene, and the thickness of one side of the coating after drying was 200. Mu.m, for Limiting Oxygen Index (LOI) and vertical burning test (UL-94).
And (2) application II: coating acrylic emulsion on the surface of a steel plate in a roller coating mode to serve as a primer, wherein the thickness is 60 mu m, coating the fire-retardant coating of the embodiment 5 on the surface of the steel plate coated with the primer to serve as a finish paint after the primer is dried, and dividing the steel plate into 6 coating steps after the coating is dried completely, so that a fire-retardant steel plate is obtained after the steel plate is dried and used for back temperature test; the flame-retardant coating of the embodiment 4 is coated on the surface of the polypropylene burnt by flame in a roller coating mode, the coating is dried at 35 ℃ for 10 h, the thickness of one side of the dried coating is 1500 mu m, the coating is divided into 6 times of coating, and the flame-retardant polypropylene obtained after drying is used for back temperature test.
Example 6
The preparation method of the bio-based intumescent water-based flame retardant coating with strong adhesive property comprises the following steps (in parts by weight):
(1) Adding 200 parts of deionized water and 12 parts of magnesium gluconate into a beaker, and stirring in a water bath kettle at 70 ℃ until the magnesium gluconate is completely dissolved;
(2) After the solution is cooled to normal temperature, 26 parts of chitosan lactate is slowly added, and the solution is stirred at the normal temperature at the speed of 200 rmp for 1h so as to be uniformly dispersed;
(3) Slowly adding 16 parts of 70 wt% phytic acid solution, and stirring at a speed of 200 rmp for 30min at normal temperature;
(4) 1.8 parts of UV-770 and 0.3 part of Genapol 2070 are added and stirred at a speed of 100 rmp for 20 min. The bio-based intumescent water-based flame retardant coating with strong adhesive property is obtained after uniform mixing.
Application: the flame retardant coating of example 6 was coated on the surfaces of wood, polyurethane foam and wallpaper respectively by means of knife coating, and the coating was dried at 20 ℃ for 18: 18 h to obtain flame retardant wood, flame retardant polyurethane foam and flame retardant wallpaper, and the thickness of one side of the coating after drying was 200 μm for vertical burning test (UL-94).
Comparative example 1
The example provides a preparation method of a flame-retardant acrylic coating, which comprises the following steps (in mass portion): 40 parts of acrylic emulsion and 5.5 parts of ammonium polyphosphate are added into a beaker, and the mixture is stirred at a speed of 200 rmp ℃ for 1h at normal temperature, so that the mixture is uniformly dispersed to obtain the flame-retardant acrylic coating.
The comparative example 1 flame retardant acrylic paint was coated on polypropylene by knife coating, dried at 20 c for 18 h a, and dried for 500 μm thickness for light transmittance, UL-94 and LOI tests.
Comparative example 2
The comparative example 1 flame retardant acrylic paint was coated on polypropylene by knife coating, dried at 20 c for 18 h a, and dried for a thickness of 200 μm for light transmittance and UL-94 test.
Performance test: the following tests were carried out on the products obtained in examples 1 to 6 and the products obtained in comparative examples 1 to 2.
The UL-94 rating of the polypropylene composite with flame retardant coating was tested using a plastic horizontal/vertical burn tester according to GB/T2408-2008. And detecting the limiting oxygen index of the polypropylene composite material with the flame retardant coating by adopting a ZR-01 intelligent oxygen index determinator according to GB/T38301-2019. The flame retardant coating was tested for light transmission using an ultraviolet visible spectrophotometer Cary 100. The results of the flame retardant property tests and the light transmittance of examples 1 to 5 and comparative examples are shown in Table 1, the coating of comparative examples is a milky opaque coating, the UL-94 test shows NR grade when the thickness of the coating is 200 μm, the flame retardant requirement cannot be met, the UL-94 grade V-0 can be passed only when the thickness of the coating is 500 μm or more, and the UL-94 grade V-0 can be passed when the thickness of the flame retardant coating of examples 1 to 5 is only 200 μm. It is further noted that the limiting oxygen index of the flame retardant polypropylene with the coating of the invention is over 40%, and the limiting oxygen index of the flame retardant polypropylene in the example 3 is as high as 46.1%, which is far beyond 18.0%. This demonstrates that the flame retardant coating of the present invention not only has high light transmittance (transmittance of example 3 is as in fig. 3), but also imparts excellent flame retardancy to polypropylene in the case of a very thin coating. Example 3 in a 550 ℃ constant temperature muffle furnace experiment of the flame-retardant coating, the expansion height of the coating is about 100 times of the original volume, and the carbon layer is compact and continuous, so that the condensed phase flame-retardant effect of the flame-retardant coating is obvious.
TABLE 1 flame retardant Property test results and light transmittance
The flame retardant properties of the polypropylene composite with flame retardant coating were tested using a cone calorimeter according to ISO 5660-1. The cone calorimetric test results of examples 1-2 are shown in Table 2 and FIG. 1; as seen from Table 2 and FIG. 1, the Peak Heat Release Rate (PHRR) and total heat release rate (THR) values of polypropylene were 823.5 kW/m 2 and 114.4 MJ/m 2, respectively, whereas the PHRR and THR values of flame retardant polypropylene in example 1 were 298.9 kW/m 2 and 76.4 MJ/m 2, respectively, were significantly reduced by 63.7% and 33.2%, respectively. The flame retardant coating of the invention is demonstrated to have a greater ability to reduce heat release. The ignition time (TTI) of polypropylene was only 34 s, whereas the TTI of example 1 was increased to 525 s. The carbon residue of polypropylene was 7%, while the flame retardant polypropylene carbon residue in example 1 was 15.89%, indicating the formation of high carbon residue. Meanwhile, the fire spread rate is estimated by detecting a fire growth rate index (FIGRA) and a Fire Performance Index (FPI). The FIGRA of the polypropylene was 5.00 kW/m 2 s and the FPI was 0.04 m 2 s/kW, whereas the FIGRA of the flame retardant polypropylene in example 1 was 0.42 kW/(m 2/s) and the FPI was 1.76 m 2 s/kW, which was 3.2 times higher than the PP. The Total Smoke Production (TSP) was also evaluated. The TSP of the flame retardant polypropylene in example 1 was 7.98 m 2, respectively 40.5% less than polypropylene. The cone calorimetric test results further demonstrate that the flame retardant coating of the present invention has excellent flame retardancy.
TABLE 2 Cone calorimetric measurements
And testing the back temperature of the steel plate and the polypropylene plate with the flame retardant coating by using a handheld thermal imager. The back temperature detection results of examples 1 to 5 are shown in table 3, and the back temperature detection result of example 3 is shown in fig. 2; from Table 3, the stable temperatures of the back temperature of the fireproof steel plate of the invention in 30 min are all lower than 250 ℃, which shows that the flame retardant coating of the invention can reduce the back temperature of the steel plate and improve the stability of the steel structure at high temperature when being used for fireproof steel plate. In addition, the back temperature of the flame retardant polypropylene of examples 1-5 is tested, and the temperature is stabilized at about 220 ℃, so that the flame retardant coating has good heat insulation and fireproof performance.
TABLE 3 Back temperature test results
The adhesion of the flame retardant coating was tested according to GB/T4893.4-2013 using a hundred-gauge knife (OU 4000) to score 5 cuts in each of the horizontal and vertical directions of the composite film, forming a 16-gauge 1cm by 1cm small square. The adhesive tape was quickly torn after being firmly adhered by a 3M hundred-cell test tape, and the degree of damage of the coating was checked and judged. According to national standard GB/T6739-1996, coating hardness is tested, a coating pencil hardness tester (QHQ-A) is used, a sample to be tested is horizontally placed on a test bed, meanwhile, the installed pencil hardness tester is lightly placed on the surface of the coating at 45 degrees, then, from the hardest pencil, the pencil is horizontally pushed at a speed of 5-10 cm/min for 10 cm to observe whether scratches exist on the surface, each grade of pencil is scratched for 5 times, if 2 times of pencil scratch the sample to be tested exists in 5 times, a softer number pencil is selected until at most 1 times of pencil scratch the sample to be tested exist in 5 times, and the pencil corresponding number is the hardness of the pencil to be tested. The results of the coating hundred test and hardness test of examples 1 to 5 are shown in Table 4. In Table 4, the flame retardant coatings obtained in examples 1-5 were subjected to a hundred-cell test on the surface of the pretreated polypropylene substrate, and all reached a 5B grade, and the hardness test reached 3H, which indicates that the coating of the invention can be firmly adhered to the surface of the polypropylene, and the hardness of the coating meets the requirements of paint film hardness.
TABLE 4 coating hundred test and hardness test results
Pull-apart adhesion experiments were performed on various coatings according to GB/T5210-2006: the adhesion between the different coatings and the polypropylene was measured by a pull test using a CMT4204 universal tester with a pull rate of 5 mm/min. The adhesion force measured by the tensile test means a force required to apply a uniform and perpendicular force above the bonding surface at a prescribed speed for determining when the adhesion force between the coating layer and the substrate is broken. The results of the coating adhesion test of the flame retardant coating prepared in example 3, the acrylic emulsion (commercially available, manufacturer: green chemical industry) and the flame retardant acrylic coating prepared in comparative example 2 with the flame-burned polypropylene are shown in fig. 4. Fig. 4 shows that: example 3 the flame retardant coating of the invention has an adhesion of 1.7 mpa on polypropylene with an acrylic emulsion coating, a flame retardant acrylic coating, and a stronger adhesion than the acrylic emulsion coating and the flame retardant acrylic coating. Indicating that the coating of the present invention has a strong adhesion far exceeding that of a typical coating.
Example 6 the results of the vertical burn test (UL-94) for the different materials are shown in table 5. From Table 5, the UL-94 test of the flame retardant coating of the invention on the surfaces of different substrates can be passed through UL-94V-0 level, which shows that the coating of the invention has wide applicability.
TABLE 5 example 6 different matrix materials UL-94 test
And (3) performing antibacterial detection on the flame-retardant coating by adopting solid plate culture medium antibacterial detection. Experimental operation: e.coli DH5 alpha to OD600 of about 0.6 and 108 CFU/mL are respectively cultured in LB culture medium at the temperature of 220 rpm and 37 ℃, bacterial liquid and melted solid culture medium are mixed according to the volume ratio of 1:1000, and 10 mL mixed culture medium is poured into each culture dish (with the diameter of 90 mm) for later use after solidification. The samples to be tested are respectively added, and the samples are cultivated for 24 hours at 37 ℃ for photographing. Example 4 flame retardant coating antibacterial test results are shown in table 6. As shown in Table 6, the number of colonies of the blank plate is far greater than that of colonies treated by the flame retardant coating of example 4, and the antibacterial rate is higher than 80%, which indicates that the flame retardant coating of the invention has antibacterial property.
Table 6 example 4 flame retardant coating antibacterial test
The flame retardant coating is used as a binder and has the performance detection: the flame retardant coating prepared in example 3 was uniformly applied to both ends of the polyurethane foam (coating thickness: about 200 μm), and after leaving at room temperature 6 h, the coating surfaces which had not been completely dried were bonded, and after leaving at room temperature 12: 12 h, the polyurethane foam after bonding was obtained. The vertical surface of the bonded polyurethane foam can bear at least 5N of force, which shows that the flame-retardant coating can bear a certain weight of force to pull the polyurethane foam when being used as a binder, and the substrates cannot be separated, thereby meeting the requirement of being used as the binder.
Claims (10)
1. The bio-based intumescent water-based flame retardant coating with strong adhesive property is characterized by being prepared from the following raw materials in parts by weight:
100-300 parts of deionized water
Gluconate 10-40 parts
10-30 Parts of chitosan salt
40-45 Parts of phytic acid
1-2 Parts of anti-aging agent
0.3-0.4 Part of freeze thawing resistant additive.
2. The bio-based intumescent aqueous flame retardant coating with strong adhesion properties of claim 1, wherein: the gluconate comprises one or a combination of calcium gluconate, sodium gluconate and magnesium gluconate.
3. The bio-based intumescent aqueous flame retardant coating with strong adhesion properties of claim 1, wherein: the chitosan salt comprises one or a combination of chitosan quaternary ammonium salt, chitosan hydrochloride, chitosan lactate and chitosan nitrate, and the substitution degree is more than or equal to 80%.
4. The bio-based intumescent aqueous flame retardant coating with strong adhesion properties of claim 1, wherein: the phytic acid is 50-70wt.% phytic acid solution.
5. The bio-based intumescent aqueous flame retardant coating with strong adhesion properties of claim 1, wherein: the anti-aging agent comprises any one of UV-770, UV-531 and anti-aging agent 1010; the freeze-thawing resistant auxiliary agent is a Coriolis environment-friendly scrubbing-resistant freeze-thawing resistant auxiliary agent Genapol 2070.
6. A method for preparing the bio-based intumescent aqueous flame retardant coating with strong adhesive properties according to any one of claims 1-5, which is characterized by comprising the following steps:
(1) Adding deionized water and gluconate into a beaker, and stirring in a water bath kettle at 50-80 ℃ until the deionized water and the gluconate are completely dissolved;
(2) Cooling the solution to normal temperature, slowly adding chitosan salt, and stirring at the speed of 100-200 rmp at normal temperature for 1-1.5 h to uniformly disperse;
(3) Slowly adding phytic acid solution, and stirring at a speed of 100-200 rmp at normal temperature for 30-60 min;
(4) Adding an anti-aging agent and an anti-freeze thawing auxiliary agent, and stirring at a speed of 100 rmp for 20 min; and uniformly mixing to obtain the bio-based intumescent water-based flame retardant coating with strong adhesive property.
7. A method for using the bio-based intumescent aqueous flame retardant coating with strong adhesive properties of any one of claims 1-5, which is characterized in that: the coating mode of the surface paint of the base material is as follows: blade coating, brush coating, dip coating or roller coating; the coating is dried for 18-24 hours at 15-35 ℃, and the coating needs to be coated for many times when the thickness of the dried coating exceeds 200 mu m.
8. The method of use according to claim 7, wherein: the base material comprises plastics, wood, wallpaper, rigid polyurethane foam or steel; when the substrate is plastic or a substrate with low surface polarity, simple pretreatment of the substrate surface is required, including one of a flame firing method, a polishing method and an adhesion treating agent treatment method.
9. The application of the bio-based intumescent water-based flame retardant coating with strong adhesive property in steel plate fireproof, which is characterized in that:
When the flame-retardant coating is applied to fire prevention of a steel plate, any one of acrylic emulsion, organic silicon resin or wood wax oil is required to be coated on the surface of the steel plate in advance as a primer, the thickness is 50-150 mu m, after the primer is dried, the surface of the steel plate coated with the primer is coated with the flame-retardant coating of the invention as a finish, the thickness of the flame-retardant coating is more than or equal to 1500 mu m, and the coating is carried out for 4-6 times.
10. Use of the bio-based intumescent aqueous flame retardant coating with strong adhesion properties of any one of claims 1-5 in flame retardant adhesives.
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