CN114940853A - LDH @ PDA @ ZrPP water-based epoxy resin intumescent fire-retardant coating - Google Patents
LDH @ PDA @ ZrPP water-based epoxy resin intumescent fire-retardant coating Download PDFInfo
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- 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
- C09D5/185—Intumescent paints
Abstract
The invention discloses an LDH @ PDA @ ZrPP waterborne epoxy resin intumescent fire retardant coating, which comprises the following steps: (1) preparing a base material; (2) preparing an LDH nano hybrid material; (3) preparing an LDH @ PDA nanometer hybrid material; (4) preparing an LDH @ PDA @ ZrPP nano hybrid material; (4) preparation of the LDH @ PDA @ ZrPP intumescent fire retardant coating: weighing the base material, the curing agent and the modified LDH @ PDA @ ZrPP, mixing, mechanically stirring and dispersing for 5 hours to form a uniform dispersion system, then coating the uniform dispersion system on the surface of a square steel sheet, curing at normal temperature for 7 days after coating, and baking at 40 ℃ for 3 days to obtain the LDH @ PDA @ ZrPP intumescent fire retardant coating. The LDH @ PDA @ ZrPP nano filler is used for improving the fireproof and smoke suppression performance and the mechanical strength of the fireproof coating. The environment-friendly fireproof coating is environment-friendly and has good market development prospect and important social value.
Description
Technical Field
The invention belongs to the field of preparation methods of epoxy nanocomposite materials, and particularly relates to a preparation method and application of a hydrotalcite-based water-based epoxy resin intumescent fire-retardant coating with quick response capability.
Background
China is a large steel structure country, and the steel structure can be reused as a form of green building, so that the construction waste is reduced to a great extent, and the method conforms to the road of green sustainable development of China. At present, subway networks, skyscrapers, related supporting facilities and the like of main cities around the world are increasing, and the consumption of steel structures is increasing. However, the steel structure is very sensitive to temperature, and the steel structure is damaged to different degrees along with the rise of temperature in a fire environment. In this regard, the most effective, simple and aesthetically pleasing means of protection is to apply a fire retardant coating to the steel structure surface, which means that the demand for fire retardant coatings is greatly increased.
The water-based epoxy resin (EP) is widely applied to the field of intumescent fire-retardant coatings because of the characteristics of environmental friendliness, no pollution, no toxicity, no harm and the like, but the pure EP fire-retardant coatings have the problems of poor barrier and fire-retardant properties, short service life and the like, so that the properties of the fire-retardant coatings in all aspects need to be improved by adding an inorganic filler.
The layered double hydroxide is a nano-layered material, which consists of a positively charged metal oxide layer and negatively charged anions. The intermediate anion being CO 3 2- Magnesium aluminum hydrotalcite, metal ions from LDH sheets are produced at high temperatures, filling the carbon layers with metal oxides. And water and CO bound between LDH layers 3 2- Can be decomposed into water and CO under the condition of high temperature 2 And the function of diluting the substrate for high-temperature combustion is achieved. The concentration of combustible gas generated by high-temperature combustion of the base material isolates oxygen to achieve the purpose of flame retardance. In addition, poor dispersion and material aggregation of LDH in a flame-retardant coating system cause cracks to appear on a dry flame-retardant coating, and the fireproof performance is reduced, so that the LDH is coated by PDA, the PDA surface contains abundant hydrophilic groups, the dispersibility of the LDH in aqueous epoxy resin can be improved, ZrPP is further uniformly loaded on the surface of the LDH PDA through a coprecipitation method, and the fireproof performance of the composite material in the coating is further improved by utilizing the characteristics of lamellar barrier property and catalytic carbon formation of the ZrPP.
Disclosure of Invention
The invention provides a preparation method of a nano water-based epoxy resin intumescent fire retardant coating aiming at the defects, and develops the application of a nano LDH @ PDA @ ZrPP composite material in the field of fire retardant coatings. In the research, PDA is coated on the surface of LDH through the self-polymerization of PDA, so that the dispersibility of LDH in aqueous epoxy resin is improved, the oxidation resistance of a carbon layer is improved through the capability of eliminating free radicals of PDA, and the combustion speed of the coating is slowed down. In addition, benzene rings in the PDA and the ZrPP form a pi-pi stacking effect, so that the ZrPP is successfully loaded on the surface of the LDH @ PDA, and the flame retardant property and the mechanical property of the carbon layer are further improved.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a high-temperature-resistant nano LDH @ PDA @ ZrPP waterborne epoxy resin intumescent fire-retardant coating comprises the following steps:
(1) preparation of LDH nano hybrid material
LDH is prepared by a hydrothermal method. First, magnesium nitrate and aluminum sulfate were dispersed in 100ml of deionized water. Anhydrous sodium carbonate and urea were dissolved in 100ml of deionized water. In addition, the two solutions were slowly added to the flask and the pH of the solution was maintained at 9-10 by adding 1mol/L NaOH solution, and the solution was reacted at 90 ℃ for 5 h. Then, the reaction solution was poured into a hydrothermal kettle and reacted at 120 ℃ for 36 hours. Finally, the resulting product was centrifuged and thoroughly washed with deionized water until the pH was neutral. The sample was then dried in an oven at 65 ℃ until a constant weight was reached.
(2) Preparation of LDH @ PDA nanometer hybrid material
First, 0.3 to 0.4g LDH and 0.3 to 0.4g Tris-HCl were added to a flask containing 200ml deionized water, and sonicated with a probe for 10 minutes. Then, dilute sodium hydroxide solution was gradually added until the pH reached 8.5. Subsequently, dopamine hydrochloride salt was added to the flask. The reaction system is reacted for 10-15 hours under continuous stirring. After the reaction, the nanoparticles were washed several times with deionized water by centrifugation at 6000 rpm for 5 minutes until the ph of the centrifuged solution became neutral. Finally, LDH @ PDA was allowed to dry in a vacuum oven at 80 ℃ for 24 hours.
(3) Preparation of LDH @ PDA @ ZrPP nano hybrid material
0.625g of phenylphosphoric acid (PPA) was first weighed into 60mL of deionized water and treated with a probe sonicator for 5 min. In addition, 0.5g LDH @ PDA was treated with a probe sonicator for 10min, and then the two solutions were poured into a three-necked flask and mixed, and put in an oil bath pan 25%The mixture was stirred for one hour to mix uniformly, and then the temperature was raised to 100 ℃. 0.5g of ZrOCl was then weighed 2 ·8H 2 And dissolving the O in 20mL of pure water, pouring the dissolved O into a three-neck flask after complete dissolution, connecting a condenser, and continuously reacting for 24 hours. Finally, the product was washed with deionized water until the solution was neutral in pH, and then placed in a vacuum oven and dried at 60 ℃ for 12 hours.
(4) Preparation of the base stock
An intumescent flame retardant system (15 g of melamine polyphosphate, 7.5g of dipentaerythritol and 2.5g of melamine) is mixed and dispersed in deionized water, and stirred vigorously for 30min to obtain a uniformly dispersed suspension. Then, the aqueous epoxy resin emulsion (50g) and curing agent (25g) were weighed out and mixed with the above suspension, and stirring was continued for 10 min. And adding 1g of defoaming agent for eliminating bubbles generated in the stirring process, and uniformly stirring at the speed of 300r/min for 1h to obtain a uniformly mixed base material.
(5) Preparation of LDH @ PDA @ ZrPP waterborne epoxy resin intumescent fire retardant coating
Weighing the base material, the modified LDH @ PDA @ ZrPP nano composite material and the defoaming agent, mixing, mechanically stirring and dispersing for 1h to form a uniform dispersion system, then coating the uniform dispersion system on the surface of a square steel sheet, curing at normal temperature for 7 days after coating, and baking at 40 ℃ for 3 days to obtain the LDH @ PDA @ ZrPP intumescent fire retardant coating.
Further, the ratio of epoxy resin to curing agent in step (1) is 2: 1.
further, in the step (1), the ratio of the epoxy resin to the expansion system is 2-2.5: 1-1.5.
Further, in the step (1), the ratio of melamine polyphosphate to dipentaerythritol to melamine is 5.5-6.5: 2.5-3.5: 1-1.5.
Further, the binder in the step (4) accounts for 96-98% of the total weight of the uniform dispersion system.
Further, in the step (4), the modified LDH @ PDA @ ZrPP hybrid material accounts for 2.5% -4.5% of the total weight of the uniform dispersion system.
Further, in the step (4), the defoaming agent accounts for 0.5-1.5% of the total weight of the homogeneous dispersion system.
The invention provides a preparation method of a hydrotalcite-based water-based epoxy resin intumescent fire retardant coating with quick response capability, which has the following beneficial effects:
(1) the preparation process is simple and feasible, low in cost, environment-friendly and suitable for industrial production.
(2) In the preparation process, the modified LDH @ PDA @ ZrPP is combined with the epoxy resin, and the prepared product is good in high-temperature resistance effect and strong in adhesive force.
Drawings
FIG. 1 is an X-ray diffraction diagram of LDH, LDH @ PDA @ ZrPP and ZrPP.
FIG. 2 is an infrared spectrum of LDH, LDH @ PDA @ ZrPP and ZrPP.
FIG. 3 is a transmission electron micrograph of LDH, LDH @ PDA @ ZrPP and ZrPP.
FIG. 4 temperature profile of the back side of the steel plate after the large plate method test.
FIG. 5 shows the morphology of the coating before and after the large plate test, wherein a is pure EP, b is LDH// EP, c is LDH @ PDA// EP, and d is LDH @ PDA @ ZrPP// EP.
FIG. 6 is the expansion height of the carbon layer after hearth test, where A is pure resin, B is LDH/epoxy, C is LDH @ PDA// epoxy, and D is LDH @ PDA @ ZrPP/epoxy.
FIG. 7 is a scanning electron microscope image of the carbon layer coated with epoxy resin, LDH/epoxy resin, LDH @ PDA @ ZrPP/epoxy resin.
Detailed Description
Example 1
A preparation method of a high-temperature-resistant nano LDH @ PDA @ ZrPP waterborne epoxy resin intumescent fire-retardant coating comprises the following steps:
(1) preparation of the base stock
An intumescent flame retardant system (15 g of melamine polyphosphate, 7.5g of dipentaerythritol and 2.5g of melamine) is mixed and dispersed in deionized water, and stirred vigorously for 30min to obtain a uniformly dispersed suspension. Then, the aqueous epoxy resin emulsion (50g) and the curing agent (25g) were weighed out and mixed with the above suspension, and stirring was continued for 10 min. And adding 1g of defoaming agent for eliminating bubbles generated in the stirring process, and uniformly stirring at the speed of 300r/min for 1h to obtain a uniformly mixed base material.
(2) Preparation of LDH nanomaterials
Layered double metal hydroxide, magnesium aluminum hydrotalcite (LDH), is prepared by a hydrothermal method. First, MgCl is added 2 ·H 2 O (5.421g,0.023mol) and Al (NO3) 3.9H 2 O (5g,0.013mol) was dissolved together in 100mL of pure water; then weighing anhydrous sodium carbonate Na 2 CO 3 (2.8263g,0.0266mol) and urea (4.805g) were dissolved in an additional beaker containing 100mL of purified water. Then, pouring the two solutions into a three-neck flask, and carrying out reaction in an oil bath kettle at the temperature of 80 ℃; then, the mixed solution is transferred to a hydrothermal pot and reacted for 36 hours at 120 ℃; washing the reacted solution with pure water for many times until the pH test value is neutral; finally, drying in a freeze-dryer.
(3) Preparation of LDH @ PDA nano material
Firstly, dissolving 0.4g of LDH in 200mL of deionized water, and treating for 10 minutes by using a probe ultrasonic device to uniformly disperse the LDH; then, 0.35g of Tris HCl was weighed and mixed with the LDH dispersion to prepare a NaOH solution and adjust the pH of the dispersion to 8.5, and then 0.5g of dopamine hydrochloride was added to the mixed solution and continuously stirred for 10 hours so that PDA could be uniformly coated on the LDH surface.
(4) Preparation of LDH @ PDA @ ZrPP composite material
0.625g of phenylphosphoric acid (PPA) was first weighed into 60mL of deionized water and treated with a probe sonicator for 5 min. In addition, 0.5g of LDH @ PDA was taken and treated with a probe ultrasonic for 10min, then the above two solutions were poured into a three-necked flask and mixed, stirred in an oil bath at 25 ℃ for one hour to be uniformly mixed, and then heated to 100 ℃. 0.5g of ZrOCl was then weighed 2 ·8H 2 And dissolving the O in 20mL of pure water, pouring the dissolved O into a three-neck flask after complete dissolution, connecting a condenser, and continuously reacting for 24 hours. Finally, the product was washed with deionized water until the solution was neutral in pH, and then placed in a vacuum oven and dried at 60 ℃ for 12 hours.
(4) Preparation of high-temperature-resistant nano LDH @ PDA @ ZrPP water-based epoxy resin intumescent fire-retardant coating
Weighing 97g of base material, 2g of LDH @ PDA @ ZrPP nano hybrid material and 1g of defoaming agent, mixing, mechanically stirring and dispersing for 5h to form a uniform dispersion system, then coating the uniform dispersion system on the surface of a rectangular steel sheet, curing at normal temperature for 7 days after coating, and baking at 40 ℃ for 3 days to obtain the high-temperature-resistant nano LDH @ PDA @ ZrPP intumescent fire-retardant coating. Wherein, the proportion of the base material and the proportion of the LDH @ PDA @ ZrPP in the total weight of the dispersion system are shown in the table 1:
TABLE 1 base material, LDH @ PDA @ ZrPP proportioning table
Experimental example 2
LDH, LDH @ PDA @ ZrPP and epoxy resin are mixed respectively, mechanical stirring is carried out for 5 hours, LDH/epoxy resin coatings, LDH @ PDA/epoxy resin coatings and LDH @ PDA @ ZrPP/epoxy resin coatings with the contents of LDH, LDH @ PDA @ ZrPP and 4 wt% are prepared, the LDH/epoxy resin coatings, the LDH @ PDA/epoxy resin coatings and the LDH @ PDA @ ZrPP/epoxy resin coatings are respectively coated on a base steel plate (Q235) which is subjected to sand blasting and welding, spraying of the coatings is carried out within 1 hour after sand blasting treatment of the base steel plate is completed, after spraying is completed, the steel plate with the coatings is cured for 7 days at room temperature, and is baked for 3 days at 40 ℃, so that a sample is obtained, and pure epoxy resin is used as a reference.
(1) Characterization of LDH, LDH @ PDA @ ZrPP and ZrPP was performed by X-ray diffraction (XRD, X Pert PRO MPD, Cu K alpha ray diffraction, 5-80 ℃). The results are shown in FIG. 1. From the first figure, the LDH and ZrPP diffraction peaks are obvious and sharp, the crystal form is complete, and the XRD diffraction peaks corresponding to the lamellar structure are met. In addition, the diffraction peaks of both LDH and ZrPP can be clearly seen in the XRD of LDH @ PDA @ ZrPP.
(2) Functional groups of LDH, LDH @ PDA @ ZrPP and ZrPP were observed by FT-IR, and the results are shown in FIG. 2. Original LDH at 3443cm -1 The broad peak comes from abundant hydroxyl (-OH) on the surface of the hydrotalcite and is 1637cm -1 And 1358cm -1 The peaks are respectively attributed to water molecules (H) between hydrotalcite layers 2 O) and CO 3 2- At 418-720cm -1 A series of characteristic peak assignmentsIs the vibration of metal-oxygen (M-O). As can be seen from the spectrum of LDH @ PDA, the characteristic peak intensity of hydrotalcite is weakened because PDA is coated on the surface of hydrotalcite. In the FT-IR spectrum of ZrPP, it is located at 3454cm -1 The broad peak at (a) is from the hydroxyl groups in the material. At 3054cm -1 The labeled peak at (A) belongs to C-H stretching vibration of a benzene ring. 1598cm -1 And 1440cm -1 The broad peak of (a) can be attributed to C ═ C stretching vibration of the benzene ring. In addition, at 1165cm -1 And 985cm -1 Stretching vibration of the P-O occurs. The characteristic peak of the benzene ring may be 749cm -1 、724cm -1 And 692cm -1 Is observed. At 567cm -1 A Zr-O absorption peak was observed. For LPZP hybrid materials, characteristic peaks belonging to LDH and ZrPP can be clearly seen in the infrared spectrum of the LPZP hybrid materials. This initially demonstrated the successful loading of ZrPP onto LDH @ PDA surfaces.
(3) The morphology of the LDH and LDH @ PDA, LDH @ PDA @ ZrPP hybrid material was observed by using a JEOL JEM-2100 high resolution transmission electron microscope (HR-TEM), and the results are shown in figure 3. Figure 3(a) is a pure LDH with a clearly intact lamellar structure visible. Fig. 3(b) shows pure ZrPP, where ZrPP of the platelet layer can be seen, and fig. 3(c) shows LDH with PDA coated on the surface, where a 30 nm-wide translucent film is present at the edge of the hydrotalcite platelet layer. FIGS. 3(d) and (e) are graphs of LDH @ PDA @ ZrPP, from which it can be seen that ZrPP is uniformly loaded on the surface of LDH @ PDA by means of pi-pi stacking.
(4) And (3) testing the temperature of the back surface of the steel plate by adopting a large plate method to detect the fireproof performance of the fireproof coating. The results are shown in FIG. 4. As can be seen from fig. 4, the steel sheet back surface temperature of the fire retardant coating comprising LDH @ PDA @ ZrPP was the lowest, indicating the best fire retardant properties. As can be seen from fig. 4(d), the fire retardant coating carbon layer containing LDH @ PDA @ ZrPP has a complete and compact structure with few voids. The result shows that the synthesized hybrid material LDH @ PDA @ ZrPP can effectively improve the carbon layer strength and the oxidation resistance of the fireproof coating, so that the fireproof performance is improved.
(5) The carbon layer formed by the coating after the large panel test was analyzed and the results are shown in FIG. 5. It can be seen from the figure that all samples (a-d) show a flat smooth surface before and after combustion, which indicates the rationality of the intumescent coating formulation. As can be seen from the graph (a'), the carbon layer surface of pure EP has large cracks and pores, which may cause the steel plate to directly contact with flame during combustion, and thus the heat cannot be effectively blocked. For LDH/EP and LDH @ PDA/EP, it can be seen from the graphs (b ') and (c'), that the carbon layer structure remains intact after the sample is subjected to flame impact, but certain cracks and pores still exist. After the LDH @ PDA @ ZrPP composite material is added, the IFR coating (d') shows a more complete and compact carbon layer, because metal ions in the LDH @ PDA @ ZrPP form metal oxides at high temperature, and the metal oxides are filled in the carbon layer as a condensed phase, so that the strength of the carbon layer is enhanced, the phenomenon of cracking of the carbon layer caused by flame impact is improved, and the release of volatile substances is reduced.
(6) The expansion performance of the fire retardant coating was tested by in-furnace experiments. The swelling behavior of the coating is shown in FIG. 6. The expansion height and expansion ratio of pure EP (fig. a) were 10.5mm, which indicates that the expansion performance of pure EP is not good, a sufficient distance between the flame and the steel plate cannot be formed, and the strength of the carbon layer is weak, and effective blocking of volatile substances is not possible. After the addition of LDH (b), the IFR coating reached a height of 14.7mm of swelling. In addition, LDH @ PDA/EP sample (c) the oxidation resistance of the carbon layer was improved by the addition of PDA, and the swelling height was increased to 16.5 mm. For the LDH @ PDA @ ZrPP/EP sample, the expansion performance of the coating is obviously enhanced, and the expansion height reaches 30.1mm, because the LDH @ PDA @ ZrPP can release a certain amount of CO in the thermal degradation process 2 And H 2 And O, so that the foaming effect of the composite coating is enhanced, and the metal oxide generated at the high temperature of the LDH @ PDA @ ZrPP can further improve the strength of the carbon layer, so that the carbon layer can expand more uniformly.
(7) The internal condition of the carbon layer after the large-plate method test was observed by using a JSM-7500F scanning electron microscope, as shown in FIG. 6. SEM images of pure EP (fig. 7(a)) show cracks and large pores on the surface of the carbon residue after combustion, which form a transfer path between heat and the steel plate, resulting in a rapid increase in the temperature of the steel surface. As can be seen from fig. 7(b), the number of pores and cracks on the surface of the carbon layer decreased with the addition of LDH, indicating that LDH can effectively improve the strength of the carbon layer. FIG. 7(c) shows the carbon layer structure of LDH @ PDA/EP, and due to the antioxidant property of PDA, it can be seen that the gaps on the surface of the carbon layer disappear, but the pores still have different sizes. The carbon layer (d) of the LDH @ PDA @ ZrPP/EP has a complete and compact cellular structure, so that the surface area of the carbon layer for adsorbing smoke is increased, and the emission of more volatile substances can be reduced.
Claims (4)
1. An LDH @ PDA @ ZrPP water-based epoxy resin intumescent fire retardant coating is prepared by the following steps:
(1) preparation of LDH nano hybrid material
Layered double hydroxides, namely magnesium aluminum hydrotalcite (LDH), are prepared by a hydrothermal method. First, MgCl 2 ·H 2 O (5.421g,0.023mol) and Al (NO) 3 ) 3 ·9H 2 O (5g,0.013mol) was dissolved together in 100mL of pure water; then anhydrous sodium carbonate Na is weighed 2 CO 3 (2.8263g,0.0266mol) and urea (4.805g), dissolved in an additional beaker containing 100mL of purified water; then, pouring the two solutions into a three-neck flask, and carrying out reaction in an oil bath kettle at the temperature of 80 ℃; then, the mixed solution is moved into a hydrothermal kettle and reacts for 36 hours at the temperature of 120 ℃; pumping and filtering the reactant by using pure water until the pH test value is neutral; finally, drying in a freeze-dryer;
(2) preparation of LDH @ PDA nanometer hybrid material
Firstly, dissolving 0.4g of LDH in 200mL of deionized water, and treating for 10 minutes by using a probe ultrasonic device to uniformly disperse the LDH; then weighing 0.35g of Tris HCl and mixing with the LDH dispersion liquid, preparing a NaOH solution, adjusting the pH value of the dispersion liquid to 8.5, then adding 0.5g of dopamine hydrochloride into the mixed solution, and continuously stirring for 10 hours to ensure that the PDA can be uniformly coated on the surface of the LDH;
(3) preparation of LDH @ PDA @ ZrPP nano hybrid material
Firstly weighing 0.625g of phenylphosphoric acid (PPA) to be dissolved in 60mL of deionized water, and treating for 5min by using a probe ultrasonic processor; in addition, 0.5g of LDH @ PDA (equivalent to 45mL of undried LDH @ PDA solution) was treated with a probe sonicator for 10min, and then the two solutions were poured into a three-necked flask and mixed, stirred in an oil bath at room temperatureStirring for one hour to uniformly mix, and then heating to 100 ℃; then 0.5g of ZrOCl.8H was weighed using an electronic scale 2 Dissolving O in 20mL of pure water, pouring the dissolved O into a three-neck flask after the O is completely dissolved, communicating a condenser, and continuously reacting for twenty-four hours; finally, washing the product with deionized water until the pH test value of the solution is neutral, and then placing the product in a freeze dryer for drying;
(4) preparation of high-temperature-resistant nano LDH @ PDA @ ZrPP water-based epoxy resin intumescent fire-retardant coating
Mixing and dispersing an expansion flame-retardant system (MPP, DPER and MEL) in deionized water according to a certain proportion, and violently stirring for 30min to obtain a uniformly dispersed suspension. Then weighing a certain amount of aqueous epoxy resin emulsion and curing agent, mixing with the suspension, and continuing stirring for 10 min; subsequently, different dispersions (LDH, LDH @ PDA @ ZrPP) of the nano-filler are respectively added, a small amount of antifoaming agent is added for eliminating bubbles generated in the stirring process, and the mixture is uniformly stirred at the speed of 300r/min for 10 min. And finally, uniformly coating the prepared mixed emulsion on the surface of a self-made steel plate, and curing for one week at normal ambient temperature to obtain the IFR coating.
2. The preparation method of the nano LDH @ PDA @ ZrPP waterborne epoxy resin intumescent fire retardant coating as claimed in claim 1, wherein the addition ratio of LDH to dopamine hydrochloride in step (1) is 4:5 by mass.
3. The preparation method of the nano LDH @ PDA @ ZrPP waterborne epoxy resin intumescent fire retardant coating as claimed in claim 1, wherein the addition amount of the LDH @ PDA @ ZrPP composite material in the step (4) is 3.5-4.5% of the total mass of the system.
4. An aqueous epoxy intumescent fire retardant coating prepared by the process of any of claims 1 to 3.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115850913A (en) * | 2022-12-02 | 2023-03-28 | 西南石油大学 | Preparation method of environment-friendly nano intumescent flame retardant mBN @ LDH @ PATP and epoxy resin nano composite material |
| CN116554757A (en) * | 2023-05-24 | 2023-08-08 | 成都大学 | Preparation method of organic solid acid modified boron nitride water-based intumescent fireproof coating |
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2022
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115850913A (en) * | 2022-12-02 | 2023-03-28 | 西南石油大学 | Preparation method of environment-friendly nano intumescent flame retardant mBN @ LDH @ PATP and epoxy resin nano composite material |
| CN115850913B (en) * | 2022-12-02 | 2024-03-08 | 西南石油大学 | Preparation method of environment-friendly nano intumescent flame retardant mBN@LDH@PATP and epoxy resin nanocomposite |
| CN116554757A (en) * | 2023-05-24 | 2023-08-08 | 成都大学 | Preparation method of organic solid acid modified boron nitride water-based intumescent fireproof coating |
| CN116554757B (en) * | 2023-05-24 | 2024-01-05 | 成都大学 | Preparation method of organic solid acid modified boron nitride water-based intumescent fireproof coating |
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Application publication date: 20220826 |