Antibacterial weather-resistant nano transparent fireproof coating and preparation method thereof

Abstract

The application discloses an antibacterial weather-resistant nano transparent fireproof coating and a preparation method thereof. The transparent fireproof material is prepared by the following method: first, a modified layered nano filler is grafted on a flexible phosphate to prepare a layered nano composite flexible phosphate; then, the layered nano filler composite flexible phosphate is prepared into an ethanol solution as component one; an amino resin is prepared into an aqueous solution as component two, and the components one and two are uniformly blended and stirred according to a mass ratio of 1:1-2 to obtain the transparent fireproof coating. The modified layered nano filler is grafted on the flexible phosphate, the peeling degree of the layered nano filler is improved, the transparency, migration and compatibility of the coating can be ensured, and the release of heat and smoke can be effectively blocked; the prepared transparent fireproof coating has a continuous and dense expanded carbon layer structure, has a good fireproof protection effect on a base material, has good decoration, flame-retardant, antibacterial and aging-resistant properties, and has low raw material cost, simple preparation process and wide application range.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of paint technology, in particular to a transparent fireproof paint and a preparation method thereof, especially to an antibacterial and weather-resistant nano transparent fireproof paint and a preparation method thereof. BACKGROUND

[0002] Transparent fireproof paint is a special paint that can be brushed on flammable substrates or objects requiring special protection, which can maintain the original appearance of the substrate and also play a role in fireproofing and decoration. Transparent fireproof paint has become a research hotspot in the field of coatings due to its excellent decorative effect and fireproof performance, and has broad application prospects in the fields of cultural relics and ancient buildings, modern buildings, and high-end furniture. However, transparent fireproof paint is often exposed to natural environment and inevitably affected by environmental factors such as light, temperature, and bacteria, which causes the fireproofing and flame-retardant performance to deteriorate and fail. Therefore, the problem of insufficient antibacterial and weather-resistant performance of the coating greatly affects the long-term use of the intumescent transparent fireproof paint in the field of cultural relics and ancient buildings, thereby limiting its industrial application. Therefore, developing high-efficiency and durable transparent fireproof paint is a new trend and focus.

[0003] Currently, there have been some studies on the design and preparation of nano fireproof paint, such as:

[0004] The Chinese patent document with publication number CN103805056A discloses a nano fireproof paint and a preparation method thereof, which can absorb heat and form a ceramic heat insulation layer at different stages of a fire, and can be widely used in various places requiring fireproofing and flame-retardant.

[0005] The Chinese patent document with publication number CN104774540A discloses a thin intumescent nano fireproof paint for steel structure and a preparation method thereof, which has high fire-retardant efficiency, good compatibility, and good uniformity of nano montmorillonite in the fireproof paint.

[0006] Layered nano fillers, such as montmorillonite and kaolin, on the one hand, due to the unique lamellar structure of layered nano fillers, not only can act as a physical barrier, but also can catalyze the formation of carbon, thereby effectively blocking the transfer of heat, oxygen, and combustible gases; on the other hand, layered nano fillers can hinder the cell division process of bacteria, thereby showing good bacteriostatic effect. However, layered nano fillers have poor dispersibility in coatings and are prone to agglomeration, causing serious light scattering and not meeting the high transparency requirement of transparent fireproof paint.

[0007] The existing research on nano fireproof coating mainly focuses on non-transparent coating field, which cannot meet the requirements of material decoration performance, and there is little research on the use of layered nano filler to enhance the multifunctional integration of transparent fireproof coating such as fire resistance, antibiosis and weather resistance, so it is necessary to provide an antibacterial and weather resistant nano transparent fireproof coating and a preparation method thereof, and promote the industrial application of layered nano filler in the field of transparent fireproof coating. SUMMARY

[0008] The technical problem to be solved by the present application is to provide an antibacterial and weather resistant nano transparent fireproof coating and a preparation method thereof.

[0009] In order to solve the above technical problems, the present application adopts the following technical solutions:

[0010] In a first aspect, a preparation method of an antibacterial and weather resistant nano transparent fireproof coating is provided, which specifically comprises the following steps:

[0011] (1) grafting the modified layered nano filler on the flexible phosphate to obtain a layered nano composite flexible phosphate, specifically blending and stirring the modified layered nano filler and the flexible phosphate uniformly, ultrasonic dispersion and mixing reaction to obtain; wherein the modified layered nano filler accounts for 0.5-3wt% of the total mass of the obtained layered nano composite flexible phosphate;

[0012] (2) preparing a 50-80wt% ethanol solution of the layered nano filler composite flexible phosphate obtained in step (1) as component one; preparing a 50-80wt% aqueous solution of amino resin as component two, then blending and stirring uniformly according to the mass ratio of component one to component two is 1:1-2, to obtain the antibacterial and weather resistant nano transparent fireproof coating.

[0013] Further, the modified layered nano filler in step (1) is one of modified boron nitride and modified zirconium phosphate.

[0014] In one aspect, the modified boron nitride is KH550 modified boron nitride.

[0015] Specifically, the KH550 modified boron nitride is prepared by the following method:

[0016] P1, 3.5-5.5g hexagonal boron nitride and 200mL of 4-6mol / L sodium hydroxide ethanol solution are sequentially added, mixed at 70-80℃ for 12h, then the product is suction filtered, washed to neutral, and dried at 50-80℃ for 7-10h to obtain hydroxylated boron nitride;

[0017] P2, 100 mL of 95% volume fraction of ethanol, 10 mL of deionized water and 0.5-1.5 g of silane coupling agent KH550 are sequentially added and mixed at 20-30°C for 5-15 min to obtain a mixed solution;

[0018] P3, the mixed solution prepared in step P2 and the hydroxylated boron nitride prepared in step P1 are mixed, and the product is filtered, washed and dried at 50-80°C for 7-10 h to obtain KH550 modified boron nitride.

[0019] In another aspect, the modified zirconium phosphate is KH550 modified zirconium phosphate.

[0020] Specifically, the KH550 modified zirconium phosphate is prepared by the following method:

[0021] 1-3 g of α-zirconium phosphate, 130-135 g of ethanol and 30-35 g of deionized water are uniformly mixed and ultrasonically dispersed at room temperature for 30 min; then 1-1.5 g of ethylamine is added and ultrasonically dispersed at room temperature for 0.5-1.5 h; then 0.4-1 g of silane coupling agent KH550 is added and ultrasonically dispersed at room temperature for 3-5 h, and the product is filtered, washed and dried at 50-80°C for 7-10 h to obtain KH550 modified zirconium phosphate.

[0022] Further, the reaction conditions for grafting the modified layered nanofiller on the flexible phosphate ester in step (1) to prepare the layered nanocomposite flexible phosphate ester are as follows: after the modified layered nanofiller and the flexible phosphate ester are uniformly blended and stirred, ultrasonic dispersion is performed at 40-60°C for 0.5-1.5 h, and then mixed reaction is performed at 120-140°C for 3-5 h.

[0023] Further, the flexible phosphate ester in step (1) is prepared by mixing and reacting polyethylene glycol borate and acid phosphate ester in a predetermined ratio.

[0024] Further, the preparation method of the flexible phosphate ester specifically comprises the following steps:

[0025] C1, polyethylene glycol and boric acid are sequentially added and mixed at a molar ratio of 2.0-3.0:1.0-1.1, and mixed reaction is performed at 120-140°C for 2-4 h under stirring and condensation reflux to obtain polyethylene glycol borate;

[0026] C2, phosphoric acid, pentaerythritol and n-butanol are sequentially added and mixed at a molar ratio of 2.5-3:0.5-1:0.3-0.5, and mixed reaction is performed at 100-120°C for 3-5 h and at 120-150°C for 1-3 h, and condensation reflux is performed to obtain acid phosphate ester;

[0027] C3, the polyethylene glycol borate prepared in step C1 and the acid phosphate prepared in step C2 are added in turn according to a mass ratio of 10-15:80-85, mixed and reacted at 40-60°C for 0.5-1.5h, then the temperature is increased to 110-120°C for mixing and reaction for 3-5h, and then distilled under reduced pressure to obtain the flexible phosphate.

[0028] Further, the amino resin in step (2) is one of methyl etherified melamine resin and butylated melamine resin.

[0029] In a second aspect, the application further provides an antibacterial and weather-resistant nano transparent fireproof coating prepared by the above method, which is mainly composed of component one and component two according to a mass ratio of 1:1-2.

[0030] The component one is an ethanol solution of the layered nano-composite flexible phosphate, which is prepared by grafting the modified layered nano-filler on the flexible phosphate, and the mass ratio of the modified layered nano-filler in the layered nano-composite flexible phosphate is 0.5-3wt%.

[0031] The component two is an aqueous solution of the amino resin.

[0032] Further, the modified layered nano-filler is one of modified boron nitride and modified zirconium phosphate.

[0033] The application has the following beneficial effects:

[0034] 1. Since the layered nano-particles are prone to agglomeration in the group to cause light scattering phenomenon, thereby reducing the light transmittance, the fireproof coating provided by the application uses the modified layered nano-filler, which has enhanced exfoliation degree and can greatly reduce the light scattering phenomenon, so that the light transmittance of the fireproof coating reaches more than 80%.

[0035] 2. The fireproof coating provided by the application uses the modified layered nano-filler with improved dispersibility, and the chemical grafting on the flexible phosphate helps to disperse more uniformly in the transparent coating, avoids the migration problem of the coating layer caused by physical blending, further improves the compatibility of the coating layer, makes the layered nano-particles fully play the role of layer barrier, effectively blocks the release of heat and smoke, and significantly improves the fireproof, heat insulation and flame-retardant and smoke-suppression effects of the transparent fireproof coating.

[0036] 3. The modified layered nano-filler of the application preferably uses modified boron nitride and modified zirconium phosphate. The use of boron nitride can produce a "labyrinth" effect in the coating layer, and the in-plane thermal conductivity is much higher than the thermal conductivity in the vertical plane direction, further enhancing the heat insulation and barrier effects. The use of zirconium phosphate is because the interlayer of zirconium phosphate has a large number of acid points (H + ) and Lewis acid points (Zr4+ ), which can catalyze the cross-linking of the polymer into carbon during the high-temperature process, further blocking the transmission of oxygen and heat.

[0037] 4, The modified layered nanofiller used in the fireproof paint provided by the application helps to promote the carbonization of the coating, can form a continuous, dense and stable expanded carbon layer, thereby inhibiting the decomposition and combustion of the matrix, and the coating exhibits more excellent flame-retardant and smoke-suppressing performance.

[0038] 5, The modified layered nanofiller used in the fireproof paint provided by the application has good anti-permeability and anti-corrosion, and the nano barrier formed by the modified layered nanofiller uniformly dispersed in the transparent coating can effectively block moisture, absorb ultraviolet rays, delay the oxidation and hydrolysis of the coating, and block the migration of the flame retardant, thereby improving the aging resistance of the coating.

[0039] 6, The modified layered nanofiller used in the fireproof paint provided by the application can effectively enhance the antibacterial performance of the coating. Among them, the boron nitride selected can be combined with the conserved site of the surface protein responsible for the shrinkage of Z ring (FtsZ ring) in bacterial cell division, destroying cell division; the zirconium element in the zirconium phosphate can destroy the structural integrity of the bacterial cell membrane and interfere with the normal metabolic activities inside the bacteria.

[0040] In summary, the nano transparent fireproof material provided by the application can ensure excellent flame-retardant effect and decorative performance of the material while enhancing the antibacterial and aging resistance of the coating. Moreover, the raw material cost is low, the preparation process is simple, and the application range is wide. BRIEF DESCRIPTION OF DRAWINGS

[0041] Figure 1 The infrared spectrum comparison chart of the modified boron nitride and the unmodified boron nitride of the embodiment 1 of the application, wherein (a) is hexagonal boron nitride, (b) is hydroxylated boron nitride, and (c) is KH550 modified boron nitride.

[0042] Figure 2 The infrared spectrum comparison chart of the modified zirconium phosphate and the unmodified zirconium phosphate of the embodiment 4 of the application, wherein (a) is zirconium phosphate, and (b) is KH550 modified zirconium phosphate.

[0043] Figure 3 The infrared spectrum comparison chart of the modified boron nitride grafted with flexible phosphate ester and the ungrafted flexible phosphate ester of the embodiment 1, wherein (a) is flexible phosphate ester, and (b) is modified boron nitride grafted with flexible phosphate ester.

[0044] Figure 4 The infrared spectrum comparison chart of the modified zirconium phosphate grafted with flexible phosphate ester and the ungrafted flexible phosphate ester of the embodiment 4, wherein (a) is flexible phosphate ester, and (b) is modified zirconium phosphate grafted with flexible phosphate ester. DETAILED DESCRIPTION

[0045] The application provides an antibacterial weather-resistant nano transparent fireproof coating and a preparation method thereof.

[0046] (1) grafting the modified layered nanofiller on the flexible phosphate to obtain the layered nanocomposite flexible phosphate, specifically, uniformly blending and stirring the modified layered nanofiller and the flexible phosphate, ultrasonic dispersing at 40-60°C for 0.5-1.5h, and then mixing and reacting at 120-140°C for 3-5h.

[0047] As a preferred embodiment, the modified layered nanofiller accounts for 0.5-5wt% of the total mass of the obtained layered nanocomposite flexible phosphate. It can be understood that the modified layered nanofiller can account for any value in 0.5-3wt% of the total mass of the obtained layered nanocomposite flexible phosphate, including but not limited to 0.5%, 1%, 1.5%, 2%, 2.5%, and 3%.

[0048] As a preferred embodiment, the modified layered nanofiller is any one of modified boron nitride and modified zirconium phosphate.

[0049] More preferably, the modified boron nitride is KH550 modified boron nitride, and the following specific embodiments are described by taking the KH550 modified boron nitride prepared by the following method as an example.

[0050] P1, 3.5-5.5g of hexagonal boron nitride and 200mL of an ethanol solution of sodium hydroxide with a concentration of 4-6mol / L are sequentially added, mixed and reacted at 70-80°C for 12h, then the product is suction filtered, washed to neutral, and dried at 50-80°C for 7-10h to obtain hydroxylated boron nitride;

[0051] P2, 100mL of ethanol with a volume fraction of 95%, 10mL of deionized water, and 0.5-1.5g of silane coupling agent KH550 are sequentially added, mixed and reacted at 20-30°C for 5-15min to obtain a mixed solution;

[0052] P3, the mixed solution prepared in step P2 and the hydroxylated boron nitride prepared in step P1 are mixed, stirred in a water bath at 60-80°C for 8-12h, the product is filtered and washed, and dried at 50-80°C for 7-10h to obtain KH550 modified boron nitride.

[0053] More preferably, the modified zirconium phosphate is KH550 modified zirconium phosphate, and the following specific embodiments are described by taking the KH550 modified zirconium phosphate prepared by the following method as an example.

[0054] Mix 1-3 g of zirconium alpha-phosphate, 130-135 g of ethanol and 30-35 g of deionized water uniformly, and ultrasonically disperse at room temperature for 30 min; then add 1-1.5 g of ethylamine, and ultrasonically disperse at room temperature for 0.5-1.5 h; then add 0.4-1 g of silane coupling agent KH550, and ultrasonically disperse at room temperature for 3-5 h; filter and wash the product, and dry at 50-80℃ for 7-10 h to obtain KH550-modified zirconium phosphate.

[0055] As a preferred embodiment, the flexible phosphate ester is prepared by mixing and reacting polyethylene glycol borate and acid phosphate ester in a preset ratio, and specifically includes the following steps:

[0056] C1, sequentially add polyethylene glycol and boric acid in a molar ratio of 2.0-3.0:1.0-1.1, and mix under stirring at 120-140℃ for 2-4 h to obtain polyethylene glycol borate by condensation reflux;

[0057] C2, sequentially add phosphoric acid, pentaerythritol and n-butanol in a molar ratio of 2.5-3:0.5-1:0.3-0.5, and mix at 100-120℃ for 3-5 h and at 120-150℃ for 1-3 h to obtain acid phosphate ester by condensation reflux;

[0058] C3, sequentially add the polyethylene glycol borate prepared in step C1 and the acid phosphate ester prepared in step C2 in a mass ratio of 10-15:80-85, and mix at 40-60℃ for 0.5-1.5 h, then heat to 110-120℃ for 3-5 h, and distill under reduced pressure to obtain the flexible phosphate ester.

[0059] (2) Mix the layered nanofiller composite flexible phosphate ester prepared in step (1) into an ethanol solution of 50-80 wt%, as component one; mix the amino resin into an aqueous solution of 50-80 wt%, as component two, then blend and stir uniformly according to a mass ratio of component one to component two of 1:1-2, to obtain the antibacterial and weather-resistant nanometer transparent fireproof coating.

[0060] As a preferred embodiment, the commonly used amino resin includes methyl etherified melamine resin and butylated melamine resin. The methyl etherified melamine resin is preferably used in the present application.

[0061] In order to more clearly understand the above-mentioned purposes, features and advantages of the present application, the present application will be further described in detail below in combination with the drawings and specific embodiments.

[0062] Many specific details are set forth in the following description to provide a thorough understanding of the invention. However, the invention may also be practiced in other ways different from those described herein, and therefore the scope of protection of the invention is not limited to the specific embodiments disclosed below. Any modifications, substitutions, or improvements made without departing from the spirit and principles of the invention are within the scope of protection claimed by the invention.

[0063] I. Preparation of Nano-Transparent Fireproof Materials

[0064] The relevant information regarding the test raw materials used in the following specific embodiments and comparative examples is shown in Table 1 below:

[0065] Table 1. Information related to experimental raw materials

[0066] Raw material name Purity or model Factory Nano hexagonal boron nitride Purity ≥ 99.9% Shanghai Maikelin Biotechnology Co., Ltd. Zirconium phosphate Purity ≥ 99.0% Wuhan Lalanbai Pharmaceutical Chemical Co., Ltd. Methyl etherified melamine resin 303-80 type Jiyang Sanjian Chemical Co., Ltd. Butylated melamine resin 582-2 type Shanghai Xinhua Resin Factory Escherichia coli ATCC25922 Beijing Biological Preservation Center Phosphoric acid 85.0% aqueous solution Hunan Huihong Reagent Co., Ltd. Pentaerythritol Analytically pure Shandong Yuxia Chemical Industry Co., Ltd. Anhydrous ethanol Purity ≥ 99.7% Tianjin Hengxing Chemical Reagent Manufacturing Co., Ltd. n-Butanol Analytically pure Taicang Hu Reagent Co., Ltd. Boric acid Analytically pure Hunan Huihong Reagent Co., Ltd. Polyethylene glycol 200 Purity ≥ 99.0% Shandong Yousuo Chemical Technology Co., Ltd. Sodium hydroxide Purity ≥ 96.0% Xilong Scientific Co., Ltd. Silane coupling agent 550 Analytically pure Kangjin New Material Technology Co., Ltd. Ethylamine 68.0-72.0% aqueous solution Shanghai Maikelin Biotechnology Co., Ltd.

[0067] Example 1

[0068] This embodiment provides a method for preparing an antibacterial and weather-resistant nano-transparent fireproof coating. The nano-transparent fireproof coating is mainly composed of layered nano-composite flexible phosphate ester and amino resin. Specifically, the layered nano-composite flexible phosphate ester is a modified boron nitride composite phosphate ester obtained by grafting modified boron nitride onto the flexible phosphate ester, and the amino resin is methyl etherified melamine resin.

[0069] The preparation method specifically includes the following steps:

[0070] (I) Preparation of modified boron nitride

[0071] P1. Add 5g of hexagonal boron nitride and 5mol / L sodium hydroxide ethanol solution to a three-necked flask in sequence, mix and react at 76℃ for 12h, then filter, wash and dry the product at 60℃ for 8h to obtain hydroxylated boron nitride.

[0072] P2. Add 100 mL of 95% ethanol, 10 mL of deionized water and 1 g of silane coupling agent KH550 to a three-necked flask in sequence, and mix and react at 25 °C for 10 min to obtain a mixture.

[0073] P3. Mix the mixture obtained in step P2 with the hydroxylated boron nitride obtained in step P1, stir in a water bath at 70°C for 10 hours, filter and wash the product, and dry it at 60°C for 8 hours to obtain KH550 modified boron nitride.

[0074] like Figure 1 As shown, hydroxylated boron nitride at 2426 cm⁻¹ -1 The absorption peaks between the two peaks are significantly broadened and enhanced, with modified boron nitride showing a peak at 2860 cm⁻¹. -1 and 2930cm -1The appearance of -CH3, -CH2 characteristic peaks indicates that KH550 is successfully grafted onto the hydroxylated boron nitride, and the modification of boron nitride is successful.

[0075] (II) Preparation of modified boron nitride grafted flexible phosphate

[0076] (1) Preparation of flexible phosphate

[0077] C1, polyethylene glycol and boric acid are added in the order of 2.8:1.0 molar ratio, stirred at 130℃ for 3h, and condensed under reflux to obtain polyethylene glycol borate;

[0078] C2, phosphoric acid, pentaerythritol and n-butanol are added in the order of 3:0.85:0.5 molar ratio, mixed at 105℃ for 4h, mixed at 120℃ for 2h, and condensed under reflux to obtain acid phosphate;

[0079] C3, the polyethylene glycol borate prepared in step C1 and the acid phosphate prepared in step C2 are added in the order of 15:85 mass ratio, mixed at 50℃ for 1h, then heated to 115℃ for 4h, and distilled under reduced pressure to obtain flexible phosphate.

[0080] (2) Modified boron nitride grafted flexible phosphate

[0081] The flexible phosphate prepared in step (1) and the modified boron nitride prepared in step (I) are uniformly mixed, ultrasonically dispersed in an ultrasonic disperser at 50℃ for 30min, and then placed in a three-necked flask for 4h at 120℃ to obtain modified boron nitride grafted flexible phosphate. The mass percentage of modified boron nitride in modified boron nitride grafted flexible phosphate is 1.5%.

[0082] As shown in Figure 3 , the P-O-C group in modified boron nitride grafted flexible phosphate moves from 972cm -1 to 965cm -1 , and at the same time, the P-OH absorption peak in modified boron nitride grafted flexible phosphate is weakened, indicating that the amino group in modified boron nitride reacts with P-OH in flexible phosphate, and modified boron nitride is successfully grafted onto the molecular chain of flexible phosphate.

[0083] (III) Preparation of nano transparent fireproof coating

[0084] The modified boron nitride grafted flexible phosphate prepared in step (II) is prepared into a 60% mass percentage modified boron nitride grafted flexible phosphate ethanol solution to obtain component one;

[0085] The methoxylated melamine resin is prepared into a 60% mass percentage methoxylated melamine resin aqueous solution to obtain component two;

[0086] The two solutions of component one and component two are blended and stirred uniformly according to a mass ratio of 1:1.2, and the anti-bacterial and weather-resistant nano transparent fireproof coating is obtained.

[0087] Example 2

[0088] The embodiment provides a preparation method of an antibacterial and weather-resistant nano transparent fireproof coating, and the specific steps are as follows:

[0089] (I) Preparation of modified boron nitride

[0090] P1, 3.5g of hexagonal boron nitride and 4mol / L sodium hydroxide ethanol solution are sequentially added into a three-necked flask, mixed and reacted at 70℃ for 12h, then the product is extracted, filtered, washed to neutral, and dried at 50℃ for 10h to obtain hydroxylated boron nitride;

[0091] P2, 100mL of 95% ethanol, 10mL of deionized water and 1.5g of silane coupling agent KH550 are sequentially added into a three-necked flask, mixed and reacted at 30℃ for 5min to obtain a mixed solution;

[0092] P3, the mixed solution prepared in step P2 and the hydroxylated boron nitride prepared in step P1 are mixed, stirred in a water bath at 80℃ for 8h, the product is filtered, washed, and dried at 80℃ for 7h to obtain KH550 modified boron nitride.

[0093] (II) Preparation of modified boron nitride grafted with flexible phosphate

[0094] (1) Preparation of flexible phosphate

[0095] C1, polyethylene glycol and boric acid are sequentially added and mixed according to a molar ratio of 3.0:1.1, mixed and reacted at 140℃ for 2h under stirring and condensation reflux to obtain polyethylene glycol borate;

[0096] C2, phosphoric acid, pentaerythritol and n-butanol are sequentially added and mixed according to a molar ratio of 2.5:0.5:0.3, mixed and reacted at 100℃ for 5h, mixed and reacted at 150℃ for 1h, and condensed and refluxed to obtain an acid phosphate ester;

[0097] C3, the polyethylene glycol borate prepared in step C1 and the acid phosphate ester prepared in step C2 are sequentially added according to a mass ratio of 10:80, mixed and reacted at 60℃ for 0.5h, then the temperature is increased to 110℃ for mixing and reaction for 5h, and the flexible phosphate ester is obtained by reduced pressure distillation.

[0098] (2) Modified boron nitride grafted with flexible phosphate

[0099] The flexible phosphate prepared in step (1) is uniformly mixed with the modified boron nitride prepared in step (1), ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixed reaction at 120°C for 4 h to obtain the modified boron nitride grafted flexible phosphate. The mass percentage of the modified boron nitride in the modified boron nitride grafted flexible phosphate is 2%.

[0100] (Three) Preparation of the nano transparent fireproof coating

[0101] The modified boron nitride grafted flexible phosphate prepared in step (two) is formulated into a 50% (mass percentage) modified boron nitride grafted flexible phosphate ethanol solution to obtain component one.

[0102] The methoxylated melamine resin is formulated into a 50% (mass percentage) methoxylated melamine resin aqueous solution to obtain component two.

[0103] The two solutions of component one and component two are uniformly blended and stirred according to a mass ratio of 1:1 to obtain the nano transparent fireproof coating.

[0104] Example 3

[0105] The present example provides a preparation method of an antibacterial and weather-resistant nano transparent fireproof coating, and the specific steps are as follows:

[0106] (One) Preparation of modified boron nitride

[0107] P1, 5.5 g of hexagonal boron nitride and 6 mol / L sodium hydroxide ethanol solution are sequentially added to a three-necked flask, mixed and reacted at 80°C for 12 h, then the product is suction filtered, washed to neutral, and dried at 80°C for 7 h to obtain hydroxylated boron nitride.

[0108] P2, 100 mL of 95% (volume fraction) ethanol, 10 mL of deionized water, and 0.5 g of silane coupling agent KH550 are sequentially added to a three-necked flask, mixed and reacted at 20°C for 15 min to obtain a mixed solution.

[0109] P3, the mixed solution prepared in step P2 and the hydroxylated boron nitride prepared in step P1 are mixed, stirred in a water bath at 60°C for 12 h, the product is filtered and washed, and dried at 50°C for 10 h to obtain KH550 modified boron nitride.

[0110] (Two) Preparation of modified boron nitride grafted flexible phosphate

[0111] (1) Preparation of flexible phosphate

[0112] C1, polyethylene glycol and boric acid are sequentially added to a three-necked flask according to a molar ratio of 2:1, mixed and reacted at 120°C for 4 h under stirring, and condensed to obtain polyethylene glycol borate.

[0113] C2. Phosphoric acid, pentaerythritol and n-butanol were added sequentially in a molar ratio of 3:0.7:0.4 and mixed. The mixture was reacted at 120°C for 3 hours. The mixture was then refluxed to obtain an acidic phosphate ester.

[0114] C3. The polyethylene glycol borate ester obtained in step C1 and the acidic phosphate ester obtained in step C2 are added sequentially at a mass ratio of 12:83. The mixture is reacted at 40°C for 1.5 hours, then heated to 120°C and reacted for 3 hours. The mixture is then distilled under reduced pressure to obtain the flexible phosphate ester.

[0115] (2) Modified boron nitride grafted flexible phosphate ester

[0116] The flexible phosphate ester prepared in step (1) was uniformly mixed with the modified boron nitride obtained in step (i), and ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min. Then, the mixture was placed in a three-necked flask and reacted at 120°C for 4 h to obtain the modified boron nitride-grafted flexible phosphate ester. The modified boron nitride accounted for 0.5% of the mass of the modified boron nitride-grafted flexible phosphate ester.

[0117] (III) Preparation of Nano-Transparent Fire-Retardant Coatings

[0118] The modified boron nitride-grafted flexible phosphate ester obtained in step (II) is prepared into an ethanol solution of modified boron nitride-grafted flexible phosphate ester with a mass percentage of 80%, to obtain component one.

[0119] The methylated melamine resin was prepared into an aqueous solution of methylated melamine resin with a mass percentage of 80%, to obtain component two;

[0120] The solution of component one and component two are mixed and stirred evenly at a mass ratio of 1:2 to obtain the final product.

[0121] Example 4

[0122] This embodiment provides a method for preparing an antibacterial and weather-resistant nano-transparent fire-retardant coating, which specifically includes the following steps:

[0123] (I) Preparation of modified zirconium phosphate

[0124] 2g of zirconium α-phosphate, 131.84g of ethanol and 32.84g of deionized water were mixed evenly and ultrasonically dispersed in an ultrasonic disperser for 30 min at room temperature. Then, 1.07g of ethylamine was added and ultrasonically dispersed in an ultrasonic disperser for 1 h at room temperature. Then, 0.5g of silane coupling agent was added and ultrasonically dispersed in an ultrasonic disperser for 4 h at room temperature. The product was filtered, washed and dried at 60℃ for 8 h to obtain KH550 modified boron nitride.

[0125] like Figure 2 As shown, the modified zirconium phosphate at 3558 cm⁻¹ -1The absorption peak disappears at 2800-2900 cm⁻¹. -1 A characteristic CH2 peak appears between the two peaks, at 1536 cm⁻¹. -1 The presence of N-H characteristic peaks indicates that ethylamine small molecules have intercalated into zirconium phosphate, and KH550 has been successfully grafted onto zirconium phosphate, indicating successful modification of zirconium phosphate.

[0126] (II) Preparation of modified zirconium phosphate grafted flexible phosphate ester

[0127] (1) Preparation of flexible phosphate ester

[0128] The preparation of the flexible phosphate ester is the same as in Example 1.

[0129] (2) Modified zirconium phosphate grafted flexible phosphate ester

[0130] The flexible phosphate ester prepared in step (1) was uniformly mixed with the modified zirconium phosphate obtained in step (i), and ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min. Then, the mixture was placed in a three-necked flask and reacted at 120°C for 4 h to obtain the modified zirconium phosphate composite phosphate ester. The modified zirconium phosphate accounted for 2% of the mass of the modified zirconium phosphate grafted flexible phosphate ester.

[0131] like Figure 4 As shown, the POC groups in the modified zirconium phosphate grafted flexible phosphate ester are 972 cm⁻¹ -1 Moved to 964cm -1 Meanwhile, the absorption peak of P-OH in the modified zirconium phosphate grafted onto the flexible phosphate ester was weakened, indicating that the amino group in the modified zirconium phosphate reacted with the P-OH group in the flexible phosphate ester, and the modified zirconium phosphate was successfully grafted onto the flexible phosphate ester molecular chain.

[0132] (III) Preparation of Nano-Transparent Fire-Retardant Coatings

[0133] The modified zirconium phosphate grafted flexible phosphate ester obtained in step (II) is prepared into an ethanol solution of modified zirconium phosphate grafted flexible phosphate ester with a mass percentage of 60%, to obtain component one.

[0134] The methylated melamine resin was prepared into an aqueous solution of 60% methylated melamine resin to obtain component two.

[0135] Mix the solutions of component one and component two at a mass ratio of 1:1.2 until homogeneous to obtain the final product.

[0136] Example 5

[0137] This embodiment provides a method for preparing an antibacterial and weather-resistant nano-transparent fire-retardant coating, which specifically includes the following steps:

[0138] (I) Preparation of modified zirconium phosphate

[0139] Mixing 1 g of zirconium phosphate, 130 g of ethanol and 30 g of deionized water uniformly, ultrasonic dispersion in ultrasonic dispersion instrument at room temperature for 30 min, then adding 1 g of ethylamine, ultrasonic dispersion in ultrasonic dispersion instrument at room temperature for 0.5 h, then adding 0.4 g of silane coupling agent, ultrasonic dispersion in ultrasonic dispersion instrument at room temperature for 3 h, filtering, washing and drying at 50℃ for 10 h to obtain KH550 modified boron nitride.

[0140] (II) Preparation of modified zirconium phosphate grafted flexible phosphate ester

[0141] (I) Preparation of flexible phosphate ester

[0142] The preparation of flexible phosphate ester is the same as that of Example 2.

[0143] (II) Modified zirconium phosphate grafted flexible phosphate ester

[0144] Mixing the flexible phosphate ester prepared in step (I) and the modified zirconium phosphate prepared in step (I) uniformly, ultrasonic dispersion in ultrasonic dispersion instrument at 50℃ for 30 min, then placing in a three-necked flask and mixing at 120℃ for 4 h to obtain modified zirconium phosphate composite phosphate ester. The mass percentage of modified zirconium phosphate in the modified zirconium phosphate grafted flexible phosphate ester is 3%.

[0145] (III) Preparation of nano transparent fireproof coating

[0146] Preparing the modified zirconium phosphate grafted flexible phosphate ester prepared in step (II) into a 50% mass percentage modified zirconium phosphate grafted flexible phosphate ester ethanol solution to obtain component one.

[0147] Preparing the methoxylated melamine resin into a 50% mass percentage methoxylated melamine resin aqueous solution to obtain component two.

[0148] Blending and stirring the two solutions of component one and component two uniformly according to a mass ratio of 1:1 to obtain the nano transparent fireproof coating.

[0149] Example 6

[0150] The present example provides a preparation method of an antibacterial and weather-resistant nano transparent fireproof coating, which specifically comprises the following steps:

[0151] (I) Preparation of modified zirconium phosphate

[0152] Mixing 3 g of zirconium phosphate, 135 g of ethanol and 35 g of deionized water uniformly, ultrasonic dispersion in ultrasonic dispersion instrument at room temperature for 30 min, then adding 1.5 g of ethylamine, ultrasonic dispersion in ultrasonic dispersion instrument at room temperature for 1.5 h, then adding 1 g of silane coupling agent, ultrasonic dispersion in ultrasonic dispersion instrument at room temperature for 5 h, filtering, washing and drying at 80℃ for 10 h to obtain KH550 modified boron nitride.

[0153] (II) Preparation of modified zirconium phosphate grafted flexible phosphate ester

[0154] (1) Preparation of flexible phosphate ester

[0155] The preparation of flexible phosphate ester is the same as Example 3.

[0156] (2) Modified zirconium phosphate grafted flexible phosphate ester

[0157] The flexible phosphate ester prepared in step (1) is uniformly mixed with the modified zirconium phosphate prepared in step (I), and ultrasonic dispersion is carried out in an ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixed reaction at 120°C for 4 h to obtain modified zirconium phosphate composite phosphate ester. The mass percentage of modified zirconium phosphate in the modified zirconium phosphate grafted flexible phosphate ester is 0.5%.

[0158] (III) Preparation of nano transparent fireproof coating

[0159] An ethanol solution of the modified zirconium phosphate grafted flexible phosphate ester prepared in step (II) is prepared with a mass percentage of 80% to obtain component one;

[0160] An aqueous solution of methoxylated melamine resin is prepared with a mass percentage of 80% to obtain component two;

[0161] The two solutions of component one and component two are uniformly blended and stirred according to a mass ratio of 1:2 to obtain the transparent fireproof coating.

[0162] Comparative Example 1

[0163] The main difference between this example and Examples 1-6 is that the transparent fireproof coating prepared in this example does not contain any modified layered nanofiller, and the specific preparation method is as follows:

[0164] (1) Preparation of flexible phosphate ester

[0165] The preparation of flexible phosphate ester is the same as Example 1.

[0166] (2) Preparation of transparent fireproof coating

[0167] An ethanol solution of the flexible phosphate ester prepared in step (1) is prepared with a mass percentage of 60% to obtain component one; an aqueous solution of methoxylated melamine resin is prepared with a mass percentage of 60% to obtain component two; and the two solutions of component one and component two are uniformly blended and stirred according to a mass ratio of 1:1.2 to obtain the transparent fireproof coating.

[0168] Comparative Example 2

[0169] The main difference between this example and Example 1 is that the layered nanofiller used is unmodified boron nitride, and the specific steps are as follows:

[0170] (1) Preparation of flexible phosphate ester

[0171] The preparation of flexible phosphate ester is the same as that of Example 1.

[0172] (2) Boron nitride grafted flexible phosphate ester

[0173] The flexible phosphate ester prepared in step (1) is uniformly mixed with unmodified boron nitride, ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixing reaction at 120°C for 4 h to obtain boron nitride grafted flexible phosphate ester. The mass percentage of boron nitride in the boron nitride grafted flexible phosphate ester is 1.5%.

[0174] (3) Preparation of nano transparent fireproof coating

[0175] The boron nitride grafted flexible phosphate ester prepared in step (2) is formulated into an ethanol solution of boron nitride grafted flexible phosphate ester with a mass percentage of 60% to obtain component one; methoxylated melamine resin is formulated into an aqueous solution of methoxylated melamine resin with a mass percentage of 60% to obtain component two;

[0176] The two solutions of component one and component two are uniformly blended and stirred according to a mass ratio of 1:1.2 to obtain the nano transparent fireproof coating.

[0177] Comparative Example 3

[0178] The main difference from Example 4 is that the layered nanofiller used is unmodified zirconium phosphate, and the specific steps are as follows:

[0179] (1) Preparation of flexible phosphate ester

[0180] The preparation of flexible phosphate ester is the same as that of Example 2.

[0181] (2) Zirconium phosphate grafted flexible phosphate ester

[0182] The flexible phosphate ester prepared in step (1) is uniformly mixed with unmodified zirconium phosphate, ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixing reaction at 120°C for 4 h to obtain zirconium phosphate grafted flexible phosphate ester. The mass percentage of zirconium phosphate in the zirconium phosphate grafted flexible phosphate ester is 2%.

[0183] (3) Preparation of nano transparent fireproof coating

[0184] The zirconium phosphate grafted flexible phosphate ester prepared in step (2) is formulated into an ethanol solution of zirconium phosphate grafted flexible phosphate ester with a mass percentage of 60% to obtain component one; methoxylated melamine resin is formulated into an aqueous solution of methoxylated melamine resin with a mass percentage of 60% to obtain component two;

[0185] The two solutions of component one and component two are blended and stirred uniformly according to a mass ratio of 1:1.2, and the mixture is obtained.

[0186] Comparative Example 4

[0187] The main difference from Example 1 is that the layered nanofiller used is modified kaolin, and the specific steps are as follows:

[0188] (I) Preparation of modified kaolin

[0189] G1, 40 mL of dimethyl sulfoxide and 4.5 mL of deionized water were mixed and stirred for 15 min to prepare a dimethyl sulfoxide solution;

[0190] G2, then, the dimethyl sulfoxide solution prepared in step G1 and 4 g of kaolin were sequentially added to a three-necked flask, stirred in an oil bath at 60°C for 24 h, the product was filtered, washed, and dried at 50-80°C for 8 h to obtain kaolin-dimethyl sulfoxide;

[0191] G3, 44 g of potassium acetate and 16 g of deionized water were mixed and stirred for 15 min to prepare a potassium acetate solution;

[0192] G4, the potassium acetate solution prepared in step G3 and 3 g of kaolin-dimethyl sulfoxide prepared in step G2 were sequentially added to a three-necked flask, stirred in an oil bath at 60°C for 24 h, the product was filtered, washed, and dried at 60°C for 8 h to obtain kaolin-potassium acetate.

[0193] (II) Preparation of modified kaolin grafted with flexible phosphate

[0194] (1) Preparation of flexible phosphate

[0195] The preparation of flexible phosphate is the same as that of Example 1.

[0196] (2) Modified kaolin grafted with flexible phosphate

[0197] The flexible phosphate prepared in step (1) and the modified kaolin prepared in step (I) were uniformly mixed, ultrasonically dispersed in a ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixed reaction at 120°C for 4 h to obtain modified kaolin grafted with flexible phosphate. The mass percentage of modified kaolin in the modified kaolin grafted with flexible phosphate is 2%.

[0198] (III) Preparation of nano transparent fireproof coating

[0199] The modified kaolin grafted with flexible phosphate prepared in step (II) was prepared into a modified kaolin grafted with flexible phosphate ethanol solution with a mass percentage of 60% to obtain component one;

[0200] The methoxylated melamine resin is prepared into a 60% by mass methoxylated melamine resin aqueous solution to obtain component two.

[0201] The two solutions of component one and component two are blended and stirred uniformly at a mass ratio of 1:1.2 to obtain the product.

[0202] Comparative Example 5

[0203] The difference from Example 1 is that the layered nanofiller used is unmodified kaolin, and the specific steps are as follows:

[0204] (1) Preparation of flexible phosphate ester

[0205] The preparation of the flexible phosphate ester is the same as in Example 1.

[0206] (2) Grafting of flexible phosphate ester onto kaolin

[0207] The flexible phosphate ester prepared in step (1) is uniformly mixed with unmodified kaolin, ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixed reaction at 120°C for 4 h to obtain the kaolin grafted flexible phosphate ester. The mass percentage of kaolin in the kaolin grafted flexible phosphate ester is 2%.

[0208] (3) Preparation of nano transparent fireproof coating

[0209] The kaolin grafted flexible phosphate ester prepared in step (2) is prepared into a 60% by mass kaolin grafted flexible phosphate ester ethanol solution to obtain component one; the methoxylated melamine resin is prepared into a 60% by mass methoxylated melamine resin aqueous solution to obtain component two.

[0210] The two solutions of component one and component two are blended and stirred uniformly at a mass ratio of 1:1.2 to obtain the product.

[0211] Comparative Example 6

[0212] The difference from Example 5 is that the layered nanofiller used is unmodified boron nitride, and the specific steps are as follows:

[0213] (1) Preparation of flexible phosphate ester

[0214] The preparation of the flexible phosphate ester is the same as in Example 1.

[0215] (2) Grafting of flexible phosphate ester onto boron nitride

[0216] The flexible phosphate ester prepared in step (1) is uniformly mixed with unmodified boron nitride, ultrasonically dispersed in an ultrasonic disperser at 50°C for 30 min, and then placed in a three-necked flask for mixed reaction at 120°C for 4 h to obtain the boron nitride grafted flexible phosphate ester. The mass percentage of boron nitride in the boron nitride grafted flexible phosphate ester is 2%.

[0217] (3) Preparation of nano transparent fireproof coating

[0218] The boron nitride grafted flexible phosphate prepared in step (2) is mixed with ethanol to form a 60% by mass of boron nitride grafted flexible phosphate ethanol solution, to obtain component one; the methoxylated melamine resin is mixed with water to form a 60% by mass of methoxylated melamine resin aqueous solution, to obtain component two;

[0219] The two solutions of component one and component two are mixed and stirred uniformly at a mass ratio of 1:1.2, to obtain the nano transparent fireproof coating.

[0220] II. Performance characterization of transparent fireproof coating

[0221] The flame retardant, smoke suppression, carbon formation, antibacterial, and weather resistance of the transparent fireproof coating prepared in Examples 1-5 and Comparative Examples 1-6 are determined by GB / T 2410-2008 “Determination of Light Transmittance and Haze of Transparent Plastics”, GB 12441-2018 “Decorative Fireproof Coating”, GB / T 15442.3-1995 “Classification and Test Method for Fire Resistance of Decorative Fireproof Coating Tunnel Combustion Method”, GB / T 8626-2007 “Smoke Density Test Method for Combustion or Decomposition of Building Materials”, GB / T 33568-2017 “Aging Grade and Evaluation Method for Wood Coated Surface”, GB / T 21866-2008 “Determination of Antibacterial Property of Antibacterial Coatings (Paint Film) and Antibacterial Effect”, and GB / T 1720-2020 “Paint Film Scratch Test”, and the results are shown in Tables 2 and 3 below.

[0222] Table 2 Comparison of performance test results of nano transparent fireproof coating materials of each example

[0223]

[0224] Table 3 Comparison of performance test results of nano transparent fireproof coating materials of each comparative example

[0225]

[0226] Based on the test results of Examples 1-6 and Comparative Examples 1-6 and Tables 2 and 3, the results are analyzed as follows:

[0227] Based on Examples 1-6 and Comparative Example 1, it is known that the transparent fireproof coating containing modified layered nanoparticles can effectively improve the flame retardant and fireproof performance, antibacterial and aging resistance of the material.

[0228] Based on Examples 1-6 and Comparative Examples 2-3 and Comparative Example 6, it is known that the modified layered nano transparent fireproof coating has more excellent light transmittance, flame retardant, antibacterial, and aging resistance, and the comprehensive performance is significantly improved.

[0229] It can be seen from the embodiments 1-6 and the comparative examples 2-6 that the exfoliation treatment of the layered nanofiller can significantly improve the light transmittance, fireproofing, heat insulation, flame retardation, smoke suppression, antibacterial and aging resistance of the layered nanocoating.

[0230] It can be seen from the embodiments 1-6 and the comparative example 4 that the transparent fireproofing coating using the exfoliated boron nitride and zirconium phosphate has more excellent performance compared to the transparent fireproofing coating containing the exfoliated kaolin.

[0231] Therefore, the nanometer transparent fireproofing material can ensure excellent flame retardation and decoration of the material, and enhance the antibacterial and aging resistance of the coating.

[0232] The above merely provides some preferred embodiments of the present application, but should not be used to limit the present application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A method for preparing an antibacterial, weather-resistant, nano-transparent fire-retardant coating, characterized in that, Specifically, the steps include the following: (1) A layered nanocomposite flexible phosphate ester is prepared by grafting modified layered nanofillers onto flexible phosphate ester. Specifically, the modified layered nanofillers and flexible phosphate ester are mixed and stirred evenly, ultrasonically dispersed at 40-60℃ for 0.5-1.5h, and then mixed and reacted at 120-140℃ for 3-5h. The modified layered nanofillers account for 0.5-3wt% of the total mass of the prepared layered nanocomposite flexible phosphate ester. The modified layered nanofiller is KH550 modified boron nitride, which is prepared by the following method: P1. 3.5-5.5g of hexagonal boron nitride and 200mL of sodium hydroxide ethanol solution with a concentration of 4-6mol / L were added sequentially and reacted at 70-80℃ for 12h. Then, the product was filtered, washed until neutral, and dried at 50-80℃ for 7-10h to obtain hydroxylated boron nitride. P2. Add 100 mL of 95% ethanol, 10 mL of deionized water and 0.5-1.5 g of silane coupling agent KH550 in sequence, and mix and react at 20-30℃ for 5-15 min to obtain a mixed solution. P3. Mix the mixture obtained in step P2 with the hydroxylated boron nitride obtained in step P1, stir in a water bath at 60-80℃ for 8-12 hours, filter and wash the product, and dry at 50-80℃ for 7-10 hours to obtain KH550 modified boron nitride. The flexible phosphate ester is prepared by mixing and reacting polyethylene glycol borate and acid phosphate ester in a preset ratio. (2) Prepare a 50-80 wt% ethanol solution of the layered nanofiller composite flexible phosphate ester obtained in step (1) as component one; prepare a 50-80 wt% aqueous solution of amino resin as component two, wherein the amino resin is one of methyl etherified melamine resin and butylated melamine resin; then mix and stir the components one and two at a mass ratio of 1:1-2 to obtain the antibacterial and weather-resistant nano transparent fireproof coating.

2. The preparation method of the antibacterial and weather-resistant nano-transparent fire-retardant coating according to claim 1, characterized in that, The modified layered nanofiller in step (1) is KH550 modified zirconium phosphate, which is prepared by the following method: Mix 1-3g of α-zirconium phosphate, 130-135g of ethanol and 30-35g of deionized water evenly and disperse ultrasonically at room temperature for 30min; then add 1-1.5g of ethylamine and disperse ultrasonically at room temperature for 0.5-1.5h; then add 0.4-1g of silane coupling agent KH550 and disperse ultrasonically at room temperature for 3-5h. Filter and wash the product and dry it at 50-80℃ for 7-10h to obtain KH550 modified zirconium phosphate.

3. The preparation method of the antibacterial and weather-resistant nano-transparent fire-retardant coating according to claim 1 or 2, characterized in that, The preparation method of the flexible phosphate ester specifically includes the following steps: C1. Polyethylene glycol and boric acid are added sequentially in a molar ratio of 2.0-3.0:1.0-1.1 and mixed. Under stirring, the mixture is reacted at 120-140℃ for 2-4 hours, and then refluxed to obtain polyethylene glycol borate. C2. Phosphoric acid, pentaerythritol and n-butanol are added sequentially in a molar ratio of 2.5-3:0.5-1:0.3-0.5 and mixed. The mixture is reacted at 100-120℃ for 3-5 hours and at 120-150℃ for 1-3 hours. The mixture is then refluxed to obtain acidic phosphate ester. C3. The polyethylene glycol borate ester obtained in step C1 and the acidic phosphate ester obtained in step C2 are added sequentially at a mass ratio of 10-15:80-85. The mixture is reacted at 40-60℃ for 0.5-1.5h, and then the temperature is raised to 110-120℃ for 3-5h. The mixture is then distilled under reduced pressure to obtain the flexible phosphate ester.

4. The antibacterial, weather-resistant, nano-transparent fire-retardant coating prepared by the method of claim 1, characterized in that, The nano-transparent fireproof coating is mainly composed of component one and component two in a mass ratio of 1:1-2; Component one is an ethanol solution of layered nanocomposite flexible phosphate ester, which is prepared by grafting modified layered nanofiller onto flexible phosphate ester. The modified layered nanofiller accounts for 0.5-3 wt% of the mass of the layered nanocomposite flexible phosphate ester. The modified layered nanofiller is modified boron nitride. Component two is an aqueous solution of an amino resin.

5. The antibacterial, weather-resistant, nano-transparent fire-retardant coating prepared by the method of claim 2, characterized in that, The nano-transparent fireproof coating is mainly composed of component one and component two in a mass ratio of 1:1-2; Component one is an ethanol solution of layered nanocomposite flexible phosphate ester, which is prepared by grafting modified layered nanofiller onto flexible phosphate ester. The modified layered nanofiller accounts for 0.5-3 wt% of the mass of the layered nanocomposite flexible phosphate ester. The modified layered nanofiller is modified zirconium phosphate. Component two is an aqueous solution of an amino resin.

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