High-temperature-resistant white latex material and preparation method thereof

Abstract

The invention discloses a high-temperature-resistant white latex material and a preparation method thereof, and belongs to the technical field of high polymer materials. The preparation method comprises the following steps: uniformly mixing a modified polyvinyl acetate emulsion, a flame retardant, modified sepiolite, modified basalt fibers, zinc oxide, castor oil, ammonium persulfate and deionized water, carrying out ultrasonic dispersion for 15-20 minutes, then stirring for 20-30 minutes at 60-80 DEG C, carrying out heat preservation, and discharging to obtain the high-temperature-resistant white latex material. Siloxane bonds have good thermal stability, N-hydroxymethyl acrylamide can greatly improve high-temperature creep resistance and thermal strength by means of covalent bond crosslinking, and the synergistic effect of the siloxane bonds and the N-hydroxymethyl acrylamide can significantly enhance the high-temperature resistance of the white latex material; a triazine ring in the flame retardant has relatively high thermal stability, and an imine bond and an adjacent benzene ring can form a conjugated system, so that the high temperature resistance of the white latex material is enhanced; the sepiolite and the basalt fiber form a stable three-dimensional network through the coupling agent and the modified polyvinyl acetate emulsion, so that the high-temperature resistance of the white latex material is further improved.

Description

Technical Field

[0001] This invention belongs to the field of polymer materials technology, and more specifically, relates to a high-temperature resistant white latex material and its preparation method. Background Technology

[0002] White glue, due to its non-toxic and harmless properties, good initial tack, and ease of use, is widely used in wood processing, building decoration, and handicraft manufacturing. However, in high-temperature environments during summer or near certain heat-generating devices, the adhesive layer of traditional white glue is prone to softening, leading to problems such as joint failure and delamination. This severely limits its application in situations requiring a certain level of heat resistance. Therefore, avoiding this phenomenon is key to solving the problem, and developing a white glue material that is simple to process, stable in storage, and possesses significant high-temperature resistance has become an important research topic. For example, patent application CN114410159A discloses a bio-based modified construction coating white glue and its preparation method. This invention's bio-based modified construction coating white glue has excellent film-forming properties, strong adhesive strength, and a wide range of applications, but its high-temperature resistance needs further improvement. Summary of the Invention

[0003] Technical problems to be solved To address the shortcomings of existing technologies, this invention provides a high-temperature resistant white latex material and its preparation method. The white latex material prepared by this invention has excellent high-temperature resistance.

[0004] Technical solution

[0005] To solve the above problems, the technical solution adopted by the present invention is as follows: The present invention discloses a method for preparing a high-temperature resistant white latex material, which includes the following steps: (1) Preparation of modified polyvinyl acetate emulsion; (2) Preparation of flame retardants; (3) Mix the modified polyvinyl acetate emulsion, flame retardant, modified sepiolite, modified basalt fiber, zinc oxide, castor oil, ammonium persulfate and deionized water evenly, ultrasonically disperse for 15-20 min, then stir at 60-80℃ for 20-30 min, keep warm, and discharge to obtain a high-temperature resistant white latex material.

[0006] Further, the preparation method of the modified polyvinyl acetate emulsion in step (1) is as follows: 4.3-4.4g of polyvinyl alcohol and 48-50g of deionized water are added to the reactor and stirred and dissolved at 90-95℃ for 1-2h. Then the temperature is lowered to 60-65℃, and 0.6-0.7g of surfactant, 3.5-3.6g of vinyl acetate, 0.04-0.05g of ammonium persulfate, and 0.15-0.18g of sodium acetate are added. The mixture is stirred evenly, and the temperature is raised to 80-90℃. After the reflux stops, the main reactants are added dropwise at the same time for 4-4.5h. The reaction temperature is maintained at 76-80℃. After the dropwise addition is completed, the temperature is kept for 1-1.5h. After cooling, 0.12-0.15g of sodium acetate is added to adjust the pH to neutral. The product is discharged to obtain the modified polyvinyl acetate emulsion.

[0007] Furthermore, the method for preparing the flame retardant in step (2) is as follows: S1: Add vanillin and anhydrous sodium carbonate to acetone solvent, stir and mix, then add cyanuric chloride, react at 80-100℃ for 6-10h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 50-60℃ for 22-26h to obtain intermediate 1. S2: Under nitrogen protection, intermediate 1, 1-(3-aminopropyl)imidazolium is added to N,N-dimethylformamide solvent, stirred evenly, and reacted at 50-60℃ for 5-8 hours. After the reaction is completed, the mixture is filtered, washed and dried, and purified to obtain the flame retardant.

[0008] Further, the modified sepiolite in step (3) is prepared by adding 20-25 mL of deionized water, 30-35 mL of anhydrous ethanol, and 5.02-5.06 g of sepiolite to a reactor, ultrasonically treating it for 10-15 min, then adding 2.13-2.17 g of γ-aminopropyltriethoxysilane dropwise, and reacting at 75-85 °C for 4-6 h. After the reaction is completed, the mixture is washed and dried to obtain the modified sepiolite.

[0009] Further, the preparation method of the modified basalt fiber in step (3) is as follows: First, place 2.34-2.38g of basalt fiber in 28-30mL of acetone solution and ultrasonically wash for 10-15min. Then, add 20-25mL of deionized water, 30-35mL of anhydrous ethanol, and ultrasonically washed basalt fiber to the reactor. Add 1.12-1.16g of γ-aminopropyltriethoxysilane dropwise to it. React at 35-45℃ for 8-12h. After the reaction is completed, wash and dry in an oven at 110-120℃ for 1-2h to obtain modified basalt fiber.

[0010] Furthermore, the main reactants consist of two parts: the first part is a mixed monomer obtained by uniformly mixing 8-10g of vinyl acetate, 0.1-0.15g of diallyl phthalate and 0.3-0.5g of vinyltrimethoxysilane; the second part is an aqueous solution obtained by dissolving 0.08-0.1g of ammonium persulfate and 0.6-0.8g of N-hydroxymethylacrylamide in 5-6g of deionized water.

[0011] Furthermore, the ratio of acetone, vanillin, anhydrous sodium carbonate, and cyanuric chloride in S1 is 40-50 mL: 10.64-10.68 g: 7.62-7.66 g: 3.68-3.72 g.

[0012] Furthermore, the ratio of N,N-dimethylformamide, intermediate 1, and 1-(3-aminopropyl)imidazole in S2 is 35-45 mL: 5.32-5.36 g: 3.75-3.8 g.

[0013] Further, the weight parts of each component in step (3) are as follows: 40-50 parts of modified polyvinyl acetate emulsion, 3-5 parts of flame retardant, 2-3 parts of modified sepiolite, 1-2 parts of modified basalt fiber, 0.5-0.8 parts of zinc oxide, 1-1.5 parts of castor oil, 0.3-0.5 parts of ammonium persulfate, and 10-12 parts of deionized water.

[0014] This invention also protects a high-temperature resistant white latex material, which is prepared by any of the preparation methods described above.

[0015] Beneficial technical effects Compared with the prior art, the beneficial effects of the present invention are as follows: (1) By copolymerizing vinyltrimethoxysilane and N-hydroxymethylacrylamide into the modified polyvinyl acetate emulsion, the siloxane bond has a high bond energy and good thermal stability. N-hydroxymethylacrylamide can significantly improve the high-temperature creep resistance and thermal strength by crosslinking with covalent bonds. The synergistic effect of the two can significantly enhance the high-temperature resistance of the white latex material. The triazine ring in the flame retardant is highly symmetrical and has high thermal stability. The imine bond also has good thermal stability and can form a conjugated system with the adjacent benzene ring, further enhancing the high-temperature resistance of the white latex material. By modifying sepiolite and basalt fiber with coupling agent, they can be uniformly dispersed in the polymer matrix. Sepiolite can restrict the movement of polymer chain segments at high temperature and increase the heat distortion temperature of the material. Basalt fiber can still maintain strength at high temperature and effectively resist the creep of the material at high temperature. Sepiolite and basalt fiber form a stable three-dimensional network through coupling agent and modified polyvinyl acetate emulsion, further improving the high-temperature resistance of the white latex material.

[0016] (2) A high-temperature resistant white latex material of the present invention is obtained by the preparation method of the present invention and has all the beneficial effects of the preparation method of the present invention. Attached Figure Description

[0017] Figure 1 It is a reactive synthesis formula for flame retardants. Detailed Implementation

[0018] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described clearly and completely. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0019] To better understand the above technical solutions, the following will provide a detailed description of the technical solutions in conjunction with the accompanying drawings and specific embodiments.

[0020] The reagents used in the following specific embodiments are of analytical grade. Additionally: Polyvinyl alcohol: Industrial grade, manufactured by Changchun Chemical (Jiangsu) Co., Ltd. Surfactant: Surfactant TO-7, industrial grade, manufactured by Guangdong Aoboshun Chemical Co., Ltd. Sepiolite: The manufacturer is Xiangtan Yuanyuan Sepiolite New Material Co., Ltd.; Basalt fiber: 6mm in length, 15µm in diameter, and 2780kg·m³ in density. -3 .

[0021] Example 1 This embodiment provides a method for preparing a high-temperature resistant white latex material, which specifically includes the following steps: (1) Add 4.3g of polyvinyl alcohol and 48g of deionized water to the reactor and stir to dissolve at 90°C for 1h. Then cool down to 60°C and add 0.6g of surfactant, 3.5g of vinyl acetate, 0.04g of ammonium persulfate and 0.15g of sodium acetate. Mix evenly and heat up to 80°C. After the reflux stops, start to add the main reactants dropwise. The first part is a mixed monomer obtained by mixing 8g of vinyl acetate, 0.1g of diallyl phthalate and 0.3g of vinyltrimethoxysilane evenly. The second part is an aqueous solution obtained by dissolving 0.08g of ammonium persulfate and 0.6g of N-hydroxymethylacrylamide in 5g of deionized water. The dropwise addition time is 4h and the reaction temperature is maintained at 76°C. After the dropwise addition is completed, keep warm for 1h. After cooling down, add 0.12g of sodium acetate to adjust the pH to neutral and discharge to obtain modified polyvinyl acetate emulsion. (2) Add 10.64g of vanillin and 7.62g of anhydrous sodium carbonate to 40mL of acetone solvent, stir and mix, then add 3.68g of cyanuric chloride, react at 80℃ for 6h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 50℃ for 22h to obtain intermediate 1. (3) Under nitrogen protection, 5.32 g of intermediate 1 and 3.75 g of 1-(3-aminopropyl)imidazolium were added to 35 mL of N,N-dimethylformamide solvent, stirred evenly, and reacted at 50 °C for 5 h. After the reaction was completed, the mixture was filtered, washed and dried, and purified to obtain the flame retardant. (4) Add 20 mL of deionized water, 30 mL of anhydrous ethanol and 5.02 g of sepiolite to the reactor, sonicate for 10 min, then add 2.13 g of γ-aminopropyltriethoxysilane dropwise, react at 75 °C for 4 h, after the reaction is completed, wash and dry to obtain modified sepiolite. (5) First, place 2.34g of basalt fiber in 28mL of acetone solution and ultrasonically wash for 10min. Then, add 20mL of deionized water, 30mL of anhydrous ethanol and ultrasonically washed basalt fiber to the reactor. Add 1.12g of γ-aminopropyltriethoxysilane dropwise. React at 35℃ for 8h. After the reaction is complete, wash and dry in an oven at 110℃ for 1h to obtain modified basalt fiber. (6) Mix 40 parts by weight of modified polyvinyl acetate emulsion, 3 parts by weight of flame retardant, 2 parts by weight of modified sepiolite, 1 part by weight of modified basalt fiber, 0.5 parts by weight of zinc oxide, 1 part by weight of castor oil, 0.3 parts by weight of ammonium persulfate and 10 parts by weight of deionized water evenly, ultrasonically disperse for 15 min, then stir at 60℃ for 20 min, keep warm, and discharge to obtain a high temperature resistant white latex material.

[0022] Example 2 This embodiment provides a method for preparing a high-temperature resistant white latex material, which specifically includes the following steps: (1) Add 4.4g of polyvinyl alcohol and 50g of deionized water to the reactor and stir to dissolve at 95°C for 2h. Then cool down to 65°C and add 0.7g of surfactant, 3.6g of vinyl acetate, 0.05g of ammonium persulfate and 0.18g of sodium acetate. Mix evenly and heat up to 90°C. After the reflux stops, start to add the main reactants dropwise. The first part is a mixed monomer obtained by mixing 10g of vinyl acetate, 0.15g of diallyl phthalate and 0.5g of vinyltrimethoxysilane evenly. The second part is an aqueous solution obtained by dissolving 0.1g of ammonium persulfate and 0.8g of N-hydroxymethylacrylamide in 6g of deionized water. The dropwise addition time is 4.5h. The reaction temperature is maintained at 80°C. After the dropwise addition is completed, keep warm for 1.5h. After cooling down, add 0.15g of sodium acetate to adjust the pH to neutral. Discharge to obtain modified polyvinyl acetate emulsion. (2) Add 10.68g of vanillin and 7.66g of anhydrous sodium carbonate to 50mL of acetone solvent, stir and mix, then add 3.72g of cyanuric chloride, react at 100℃ for 10h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 60℃ for 26h to obtain intermediate 1. (3) Under nitrogen protection, 5.36 g of intermediate 1 and 3.8 g of 1-(3-aminopropyl)imidazolium were added to 45 mL of N,N-dimethylformamide solvent, stirred evenly, and reacted at 60 °C for 8 h. After the reaction was completed, the mixture was filtered, washed and dried, and purified to obtain the flame retardant. (4) Add 25 mL of deionized water, 35 mL of anhydrous ethanol and 5.06 g of sepiolite to the reactor, sonicate for 15 min, then add 2.17 g of γ-aminopropyltriethoxysilane dropwise, react at 85 °C for 6 h, after the reaction is completed, wash and dry to obtain modified sepiolite. (5) First, place 2.38g of basalt fiber in 30mL of acetone solution and ultrasonically wash for 15min. Then, add 25mL of deionized water, 35mL of anhydrous ethanol, and ultrasonically washed basalt fiber to the reactor. Add 1.16g of γ-aminopropyltriethoxysilane to it. React at 45℃ for 12h. After the reaction is completed, wash and dry in an oven at 120℃ for 2h to obtain modified basalt fiber. (6) Mix 50 parts by weight of modified polyvinyl acetate emulsion, 5 parts by weight of flame retardant, 3 parts by weight of modified sepiolite, 2 parts by weight of modified basalt fiber, 0.8 parts by weight of zinc oxide, 1.5 parts by weight of castor oil, 0.5 parts by weight of ammonium persulfate and 12 parts by weight of deionized water evenly, ultrasonically disperse for 20 min, then stir at 80℃ for 30 min, keep warm, and discharge to obtain a high temperature resistant white latex material.

[0023] Example 3

[0024] This embodiment provides a method for preparing a high-temperature resistant white latex material, which specifically includes the following steps: (1) Add 4.35g of polyvinyl alcohol and 49g of deionized water to the reactor and stir to dissolve at 92℃ for 1.5h. Then cool down to 62℃ and add 0.65g of surfactant, 3.55g of vinyl acetate, 0.04g of ammonium persulfate and 0.16g of sodium acetate. Mix evenly and heat up to 85℃. After the reflux stops, start to add the main reactants dropwise. The first part is a mixed monomer obtained by mixing 9g of vinyl acetate, 0.13g of diallyl phthalate and 0.4g of vinyltrimethoxysilane evenly. The second part is an aqueous solution obtained by dissolving 0.09g of ammonium persulfate and 0.7g of N-hydroxymethylacrylamide in 5.5g of deionized water. The dropwise addition time is 4h and the reaction temperature is maintained at 78℃. After the dropwise addition is completed, keep warm for 1h. After cooling down, add 0.13g of sodium acetate to adjust the pH to neutral and discharge to obtain modified polyvinyl acetate emulsion. (2) Add 10.66g of vanillin and 7.64g of anhydrous sodium carbonate to 45mL of acetone solvent, stir and mix, then add 3.7g of cyanuric chloride, react at 90℃ for 8h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 55℃ for 24h to obtain intermediate 1. (3) Under nitrogen protection, 5.34 g of intermediate 1 and 3.77 g of 1-(3-aminopropyl)imidazolium were added to 40 mL of N,N-dimethylformamide solvent, stirred evenly, and reacted at 55 °C for 6 h. After the reaction was completed, the mixture was filtered, washed and dried, and purified to obtain the flame retardant. (4) Add 22 mL of deionized water, 32 mL of anhydrous ethanol and 5.04 g of sepiolite to the reactor, sonicate for 13 min, then add 2.15 g of γ-aminopropyltriethoxysilane dropwise, react at 80 °C for 5 h, after the reaction is completed, wash and dry to obtain modified sepiolite. (5) First, place 2.36g of basalt fiber in 29mL of acetone solution and ultrasonically wash for 12min. Then, add 22mL of deionized water, 33mL of anhydrous ethanol and ultrasonically washed basalt fiber to the reactor. Add 1.14g of γ-aminopropyltriethoxysilane to it. React at 40℃ for 10h. After the reaction is completed, wash and dry in an oven at 115℃ for 1h to obtain modified basalt fiber. (6) Mix 45 parts by weight of modified polyvinyl acetate emulsion, 4 parts by weight of flame retardant, 2 parts by weight of modified sepiolite, 1.5 parts by weight of modified basalt fiber, 0.6 parts by weight of zinc oxide, 1.2 parts by weight of castor oil, 0.4 parts by weight of ammonium persulfate and 11 parts by weight of deionized water evenly, ultrasonically disperse for 18 min, then stir at 70℃ for 25 min, keep warm, and discharge to obtain a high temperature resistant white latex material.

[0025] Example 4

[0026] This embodiment provides a method for preparing a high-temperature resistant white latex material, which specifically includes the following steps: (1) Add 4.32g of polyvinyl alcohol and 48.5g of deionized water to the reactor, stir and dissolve at 91℃ for 1h, then cool to 61℃, add 0.62g of surfactant, 3.52g of vinyl acetate, 0.04g of ammonium persulfate, and 0.16g of sodium acetate, mix well, heat to 82℃, and after reflux stops, start adding the main reactants dropwise simultaneously. The first portion is 8.5g of vinyl acetate and 0.11g of... A mixed monomer was obtained by uniformly mixing dipropylene phthalate and 0.35 g of vinyltrimethoxysilane. The second part was an aqueous solution obtained by dissolving 0.08 g of ammonium persulfate and 0.65 g of N-hydroxymethylacrylamide in 5.2 g of deionized water. The addition time was 4 h, the reaction temperature was maintained at 77 °C, and the temperature was kept at 1.1 h after the addition was completed. After cooling, 0.13 g of sodium acetate was added to adjust the pH to neutral, and the product was discharged to obtain modified polyvinyl acetate emulsion. (2) Add 10.65g of vanillin and 7.63g of anhydrous sodium carbonate to 42mL of acetone solvent, stir and mix, then add 3.69g of cyanuric chloride, react at 85℃ for 7h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 52℃ for 23h to obtain intermediate 1. (3) Under nitrogen protection, 5.33 g of intermediate 1 and 3.76 g of 1-(3-aminopropyl)imidazolium were added to 38 mL of N,N-dimethylformamide solvent, stirred evenly, and reacted at 52 °C for 6 h. After the reaction was completed, the mixture was filtered, washed and dried, and purified to obtain the flame retardant. (4) Add 21 mL of deionized water, 32 mL of anhydrous ethanol and 5.03 g of sepiolite to the reactor, sonicate for 11 min, then add 2.14 g of γ-aminopropyltriethoxysilane dropwise, react at 78 °C for 4 h, after the reaction is completed, wash and dry to obtain modified sepiolite. (5) First, place 2.35g of basalt fiber in 28mL of acetone solution and ultrasonically wash for 11min. Then, add 21mL of deionized water, 32mL of anhydrous ethanol and ultrasonically washed basalt fiber to the reactor. Add 1.13g of γ-aminopropyltriethoxysilane dropwise. React at 38℃ for 9h. After the reaction is complete, wash and dry in an oven at 112℃ for 1h to obtain modified basalt fiber. (6) Mix 42 parts by weight of modified polyvinyl acetate emulsion, 3 parts by weight of flame retardant, 2 parts by weight of modified sepiolite, 1 part by weight of modified basalt fiber, 0.6 parts by weight of zinc oxide, 1.1 parts by weight of castor oil, 0.4 parts by weight of ammonium persulfate and 11 parts by weight of deionized water evenly, ultrasonically disperse for 16 min, then stir at 65℃ for 22 min, keep warm, and discharge to obtain a high temperature resistant white latex material.

[0027] Example 5

[0028] This embodiment provides a method for preparing a high-temperature resistant white latex material, which specifically includes the following steps: (1) Add 4.38g of polyvinyl alcohol and 49.5g of deionized water to the reactor, stir and dissolve at 94℃ for 2h, then cool to 64℃, add 0.68g of surfactant, 3.58g of vinyl acetate, 0.05g of ammonium persulfate, and 0.17g of sodium acetate, mix well, heat to 88℃, and after reflux stops, start adding the main reactants dropwise simultaneously. The first portion is 9.5g of vinyl acetate and 0.14g of... A mixed monomer was obtained by uniformly mixing dipropylene phthalate and 0.45 g of vinyltrimethoxysilane. The second part was an aqueous solution obtained by dissolving 0.1 g of ammonium persulfate and 0.75 g of N-hydroxymethylacrylamide in 5.8 g of deionized water. The addition time was 4.5 h, the reaction temperature was maintained at 79 °C, and the temperature was kept at 1.5 h after the addition was completed. After cooling, 0.14 g of sodium acetate was added to adjust the pH to neutral, and the product was discharged to obtain modified polyvinyl acetate emulsion. (2) Add 10.67g of vanillin and 7.65g of anhydrous sodium carbonate to 48mL of acetone solvent, stir and mix, then add 3.71g of cyanuric chloride, react at 95℃ for 9h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 58℃ for 25h to obtain intermediate 1. (3) Under nitrogen protection, 5.35 g of intermediate 1 and 3.79 g of 1-(3-aminopropyl)imidazolium were added to 42 mL of N,N-dimethylformamide solvent, stirred evenly, and reacted at 58 °C for 7 h. After the reaction was completed, the mixture was filtered, washed and dried, and purified to obtain the flame retardant. (4) Add 24 mL of deionized water, 34 mL of anhydrous ethanol and 5.05 g of sepiolite to the reactor, sonicate for 14 min, then add 2.16 g of γ-aminopropyltriethoxysilane dropwise, react at 82 °C for 6 h, after the reaction is completed, wash and dry to obtain modified sepiolite. (5) First, place 2.37g of basalt fiber in 30mL of acetone solution and ultrasonically wash for 14min. Then, add 24mL of deionized water, 34mL of anhydrous ethanol and ultrasonically washed basalt fiber to the reactor. Add 1.15g of γ-aminopropyltriethoxysilane dropwise. React at 42℃ for 11h. After the reaction is complete, wash and dry in an oven at 118℃ for 2h to obtain modified basalt fiber. (6) Mix 48 parts by weight of modified polyvinyl acetate emulsion, 4 parts by weight of flame retardant, 3 parts by weight of modified sepiolite, 2 parts by weight of modified basalt fiber, 0.7 parts by weight of zinc oxide, 1.5 parts by weight of castor oil, 0.5 parts by weight of ammonium persulfate and 12 parts by weight of deionized water evenly, ultrasonically disperse for 19 min, then stir at 75°C for 28 min, keep warm, and discharge to obtain a high-temperature resistant white latex material.

[0029] Comparative Example 1 The proportions of the high-temperature resistant white latex material in Comparative Example 1 and Example 1 are basically the same, the main difference being that vinyltrimethoxysilane is not added in step (1).

[0030] Comparative Example 2 The proportions of the high-temperature resistant white latex material in Comparative Example 1 and Example 1 are basically the same, the main difference being that N-hydroxymethylacrylamide is not added in step (1).

[0031] Comparative Example 3 The proportions of the high-temperature resistant white latex material in Comparative Example 1 and Example 1 are basically the same, the main difference being that intermediate 1 is used instead of flame retardant.

[0032] Comparative Example 4 The high-temperature resistant white latex material formulation of Comparative Example 1 is basically the same as that of Example 1, the main difference being that sepiolite is used instead of modified sepiolite.

[0033] Performance testing Ash wood meeting the standard specifications was selected and processed into specimens with specific overlapping surfaces. The high-temperature resistant white latex materials prepared in Examples 1-5 and Comparative Examples 1-4 were precisely and evenly applied to the overlapping surfaces of the specimens, with an adhesive application rate of 120 g / m². 2 The two overlapping surfaces are then aligned and joined together, placed in a press, and pressed together at a pressure of 1.2 MPa for 24 hours. After that, they are cured at room temperature for 7 days to obtain a standard specimen.

[0034] (1) Bond strength test: The dry and wet bond strength of each group of standard specimens were tested in accordance with HG / T2727-2010. The test results are shown in Table 1.

[0035] Table 1: Bond Strength Test

[0036] As can be seen from Table 1, the high-temperature resistant white latex materials prepared in Examples 1-5 have good bonding strength.

[0037] (2) High temperature resistance test: The standard adhesive specimens were randomly divided into experimental group and control group. The tensile shear strength of the standard specimens in the control group was tested directly according to GB / T7124-2008. The experimental group was dried in a drying oven at 100℃ for 24h, and then the tensile shear strength of the standard specimens in the experimental group was tested according to GB / T7124-2008. The strength retention rate was calculated as follows: Strength retention rate (%) = (tensile shear strength of experimental group / tensile shear strength of control group) × 100%. The test results are shown in Table 2.

[0038] Table 2: High Temperature Resistance Test

[0039] As can be seen from Table 2, the high-temperature resistant white latex materials prepared in Examples 1-5 have good high-temperature resistance.

[0040] The comparison shows that the high-temperature resistant white latex materials prepared in Examples 1-5 have better adhesion and high-temperature resistance than the high-temperature resistant white latex materials prepared in Comparative Examples 1-4. In Comparative Example 1, the lack of vinyltrimethoxysilane weakened the interfacial bonding strength and cross-linking density of the white latex material. Furthermore, the siloxane bond exhibits extremely high thermal stability, resulting in decreased adhesive strength and high-temperature resistance. Comparative Example 2 lacked N-hydroxymethylacrylamide, leading to an incomplete cross-linking network, decreased cohesive strength, and lower creep resistance at high temperatures compared to the examples, thus also reducing adhesive strength and high-temperature resistance. Comparative Example 3 lacked the hydrogen bond network formed by the imidazole ring and various functional groups on the material surface, reducing the overall material integrity. The absence of imine bonds prevented the formation of a conjugated system with adjacent benzene rings, significantly reducing adhesive strength and high-temperature resistance. Comparative Example 4, due to the lack of surface modification of sepiolite, was prone to agglomeration, forming stress concentration points. Its poor interfacial bonding with the material led to overall material disintegration at high temperatures, resulting in the most significant decrease in adhesive strength and high-temperature resistance.

[0041] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0042] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

[0043] Those skilled in the art should understand that the above descriptions are merely several specific embodiments of the present invention, and not all embodiments. It should be noted that many modifications and improvements can be made by those skilled in the art, and all modifications or improvements not exceeding the scope of the claims should be considered within the protection scope of the present invention.

Claims

1. A method for preparing a high-temperature resistant white latex material, characterized in that, Includes the following steps: (1) Preparation of modified polyvinyl acetate emulsion; (2) Preparation of flame retardants; (3) Mix the modified polyvinyl acetate emulsion, flame retardant, modified sepiolite, modified basalt fiber, zinc oxide, castor oil, ammonium persulfate and deionized water evenly, ultrasonically disperse for 15-20 min, then stir at 60-80℃ for 20-30 min, keep warm, and discharge to obtain a high-temperature resistant white latex material.

2. The method for preparing the high-temperature resistant white latex material according to claim 1, characterized in that, The preparation method of the modified polyvinyl acetate emulsion in step (1) is as follows: 4.3-4.4g of polyvinyl alcohol and 48-50g of deionized water are added to the reactor and stirred and dissolved at 90-95℃ for 1-2h. Then the temperature is lowered to 60-65℃, and 0.6-0.7g of surfactant, 3.5-3.6g of vinyl acetate, 0.04-0.05g of ammonium persulfate, and 0.15-0.18g of sodium acetate are added. The mixture is stirred evenly and heated to 80-90℃. After the reflux stops, the main reactants are added dropwise at the same time for 4-4.5h. The reaction temperature is maintained at 76-80℃. After the addition is completed, the temperature is kept for 1-1.5h. After cooling, 0.12-0.15g of sodium acetate is added to adjust the pH to neutral. The product is discharged to obtain the modified polyvinyl acetate emulsion.

3. The method for preparing the high-temperature resistant white latex material according to claim 1, characterized in that, The method for preparing the flame retardant in step (2) is as follows: S1: Add vanillin and anhydrous sodium carbonate to acetone solvent, stir and mix, then add cyanuric chloride, react at 80-100℃ for 6-10h, after the reaction is completed, cool to room temperature, filter, wash, and dry in an oven at 50-60℃ for 22-26h to obtain intermediate 1. S2: Under nitrogen protection, intermediate 1, 1-(3-aminopropyl)imidazolium is added to N,N-dimethylformamide solvent, stirred evenly, and reacted at 50-60℃ for 5-8 hours. After the reaction is completed, the mixture is filtered, washed and dried, and purified to obtain the flame retardant.

4. The method for preparing the high-temperature resistant white latex material according to claim 1, characterized in that, The modified sepiolite in step (3) is prepared by adding 20-25 mL of deionized water, 30-35 mL of anhydrous ethanol, and 5.02-5.06 g of sepiolite to a reactor, sonicating for 10-15 min, then adding 2.13-2.17 g of γ-aminopropyltriethoxysilane, and reacting at 75-85 °C for 4-6 h. After the reaction is completed, the mixture is washed and dried to obtain the modified sepiolite.

5. The method for preparing the high-temperature resistant white latex material according to claim 1, characterized in that, The method for preparing modified basalt fiber in step (3) is as follows: First, place 2.34-2.38g of basalt fiber in 28-30mL of acetone solution and ultrasonically wash for 10-15min. Then, add 20-25mL of deionized water, 30-35mL of anhydrous ethanol, and ultrasonically washed basalt fiber to the reactor. Add 1.12-1.16g of γ-aminopropyltriethoxysilane dropwise. React at 35-45℃ for 8-12h. After the reaction is completed, wash and dry in an oven at 110-120℃ for 1-2h to obtain modified basalt fiber.

6. The method for preparing the high-temperature resistant white latex material according to claim 2, characterized in that, The main reactants consist of two parts. The first part is a mixed monomer obtained by uniformly mixing 8-10g of vinyl acetate, 0.1-0.15g of diallyl phthalate and 0.3-0.5g of vinyltrimethoxysilane. The second part is an aqueous solution obtained by dissolving 0.08-0.1g of ammonium persulfate and 0.6-0.8g of N-hydroxymethylacrylamide in 5-6g of deionized water.

7. The method for preparing the high-temperature resistant white latex material according to claim 3, characterized in that, The ratio of acetone, vanillin, anhydrous sodium carbonate, and cyanuric chloride in S1 is 40-50 mL: 10.64-10.68 g: 7.62-7.66 g: 3.68-3.72 g.

8. The method for preparing the high-temperature resistant white latex material according to claim 3, characterized in that, The ratio of N,N-dimethylformamide, intermediate 1, and 1-(3-aminopropyl)imidazole in S2 is 35-45 mL: 5.32-5.36 g: 3.75-3.8 g.

9. The method for preparing the high-temperature resistant white latex material according to claim 1, characterized in that, The weight parts of each component in step (3) are as follows: 40-50 parts of modified polyvinyl acetate emulsion, 3-5 parts of flame retardant, 2-3 parts of modified sepiolite, 1-2 parts of modified basalt fiber, 0.5-0.8 parts of zinc oxide, 1-1.5 parts of castor oil, 0.3-0.5 parts of ammonium persulfate, and 10-12 parts of deionized water.

10. A high-temperature resistant white latex material, characterized in that, It is prepared by the preparation method described in any one of claims 1-9.

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