Flame-retardant pressure-sensitive adhesive, preparation method and adhesive tape prepared therefrom

Abstract

The present invention discloses a method for preparing a flame-retardant pressure-sensitive adhesive, comprising the following steps: (1) preparing a mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate, and ethyl acetate, and adding azobisisobutyronitrile to the mixed solution to obtain a mixed solution; (2) adding modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution to obtain a coating adhesive; and (3) immediately coating the coating adhesive on a PET film and drying it at 100° C. for 90 seconds to obtain an adhesive tape containing the flame-retardant pressure-sensitive adhesive. The adhesive tape prepared by the method of the present invention has high peel strength and good flame retardant properties, thereby improving the safety and reliability of the adhesive tape.

Description

Technical Field

[0001] The present invention relates to the technical field of pressure-sensitive adhesives, and in particular to a flame-retardant pressure-sensitive adhesive, a preparation method and an adhesive tape prepared therefrom. Background Art

[0002] Pressure-sensitive adhesive (PSA) is a soft polymer material with long-lasting adhesion at room temperature. It adheres to the surface of the adhesive through non-covalent bonds under light pressure and leaves no residue after being peeled off. With the advancement of pressure-sensitive adhesive technology and the increasing demand for its application, functionally modified acrylic pressure-sensitive adhesives have become a major development trend in this field. Functional polymers are made by adding other functional materials to polymers. Typically, acrylic resins are mixed with other organic resins, inorganic fillers, organic small molecules, and other substances to produce polymer materials with special properties. This functional polymer material not only has the excellent properties of acrylic resin, but also has the thermal conductivity, flame retardancy, and electrical conductivity functions imparted by the modifier. Summary of the Invention

[0003] The present invention provides a method for preparing a flame retardant pressure-sensitive adhesive, comprising the following steps:

[0004] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate, and ethyl acetate, and maintaining the mixture in a water bath at a constant temperature of 70° C., condensing and refluxing during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, and continuing to maintain the mixture at 70° C. and condensing and refluxing for more than 5 hours after the addition is completed;

[0005] (2) cooling the mixed solution to 50° C., preserving the mixture, condensing and refluxing, and then stirring the mixed solution. Adding modified magnesium hydroxide powder to the mixed solution under stirring, stirring the mixed solution for more than 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution under stirring. After the addition is completed, continue to keep the mixture at 50° C., condensing and refluxing, and stirring for more than 2 hours. Air-cooling to room temperature under stirring to obtain a coating glue;

[0006] (3) immediately coating the coating adhesive on a PET film and drying at 100° C. to obtain the flame retardant pressure-sensitive adhesive;

[0007] The preparation method of the modified magnesium hydroxide powder is as follows:

[0008] Step 1, preparing ammonia water with a solute mass percentage of 20%; stirring the ammonia water, adding nitrilotriacetic acid to the ammonia water under stirring, and continuing to stir the solution for more than 10 minutes after the addition is completed; then adding magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, and keeping the temperature in a water bath at 35±2° C. for more than 30 minutes after the addition is completed, stirring the solution and condensing and refluxing during the insulation process, and separating the solid and liquid after the insulation is completed, washing the solid phase with deionized water, and drying to obtain a solid phase powder;

[0009] Step 2: Prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; soak the solid phase powder in the acetone solution of palladium acetate, then place the solution under 0.01 standard atmospheric pressure for more than 10 minutes, then separate the solid and liquid, soak the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for more than 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water for more than 3 times, then soak it in the aqueous solution of neodymium acetate, place the solution under 0.01 standard atmospheric pressure for more than 10 minutes, then separate the solid and liquid. The solid phase is again immersed in an aqueous solution of sodium borohydride kept at 40±5°C for more than 20 minutes; then the solid-liquid separation is carried out, the solid phase is washed with deionized water for more than 3 times, and then immersed in the acetone solution of palladium acetate again; the above-mentioned soaking steps of palladium acetate in acetone solution, sodium borohydride aqueous solution, neodymium acetate aqueous solution, and sodium borohydride aqueous solution are combined into one group, and a total of 5 groups are repeated, followed by solid-liquid separation, the solid phase is washed with deionized water for more than 3 times, and dried at 60°C for more than 30 minutes to obtain a treated solid phase;

[0010] Step three, preparing an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; dispersing the once treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, the suspension is kept constant temperature at 60±2°C in a water bath, the suspension is stirred, and then triethylamine is added to the suspension under stirring. After the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2°C for more than 5h, and then the solid-liquid separation is performed, the solid phase is washed with ethanol for more than 3 times, and dried at 60°C for more than 30min to obtain the modified magnesium hydroxide powder.

[0011] Furthermore, in the step (1), in the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, the mixing mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid:methyl acrylate:2-ethylhexyl acrylate:ethyl acetate=12-16:25-30:70-80:120; and the mass ratio of the added mass of azobisisobutyronitrile to the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile:mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate=0.13-0.16:100.

[0012] Furthermore, in the step (2), the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed liquid is modified magnesium hydroxide powder: aluminum acetylacetonate: mixed liquid = 17-22: 0.08-0.09:100.

[0013] Furthermore, in the step 1, the amount ratio of nitrilotriacetic acid added to the ammonia water is nitrilotriacetic acid: ammonia water = 8-10 g: 1 L; in the magnesium chloride solution, the concentration of magnesium chloride is 80-100 g / L, and the solvent is water; in the sodium hydroxide solution, the concentration of sodium hydroxide is 40-50 g / L, and the solvent is water; in the sodium dodecylbenzenesulfonate solution, the concentration of sodium dodecylbenzenesulfonate is 0.3-0.6 g / L, and the solvent is water; the volume ratio of the magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution added to the solution is magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzenesulfonate solution: solution = 15-18:16-20:8-10:100.

[0014] Furthermore, in step 2, the concentration of palladium acetate in the acetone solution of palladium acetate is 1.2-1.3 g / L, and the solvent is acetone; the concentration of neodymium acetate in the aqueous solution of neodymium acetate is 20-22 g / L, and the solvent is water.

[0015] Furthermore, in the step three, the concentration of 4,4'-dihydroxydiphenyl sulfone in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone is 2 to 3 g / 100 mL, and the solvent is acetonitrile; the solid-liquid mass ratio of the once-treated solid phase dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone is once-treated solid phase: 4,4'-dihydroxydiphenyl sulfone acetonitrile solution = 1:50; the volume ratio of triethylamine added to the suspension to the volume of the suspension is triethylamine: suspension = 0.7 to 0.8:100.

[0016] The invention also discloses an adhesive tape. The adhesive tape is obtained by coating the coating adhesive on a PET film and drying the film at 100° C. for 90 seconds.

[0017] The beneficial effects of the present invention are that the adhesive tape prepared by the method of the present invention has high peel strength and good flame retardant performance, thereby improving the safety and reliability of the adhesive tape. DETAILED DESCRIPTION

[0018] The present invention will be further described below with reference to the embodiments.

[0019] Example 1

[0020] A method for preparing a flame retardant pressure-sensitive adhesive, comprising the following steps:

[0021] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 12:25:70:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condenses and refluxes during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.13:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0022] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing and refluxing, and then stirring the mixed solution. Adding modified magnesium hydroxide powder to the mixed solution under stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution under stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 17:0.08:100; after the addition is completed, continue to keep the mixture at 50° C., condensing and refluxing, and stirring for 2 hours, and air-cool to room temperature under stirring to obtain a coating glue;

[0023] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the flame retardant pressure sensitive adhesive; the thickness of the flame retardant pressure sensitive adhesive was 20 μm.

[0024] The preparation method of the modified magnesium hydroxide powder is as follows:

[0025] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 8g: 1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 80g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 40g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.3 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 15:16:8:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0026] Step 2: prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.2 g / L, and the solvent is acetone; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 20 g / L, and the solvent is water; immerse the solid phase powder in the acetone solution of palladium acetate, and then place the solution under 0.01 standard atmospheric pressure for 10 minutes, then separate the solid and liquid, and immerse the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water 3 times, and then immerse it in the aqueous solution of neodymium acetate. The solution is placed under 0.01 standard atmospheric pressure for 10 minutes, and then the solid-liquid separation is performed, and the solid phase is immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes again; then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and then immersed in the acetone solution of palladium acetate again; the above-mentioned soaking process of palladium acetate in acetone solution, soaking process of sodium borohydride aqueous solution, soaking process of neodymium acetate aqueous solution, and soaking process of sodium borohydride aqueous solution are a whole group, and a total of 5 groups are repeated, and then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and dried at 60°C for 30 minutes to obtain a treated solid phase;

[0027] Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 2g / 100mL, and the solvent is acetonitrile; disperse the once-treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of once-treated solid phase: 4,4'-dihydroxy The suspension is kept at a constant temperature of 60±2° C. in a water bath, stirred, and then triethylamine is added to the suspension under stirring, with the volume ratio of triethylamine added to the suspension to the volume of the suspension being triethylamine:suspension=0.7:100; after the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for 5 hours, and then solid-liquid separation is performed, the solid phase is washed with ethanol three times, and dried at 60° C. for 30 minutes to obtain the modified magnesium hydroxide powder.

[0028] Example 2

[0029] A method for preparing a flame retardant pressure-sensitive adhesive, comprising the following steps:

[0030] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 14:27:74:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condenses and refluxes during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.14:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0031] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 19:0.08:100; after the addition is completed, continue to keep the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cool to room temperature while stirring to obtain a coating adhesive;

[0032] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the flame retardant pressure sensitive adhesive; the thickness of the flame retardant pressure sensitive adhesive was 20 μm.

[0033] The preparation method of the modified magnesium hydroxide powder is as follows:

[0034] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 9g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 90g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 45g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.4 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 16:18:9:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0035] Step 2: prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.2 g / L, and the solvent is acetone; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 21 g / L, and the solvent is water; immerse the solid phase powder in the acetone solution of palladium acetate, and then place the solution under 0.01 standard atmospheric pressure for 10 minutes, then separate the solid and liquid, and immerse the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water 3 times, and then immerse it in the aqueous solution of neodymium acetate. The solution is placed under 0.01 standard atmospheric pressure for 10 minutes, and then the solid-liquid separation is performed, and the solid phase is immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes again; then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and then immersed in the acetone solution of palladium acetate again; the above-mentioned soaking process of palladium acetate in acetone solution, soaking process of sodium borohydride aqueous solution, soaking process of neodymium acetate aqueous solution, and soaking process of sodium borohydride aqueous solution are a whole group, and a total of 5 groups are repeated, and then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and dried at 60°C for 30 minutes to obtain a treated solid phase;

[0036] Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 2g / 100mL, and the solvent is acetonitrile; disperse the once-treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of once-treated solid phase: 4,4'-dihydroxy The suspension is kept at a constant temperature of 60±2° C. in a water bath, stirred, and then triethylamine is added to the suspension under stirring, with the volume ratio of triethylamine added to the suspension to the volume of the suspension being triethylamine:suspension=0.7:100; after the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for 5 hours, and then solid-liquid separation is performed, the solid phase is washed with ethanol three times, and dried at 60° C. for 30 minutes to obtain the modified magnesium hydroxide powder.

[0037] Example 3

[0038] A method for preparing a flame retardant pressure-sensitive adhesive, comprising the following steps:

[0039] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 14:28:75:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condensed and refluxed during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.15:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0040] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 20:0.09:100; after the addition is completed, continue preserving the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cooling to room temperature while stirring to obtain a coating adhesive;

[0041] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the flame retardant pressure sensitive adhesive; the thickness of the flame retardant pressure sensitive adhesive was 20 μm.

[0042] The preparation method of the modified magnesium hydroxide powder is as follows:

[0043] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 9g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 90g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 45g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.5 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 17:18:9:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0044] Step 2: prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.3 g / L, and the solvent is acetone; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 21 g / L, and the solvent is water; immerse the solid phase powder in the acetone solution of palladium acetate, and then place the solution under 0.01 standard atmospheric pressure for 10 minutes, then separate the solid and liquid, and immerse the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water 3 times, and then immerse it in the aqueous solution of neodymium acetate. The solution is placed under 0.01 standard atmospheric pressure for 10 minutes, and then the solid-liquid separation is performed, and the solid phase is immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes again; then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and then immersed in the acetone solution of palladium acetate again; the above-mentioned soaking process of palladium acetate in acetone solution, soaking process of sodium borohydride aqueous solution, soaking process of neodymium acetate aqueous solution, and soaking process of sodium borohydride aqueous solution are a whole group, and a total of 5 groups are repeated, and then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and dried at 60°C for 30 minutes to obtain a treated solid phase;

[0045] Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 3g / 100mL, and the solvent is acetonitrile; disperse the once-treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of once-treated solid phase: 4,4'-dihydroxy The suspension is kept at a constant temperature of 60±2° C. in a water bath, stirred, and then triethylamine is added to the suspension under stirring, with the volume ratio of triethylamine added to the suspension to the volume of the suspension being triethylamine:suspension=0.8:100. After the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for 5 hours, and then solid-liquid separation is performed, the solid phase is washed with ethanol three times, and dried at 60° C. for 30 minutes to obtain the modified magnesium hydroxide powder.

[0046] Example 4

[0047] A method for preparing a flame retardant pressure-sensitive adhesive, comprising the following steps:

[0048] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 16:30:80:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condenses and refluxes during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.16:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0049] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 22:0.09:100; after the addition is completed, continue to keep the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cool to room temperature while stirring to obtain a coating adhesive;

[0050] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the flame retardant pressure sensitive adhesive; the thickness of the flame retardant pressure sensitive adhesive was 20 μm.

[0051] The preparation method of the modified magnesium hydroxide powder is as follows:

[0052] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 10g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, wherein the concentration of magnesium chloride in the magnesium chloride solution is 100g / L and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 50g / L and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.6 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 18:20:10:100; after the addition is completed, the water bath is kept constant at 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0053] Step 2: prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.3 g / L, and the solvent is acetone; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 22 g / L, and the solvent is water; immerse the solid phase powder in the acetone solution of palladium acetate, and then place the solution under 0.01 standard atmospheric pressure for 10 minutes, then separate the solid and liquid, and immerse the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water 3 times, and then immerse it in the aqueous solution of neodymium acetate. The solution is placed under 0.01 standard atmospheric pressure for 10 minutes, and then the solid-liquid separation is performed, and the solid phase is immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes again; then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and then immersed in the acetone solution of palladium acetate again; the above-mentioned soaking process of palladium acetate in acetone solution, soaking process of sodium borohydride aqueous solution, soaking process of neodymium acetate aqueous solution, and soaking process of sodium borohydride aqueous solution are a whole group, and a total of 5 groups are repeated, and then the solid-liquid separation is performed, the solid phase is washed with deionized water 3 times, and dried at 60°C for 30 minutes to obtain a treated solid phase;

[0054] Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 3g / 100mL, and the solvent is acetonitrile; disperse the once-treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of once-treated solid phase: 4,4'-dihydroxy The suspension is kept at a constant temperature of 60±2° C. in a water bath, stirred, and then triethylamine is added to the suspension under stirring, with the volume ratio of triethylamine added to the suspension to the volume of the suspension being triethylamine:suspension=0.8:100. After the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for 5 hours, and then solid-liquid separation is performed, the solid phase is washed with ethanol three times, and dried at 60° C. for 30 minutes to obtain the modified magnesium hydroxide powder.

[0055] Comparative Example 1

[0056] A method for preparing a comparative glue comprises the following steps:

[0057] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 14:28:75:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condensed and refluxed during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.15:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0058] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 20:0.09:100; after the addition is completed, continue preserving the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cooling to room temperature while stirring to obtain a coating adhesive;

[0059] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the comparative adhesive; the thickness of the comparative adhesive was 20 μm.

[0060] The preparation method of the modified magnesium hydroxide powder is as follows:

[0061] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 9g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 90g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 45g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.5 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 17:18:9:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0062] Step 2: Prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 3g / 100mL, and the solvent is acetonitrile; disperse the solid phase powder in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the solid-liquid mass ratio of the solid phase powder to the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone is solid phase powder: 4,4'-dihydroxydiphenyl sulfone Nitrile solution = 1:50; the suspension was kept warm in a water bath at 60±2°C, the suspension was stirred, and then triethylamine was added to the suspension under stirring, the volume ratio of triethylamine added to the suspension to the volume of the suspension was triethylamine: suspension = 0.8:100; after the addition was completed, the suspension was stirred at a constant temperature of 60±2°C for 5h, and then the solid-liquid separation was carried out, the solid phase was washed 3 times with ethanol, and dried at 60°C for 30min to obtain the modified magnesium hydroxide powder described in this comparative example.

[0063] Comparative Example 2

[0064] A method for preparing a comparative glue comprises the following steps:

[0065] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 14:28:75:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condensed and refluxed during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.15:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0066] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 20:0.09:100; after the addition is completed, continue preserving the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cooling to room temperature while stirring to obtain a coating adhesive;

[0067] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the comparative adhesive; the thickness of the comparative adhesive was 20 μm.

[0068] The preparation method of the modified magnesium hydroxide powder is as follows:

[0069] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 9g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 90g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 45g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.5 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 17:18:9:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0070] Step 2, preparing an acetone solution of palladium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.3 g / L, and the solvent is acetone; soaking the solid phase powder in the acetone solution of palladium acetate, and then placing the solution under 0.01 standard atmospheric pressure for 10 minutes, followed by solid-liquid separation, and soaking the solid phase in an aqueous solution of sodium borohydride insulated at 40±5°C for 20 minutes; then solid-liquid separation, the solid phase is washed 3 times with deionized water, and then soaked in the acetone solution of palladium acetate again, the solution is placed under 0.01 standard atmospheric pressure for 10 minutes, and then solid-liquid separation, and the solid phase is again soaked in an aqueous solution of sodium borohydride insulated at 40±5°C for 20 minutes; the above-mentioned soaking process of palladium acetate in acetone solution and soaking process of sodium borohydride aqueous solution are a whole group, repeated for a total of 5 groups, and then solid-liquid separation, the solid phase is washed 3 times with deionized water, and dried at 60°C for 30 minutes to obtain a treated solid phase;

[0071] Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 3g / 100mL, and the solvent is acetonitrile; disperse the once-treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of once-treated solid phase: 4,4'-dihydroxy The suspension is kept at a constant temperature of 60±2° C. in a water bath, stirred, and then triethylamine is added to the suspension under stirring, with the volume ratio of triethylamine added to the suspension to the volume of the suspension being triethylamine:suspension=0.8:100. After the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for 5 hours, and then solid-liquid separation is performed, the solid phase is washed with ethanol three times, and dried at 60° C. for 30 minutes to obtain the modified magnesium hydroxide powder.

[0072] Comparative Example 3

[0073] A method for preparing a comparative glue comprises the following steps:

[0074] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 14:28:75:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condensed and refluxed during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.15:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0075] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 20:0.09:100; after the addition is completed, continue preserving the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cooling to room temperature while stirring to obtain a coating adhesive;

[0076] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the comparative adhesive; the thickness of the comparative adhesive was 20 μm.

[0077] The preparation method of the modified magnesium hydroxide powder is as follows:

[0078] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 9g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 90g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 45g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.5 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 17:18:9:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0079] Step 2, prepare an aqueous solution of neodymium acetate; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 21g / L, and the solvent is water; soak the solid phase powder in the aqueous solution of neodymium acetate, the solution is placed at 0.01 standard atmospheric pressure and maintained for 10 minutes, then the solid-liquid separation is performed, and the solid phase is immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; then the solid-liquid separation is performed, the solid phase is washed 3 times with deionized water, and then immersed in the aqueous solution of neodymium acetate again, the solution is placed at 0.01 standard atmospheric pressure and maintained for 10 minutes, then the solid-liquid separation is performed, and the solid phase is immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; the above-mentioned aqueous solution soaking process of neodymium acetate and the aqueous solution soaking process of sodium borohydride are a whole group, repeated for a total of 5 groups, and then the solid-liquid separation is performed, the solid phase is washed 3 times with deionized water, and dried at 60°C for 30 minutes to obtain a treated solid phase;

[0080] Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 3g / 100mL, and the solvent is acetonitrile; disperse the once-treated solid phase in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of once-treated solid phase: 4,4'-dihydroxy The suspension is kept at a constant temperature of 60±2° C. in a water bath, stirred, and then triethylamine is added to the suspension under stirring, with the volume ratio of triethylamine added to the suspension to the volume of the suspension being triethylamine:suspension=0.8:100. After the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for 5 hours, and then solid-liquid separation is performed, the solid phase is washed with ethanol three times, and dried at 60° C. for 30 minutes to obtain the modified magnesium hydroxide powder.

[0081] Comparative Example 4

[0082] A method for preparing a comparative glue comprises the following steps:

[0083] (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, wherein the mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 14:28:75:120; the mixture is kept at a constant temperature of 70° C. in a water bath, and condensed and refluxed during the insulation process; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, wherein the mass ratio of the added azobisisobutyronitrile to the mass ratio of the mixed solution of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.15:100; after the addition is completed, the mixture is kept at 70° C. and condensed and refluxed for 5 hours;

[0084] (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing, and refluxing, then stirring the mixed solution, adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring, with the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed solution being modified magnesium hydroxide powder: aluminum acetylacetonate: mixed solution = 20:0.09:100; after the addition is completed, continue preserving the mixture at 50° C., condensing, and refluxing, stirring for 2 hours, and air-cooling to room temperature while stirring to obtain a coating adhesive;

[0085] (3) The coating adhesive was immediately coated on a PET film and dried at 100° C. for 90 seconds to obtain an adhesive tape containing the comparative adhesive; the thickness of the comparative adhesive was 20 μm.

[0086] The preparation method of the modified magnesium hydroxide powder is as follows:

[0087] Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 9g:1L; continue to stir the solution for 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, the concentration of magnesium chloride in the magnesium chloride solution is 90g / L, and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 45g / L, and the solvent is water; in the sodium dodecylbenzene sulfonate solution, the concentration of sodium dodecylbenzene sulfonate is 0.5 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzene sulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzene sulfonate solution: solution = 17:18:9:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2°C for 30 minutes, the solution is stirred during the insulation process and condensed and refluxed, and after the insulation is completed, solid-liquid separation is carried out, the solid phase is washed three times with deionized water, and dried at 60°C for 30 minutes to obtain a solid phase powder;

[0088] Step 2: prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.3 g / L, and the solvent is acetone; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 21 g / L, and the solvent is water; immerse the solid phase powder in the acetone solution of palladium acetate, and then place the solution under 0.01 standard atmospheric pressure for 10 minutes, then separate the solid and liquid, and immerse the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water 3 times, and then immerse it in the aqueous solution of neodymium acetate, and the solution The mixture was placed under 0.01 standard atmospheric pressure and maintained for 10 minutes, and then the solid-liquid separation was performed, and the solid phase was immersed in an aqueous solution of sodium borohydride kept at 40±5°C for 20 minutes again; the solid-liquid separation was then performed, the solid phase was washed three times with deionized water, and immersed in the acetone solution of palladium acetate again; the above-mentioned soaking process of palladium acetate in acetone solution, soaking process of sodium borohydride aqueous solution, soaking process of neodymium acetate aqueous solution, and soaking process of sodium borohydride aqueous solution were combined into one group, and repeated for a total of 5 groups, and then the solid-liquid separation was performed, the solid phase was washed three times with deionized water, and dried at 60°C for 30 minutes to obtain the modified magnesium hydroxide powder described in this comparative example.

[0089] Example 5

[0090] The 180° peel strength (Method 1) of the adhesive tapes prepared by the methods described in the above embodiments and comparative examples was tested in accordance with the requirements of standard GB / T 2792-2014. The flame retardancy of the adhesive tapes prepared by the methods described in the above embodiments and comparative examples was tested in accordance with the requirements of standard GB / T 15903-1995. The test tape length was 300 mm and the width was 25 mm. The results are shown in Table 1.

[0091] Table 1

[0092]

[0093]

[0094] As shown in Table 1, the adhesive tape prepared by the method of the present invention has high peel strength and good flame retardant properties, which improves the safety and reliability of the adhesive tape. This may be because the modified magnesium hydroxide can further promote the decomposition and absorption of heat of magnesium hydroxide compared to unmodified magnesium hydroxide when burned and heated, while absorbing oxygen from the combustion interface, reducing the oxygen concentration on the contact surface, and the products generated by the combustion of the modified material can promote the cross-linking of polymers into carbon, causing the surface of the pressure-sensitive adhesive matrix to dehydrate and carbonize to form a non-combustible carbon layer, while also forming a condensed phase flame retardant layer, delaying the exchange of combustible substances and achieving a flame retardant effect.

[0095] The technical solutions provided by the present invention are described in detail above. For those skilled in the art, according to the ideas of the embodiments of the present invention, there may be changes in the specific implementation methods and application scopes. In summary, the contents of this specification should not be understood as limiting the present invention.

Claims

1. A method for preparing a flame retardant pressure sensitive adhesive, characterized in that the steps include: (1) preparing a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, and keeping the mixture in a water bath at a constant temperature of 70° C., condensing and refluxing during the keeping temperature; stirring the mixture, and adding azobisisobutyronitrile to the mixture during the stirring process to obtain a mixed solution, and continuing to keep the mixture at 70° C. and condensing and refluxing for more than 5 hours after the addition is completed; in the mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate, the mixing mass ratio of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is acrylic acid: methyl acrylate: 2-ethylhexyl acrylate: ethyl acetate = 12-16:25-30:70-80:120; the mass ratio of the added azobisisobutyronitrile to the mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate is azobisisobutyronitrile: a mixture of acrylic acid, methyl acrylate, 2-ethylhexyl acrylate and ethyl acetate = 0.13-0.16:100; (2) Cooling the mixed solution to 50° C., preserving the mixture, condensing and refluxing, and then stirring the mixed solution. Adding modified magnesium hydroxide powder to the mixed solution while stirring, stirring the mixed solution for more than 30 minutes after the addition is completed, and then adding aluminum acetylacetonate to the mixed solution while stirring. After the addition is completed, continue to keep the mixture at 50° C., condensing and refluxing, and stirring for more than 2 hours. Air-cooling to room temperature while stirring to obtain a coating glue; (3) immediately coating the coating adhesive on a PET film and drying at 100° C. to obtain the flame retardant pressure sensitive adhesive; The preparation method of the modified magnesium hydroxide powder is as follows: Step 1, prepare ammonia water with a solute mass percentage of 20%; stir the ammonia water, add nitrilotriacetic acid to the ammonia water under stirring, and add nitrilotriacetic acid to the ammonia water in a ratio of nitrilotriacetic acid: ammonia water = 8-10g:1L; continue to stir the solution for more than 10 minutes after the addition is completed; then add magnesium chloride solution, sodium hydroxide solution and sodium dodecylbenzenesulfonate solution to the solution under stirring, wherein the concentration of magnesium chloride in the magnesium chloride solution is 80-100g / L and the solvent is water; the concentration of sodium hydroxide in the sodium hydroxide solution is 40-50g / L, The solvent is water; the concentration of sodium dodecylbenzenesulfonate in the sodium dodecylbenzenesulfonate solution is 0.3-0.6 g / L, and the solvent is water; magnesium chloride solution, sodium hydroxide solution, and sodium dodecylbenzenesulfonate solution are added to the solution in a volume ratio of magnesium chloride solution: sodium hydroxide solution: sodium dodecylbenzenesulfonate solution: solution = 15-18:16-20:8-10:100; after the addition is completed, the water bath is kept at a constant temperature of 35±2° C. for more than 30 minutes, the solution is stirred and condensed and refluxed during the insulation process, and after the insulation is completed, solid-liquid separation is performed, the solid phase is washed with deionized water, and dried to obtain a solid phase powder; Step 2: prepare an acetone solution of palladium acetate and an aqueous solution of neodymium acetate; in the acetone solution of palladium acetate, the concentration of palladium acetate is 1.2-1.3 g / L, and the solvent is acetone; in the aqueous solution of neodymium acetate, the concentration of neodymium acetate is 20-22 g / L, and the solvent is water; immerse the solid phase powder in the acetone solution of palladium acetate, and then place the solution under 0.01 standard atmospheric pressure for more than 10 minutes, then separate the solid and liquid, and immerse the solid phase in an aqueous solution of sodium borohydride kept at 40±5°C for more than 20 minutes; then separate the solid and liquid, wash the solid phase with deionized water for more than 3 times, and then immerse it in the neodymium acetate solution. aqueous solution, the solution is placed under 0.01 standard atmospheric pressure and maintained for more than 10 minutes, then solid-liquid separation is performed, and the solid phase is again immersed in an aqueous solution of sodium borohydride kept at 40±5°C for more than 20 minutes; then solid-liquid separation is performed, the solid phase is washed with deionized water for more than 3 times, and then immersed in the acetone solution of palladium acetate again; the above-mentioned soaking process of palladium acetate in acetone solution, soaking process of sodium borohydride aqueous solution, soaking process of neodymium acetate aqueous solution, and soaking process of sodium borohydride aqueous solution are a whole group, and are repeated for a total of 5 groups, and then solid-liquid separation is performed, the solid phase is washed with deionized water for more than 3 times, and dried at 60°C for more than 30 minutes to obtain a treated solid phase; Step 3, prepare an acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone; in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone, the concentration of 4,4'-dihydroxydiphenyl sulfone is 2 to 3 g / 100 mL, and the solvent is acetonitrile; the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone to form a suspension, and the once-treated solid phase is dispersed in the acetonitrile solution of 4,4'-dihydroxydiphenyl sulfone at a solid-liquid mass ratio of the once-treated solid phase to 4,4'-dihydroxydiphenyl sulfone. Acetonitrile solution = 1:50; the suspension is kept constant temperature at 60±2° C. in a water bath, the suspension is stirred, and then triethylamine is added to the suspension under stirring, and the volume ratio of triethylamine added to the suspension to the volume of the suspension is triethylamine: suspension = 0.7-0.8:100; after the addition is completed, the suspension is continued to be stirred at a constant temperature of 60±2° C. for more than 5 hours, and then solid-liquid separation is carried out, the solid phase is washed with ethanol for more than 3 times, and dried at 60° C. for more than 30 minutes to obtain the modified magnesium hydroxide powder.

2. The method for preparing a flame retardant pressure sensitive adhesive according to claim 1, characterized in that: In the step (2), the mass ratio of the added modified magnesium hydroxide powder and aluminum acetylacetonate to the mixed liquid is modified magnesium hydroxide powder: aluminum acetylacetonate: mixed liquid = 17-22: 0.08-0.09:

100.

3. An adhesive tape, characterized in that: The adhesive tape is obtained by coating the coating adhesive prepared by the method according to claim 1 on a PET film and drying at 100° C. for 90 seconds.

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