Polyacrylate pressure-sensitive adhesive and preparation method thereof

Abstract

The invention discloses a polyacrylate pressure-sensitive adhesive and a preparation method thereof. The preparation method comprises the following steps: firstly, mixing a hard monomer, a soft monomer, a functional monomer and a solvent, titrating an initiator A, then adding polyether phosphate (V-100P) containing double bonds and a polyacetylene benzene polymer, finally adding an initiator B, carrying out a reaction, and carrying out heat preservation and cooling to prepare the strong-acid-resistant and strong-alkali-resistant flame-retardant polypolyacrylate pressure-sensitive adhesive. Wherein the mass ratio of the hard monomer to the soft monomer to the solvent to the functional monomer to the initiator is (6-10): (35-45): (40-50): (8-12): (0.2-0.4). By adjusting the proportion of the etherified amino resin, the polyisocyanate and the polyacrylate pressure-sensitive adhesive, the purposes of controlling the stripping force, temperature resistance, moisture resistance and acid and alkali resistance are achieved.

Description

Technical Field

[0001] The invention relates to the technical field of pressure-sensitive adhesives, and in particular to a polyacrylate pressure-sensitive adhesive and a preparation method thereof. Background Art

[0002] Traditional flame-retardant pressure-sensitive adhesive tapes are mostly made of ordinary glue with phosphorus-nitrogen flame retardants or halogen-containing flame retardants added externally. The amount of addition is large, the flame retardant effect is average, the halogen is not environmentally friendly and toxic, the glue performance is poor, and the resistance to strong acids and alkalis is poor. It cannot meet the current use standards of electronic product batteries that require resistance to strong acids and alkalis and have flame retardant properties.

[0003] Existing products have poor acid and alkali resistance, and the flame retardant solution is not environmentally friendly, mainly because the adhesive itself has defects. This solution introduces special functional monomers trimethylolpropane monoallyl ether and di-trimethylolpropane in the synthesis process, and introduces double-bond polyether phosphate (V-100P) and polyacetylene benzene polymers. Through the design of the synthesis process, a polyacrylate pressure-sensitive adhesive with strong acid (PH=1) and strong alkali (PH=13) resistance and flame retardant properties (UL94-V0) is developed. Summary of the invention

[0004] To overcome the deficiencies of the prior art, the present invention provides a polyacrylate pressure-sensitive adhesive and a preparation method thereof.

[0005] The technical problem to be solved by the present invention is achieved through the following technical solutions:

[0006] In a first aspect, a method for preparing a polyacrylate pressure-sensitive adhesive comprises the following steps: firstly mixing a hard monomer, a soft monomer, a functional monomer and a solvent, titrating an initiator A, then adding a double-bond-containing polyether phosphate (V-100P) and a polyacetylene benzene polymer, and finally adding an initiator B for reaction, followed by heat preservation and cooling to obtain a strong acid and alkali resistant flame retardant polyacrylate pressure-sensitive adhesive; wherein the mass ratio of the hard monomer, the soft monomer, the solvent, the functional monomer and the initiator is (6-10): (35-45): (40-50): (8-12): (0.2-0.4).

[0007] As a further improvement of the present invention, the hard monomer includes 1 to 3 parts of acrylic acid, 4 to 5 parts of methyl methacrylate and 3 to 4 parts of vinyl acetate.

[0008] As a further improvement of the present invention, the soft monomer includes 10-12 parts of butyl acrylate and 30-32 parts of isooctyl acrylate.

[0009] As a further improvement of the present invention, the solvent is 40-45 parts of a mixture of ethyl acetate and acetone in a weight ratio of 3:1.

[0010] As a further improvement of the present invention, the functional monomer includes 1-2 parts of trimethylolpropane monoallyl ether, 0.5-1 parts of di-trimethylolpropane, 2.2-3 parts of polyether phosphate, and 2-4 parts of polyethynylbenzene polymer.

[0011] As a further improvement of the present invention, the initiator A is 0.2-0.3 parts of azobisisobutyronitrile.

[0012] As a further improvement of the present invention, the initiator B is 0.1-0.3 parts of dibenzoyl peroxide.

[0013] A polyacrylate pressure-sensitive adhesive is prepared by the above preparation method.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] Develop a polyacrylate pressure-sensitive adhesive that is resistant to strong acid (PH=1) and strong alkali (PH=13) and has flame retardant properties (UL94-V0). The difficulty lies in the fact that it not only needs to have the performance requirements of strong acid (PH=1) and strong alkali (PH=13) resistance and flame retardant properties (UL94-V0), but also the finished tape has good adhesive properties, weather resistance, and high and low temperature resistance.

[0016] The present invention adjusts the ratio and synthesis process of acrylic acid ester monomers and active monomers containing functional groups, as well as the influence on the next step of etherified amino resin and polyisocyanate modification when synthesizing pressure-sensitive adhesive. When used, the purpose of controlling peeling force, temperature resistance, moisture resistance, acid and alkali resistance is achieved by adjusting the ratio of polyacrylate pressure-sensitive adhesive to etherified amino resin and polyisocyanate. During the synthesis process, polyether phosphate (V-100P) containing double bonds and polyacetylene benzene polymers are introduced. The polyacetylene benzene polymer contains compounds with 3 or more acetylenes on the benzene ring, which are easy to polymerize and are thermosetting resins that can form copolymers with other monomers. This copolymer absorbs heat and decomposes into carbon at high temperature to form a compact carbon layer, which is resistant to high temperature and oxidation. The glue has excellent flame retardant effect. DETAILED DESCRIPTION

[0017] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0018] Embodiment 1

[0019] A method for preparing a polyacrylate pressure-sensitive adhesive that is resistant to strong acid (PH=1) and strong alkali (PH=13) and has flame retardant properties (UL94-V0), comprising the following steps:

[0020] (1) Weigh the following raw materials in parts by weight: 10 parts of butyl acrylate, 30 parts of isooctyl acrylate, 2 parts of acrylic acid, 3 parts of vinyl acetate, 4 parts of methyl methacrylate, 1 part of trimethylolpropane monoallyl ether, 0.5 parts of di-trimethylolpropane, 2.2 parts of polyether phosphate, 2 parts of polyethynylbenzene polymer, 42 parts of solvent, 0.2 parts of initiator A, and 0.1 parts of initiator B. The solvent is a mixture of ethyl acetate and acetone in a weight ratio of 3:1. Initiator A is azobisisobutyronitrile, and initiator B is dibenzoyl peroxide.

[0021] (2) dissolving polyether phosphate in ethyl acetate and adjusting the concentration to 23% for later use;

[0022] (3) adding all of butyl acrylate, isooctyl acrylate, acrylic acid, vinyl acetate, methyl methacrylate, trimethylolpropane monoallyl ether, di-trimethylolpropane, and solvent into a reaction kettle, and stirring evenly with a stirrer at 120 rpm;

[0023] (4) Slowly raise the temperature to 68-70°C, put the dissolved initiator A into a burette with ethyl acetate, and stir while titrating to react. After 1 hour of reaction, take the prepared polyether phosphate and polyethynylbenzene polymer mixed solution and put it into another burette, and titrate the reaction at the same time. The reaction temperature is controlled at 80-85°C and the reaction time is 1.5 hours;

[0024] (5) After the titration of initiator A is completed, initiator B is dissolved in ethyl acetate and placed in a burette for titration reaction. The reaction temperature is controlled at 75-80°C and the reaction time is 3h;

[0025] (6) After the titration is completed, keep warm for 3 hours;

[0026] (7) After the insulation is completed, the material is discharged when the temperature drops below 45°C.

[0027] Embodiment 2

[0028] A method for preparing a polyacrylate pressure-sensitive adhesive that is resistant to strong acid (PH=1) and strong alkali (PH=13) and has flame retardant properties (UL94-V0), comprising the following steps:

[0029] (1) Weigh the following raw materials in parts by weight: 11 parts of butyl acrylate, 32 parts of isooctyl acrylate, 3 parts of acrylic acid, 4 parts of vinyl acetate, 4.5 parts of methyl methacrylate, 1 part of trimethylolpropane monoallyl ether, 0.8 parts of di-trimethylolpropane, 2.5 parts of polyether phosphate, 3 parts of polyethynylbenzene polymer, 40 parts of solvent, 0.25 parts of initiator A, and 0.2 parts of initiator B. The solvent is a mixture of ethyl acetate and acetone in a weight ratio of 3:1. Initiator A is azobisisobutyronitrile, and initiator B is dibenzoyl peroxide.

[0030] (2) dissolving polyether phosphate in ethyl acetate and adjusting the concentration to 23% for later use;

[0031] (3) adding all of butyl acrylate, isooctyl acrylate, acrylic acid, vinyl acetate, methyl methacrylate, trimethylolpropane monoallyl ether, di-trimethylolpropane, and solvent into a reaction kettle, and stirring evenly with a stirrer at 120 rpm;

[0032] (4) Slowly raise the temperature to 68-70°C, put the dissolved initiator A into a burette with ethyl acetate, and stir while titrating to react. After 1 hour of reaction, take the prepared polyether phosphate and polyethynylbenzene polymer mixed solution and put it into another burette, and titrate the reaction at the same time. The reaction temperature is controlled at 80-85°C and the reaction time is 1.5 hours;

[0033] (5) After the titration of initiator A is completed, initiator B is dissolved in ethyl acetate and placed in a burette for titration reaction. The reaction temperature is controlled at 75-80°C and the reaction time is 3h;

[0034] (6) After the titration is completed, keep warm for 3 hours;

[0035] (7) After the insulation is completed, the material is discharged when the temperature drops below 45°C.

[0036] Embodiment 3

[0037] A method for preparing a polyacrylate pressure-sensitive adhesive that is resistant to strong acid (PH=1) and strong alkali (PH=13) and has flame retardant properties (UL94-V0), comprising the following steps:

[0038] (1) Weigh the following raw materials in parts by weight: 12 parts of butyl acrylate, 31 parts of isooctyl acrylate, 1 part of acrylic acid, 3.5 parts of vinyl acetate, 5 parts of methyl methacrylate, 2 parts of trimethylolpropane monoallyl ether, 1 part of di-trimethylolpropane, 3 parts of polyether phosphate, 4 parts of polyethynylbenzene polymer, 45 parts of solvent, 0.3 parts of initiator A, and 0.3 parts of initiator B. The solvent is a mixture of ethyl acetate and acetone in a weight ratio of 3:1. Initiator A is azobisisobutyronitrile, and initiator B is dibenzoyl peroxide.

[0039] (2) dissolving polyether phosphate in ethyl acetate and adjusting the concentration to 23% for later use;

[0040] (3) adding all of butyl acrylate, isooctyl acrylate, acrylic acid, vinyl acetate, methyl methacrylate, trimethylolpropane monoallyl ether, di-trimethylolpropane, and solvent into a reaction kettle, and stirring evenly with a stirrer at 120 rpm;

[0041] (4) Slowly raise the temperature to 68-70°C, put the dissolved initiator A into a burette with ethyl acetate, and stir while titrating to react. After 1 hour of reaction, take the prepared polyether phosphate and polyethynylbenzene polymer mixed solution and put it into another burette, and titrate the reaction at the same time. The reaction temperature is controlled at 80-85°C and the reaction time is 1.5 hours;

[0042] (5) After the titration of initiator A is completed, initiator B is dissolved in ethyl acetate and placed in a burette for titration reaction. The reaction temperature is controlled at 75-80°C and the reaction time is 3h;

[0043] (6) After the titration is completed, keep warm for 3 hours;

[0044] (7) After the insulation is completed, the material is discharged when the temperature drops below 45°C.

[0045] The above-mentioned embodiments merely express the implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the patent scope of the present invention. Any technical solution obtained in the form of equivalent replacement or equivalent transformation shall fall within the protection scope of the present invention.

Claims

1. A method for preparing a polyacrylate pressure-sensitive adhesive, characterized in that: It includes the following steps: Firstly, a hard monomer, a soft monomer, a functional monomer and a solvent are mixed, an initiator A is titrated, and then a double-bond polyether phosphate (V-100P) and a polyacetylene benzene polymer are added, and finally an initiator B is added to react, and then the mixture is kept warm and cooled to obtain a strong acid and alkali resistant flame retardant polyacrylate pressure-sensitive adhesive; wherein the mass ratio of the hard monomer, the soft monomer, the solvent, the functional monomer and the initiator is (6-10): (35-45): (40-50): (8-12): (0.2-0.4).

2. The method for preparing the polyacrylate pressure-sensitive adhesive according to claim 1, characterized in that: The hard monomer comprises 1-3 parts of acrylic acid, 4-5 parts of methyl methacrylate and 3-4 parts of vinyl acetate.

3. The method for preparing the polyacrylate pressure-sensitive adhesive according to claim 1, characterized in that: The soft monomer includes 10-12 parts of butyl acrylate and 30-32 parts of isooctyl acrylate.

4. The method for preparing the polyacrylate pressure-sensitive adhesive according to claim 1, characterized in that: The solvent is 40-45 parts of a mixture of ethyl acetate and acetone in a weight ratio of 3:

1.

5. The method for preparing the polyacrylate pressure-sensitive adhesive according to claim 1, characterized in that: The functional monomers include 1-2 parts of trimethylolpropane monoallyl ether, 0.5-1 parts of di-trimethylolpropane, 2.2-3 parts of polyether phosphate, and 2-4 parts of polyethynylbenzene polymer.

6. The method for preparing the polyacrylate pressure-sensitive adhesive according to claim 1, characterized in that: The initiator A is 0.2-0.3 parts of azobisisobutyronitrile.

7. The method for preparing the polyacrylate pressure-sensitive adhesive according to claim 1, characterized in that: The initiator B is 0.1-0.3 parts of dibenzoyl peroxide.

8. A polyacrylate pressure-sensitive adhesive, characterized in that: It is prepared by the preparation method according to any one of claims 1 to 7.