阅读说明：本技术 高粘阻燃环保的压敏胶及制备方法和压敏胶膜的制备方法 (High-viscosity flame-retardant environment-friendly pressure-sensitive adhesive, preparation method thereof and preparation method of pressure-sensitive adhesive film ) 是由 胡文光 樊勤海 樊秋实 魏彦龙 于 2019-10-31 设计创作，主要内容包括：本发明公开一种高粘阻燃环保的压敏胶及制备方法和压敏胶膜的制备方法,压敏胶的组分为：丙烯酸酯硬单体：5-10份,丙烯酸酯软单体：15-25份,丙烯酸酯功能单体：2-5份、含磷活性单体：5-10份、引发剂：0.5-2份、有机溶剂：30-40份、高效复合阻燃剂：10-20份、固化剂：0.5-2份；通过化学合成和物理复配的方法制备压敏胶,选择定量的丙烯酸酯类单体以及具有阻燃效果的含磷功能单体,合成出具有高粘着性且有一定阻燃效果的压敏胶聚合物,并在合成后期添加多种环保高效阻燃剂,协同增效机理,提高了阻燃效果,并且使得压敏胶具有高粘着性、高温持粘性和阻燃效果显著的特点,且阻燃等级达到Vo等级,满足电子工业固定、粘接等加工需求。(The invention discloses a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive, a preparation method thereof and a preparation method of a pressure-sensitive adhesive film, wherein the pressure-sensitive adhesive comprises the following components: acrylate hard monomer: 5-10 parts of acrylate soft monomer: 15-25 parts of acrylate functional monomer: 2-5 parts of phosphorus-containing active monomer: 5-10 parts of initiator: 0.5-2 parts of organic solvent: 30-40 parts of efficient composite flame retardant: 10-20 parts of curing agent: 0.5-2 parts; the pressure-sensitive adhesive is prepared by a chemical synthesis and physical compounding method, a certain amount of acrylate monomers and phosphorus-containing functional monomers with flame retardant effects are selected to synthesize a pressure-sensitive adhesive polymer with high adhesiveness and certain flame retardant effect, a plurality of environment-friendly and efficient flame retardants are added at the later stage of synthesis, the synergistic mechanism is cooperated, the flame retardant effect is improved, the pressure-sensitive adhesive has the characteristics of high adhesiveness, high-temperature viscosity and remarkable flame retardant effect, the flame retardant grade reaches the Vo grade, and the processing requirements of electronic industry on fixation, bonding and the like are met.)

1. The high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive is characterized by comprising the following components:

acrylate hard monomer: 5-10 parts of

Acrylate soft monomer: 15-25 parts of

Acrylate functional monomer: 2-5 parts of

Phosphorus-containing reactive monomers: 5-10 parts of

Initiator: 0.5 to 2 portions of

Organic solvent: 30-40 parts of

High-efficiency composite flame retardant: 10-20 parts of

Curing agent: 0.5-2 parts.

2. The high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive according to claim 1, which is characterized by comprising the following components:

acrylate hard monomer: 6-10 parts of

Acrylate soft monomer: 15-22 parts of

Acrylate functional monomer: 2.5 to 5 portions of

Phosphorus-containing reactive monomers: 9-10 parts of

Initiator: 1-2 parts of

Organic solvent: 36-40 parts of

High-efficiency composite flame retardant: 10 to 18 portions of

Curing agent: 1.5-2 parts.

3. The high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive according to claim 1, which is characterized by comprising the following components:

acrylate hard monomer: 8-10 parts of

Acrylate soft monomer: 15-20 parts of

Acrylate functional monomer: 3-5 parts of

Phosphorus-containing reactive monomers: 9-10 parts of

Initiator: 1-2 parts of

Organic solvent: 36-40 parts of

High-efficiency composite flame retardant: 10 to 18 portions of

Curing agent: 1.5-2 parts.

4. The high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive according to claim 1, wherein the acrylate hard monomer comprises one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate and ethyl acrylate; the acrylate soft monomer comprises one or more of butyl acrylate, isooctyl acrylate, butyl methacrylate, isooctyl methacrylate and lauryl methacrylate.

5. The high viscosity flame retardant environment friendly pressure sensitive adhesive of claim 1, wherein the acrylate functional monomer comprises one or more of acrylic acid, methacrylic acid, hydroxypropyl methacrylate, glycidyl methacrylate and methylol acrylamide.

6. The high viscosity flame retardant environment friendly pressure sensitive adhesive according to claim 1, wherein the phosphorus containing reactive monomer comprises mainly one or more of hydroxyethyl acrylate phosphate, 2-ethyl (acyloxymethyl methacrylate) phosphate, 2-ethyl acryloyloxymethyl phosphate and 2-ethyl (acyloxymethyl methacrylate) phosphate.

7. The high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive according to claim 1, wherein the initiator comprises one of benzoyl peroxide, iso-phenylpropyl hydroperoxide, dicumyl peroxide, methyl ethyl ketone peroxide and azobisisobutyronitrile; the organic solvent comprises two or more of ethyl acetate, butyl acetate, butanone, methyl butyl ketone, N-dimethylformamide and N, N-dimethylacetamide.

8. The high viscosity flame retardant environmental friendly pressure sensitive adhesive according to claim 1, wherein the high efficiency flame retardant comprises two or more of ammonium polyphosphate, triethyl phosphate, trimethyl phosphite, cyclic phosphate, tricresyl phosphate, melamine pyrophosphate, zinc borate, magnesium hydroxide, aluminum hydroxide; the curing agent comprises one or more of triethylene tetramine, methylene bis (phenylenediamine) and aminoethyl piperazine.

9. A preparation method of a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive is characterized by comprising the following steps:

s1: dividing the organic solvent into two parts according to the ratio of 3: 1;

s2: adding an acrylate monomer and a large amount of organic solvent into a reaction vessel, and stirring at the speed of 150-250 r/min;

s3: introducing nitrogen into the reaction vessel, and setting the temperature to be 80-90 ℃;

s4: dissolving an initiator into a small amount of organic solvent to form an initiator solution, slowly dropwise adding the initiator solution and a phosphorus-containing active monomer into a reactor, and keeping the dropwise adding time for 2-3 h;

s5: waiting for reaction for 1-2 hours, cooling to 40 ℃, adjusting the stirring speed to 800-;

s6: and adding a curing agent, and uniformly stirring to obtain the high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive product.

10. A preparation method of a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive film is characterized in that,

s1: coating the pressure-sensitive adhesive prepared in claim 10 on a double-sided release paper;

s2: baking at 100-120 deg.C for 2-5 min; after curing, the flame-retardant adhesive film with the dry adhesive thickness of 50-60um is prepared.

Technical Field

The invention relates to the field of adhesives, in particular to a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive, a preparation method thereof and a preparation method of a pressure-sensitive adhesive film.

Background

The pressure-sensitive adhesive is an adhesive sensitive to pressure, is a high molecular polymer which can be firmly combined with an adherend by only lightly pressing without solvent, heat or other means, is widely applied to various fields such as electronics, electric appliances, automobiles, machinery, aerospace, light industry, medical treatment, family life and the like, but is extremely easy to burn, easily brings potential safety hazards and limits the application range of the pressure-sensitive adhesive because most of the pressure-sensitive adhesive is an acrylic polymer;

in the invention patent with the patent application number of 201410109500.9 and the name of a halogen-free flame-retardant pressure-sensitive adhesive and a preparation method thereof, the halogen-free flame-retardant pressure-sensitive adhesive is prepared by physically mixing the pressure-sensitive adhesive and a flame retardant, and the flame-retardant adhesive prepared by the method is often insufficient in cohesive strength and poor in sustained viscosity under a high-temperature condition; in the invention patent with the patent application number of 201710760770.X and the name of the flame-retardant acrylate pressure-sensitive adhesive for cold lamination and the preparation method thereof, the flame-retardant acrylate pressure-sensitive adhesive is prepared by introducing a phosphorus-containing flame-retardant monomer in the polymerization process, but the flame-retardant effect of the pressure-sensitive adhesive is not ideal; in the invention patent with the patent application number of 201310586418.0 and the name of a flame-retardant waterproof sealing hot-melt pressure-sensitive adhesive and a preparation method thereof, the pressure-sensitive adhesive contains decabromodiphenyl ether flame retardant, so that the halogen limit standard is not reached, and the environment is not protected;

therefore, a pressure-sensitive adhesive with good flame retardant effect, good adhesion and environmental protection is urgently needed.

Disclosure of Invention

Aiming at the defects in the technology, the invention provides a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive, a preparation method thereof and a preparation method of the pressure-sensitive adhesive film.

In order to achieve the purpose, the invention adopts the following technical scheme:

the high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive comprises the following components:

wherein, the components of the pressure-sensitive adhesive are as follows:

wherein, the components of the pressure-sensitive adhesive are as follows:

wherein the acrylate hard monomer comprises one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate and ethyl acrylate; the acrylate soft monomer comprises one or more of butyl acrylate, isooctyl acrylate, butyl methacrylate, isooctyl methacrylate, and lauryl methacrylate.

Wherein the acrylate functional monomer comprises one or more of acrylic acid, methacrylic acid, hydroxypropyl methacrylate, glycidyl methacrylate and hydroxymethyl acrylamide.

Wherein the phosphorus-containing active monomer mainly comprises one or more of acrylic acid hydroxyethyl phosphate, 2-ethyl (acyloxymethyl methacrylate) phosphate, 2-ethyl acryloyloxymethyl phosphate and 2-ethyl (acyloxymethyl methacrylate) phosphate.

Wherein the initiator comprises one of benzoyl peroxide, isopropyl phenyl hydroperoxide, dicumyl peroxide, methyl ethyl ketone peroxide and azodiisobutyronitrile; the organic solvent comprises two or more of ethyl acetate, butyl acetate, butanone, methyl butyl ketone, N-dimethylformamide and N, N-dimethylacetamide.

Wherein the high-efficiency flame retardant comprises two or more of ammonium polyphosphate, triethyl phosphate, trimethyl phosphite, cyclic phosphate, tricresyl phosphate, melamine pyrophosphate, zinc borate, magnesium hydroxide and aluminum hydroxide

Wherein the curing agent comprises one or more of triethylene tetramine, methylene bisphenyldiamine and aminoethyl piperazine.

A preparation method of a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive comprises the following steps:

s1: dividing the organic solvent into two parts according to the ratio of 3: 1;

s2: adding an acrylate monomer and a large amount of organic solvent into a reaction vessel, and stirring at the speed of 150-250 r/min;

s3: introducing nitrogen into the reaction vessel, and setting the temperature to be 80-90 ℃;

s4: dissolving an initiator into a small amount of organic solvent to form an initiator solution, slowly dropwise adding the initiator solution and a phosphorus-containing active monomer into a reactor, and keeping the dropwise adding time for 2-3 h;

s5: waiting for reaction for 1-2 hours, cooling to 40 ℃, adjusting the stirring speed to 800-;

s6: and adding a curing agent, and uniformly stirring to obtain the high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive product.

A preparation method of a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive film,

s1: coating the pressure-sensitive adhesive prepared in claim 10 on a double-sided release paper;

s2: baking at 100-120 deg.C for 2-5 min; after curing, the flame-retardant adhesive film with the dry adhesive thickness of 50-60um is prepared.

The invention has the beneficial effects that: compared with the prior art, the high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive comprises the following components in parts by weight: acrylate hard monomer: 5-10 parts of acrylate soft monomer: 15-25 parts of acrylate functional monomer: 2-5 parts of phosphorus-containing active monomer: 5-10 parts of initiator: 0.5-2 parts of organic solvent: 30-40 parts of efficient composite flame retardant: 10-20 parts of curing agent: 0.5-2 parts; the preparation method of the high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive comprises the following steps: s1: dividing the organic solvent into two parts according to the ratio of 3: 1; s2: adding an acrylate monomer and a large amount of organic solvent into a reaction vessel, and stirring at the speed of 150-250 r/min; s3: introducing nitrogen into the reaction vessel, and setting the temperature to be 80-90 ℃; s4: dissolving an initiator into a small amount of organic solvent to form an initiator solution, slowly dropwise adding the initiator solution and a phosphorus-containing active monomer into a reactor, and keeping the dropwise adding time for 2-3 h; s5: waiting for reaction for 1-2 hours, cooling to 40 ℃, adjusting the stirring speed to 800-; s6: adding a curing agent, and uniformly stirring to obtain a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive product; the pressure-sensitive adhesive is prepared by a chemical synthesis and physical compounding method, a certain amount of acrylate monomers and phosphorus-containing functional monomers with flame retardant effect are selected to synthesize a pressure-sensitive adhesive polymer with high adhesiveness and certain flame retardant effect, a plurality of environment-friendly and efficient flame retardants are added at the later stage of synthesis, the synergistic mechanism is cooperated, the flame retardant effect is improved, the pressure-sensitive adhesive has the characteristics of high adhesiveness, high-temperature lasting adhesiveness and remarkable flame retardant effect, the flame retardant grade reaches the Vo grade, and the processing requirements of electronic industry on fixation, bonding and the like are met.

Drawings

FIG. 1 is a flow chart of the method of the present invention.

Detailed Description

In order to more clearly illustrate the technical solutions in the present technology, the drawings used in the description of the embodiments or the prior art will be described below.

In recent years, the electronic and automobile industries have rapidly developed, and great progress is made. The adhesive has wide application in the industries of electronics, electric appliances, automobiles and the like, and mainly plays roles in protecting the production process and pasting and fixing components. With the technology upgrading of the industries becoming faster and faster, the requirements on the performance of the adhesive are higher and higher, and especially the requirements on the flame retardance, the viscosity, the temperature resistance, the content control of harmful components and the like of the adhesive are stricter and stricter. The high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive has the characteristics of environmental protection, flame retardance, high viscosity and convenience in use, can be used for fixing electronic and automobile parts, can be applied to the fields of laminating of EVA, PU and other fireproof foam cotton, and has very wide application and very wide market prospect and economic value. Therefore, the flame-retardant pressure-sensitive adhesive product with excellent performance is developed, can meet the urgent needs of the current market, and obtains huge economic return.

The embodiment provides a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive, which comprises the following components:

the composition of the pressure sensitive adhesive of this example was:

the composition of the pressure sensitive adhesive of this example was:

the acrylate hard monomer of the present embodiment includes one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate, and ethyl acrylate; the acrylate soft monomer comprises one or more of butyl acrylate, isooctyl acrylate, butyl methacrylate, isooctyl methacrylate, and lauryl methacrylate.

The acrylate functional monomer of this embodiment includes one or more of acrylic acid, methacrylic acid, hydroxypropyl methacrylate, glycidyl methacrylate, and methylol acrylamide.

The phosphorus-containing reactive monomer of this example comprises primarily one or more of hydroxyethyl acrylate phosphate, 2-ethyl (acyloxymethyl methacrylate) phosphate, 2-ethyl acryloyloxymethyl phosphate and 2-ethyl (acyloxymethyl methacrylate) phosphate.

The initiator of the embodiment comprises one of benzoyl peroxide, isopropyl phenyl hydroperoxide, dicumyl peroxide, methyl ethyl ketone peroxide and azobisisobutyronitrile; the organic solvent comprises two or more of ethyl acetate, butyl acetate, butanone, methyl butyl ketone, N-dimethylformamide and N, N-dimethylacetamide.

The high-efficiency flame retardant of the embodiment comprises two or more of ammonium polyphosphate, triethyl phosphate, trimethyl phosphite, cyclic phosphate, tricresyl phosphate, melamine pyrophosphate, zinc borate, magnesium hydroxide and aluminum hydroxide

The curing agent of the embodiment comprises one or more of triethylene tetramine, methylene bis (phenylenediamine) and aminoethyl piperazine.

The preparation method of the high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive comprises the following steps:

s1: dividing the organic solvent into two parts according to the ratio of 3: 1;

s2: adding an acrylate monomer and a large amount of organic solvent into a reaction vessel, and stirring at the speed of 150-250 r/min;

s3: introducing nitrogen into the reaction vessel, and setting the temperature to be 80-90 ℃;

s4: dissolving an initiator into a small amount of organic solvent to form an initiator solution, slowly dropwise adding the initiator solution and a phosphorus-containing active monomer into a reactor, and keeping the dropwise adding time for 2-3 h;

s5: waiting for reaction for 1-2 hours, cooling to 40 ℃, adjusting the stirring speed to 800-;

s6: adding a curing agent, and uniformly stirring to obtain a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive product;

a preparation method of a high-viscosity flame-retardant environment-friendly pressure-sensitive adhesive film,

s1: coating the pressure-sensitive adhesive prepared in claim 10 on a double-sided release paper;

s2: baking at 100-120 deg.C for 2-5 min; after curing, the flame-retardant adhesive film with the dry adhesive thickness of 50-60um is prepared.

The pressure-sensitive adhesive is prepared by a chemical synthesis and physical compounding method, a certain amount of acrylate monomers and phosphorus-containing functional monomers with flame retardant effect are selected to synthesize a pressure-sensitive adhesive polymer with high adhesiveness and certain flame retardant effect, a plurality of environment-friendly and efficient flame retardants are added at the later stage of synthesis, the synergistic mechanism is cooperated, the flame retardant effect is improved, the pressure-sensitive adhesive has the characteristics of high adhesiveness, high-temperature lasting adhesiveness and remarkable flame retardant effect, the flame retardant grade reaches the Vo grade, and the processing requirements of electronic industry on fixation, bonding and the like are met.