CN113755103A - Epoxy adhesive with initial pressure sensitivity and preparation method thereof - Google Patents

Epoxy adhesive with initial pressure sensitivity and preparation method thereof Download PDF

Info

Publication number
CN113755103A
CN113755103A CN202111102804.9A CN202111102804A CN113755103A CN 113755103 A CN113755103 A CN 113755103A CN 202111102804 A CN202111102804 A CN 202111102804A CN 113755103 A CN113755103 A CN 113755103A
Authority
CN
China
Prior art keywords
parts
acrylate
mixture
methacrylate
epoxy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111102804.9A
Other languages
Chinese (zh)
Inventor
周国庆
王建斌
陈田安
解海华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yantai Darbond Technology Co Ltd
Original Assignee
Yantai Darbond Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yantai Darbond Technology Co Ltd filed Critical Yantai Darbond Technology Co Ltd
Priority to CN202111102804.9A priority Critical patent/CN113755103A/en
Publication of CN113755103A publication Critical patent/CN113755103A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention discloses an epoxy adhesive with initial pressure sensitivity, which comprises the following components in parts by weight: 40-60 parts of low-viscosity epoxy resin, 5-40 parts of curing agent, 5-15 parts of acrylate tackifier, 2-5 parts of methacrylate, 0.5-2 parts of accelerator and 0.2-1.0 part of stabilizer; the acrylate tackifier comprises the following raw materials in parts by weight: 40-60 parts of acrylate soft monomer, 5-15 parts of acrylate containing epoxy group, 2-5 parts of acrylic acid crosslinking monomer and 0.5-2 parts of initiator; and 100-500 ppm of a polymerization inhibitor. The single-component epoxy adhesive can be fixed in the initial stage, has high bonding strength after curing, and is convenient to produce and apply.

Description

Epoxy adhesive with initial pressure sensitivity and preparation method thereof
Technical Field
The invention belongs to the field of adhesives, and particularly relates to an epoxy adhesive with initial pressure sensitivity and a preparation method thereof.
Background
Epoxy resins have many excellent properties. The colorless transparent adhesive is commonly used in the optical field due to its excellent light transmittance and refractive index, especially for the bonding of special parts of optical instruments such as distance measuring instruments, altimeters, telescopes, microscopes, lenses of projectors, magnifying glasses and the like, and is generally positioned and bonded by pressure-sensitive adhesive abroad, but the bonding strength is not high. And the initial pasting and positioning are difficult by only using the epoxy adhesive, the mold is needed for positioning, and the construction efficiency is not high. Therefore, further improvements are awaited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an epoxy adhesive with initial pressure sensitivity and a preparation method thereof. The single-component epoxy adhesive can be fixed in the initial stage, has high bonding strength after curing, and is convenient to produce and apply.
The specific technical scheme is as follows:
the invention aims to provide an epoxy adhesive with initial pressure-sensitive property, which comprises the following components in parts by weight:
40-60 parts of low-viscosity epoxy resin, 5-40 parts of curing agent, 5-15 parts of acrylate tackifier, 2-5 parts of methacrylate, 0.5-2 parts of accelerator and 0.2-1.0 part of stabilizer;
the acrylate tackifier comprises the following raw materials in parts by weight: 40-60 parts of acrylate soft monomer, 5-15 parts of acrylate containing epoxy group, 2-5 parts of acrylic acid crosslinking monomer and 0.5-2 parts of initiator; and 100-500 ppm of a polymerization inhibitor.
Furthermore, the raw materials of the acrylate tackifier also comprise 50-105 parts by weight of a solvent. And removing the solvent in a vacuumizing mode after the synthesis is finished. The solvent is preferably one or more of toluene, ethyl acetate, methyl ethyl ketone, isopropyl alcohol, cyclohexane, tetrahydrofuran, and N, N-dimethylformamide, and ethyl acetate and toluene are preferably used.
Further, the acrylate soft monomer is one or more than two of ethyl acrylate, n-butyl acrylate, isobutyl acrylate, n-octyl acrylate, isooctyl methacrylate, n-dodecyl methacrylate and isododecyl methacrylate; among them, n-butyl acrylate and/or isooctyl acrylate are preferably used.
Further, the acrylate containing epoxy groups is glycidyl acrylate or/and glycidyl methacrylate; among them, glycidyl methacrylate is preferably used.
Further, the acrylic acid crosslinking monomer is one or more than two of acrylonitrile, acrylic acid, methacrylic acid and acrylamide; among them, acrylonitrile is preferably used.
Further, the initiator is one or more than two of benzoyl peroxide, azodiisobutyronitrile, tert-butyl peroxy-2-ethylhexanoate and tert-butyl peroxybenzoate; among them, azobisisobutyronitrile is preferably used.
Further, the polymerization inhibitor is hydroquinone, 2-tert-butyl hydroquinone, p-hydroxyanisole and p-benzoquinone; among them, hydroquinone is preferably used.
Further, the low-viscosity epoxy resin is one or more of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin, aliphatic epoxy resin and alicyclic epoxy resin; bisphenol a type epoxy resin, hydrogenated bisphenol a type epoxy resin, or bisphenol F type epoxy resin is preferable. The low-viscosity epoxy resin can increase the toughness of the adhesive and improve the compatibility with the acrylate tackifier.
Further, the viscosity of the low-viscosity epoxy resin is 500-5000 cps.
Further, the curing agent is one or more of dicyandiamide and derivatives thereof, organic acid hydrazide and imidazole epoxy-amine adducts, and the imidazole epoxy-amine adducts are preferred.
The methacrylate is one or more selected from methyl methacrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate, preferably hydroxypropyl methacrylate.
Further, the accelerant is acetylacetone metal salt. Among them, aluminum acetylacetonate is preferably used.
Further, the stabilizer is an ultraviolet absorber and/or a light stabilizer. Among them, UV-531 and/or light stabilizer 770 are preferably used.
The invention also aims to provide a preparation method of the epoxy adhesive with initial pressure sensitivity, which comprises the following steps:
(1) mixing low-viscosity epoxy resin, a curing agent and a stabilizer, and stirring for 40-60 min to obtain a first adhesive liquid;
(2) adding an acrylate tackifier and an accelerant into the first adhesive liquid obtained in the step (1), and stirring for 40-60 min to obtain a second adhesive liquid;
(3) and (3) adding methacrylate into the second adhesive liquid obtained in the step (2), continuously stirring for 30-40 min, vacuumizing for 1-2 h, and filtering.
The stirring in steps (1) to (3) may be performed in a vacuum stirrer.
Wherein, the filtration in the step (3) can be directly filtered into a container by adopting a 300-mesh filter screen or filtered by adopting a filter with a 30-40um filter bag.
Further, the preparation method of the acrylate tackifier comprises the following steps:
(1) mixing 70% of acrylate soft monomer, 50% of acrylic acid crosslinking monomer, 30% of initiator and 40% of solvent to obtain a mixture A; mixing 30% of acrylate soft monomer, 30% of acrylic acid crosslinking monomer, 30% of initiator and 30% of solvent to obtain a mixture B; mixing 100% of epoxy group-containing acrylate, 20% of acrylic acid crosslinking monomer, 30% of initiator and 20% of solvent to obtain a mixture C; mixing 10% of initiator and 5% of solvent to obtain a mixture D; mixing 100% of polymerization inhibitor and 5% of solvent to obtain a mixture E;
(2) adding the mixture A into a reaction kettle, controlling the reaction temperature at 64-66 ℃, and reacting for 30-45 min;
(3) raising the reaction temperature to 74-76 ℃, and dropwise adding the mixture B into the reaction kettle at a constant speed within 50-70 min;
(4) continuously reacting for 25-35 min at the reaction temperature of 74-76 ℃;
(5) raising the reaction temperature to 80-82 ℃, and dropwise adding the mixture C into the reaction kettle at a constant speed within 50-70 min;
(6) continuously reacting for 90-120 min at the reaction temperature of 80-82 ℃;
(7) raising the reaction temperature to 84-86 ℃, and dropwise adding the mixture D into the reaction kettle at a constant speed within 5-10 min;
(8) continuously reacting for 120-150 min at the reaction temperature of 84-86 ℃;
(9) and adding the mixture E into a reaction kettle, stirring for 30-60 min, and vacuumizing to remove the solvent.
Further, the reaction steps (1) to (8) are all protected with nitrogen.
The invention has the following beneficial effects:
1. the acrylic ester tackifier is added, so that the pressure-sensitive adhesive has initial pressure-sensitive property and high strength after curing.
2. The invention has simple production process and meets the requirement of industrial production.
3. The invention has simple sizing process and greatly improves the application and use efficiency of the epoxy resin.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
The epoxy adhesive with initial pressure sensitivity comprises the following raw materials in parts by weight:
60 parts of low-viscosity epoxy resin (Yueyang Barlin Huaxing petrochemical Co., Ltd., bisphenol A type epoxy resin, the trade name CYD-115, the viscosity of 700-1100), 40 parts of curing agent (Japan monosodium salt, imidazole epoxy-amine adduct, the trade name PN23J), 15 parts of acrylate tackifier, 5 parts of hydroxypropyl methacrylate, 2 parts of accelerator (aluminum acetylacetonate) and 1.0 part of stabilizer (UV-531).
The acrylate tackifier comprises the following components in parts by weight:
40 parts of butyl acrylate, 5 parts of glycidyl methacrylate, 3 parts of acrylonitrile, 0.5 part of azodiisobutyronitrile serving as an initiator, 200ppm of hydroquinone serving as a polymerization inhibitor, 20 parts of toluene and 31.5 parts of ethyl acetate.
The preparation method of the epoxy adhesive comprises the following steps:
step one, preparing an acrylate tackifier:
(1) mixing 70% of acrylate soft monomer, 50% of acrylic acid crosslinking monomer, 30% of initiator and 40% of solvent to obtain a mixture A; mixing 30% of acrylate soft monomer, 30% of acrylic acid crosslinking monomer, 30% of initiator and 30% of solvent to obtain a mixture B; mixing 100% of epoxy group-containing acrylate, 20% of acrylic acid crosslinking monomer, 30% of initiator and 20% of solvent to obtain a mixture C; mixing 10% of initiator and 5% of solvent to obtain a mixture D; mixing 100% of polymerization inhibitor and 5% of solvent to obtain a mixture E;
(2) adding the mixture A into a reaction kettle, controlling the reaction temperature at 64-66 ℃, and reacting for 30 min;
(3) raising the reaction temperature to 74-76 ℃, and dropwise adding the mixture B at a constant speed within 50 min;
(4) continuously reacting for 35min at the reaction temperature of 74-76 ℃;
(5) raising the reaction temperature to 80-82 ℃, and dropwise adding the mixture C at a constant speed within 60 min;
(6) continuously reacting for 90min at the reaction temperature of 80-82 ℃;
(7) raising the reaction temperature to 84-86 ℃, and dropwise adding the mixture D at a constant speed within 5 min;
(8) continuously reacting for 150min at the reaction temperature of 84-86 ℃;
(9) the mixture E was added to the reaction kettle, stirred for 30min and vacuumed to remove all solvents.
The reaction steps (1) to (8) are all protected by nitrogen.
Step two, preparing an epoxy adhesive:
(1) adding low-viscosity epoxy resin, a curing agent and a stabilizing agent into a vacuum stirrer, and stirring for 40min to obtain a first adhesive liquid;
(2) adding an acrylate tackifier and an accelerant into the first adhesive liquid obtained in the step (1), and stirring for 60min to obtain a second adhesive liquid;
(3) and (3) adding methacrylate into the second adhesive liquid obtained in the step (2), continuously stirring for 30min, and then vacuumizing for 1 h.
Example 2
The epoxy adhesive with initial pressure sensitivity comprises the following raw materials in parts by weight:
40 parts of low-viscosity epoxy resin (bisphenol F type epoxy resin, name YDF-175S, viscosity 2000-5000, national chemical Co., Ltd.), 10 parts of curing agent (imidazole epoxy-amine adduct, name PN23J, Japan monosodium glutamate Co., Ltd.), 10 parts of acrylate tackifier, 3 parts of hydroxypropyl methacrylate, 1 part of accelerator (aluminum acetylacetonate), and 1 part of stabilizer (light stabilizer 770).
The acrylate tackifier comprises the following components in parts by weight:
60 parts of isooctyl acrylate, 15 parts of glycidyl methacrylate, 5 parts of acrylonitrile, 1.2 parts of initiator azobisisobutyronitrile, 500ppm of polymerization inhibitor hydroquinone, 35 parts of toluene and 70 parts of ethyl acetate.
The preparation method of the epoxy adhesive comprises the following steps:
step one, preparing an acrylate tackifier:
(1) mixing 70% of soft monomer, 50% of crosslinking monomer, 30% of initiator and 40% of solvent to obtain a mixture A; mixing 30% of soft monomer, 30% of crosslinking monomer, 30% of initiator and 30% of solvent to obtain a mixture B; mixing 100% of epoxy group-containing acrylate, 20% of crosslinking monomer, 30% of initiator and 20% of solvent to obtain a mixture C; mixing 10% of initiator and 5% of solvent to obtain a mixture D; mixing 100% of polymerization inhibitor and 5% of solvent to obtain a mixture E;
(2) adding the mixture A into a reaction kettle, controlling the reaction temperature to be 64-66 ℃, and reacting for 45 min;
(3) raising the reaction temperature to 74-76 ℃, and dropwise adding the mixture B at a constant speed within 70 min;
(4) continuously reacting for 25min at the reaction temperature of 74-76 ℃;
(5) raising the reaction temperature to 80-82 ℃, and dropwise adding the mixture C at a constant speed within 50 min;
(6) continuously reacting for 120min at the reaction temperature of 80-82 ℃;
(7) raising the reaction temperature to 84-86 ℃, and dropwise adding the mixture D at a constant speed within 10 min;
(8) continuously reacting for 120min at the reaction temperature of 84-86 ℃;
(9) the mixture E was added to the reaction kettle, stirred for 60min and vacuumed to remove all solvents.
The reaction steps (1) to (8) are all protected by nitrogen.
Step two, preparing an epoxy adhesive:
(1) adding low-viscosity epoxy resin, a curing agent and a stabilizing agent into a vacuum stirrer, and stirring for 60min to obtain a first adhesive liquid;
(2) adding an acrylate tackifier and an accelerant into the first adhesive liquid obtained in the step (1), and stirring for 40min to obtain a second adhesive liquid;
(3) and (3) adding methacrylate into the second adhesive liquid obtained in the step (2), continuously stirring for 40min, vacuumizing for 2h, and directly filtering to a container by using a 300-mesh filter screen.
Example 3
The epoxy adhesive with initial pressure sensitivity comprises the following raw materials in parts by weight:
50 parts of low-viscosity epoxy resin (Yueyang Barlin Huaxing petrochemical Co., Ltd., hydrogenated bisphenol A type epoxy resin, trade name ST-1000, viscosity 1000-2000), 5 parts of curing agent (Japanese monosodium glutamate, imidazole epoxy-amine adduct, trade name PN23), 5 parts of acrylate tackifier, 2 parts of hydroxypropyl methacrylate, 0.5 part of accelerator (aluminum acetylacetonate), and 0.2 part of stabilizer (UV-531).
The acrylate tackifier comprises the following components in parts by weight:
30 parts of butyl acrylate, 20 parts of isooctyl acrylate, 10 parts of glycidyl methacrylate, 2 parts of acrylonitrile, 2 parts of azodiisobutyronitrile serving as an initiator, 500ppm of hydroquinone serving as a polymerization inhibitor, 28 parts of toluene and 62 parts of ethyl acetate.
The preparation method of the epoxy adhesive comprises the following steps:
step one, preparing an acrylate tackifier:
(1) mixing 70% of soft monomer, 50% of crosslinking monomer, 30% of initiator and 40% of solvent to obtain a mixture A; mixing 30% of soft monomer, 30% of crosslinking monomer, 30% of initiator and 30% of solvent to obtain a mixture B; mixing 100% of epoxy group-containing acrylate, 20% of crosslinking monomer, 30% of initiator and 20% of solvent to obtain a mixture C; mixing 10% of initiator and 5% of solvent to obtain a mixture D; 100% of a polymerization inhibitor and 5% of a solvent were mixed to obtain a mixture E.
(2) Adding the mixture A into a reaction kettle, controlling the reaction temperature to be 64-66 ℃, and reacting for 45 min;
(3) raising the reaction temperature to 74-76 ℃, and dropwise adding the mixture B at a constant speed within 70 min;
(4) continuously reacting for 30min at the reaction temperature of 74-76 ℃;
(5) raising the reaction temperature to 80-82 ℃, and dropwise adding the mixture C at a constant speed within 70 min;
(6) continuously reacting for 120min at the reaction temperature of 80-82 ℃;
(7) raising the reaction temperature to 84-86 ℃, and dropwise adding the mixture D at a constant speed within 5 min;
(8) continuously reacting for 135min at the reaction temperature of 84-86 ℃;
(9) the mixture E was added to the reaction kettle, stirred for 45min and all solvents were removed by vacuum.
The reaction steps (1) to (8) are all protected by nitrogen.
Step two, preparing an epoxy adhesive:
(1) adding low-viscosity epoxy resin, a curing agent and a stabilizing agent into a vacuum stirrer, and stirring for 50min to obtain a first adhesive liquid;
(2) adding an acrylate tackifier and an accelerant into the first adhesive liquid obtained in the step (1), and stirring for 60min to obtain a second adhesive liquid;
(3) and (3) adding methacrylate into the second adhesive liquid obtained in the step (2), continuously stirring for 30min, vacuumizing for 1.5h, and directly filtering into a container by using a 300-mesh filter screen.
Example 4
The epoxy adhesive with initial pressure sensitivity comprises the following raw materials in parts by weight:
50 parts of low-viscosity epoxy resin (Myzuki Co., Ltd., bisphenol A epoxy resin, trade name EPON 9504, viscosity 1300-2000), 20 parts of curing agent (NOKO, imidazole epoxy-amine adduct, trade name PN40J), 10 parts of acrylate tackifier, 4 parts of hydroxypropyl methacrylate, 1.5 parts of accelerator (aluminum acetylacetonate), 0.4 part of stabilizer (UV-531) and 0.4 part of stabilizer (light stabilizer 770).
The acrylate tackifier comprises the following components in parts by weight:
15 parts of butyl acrylate, 30 parts of isooctyl acrylate, 8 parts of glycidyl methacrylate, 3 parts of acrylonitrile, 0.8 part of azodiisobutyronitrile serving as an initiator, 100ppm of hydroquinone serving as a polymerization inhibitor, 8 parts of toluene and 60 parts of ethyl acetate.
The preparation method of the epoxy adhesive comprises the following steps:
step one, preparing an acrylate tackifier:
(1) mixing 70% of soft monomer, 50% of crosslinking monomer, 30% of initiator and 40% of solvent to obtain a mixture A; mixing 30% of soft monomer, 30% of crosslinking monomer, 30% of initiator and 30% of solvent to obtain a mixture B; mixing 100% of epoxy group-containing acrylate, 20% of crosslinking monomer, 30% of initiator and 20% of solvent to obtain a mixture C; mixing 10% of initiator and 5% of solvent to obtain a mixture D; mixing 100% of polymerization inhibitor and 5% of solvent to obtain a mixture E;
(2) adding the mixture A into a reaction kettle, controlling the reaction temperature to be 64-66 ℃, and reacting for 45 min;
(3) raising the reaction temperature to 74-76 ℃, and dropwise adding the mixture B at a constant speed within 65 min;
(4) continuously reacting for 35min at the reaction temperature of 74-76 ℃;
(5) raising the reaction temperature to 80-82 ℃, and dropwise adding the mixture C at a constant speed within 60 min;
(6) continuously reacting for 105min at the reaction temperature of 80-82 ℃;
(7) raising the reaction temperature to 84-86 ℃, and dropwise adding the mixture D at a constant speed within 10 min;
(8) continuously reacting for 150min at the reaction temperature of 84-86 ℃;
(9) the mixture E was added to the reaction kettle, stirred for 50min and vacuumed to remove all solvents.
The reaction steps (1) to (8) are all protected by nitrogen.
Step two, preparing an epoxy adhesive:
(1) adding low-viscosity epoxy resin, a curing agent and a stabilizing agent into a vacuum stirrer, and stirring for 50min to obtain a first adhesive liquid;
(2) adding an acrylate tackifier and an accelerant into the first adhesive liquid obtained in the step (1), and stirring for 60min to obtain a second adhesive liquid;
(3) and (3) adding methacrylate into the second adhesive liquid obtained in the step (2), continuously stirring for 30min, vacuumizing for 1.5h, and directly filtering into a container by using a 300-mesh filter screen.
Comparative example 1
Referring to example 3, the difference from example 3 is that the synthesis of the acrylate tackifier is not performed and the acrylate tackifier is not added to the raw material components of the epoxy adhesive;
the remaining technical features are the same as those of example 3.
Testing
The epoxy adhesives obtained in examples 1 to 4 and comparative example 1 were coated on a 0.200mm thick PET film with a bond line thickness of 0.200mm, cured at 120 ℃ for 60min, and tested in the following ways (1) and (2):
(1) initial viscosity: the test was carried out according to method B of GB/T31125 & 2014 adhesive tape initial tack test method Loop method.
(2)180 ° peel strength: the test was carried out according to method 1 of GB/T2792 + 2014 adhesive tape peel strength test method.
The epoxy adhesives obtained in examples 1 to 4 and comparative example 1 were coated on a stainless steel sheet, the thickness of the adhesive layer was 0.200mm, and cured at 120 ℃ for 60min, and the following tests (3) and (4) were carried out:
(3) shear strength: the tensile shear strength of the adhesive is tested according to GB/T7124 and 2008 (rigid material to rigid material);
(4) tensile strength: the tensile shear strength of the adhesive is tested according to GB/T7124 and 2008 (rigid material to rigid material).
The results of the above tests are shown in table 1.
TABLE 1
Item Example 1 Example 2 Example 3 Example 4 Comparative example 1
Initial tack (N) 7.42 3.26 8.22 7.46 0
180 degree peel strength (N/mm) 0.36 0.44 0.56 0.46 0
Shear strength (MPa) 11.58 10.82 12.84 9.30 14.8
Tensile Strength (MPa) 30.23 36.58 35.66 28.20 40.28
As can be seen from the test results of table 1, example 3 exhibited excellent effects, and can be considered as the best example of the present application. As can be seen from the results shown in Table 1, an epoxy adhesive having initial pressure-sensitive properties of the present invention satisfies the requirements.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The epoxy adhesive with initial pressure sensitivity is characterized by comprising the following components in parts by weight:
40-60 parts of low-viscosity epoxy resin, 5-40 parts of curing agent, 5-15 parts of acrylate tackifier, 2-5 parts of methacrylate, 0.5-2 parts of accelerator and 0.2-1.0 part of stabilizer;
the acrylate tackifier comprises the following raw materials in parts by weight: 40-60 parts of acrylate soft monomer, 5-15 parts of acrylate containing epoxy group, 2-5 parts of acrylic acid crosslinking monomer and 0.5-2 parts of initiator; and 100-500 ppm of a polymerization inhibitor.
2. The epoxy adhesive as claimed in claim 1, wherein the acrylate tackifier further comprises 50-105 parts by weight of a solvent.
3. The epoxy adhesive according to claim 2, wherein the solvent is one or more of toluene, ethyl acetate, methyl ethyl ketone, isopropyl alcohol, cyclohexane, tetrahydrofuran, and N, N-dimethylformamide.
4. The epoxy adhesive according to any one of claims 1 to 3, wherein the acrylate soft monomer is one or more of ethyl acrylate, n-butyl acrylate, isobutyl acrylate, n-octyl acrylate, isooctyl methacrylate, n-dodecyl methacrylate, and isododecyl methacrylate.
5. The epoxy adhesive according to claim 1 to 3, wherein the acrylate containing an epoxy group is glycidyl acrylate or/and glycidyl methacrylate.
6. The epoxy adhesive according to claim 1 to 3,
the acrylic acid crosslinking monomer is one or more than two of acrylonitrile, acrylic acid, methacrylic acid and acrylamide;
the initiator is one or more than two of benzoyl peroxide, azobisisobutyronitrile, tert-butyl peroxy-2-ethylhexanoate and tert-butyl peroxybenzoate;
the polymerization inhibitor is one or more than two of hydroquinone, 2-tert-butyl hydroquinone, p-hydroxyanisole and p-benzoquinone.
7. The epoxy adhesive according to claim 1 to 3, wherein the low-viscosity epoxy resin is one or more of bisphenol A type epoxy resin, bisphenol F type epoxy resin, aliphatic epoxy resin, and alicyclic epoxy resin.
8. The epoxy adhesive according to claim 1 to 3,
the curing agent is one or more than two of dicyandiamide and derivatives thereof, organic acid hydrazide and imidazole epoxy-amine addition products;
the methacrylate is one or more than two of methyl methacrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate;
the accelerant is acetylacetone metal salt;
the stabilizer is an ultraviolet absorbent and/or a light stabilizer.
9. A method for preparing an epoxy adhesive having initial pressure-sensitive properties according to any one of claims 1 to 8, comprising the steps of:
(1) mixing low-viscosity epoxy resin, a curing agent and a stabilizer, and stirring for 40-60 min to obtain a first adhesive liquid;
(2) adding an acrylate tackifier and an accelerant into the first adhesive liquid obtained in the step (1), and stirring for 40-60 min to obtain a second adhesive liquid;
(3) and (3) adding methacrylate into the second adhesive liquid obtained in the step (2), continuously stirring for 30-40 min, vacuumizing for 1-2 h, and filtering.
10. The method of claim 9, wherein the acrylate tackifier is prepared by the method comprising the steps of:
(1) mixing 70% of acrylate soft monomer, 50% of acrylic acid crosslinking monomer, 30% of initiator and 40% of solvent to obtain a mixture A; mixing 30% of acrylate soft monomer, 30% of acrylic acid crosslinking monomer, 30% of initiator and 30% of solvent to obtain a mixture B; mixing 100% of epoxy group-containing acrylate, 20% of acrylic acid crosslinking monomer, 30% of initiator and 20% of solvent to obtain a mixture C; mixing 10% of initiator and 5% of solvent to obtain a mixture D; mixing 100% of polymerization inhibitor and 5% of solvent to obtain a mixture E;
(2) adding the mixture A into a reaction kettle, controlling the reaction temperature at 64-66 ℃, and reacting for 30-45 min;
(3) raising the reaction temperature to 74-76 ℃, and dropwise adding the mixture B into the reaction kettle at a constant speed within 50-70 min;
(4) continuously reacting for 25-35 min at the reaction temperature of 74-76 ℃;
(5) raising the reaction temperature to 80-82 ℃, and dropwise adding the mixture C into the reaction kettle at a constant speed within 50-70 min;
(6) continuously reacting for 90-120 min at the reaction temperature of 80-82 ℃;
(7) raising the reaction temperature to 84-86 ℃, and dropwise adding the mixture D into the reaction kettle at a constant speed within 5-10 min;
(8) continuously reacting for 120-150 min at the reaction temperature of 84-86 ℃;
(9) and adding the mixture E into a reaction kettle, stirring for 30-60 min, and vacuumizing to remove the solvent.
CN202111102804.9A 2021-09-18 2021-09-18 Epoxy adhesive with initial pressure sensitivity and preparation method thereof Pending CN113755103A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111102804.9A CN113755103A (en) 2021-09-18 2021-09-18 Epoxy adhesive with initial pressure sensitivity and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111102804.9A CN113755103A (en) 2021-09-18 2021-09-18 Epoxy adhesive with initial pressure sensitivity and preparation method thereof

Publications (1)

Publication Number Publication Date
CN113755103A true CN113755103A (en) 2021-12-07

Family

ID=78796525

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111102804.9A Pending CN113755103A (en) 2021-09-18 2021-09-18 Epoxy adhesive with initial pressure sensitivity and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113755103A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114874750A (en) * 2022-06-16 2022-08-09 东莞市奥嘉特高分子材料有限公司 Water-based adhesive for bonding rubber and metal and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04189885A (en) * 1990-04-26 1992-07-08 Nippon Carbide Ind Co Inc Thermosetting pressure-sensitive adhesive composition and thermosetting pressure-sensitive adhesive sheet
CN103980847A (en) * 2014-05-21 2014-08-13 天津大学 Self-curing polyacrylate-epoxy resin adhesive as well as preparation method and application of self-curing polyacrylate-epoxy resin adhesive
CN112646517A (en) * 2020-12-24 2021-04-13 苏州赛伍应用技术股份有限公司 Pressure-sensitive adhesive, pressure-sensitive adhesive tape, and preparation method and application thereof
CN112940662A (en) * 2021-04-26 2021-06-11 苏州赛伍应用技术股份有限公司 Reactive pressure-sensitive adhesive, pressure-sensitive adhesive tape and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04189885A (en) * 1990-04-26 1992-07-08 Nippon Carbide Ind Co Inc Thermosetting pressure-sensitive adhesive composition and thermosetting pressure-sensitive adhesive sheet
CN103980847A (en) * 2014-05-21 2014-08-13 天津大学 Self-curing polyacrylate-epoxy resin adhesive as well as preparation method and application of self-curing polyacrylate-epoxy resin adhesive
CN112646517A (en) * 2020-12-24 2021-04-13 苏州赛伍应用技术股份有限公司 Pressure-sensitive adhesive, pressure-sensitive adhesive tape, and preparation method and application thereof
CN112940662A (en) * 2021-04-26 2021-06-11 苏州赛伍应用技术股份有限公司 Reactive pressure-sensitive adhesive, pressure-sensitive adhesive tape and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114874750A (en) * 2022-06-16 2022-08-09 东莞市奥嘉特高分子材料有限公司 Water-based adhesive for bonding rubber and metal and preparation method thereof

Similar Documents

Publication Publication Date Title
JP5801514B1 (en) Photocurable pressure-sensitive adhesive composition, pressure-sensitive adhesive sheet, and laminate
JP6545251B2 (en) Photocurable liquid optically clear adhesive composition and use thereof
US6683147B2 (en) Method for the production of glass or plastic laminates by use of a curable blend of an epoxy resin and a high Tg polymer
CN114806418B (en) Preparation and application of OCA (optically clear adhesive) for touch screen
CN111808534B (en) Ultraviolet light curing liquid optical cement and preparation method and application thereof
CN109593497B (en) UV-cured acrylate pressure-sensitive adhesive suitable for plastic material and preparation method and application thereof
CN101910344A (en) Adhesive composition, and an adhesive polarising plate and liquid crystal display device comprising the same
WO2016117045A1 (en) Pressure-sensitive adhesive sheet, process for producing same, and process for producing optical member using same
JP2004091499A (en) Pressure-sensitive adhesive composition for optical member and pressure-sensitive adhesive sheet for optical member using the same pressure-sensitive adhesive composition
CN113999632A (en) Water-based acrylate pressure-sensitive adhesive and preparation method thereof
CN113755103A (en) Epoxy adhesive with initial pressure sensitivity and preparation method thereof
CN112778916B (en) Special fluorine-containing pressure-sensitive adhesive and preparation method thereof
CN110437792A (en) Optical cement and preparation method thereof suitable for the fitting of curved surface polycarbonate plate
EP1858999B1 (en) Pressure sensitive adhesive composition as well as a method of applying it and a method for the preparation thereof
JP6002145B2 (en) Method for producing radiation curable composition
CN104559854B (en) Hydroxyl-terminated polybutadiene modified acrylic pressure-sensitive adhesive for refrigerator fixing adhesive tape
JP2017082168A (en) Optical active energy ray polymerizable adhesive and optical laminate
CN108359400A (en) A kind of environment-friendly type UV curing adhesives and preparation method thereof
CN115477900B (en) Acrylic optical adhesive with three-layer structure and preparation method thereof
CN112961613B (en) Adhesive applied to AF display screen protective film, preparation method of adhesive and protective film
CN115627124A (en) Low-whitening impact-resistant quick-drying adhesive composition and preparation method thereof
JP2022085858A (en) Photocurable adhesive composition and adhesive film
CN115287026B (en) Water-based acrylate pressure-sensitive adhesive and preparation method thereof
KR102293568B1 (en) Composition for foam adhesive tape and foam adhesive tape comprising cured product thereof
CN109929492B (en) Single-component acrylic acid adhesive for window film and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20211207