CN115141589A - Conductive epoxy adhesive for floor cloth bonding and preparation method thereof - Google Patents

Conductive epoxy adhesive for floor cloth bonding and preparation method thereof Download PDF

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Publication number
CN115141589A
CN115141589A CN202210931757.7A CN202210931757A CN115141589A CN 115141589 A CN115141589 A CN 115141589A CN 202210931757 A CN202210931757 A CN 202210931757A CN 115141589 A CN115141589 A CN 115141589A
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parts
agent
epoxy resin
component
mixing
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王倩
聂琦思
王子平
赫长生
丛斌
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Nantong Comens New Materials Co ltd
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Nantong Comens New Materials Co ltd
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Priority to CN202210931757.7A priority Critical patent/CN115141589A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02Electrically-conducting adhesives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0812Aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives

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  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a conductive epoxy adhesive for floor cloth bonding and a preparation method thereof, wherein the adhesive comprises a component A and a component B, and the mass ratio of the component A to the component B is 100: 40-60; the component A comprises the following raw materials in parts by mass: 30-45 parts of first epoxy resin, 10-20 parts of modified flexible epoxy resin, 10-20 parts of first toughening agent, 5-10 parts of reactive diluent, 1-2 parts of coupling agent, 1-2 parts of first auxiliary agent and 55-80 parts of conductive filler; the component B comprises the following raw materials in parts by mass: 40-60 parts of modified amine curing agent, 20-30 parts of polyamide curing agent, 10-20 parts of second toughening agent, 1-2 parts of second auxiliary agent and 20-30 parts of second filler. The adhesive has the advantages of environment-friendly components, small smell, excellent adhesion effect on PVC or rubber, good toughness, aging resistance and conductivity, and capability of well meeting the adhesion requirement of floor cloth.

Description

Conductive epoxy adhesive for floor cloth bonding and preparation method thereof
Technical Field
The invention relates to the technical field of conductive epoxy adhesives, in particular to a conductive epoxy adhesive for floor cloth bonding and a preparation method thereof.
Background
In industrial production, places involving electric equipment mostly need to be subjected to antistatic treatment, particularly floors need to be subjected to antistatic treatment, and similarly, logistics transport carriages also need to be subjected to antistatic treatment, and the adoption of antistatic floor cloth is a practical and effective antistatic method.
The antistatic floor cloth is made of material capable of conducting static electricity, and its working principle is that firstly, one layer or several layers of antistatic floor cloth are laid on the floor or carriage plate, when the static electricity is produced, the layered antistatic floor cloth laid on the floor or carriage plate can make the static electricity be led into the ground, the ground is the medium for spreading static electricity, and the antistatic floor cloth is the product for conducting static electricity and connecting the ground with workplace. Antistatic floorings are typically required to be adhered to the floor or the bed panel using conductive glue.
At present, the materials of the common antistatic floor cloth mainly comprise two types, namely PVC (polyvinyl chloride) and rubber, and the conductive adhesive commonly used for the antistatic floor cloth mainly comprises acrylate adhesive and polyurethane adhesive. Acrylate adhesives have a heavy odor; the polyurethane adhesive has long curing time, strict requirements on curing environment, poor stability after long-term use and easy bulge. In the field of the existing adhesive, the epoxy adhesive has good bonding strength to various base materials, has small smell, no solvent and good environmental protection property, and is more suitable for occasions for bonding antistatic floor cloth; however, the epoxy adhesive has poor general toughness and low anti-peeling capability, the addition of the conductive filler also affects the toughness of the adhesive, the bonding effect of the epoxy adhesive on PVC and rubber materials is general, and the antistatic floor cloth is often in various vibration and friction environments or even in high and low temperature environments in the application process, and the problem of floor cloth detachment is easily caused by bonding with the epoxy adhesive, so that the conductive epoxy adhesive for bonding the floor cloth, which is environment-friendly, good in toughness, fatigue shock resistant and aging resistant, is urgently needed to be developed.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a conductive epoxy adhesive for floor cloth bonding and a preparation method thereof, which are used for solving the technical problems in the prior art. The adhesive has the advantages of environment-friendly components, no solvent, small smell, proper fluidity, proper operation time at normal temperature, excellent adhesion effect on PVC or rubber base materials, good toughness, fatigue vibration resistance, aging resistance, high humidity resistance and certain conductivity, and can well meet the adhesion requirement of floor cloth.
The purpose of the invention is realized by the following technical scheme:
a conductive epoxy adhesive for bonding floor cloth comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 100: 40-60; the component A comprises the following raw materials in parts by mass: 30-45 parts of first epoxy resin, 10-20 parts of modified flexible epoxy resin, 10-20 parts of first toughening agent, 5-10 parts of reactive diluent, 1-2 parts of coupling agent, 1-2 parts of first auxiliary agent and 55-80 parts of conductive filler; the component B comprises the following raw materials in parts by mass: 40-60 parts of modified amine curing agent, 20-30 parts of polyamide curing agent, 10-20 parts of second toughening agent, 1-2 parts of second auxiliary agent and 20-30 parts of second filler.
Preferably, the modified flexible epoxy resin is at least one of polyurethane modified epoxy resin, castor oil modified epoxy resin, organic silicon modified epoxy resin, liquid nitrile rubber modified epoxy resin, furan modified epoxy resin and vinyl modified epoxy resin.
Preferably, the first toughening agent in the component A is at least one of a nano core-shell rubber epoxy resin toughening agent, liquid silicone rubber, a Qishi toughening agent, polyether and liquid polyurethane.
Preferably, the second toughening agent in the component B is at least one of a Qishi toughening agent VL-1, a Qishi toughening agent VL-2, a Qishi toughening agent VL-3 and a Qishi toughening agent VL-4.
Preferably, the modified amine curing agent is at least one of a modified alicyclic amine curing agent and a modified aliphatic amine curing agent.
Preferably, the polyamide curing agent is at least one of a curing agent XH429, a curing agent XH351, a curing agent V140, a curing agent Ancamide 910 and a curing agent Ancamide 2766.
Preferably, the coupling agent is at least one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, and 3-methacryloxypropyltrimethoxysilane.
Preferably, the reactive diluent is one of monofunctional glycidyl ether and difunctional glycidyl ether; the monofunctional glycidyl ether is one of benzyl glycidyl ether, n-butyl glycidyl ether and polyene phenol glycidyl ether; the difunctional glycidyl ether is one of 1, 4-butanediol glycidyl ether, ethylene glycol diglycidyl ether and polyene phenol glycidyl ether.
Preferably, the first epoxy resin is at least one of bisphenol a type epoxy resin, hydrogenated bisphenol a type epoxy resin, bisphenol F type epoxy resin, and bisphenol S type epoxy resin.
A preparation method of the conductive epoxy adhesive for bonding the floor cloth comprises the following steps:
s1, preparation of a component A: adding the first epoxy resin, the modified flexible epoxy resin, the first toughening agent, the active diluent, the coupling agent and the first auxiliary agent into a reaction kettle according to the mass ratio of 30-45 parts of the first epoxy resin, 10-20 parts of the modified flexible epoxy resin, 10-20 parts of the first toughening agent, 5-10 parts of the active diluent, 1-2 parts of the coupling agent, 1-2 parts of the first auxiliary agent and 55-80 parts of the conductive filler, mixing and dispersing at normal temperature, vacuumizing in the mixing and dispersing process, adding the conductive filler into the reaction kettle after mixing and dispersing for a certain time, mixing and dispersing, vacuumizing in the mixing and dispersing process, and defoaming after mixing and dispersing for a certain time, thereby preparing a component A;
s2, preparation of a component B: adding the modified amine curing agent, the polyamide curing agent, the second toughening agent and the second auxiliary agent into a reaction kettle according to the mass ratio of 40-60 parts of the modified amine curing agent, 20-30 parts of the polyamide curing agent, 10-20 parts of the second toughening agent, 1-2 parts of the second auxiliary agent and 20-30 parts of the second filler, mixing and dispersing at normal temperature, vacuumizing in the mixing and dispersing process, adding the second filler into the reaction kettle after mixing and dispersing for a certain time, mixing and dispersing, vacuumizing in the mixing and dispersing process, and defoaming after mixing and dispersing for a certain time to obtain a component B;
and S3, matching the component A with the component B according to the mass ratio of 100: 40-60 to obtain the conductive epoxy adhesive for bonding the floor cloth.
Compared with the prior art, the special modified flexible epoxy resin is adopted, and the modified flexible epoxy resin, the first toughening agent, the second toughening agent, the modified amine curing agent, the polyamide curing agent and the coupling agent are matched according to a specific proportion for use, so that the technical effect of greatly toughening and softening is realized under the combined action of the modified flexible epoxy resin, the first toughening agent and the second toughening agent, the prepared conductive epoxy adhesive achieves good toughness and fatigue vibration resistance, the toughening and softening effects are far better than those of the conductive epoxy adhesive which is only used by the toughening agent, the bonding force of the conductive epoxy adhesive to PVC/rubber floor cloth is greatly improved under the combined action of the modified flexible epoxy resin, the modified amine curing agent, the polyamide curing agent and the coupling agent, and the bonding requirement of the floor cloth can be well met. The invention adopts the special active diluent, and the active diluent and the dispersant are matched according to the specific proportion, thereby effectively improving the fluidity of the epoxy adhesive system and leading the prepared conductive epoxy adhesive to have proper fluidity. The conductive filler with a special proportion is added into the component A, so that the prepared conductive epoxy adhesive has certain conductivity, and when the conductive epoxy adhesive is applied to the anti-static floor cloth, the anti-static floor cloth can have a good anti-static effect. The conductive epoxy adhesive for floor cloth bonding provided by the invention has the advantages of environment-friendly components, no solvent and small odor, meets the requirement of environment protection, has proper fluidity and room temperature operation time, meets the process requirement, has excellent bonding effect on PVC or rubber and other difficult-to-bond base materials, has excellent toughness, fatigue vibration resistance, aging resistance, high humidity resistance and certain conductivity, and can well meet the bonding requirement of the floor cloth.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below; it should be understood that the described embodiments are only some of the embodiments of the present invention, not all of the embodiments, and are not intended to limit the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The terms that may be used herein are first described as follows:
the terms "comprising," "including," "containing," "having," or other similar terms of meaning should be construed as non-exclusive inclusions. For example: including a feature (e.g., material, component, ingredient, carrier, formulation, material, dimension, part, component, mechanism, device, process, procedure, method, reaction condition, processing condition, parameter, algorithm, signal, data, product, or article of manufacture), is to be construed as including not only the particular feature explicitly listed but also other features not explicitly listed as such which are known in the art.
The term "parts by mass" is intended to indicate a mass ratio relationship between a plurality of components, for example: if X component is X parts by mass and Y component is Y parts by mass, the mass ratio of the X component to the Y component is X: Y;1 part by mass may represent any mass, for example: 1 part by mass may be 1kg or 3.1415926 kg. The sum of the parts by mass of all the components is not necessarily 100 parts, and may be more than 100 parts, less than 100 parts, or equal to 100 parts. Unless otherwise indicated, parts, ratios, and percentages described herein are by mass.
When concentrations, temperatures, pressures, dimensions, or other parameters are expressed as ranges of values, the ranges are to be understood as specifically disclosing all ranges formed from any pair of upper, lower, and preferred values within the range, regardless of whether ranges are explicitly recited; for example, if a numerical range of "2 to 8" is recited, then that numerical range should be interpreted to include ranges such as "2 to 7," "2 to 6," "5 to 7," "3 to 4 and 6 to 7," "3 to 5 and 7," "2 and 5 to 7," and the like. Unless otherwise indicated, the numerical ranges recited herein include both the endpoints thereof and all integers and fractions within the numerical range.
The conductive epoxy adhesive for flooring adhesion and the method for preparing the same according to the present invention will be described in detail. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art. Those not specifically mentioned in the examples of the present invention were carried out according to the conventional conditions in the art or conditions suggested by the manufacturer. The reagents or instruments used in the examples of the present invention are not specified by manufacturers, and are all conventional products available by commercial purchase.
The invention provides a conductive epoxy adhesive for bonding floor cloth, which mainly comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 100: 40-60; the component A comprises the following raw materials in parts by mass: 30-45 parts of first epoxy resin, 10-20 parts of modified flexible epoxy resin, 10-20 parts of first toughening agent, 5-10 parts of reactive diluent, 1-2 parts of coupling agent, 1-2 parts of first auxiliary agent and 55-80 parts of conductive filler; the component B comprises the following raw materials in parts by mass: 40-60 parts of modified amine curing agent, 20-30 parts of polyamide curing agent, 10-20 parts of second toughening agent, 1-2 parts of second auxiliary agent and 20-30 parts of second filler.
In some embodiments of the present invention, the mass ratio of the a component to the B component is 100:40 to 60, such as 100.
In some embodiments of the present invention, the first epoxy resin is selected from at least one of bisphenol a type epoxy resin, hydrogenated bisphenol a type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin.
In some embodiments of the present invention, the modified flexible epoxy resin is selected from at least one of polyurethane modified epoxy resin, castor oil modified epoxy resin, silicone modified epoxy resin, liquid nitrile rubber modified epoxy resin, furan modified epoxy resin, vinyl modified epoxy resin.
In some embodiments of the present invention, the first toughening agent is selected from at least one of a nano core shell rubber epoxy toughening agent, a liquid silicone rubber, a Qishi toughening agent, a polyether, and a liquid polyurethane.
In some embodiments of the present invention, the reactive diluent is selected from one of monofunctional glycidyl ethers, difunctional glycidyl ethers; the monofunctional glycidyl ether is one of benzyl glycidyl ether, n-butyl glycidyl ether and polyene phenol glycidyl ether; the bifunctional glycidyl ether is one of 1, 4-butanediol glycidyl ether, ethylene glycol diglycidyl ether and polyene phenol glycidyl ether.
In some embodiments of the invention, the coupling agent is selected from at least one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, and 3-methacryloxypropyltrimethoxysilane.
In some embodiments of the present invention, the first auxiliary agent comprises a defoamer and a dispersant. The defoaming agent is selected from BYK066N in the prior art. The dispersant is selected from BYK111 in the prior art.
In some embodiments of the present invention, the conductive filler is at least one selected from the group consisting of silver-based conductive powder, gold powder, copper powder, aluminum powder, nickel powder, conductive graphite, carbon black, metallic conductive particles, non-metallic conductive particles, and conductive high molecular polymer.
In some embodiments of the present invention, the modified amine curing agent is selected from at least one of a modified alicyclic amine curing agent and a modified aliphatic amine curing agent.
In some embodiments of the present invention, the polyamide curing agent is selected from at least one of curing agent XH429, curing agent XH351, curing agent V140, curing agent Ancamide 910, curing agent Ancamide 2766.
In some embodiments of the invention, the second toughening agent in the B component is selected from at least one of a Qishi toughening agent VL-1, a Qishi toughening agent VL-2, a Qishi toughening agent VL-3 and a Qishi toughening agent VL-4.
In some embodiments of the invention, the second auxiliary agent comprises an antifoaming agent and a dispersing agent. The defoaming agent is selected from BYK066N in the prior art. The dispersant is selected from BYK111 in the prior art.
In some embodiments of the present invention, the second filler is at least one selected from the group consisting of calcium carbonate, calcium silicate, barium sulfate, talc, silica powder, and glass powder.
The invention also provides a preparation method of the conductive epoxy adhesive for floor cloth bonding, which is used for preparing the conductive epoxy adhesive for floor cloth bonding and specifically comprises the following steps:
s1, preparation of a component A: adding the first epoxy resin, the modified flexible epoxy resin, the first toughening agent, the active diluent, the coupling agent and the first auxiliary agent into a reaction kettle according to the mass ratio of 30-45 parts of the first epoxy resin, 10-20 parts of the modified flexible epoxy resin, 10-20 parts of the first toughening agent, 5-10 parts of the active diluent, 1-2 parts of the coupling agent, 1-2 parts of the first auxiliary agent and 55-80 parts of the conductive filler, stirring, mixing and dispersing at normal temperature, wherein the planetary rotation speed is 15-20 rpm, the dispersion rotation speed is 650rpm, vacuumizing is required in the stirring, mixing and dispersing process, stirring, mixing and dispersing for 30min, adding the conductive filler into the reaction kettle, increasing the dispersion rotation speed to 750rpm, stirring, mixing and dispersing, vacuumizing is required in the stirring, mixing and dispersing process for 2h, twice cleaning the kettle, defoaming is performed after stirring, mixing and dispersing are finished, and the component A is prepared.
S2, preparation of a component B: adding the modified amine curing agent, the polyamide curing agent, the second toughening agent and the second auxiliary agent into a reaction kettle according to the mass ratio of 40-60 parts of the modified amine curing agent, 20-30 parts of the polyamide curing agent, 10-20 parts of the second toughening agent, 1-2 parts of the second auxiliary agent and 20-30 parts of the second filler, stirring, mixing and dispersing at normal temperature, wherein the planetary rotation speed is 15-20 rpm, the dispersion rotation speed is 650rpm, vacuumizing is required in the stirring, mixing and dispersing process, after stirring, mixing and dispersing for 30min, adding the second filler into the reaction kettle, increasing the dispersion rotation speed to 750rpm, stirring, mixing and dispersing, vacuumizing is required in the stirring, mixing and dispersing process, stirring, mixing and dispersing for 2h, cleaning the kettle twice during the period, and defoaming for 30min after stirring, mixing and dispersing are finished, thereby preparing the component B.
And S3, matching the component A with the component B according to the mass ratio of 100: 40-60 to obtain the conductive epoxy adhesive for bonding the floor cloth.
Compared with the prior art, the conductive epoxy adhesive for bonding the floor cloth and the preparation method thereof provided by the invention at least have the following advantages:
(1) According to the invention, the special modified flexible epoxy resin is adopted, and the modified flexible epoxy resin, the first toughening agent, the second toughening agent, the modified amine curing agent, the polyamide curing agent and the coupling agent are matched according to a specific proportion for use, and the matching of the specific proportion not only realizes the technical effects of greatly toughening and softening under the combined action of the modified flexible epoxy resin, the first toughening agent and the second toughening agent, so that the prepared conductive epoxy adhesive achieves good toughness and fatigue vibration resistance, the toughening and softening effects are far better than those of the conductive epoxy adhesive which is only used by the toughening agent, but also greatly improves the bonding force of the conductive epoxy adhesive on PVC/rubber floor cloth under the combined action of the modified flexible epoxy resin, the modified amine curing agent, the polyamide curing agent and the coupling agent, and compared with products commonly used in the field at present, the conductive epoxy adhesive has higher bonding strength, even can achieve substrate destruction, and can well meet the bonding requirements of the floor cloth.
(2) The invention adopts the special active diluent, and the active diluent and the dispersant are matched according to the specific proportion, thereby effectively improving the fluidity of the epoxy adhesive system and leading the prepared conductive epoxy adhesive to have proper fluidity.
(3) The conductive filler with a special proportion is added into the component A, so that the prepared conductive epoxy adhesive has certain conductivity, and when the conductive epoxy adhesive is applied to the anti-static floor cloth, the anti-static floor cloth can have a good anti-static effect.
(4) The invention reduces the internal stress of the system by the combined use of the flexible epoxy resin and the toughening agent; the thermal expansion coefficient of the system is reduced by using the filler with a specific proportion; through the use of the coupling agent with a specific proportion, the system cohesion is improved, the bonding interface is firmer, and the prepared conductive epoxy adhesive for bonding floor cloth has good aging resistance and high humidity resistance.
(5) The conductive epoxy adhesive for bonding the floor cloth, provided by the invention, is environment-friendly in components, free of solvent and small in smell, and can meet the environment-friendly requirement of the conductive epoxy adhesive for bonding the floor cloth.
(6) The conductive epoxy adhesive for floor cloth bonding provided by the invention has the advantages of environment-friendly components, no solvent, small smell, capability of meeting the environment-friendly requirement, proper fluidity and room-temperature operation time, capability of meeting the process requirement, excellent bonding effect on PVC or rubber and other difficult-to-bond base materials, excellent toughness, fatigue vibration resistance, aging resistance, high humidity resistance and certain conductivity, and capability of well meeting the bonding requirement of the floor cloth.
In conclusion, the adhesive disclosed by the embodiment of the invention is environment-friendly in components, free of solvent, less in smell, capable of meeting the environment-friendly requirement, appropriate in fluidity and room-temperature operation time, capable of meeting the process requirement, excellent in adhesion effect on PVC or rubber and other difficult-to-adhere base materials, excellent in toughness, fatigue vibration resistance, aging resistance, high humidity resistance and certain conductivity, and capable of well meeting the adhesion requirement of the floor cloth.
In order to more clearly show the technical solutions and effects provided by the present invention, the following detailed description will be made of specific embodiments of the conductive epoxy adhesive for bonding floor cloth and the method for preparing the same provided by the present invention.
Example 1
The preparation method of the conductive epoxy adhesive for bonding floor cloth can comprise the following steps:
s1, preparation of a component A: adding 40 parts of bisphenol A type epoxy resin, 15 parts of organosilicon modified epoxy resin, 10 parts of a Qishi toughening agent, 5 parts of N-butyl glycidyl ether, 2 parts of 3-methacryloxypropyl trimethoxy silane, 1 part of BYK066N and 1 part of BYK111 into a reaction kettle, stirring, mixing and dispersing at normal temperature, wherein the planetary rotation speed is 15-20 rpm, the dispersing rotation speed is 650rpm, vacuumizing is needed in the stirring, mixing and dispersing process, adding 60 parts of conductive graphite into the reaction kettle after stirring, mixing and dispersing for 30min, increasing the dispersing rotation speed to 750rpm, stirring, mixing and dispersing, vacuumizing is needed in the stirring, mixing and dispersing process, stirring, mixing and dispersing for 2h, cleaning the kettle twice in the period, defoaming for 30min after stirring, mixing and dispersing are finished, and thus obtaining the component A.
S2, preparing a component B: adding 50 parts of modified alicyclic amine curing agent, 25 parts of curing agent XH351, 15 parts of Qishi toughening agent VL-1, 0.5 part of BYK066N and 0.5 part of BYK111 into a reaction kettle, stirring, mixing and dispersing at normal temperature, wherein the planetary rotation speed is 15-20 rpm, the dispersion rotation speed is 650rpm, vacuumizing is needed in the stirring, mixing and dispersing process, stirring, mixing and dispersing for 30min, adding 10 parts of calcium carbonate and 15 parts of silicon micropowder into the reaction kettle, increasing the dispersion rotation speed to 750rpm, stirring, mixing and dispersing, vacuumizing is needed in the stirring, mixing and dispersing process, stirring, mixing and dispersing for 2h, cleaning the kettle twice in the period, and defoaming for 30min after stirring, mixing and dispersing are completed, thereby preparing the component B.
And S3, uniformly stirring and mixing the component A and the component B according to the mass ratio of 100:50 to obtain the conductive epoxy adhesive for bonding the floor cloth.
Example 2
The preparation method of the conductive epoxy adhesive for bonding floor cloth can comprise the following steps:
s1, preparation of a component A: according to the mass parts, 20 parts of bisphenol A type epoxy resin, 20 parts of bisphenol F type epoxy resin, 15 parts of polyurethane modified epoxy resin, 5 parts of nano core-shell rubber epoxy resin toughening agent, 5 parts of liquid polyurethane, 6 parts of N-butyl glycidyl ether, 2 parts of gamma-glycidyl ether oxypropyltrimethoxysilane, 1 part of BYK066N and 1 part of BYK111 are added into a reaction kettle, stirring, mixing and dispersing are carried out under the normal temperature condition, the planetary rotation speed is 15-20 rpm, the dispersing rotation speed is 650rpm, vacuumizing is required in the stirring, mixing and dispersing process, 60 parts of aluminum powder is added into the reaction kettle after stirring, mixing and dispersing are carried out for 30min, the dispersing rotation speed is increased to 750rpm, stirring, mixing and dispersing are carried out, vacuumizing is required in the stirring, mixing and dispersing process for 2h, the kettle is cleaned twice during the stirring, mixing and dispersing are carried out for 30min, and then defoaming treatment is carried out, so that the A component is prepared.
S2, preparation of a component B: adding 45 parts by mass of modified alicyclic amine curing agent, 30 parts by mass of curing agent Ancamide2766, 15 parts by mass of Qishi toughening agent VL-1, 0.5 part by mass of BYK066N and 0.5 part by mass of BYK111 into a reaction kettle, stirring, mixing and dispersing at normal temperature, wherein the planetary rotation speed is 15-20 rpm, the dispersing rotation speed is 650rpm, vacuumizing is needed in the stirring, mixing and dispersing processes, stirring, mixing and dispersing for 30min, adding 30 parts by mass of calcium carbonate into the reaction kettle, increasing the dispersing rotation speed to 750rpm, stirring, mixing and dispersing, vacuumizing is needed in the stirring, mixing and dispersing processes, stirring, mixing and dispersing for 2h, cleaning the kettle twice in the period, and defoaming for 30min after stirring, mixing and dispersing are completed, thereby obtaining the component B.
And S3, uniformly stirring and mixing the component A and the component B according to the mass ratio of 100:55 to obtain the conductive epoxy adhesive for bonding the floor cloth.
Example 3
The preparation method of the conductive epoxy adhesive for bonding floor cloth can comprise the following steps:
s1, preparation of a component A: according to the mass parts, 45 parts of bisphenol F type epoxy resin, 10 parts of furan modified epoxy resin, 10 parts of Qishi toughening agent, 5 parts of 1, 4-butanediol glycidyl ether, 2 parts of gamma-glycidyl ether oxypropyltrimethoxysilane, 1 part of BYK066N and 1 part of BYK111 are added into a reaction kettle, stirring, mixing and dispersing are carried out under the normal temperature condition, the planetary rotation speed is 15-20 rpm, the dispersing rotation speed is 650rpm, vacuumizing is needed in the stirring, mixing and dispersing process, after stirring, mixing and dispersing for 30min, 65 parts of conductive graphite is added into the reaction kettle, the dispersing rotation speed is increased to 750rpm, stirring, mixing and dispersing are carried out, vacuumizing is needed in the stirring, mixing and dispersing process, stirring, mixing and dispersing are carried out for 2h, the kettle is cleaned twice in the period, and defoaming treatment is carried out for 30min after stirring, so that the component A is prepared.
S2, preparation of a component B: adding 55 parts of modified aliphatic amine curing agent, 10 parts of curing agent XH351, 10 parts of curing agent Ancamide2766, 10 parts of Qishi toughening agent VL-4, 0.5 part of BYK066N and 0.5 part of BYK111 into a reaction kettle, stirring, mixing and dispersing at normal temperature, wherein the planetary rotation speed is 15-20 rpm, the dispersing rotation speed is 650rpm, vacuumizing is needed in the stirring, mixing and dispersing process, adding 30 parts of talcum powder into the reaction kettle after stirring, mixing and dispersing for 30min, and increasing the dispersing rotation speed to 750rpm, stirring, mixing and dispersing for 2h, cleaning the kettle twice in the stirring, mixing and dispersing for 30min after stirring, thereby preparing the component B.
And S3, uniformly stirring and mixing the component A and the component B according to the mass ratio of 100:50 to obtain the conductive epoxy adhesive for bonding the floor cloth.
Comparative example 1
A conductive epoxy adhesive, prepared substantially as in example 1, except that: the modified flexible epoxy resin is not adopted in the step S1, and the polyamide curing agent is not adopted in the step S1.
Performance detection
The following performance tests were performed on the conductive epoxy adhesives for flooring adhesion prepared in examples 1, 2 and 3 of the present invention and the conductive epoxy adhesive prepared in comparative example 1, respectively:
viscosity of component A: the measurement was carried out according to GB/T2794-2013 Single-Cylinder rotational viscometer method for measuring viscosity of adhesives.
Viscosity of the component B: measured according to GB/T2794-2013 Single-Cylinder rotational viscometer method for measuring viscosity of adhesive.
Viscosity after mixing: the measurement was carried out according to GB/T2794-2013 Single-Cylinder rotational viscometer method for measuring viscosity of adhesives.
The operation time is as follows: measured according to GB/T7123.1-2015 "working time for Multi-component Adhesives".
Shear strength/6061 aluminum: measured according to GB/T7124-2008 "determination of tensile shear strength of adhesive (rigid material to rigid material)".
Shear strength/304 stainless steel: measured according to GB/T7124-2008 "determination of tensile shear strength of adhesive (rigid material to rigid material)".
Shear strength/PVC: measured according to GB/T33334-2016 test method for Single Lap tensile shear Strength of Adhesives (composite to composite).
90 ° peel strength/rubber-1060 aluminum alloy: according to GB/T7122-1996, determination of peel strength of high-strength adhesive-floating roll method.
90 ° peel strength/PVC-1060 aluminum alloy: according to GB/T7122-1996, determination of peel strength of high-strength adhesive-floating roll method.
High temperature and high humidity: according to GB/T2423.50 environmental test part 2: test method test Cy constant moist heat was mainly used for the accelerated test of elements, test for 15 days.
Fatigue vibration: the fatigue vibration was carried out 100 ten thousand times in accordance with ISO 9664.
Volume resistivity: according to GB/T31838.2-2019 part 2 dielectric and resistance characteristics of solid insulating materials: resistance characteristics (DC method) volume resistance and volume resistivity.
The detection results of the above performance detection are shown in table 1 below:
TABLE 1
Figure BDA0003781809050000101
Figure BDA0003781809050000111
From the above examples and table 1 it can be seen that: the conductive epoxy adhesive for bonding floor cloths prepared in the embodiments 1, 2 and 3 has a proper operation time of 55-60 min at a normal temperature of 25 ℃, a viscosity of 13500-14720 mPa.s after mixing, proper fluidity, good bonding performance to aluminum-aluminum and stainless steel-stainless steel, a bonding strength to 6061 aluminum and 6061 aluminum of 19.10-20.01 MPa, a bonding strength to 304 stainless steel and 304 stainless steel of 23.35-24.01 MPa, excellent bonding effects to metal, rubber and PVC, is suitable for bonding metal, rubber/metal and PVC, can resist damp and heat for a long time, has small strength attenuation (not more than 7.5%) after 100 ten thousand fatigue vibrations, is obviously stronger than a comparative example 1, and has a strength of 5.12 × 10 5 ~5.78×10 5 The proper volume resistivity of omega cm can well meet the conductive requirement of the floor cloth; according to the embodiment of the invention, multiple toughening and flexibility increasing effects are realized by skillfully matching and using the modified flexible epoxy resin, the first toughening agent, the second toughening agent, the modified amine curing agent, the polyamide curing agent and the coupling agent, the peel strength test is superior to that of comparative example 1, the high-temperature and high-humidity resistance is superior to that of comparative example 1, and the excellent toughness is proved; the prepared conductive epoxy adhesive has obviously enhanced bonding performance on PVC or rubber base materials, has excellent toughness, fatigue and vibration resistance, aging resistance, high humidity resistance and certain conductivity, and can well meet the requirementsAnd (4) the bonding requirement of the plate cloth.
In conclusion, the components of the embodiment of the invention are environment-friendly, solvent-free, less in smell and suitable in fluidity, the operation time is suitable at normal temperature, the PVC or rubber base material has excellent bonding effect, and the bonding agent has good toughness, fatigue vibration resistance, aging resistance, high humidity resistance and certain conductivity, and can well meet the bonding requirement of the floor cloth.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.

Claims (10)

1. The conductive epoxy adhesive for bonding floor cloth is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 100: 40-60;
the component A comprises the following raw materials in parts by mass: 30-45 parts of first epoxy resin, 10-20 parts of modified flexible epoxy resin, 10-20 parts of first toughening agent, 5-10 parts of reactive diluent, 1-2 parts of coupling agent, 1-2 parts of first auxiliary agent and 55-80 parts of conductive filler;
the component B comprises the following raw materials in parts by mass: 40-60 parts of modified amine curing agent, 20-30 parts of polyamide curing agent, 10-20 parts of second toughening agent, 1-2 parts of second auxiliary agent and 20-30 parts of second filler.
2. The conductive epoxy adhesive for bonding floor cloth according to claim 1, wherein the modified flexible epoxy resin is at least one of polyurethane modified epoxy resin, castor oil modified epoxy resin, silicone modified epoxy resin, liquid nitrile rubber modified epoxy resin, furan modified epoxy resin, and vinyl modified epoxy resin.
3. The conductive epoxy adhesive for floor cloth bonding according to claim 1 or 2, wherein the first toughening agent in the component A is at least one of a nano core-shell rubber epoxy resin toughening agent, a liquid silicone rubber, a Qishi toughening agent, a polyether and a liquid polyurethane.
4. The conductive epoxy adhesive for floor cloth bonding according to claim 1 or 2, wherein the second toughening agent in the component B is at least one of a qishi toughening agent VL-1, a qishi toughening agent VL-2, a qishi toughening agent VL-3 and a qishi toughening agent VL-4.
5. The conductive epoxy adhesive for bonding floor cloth according to claim 1 or 2, wherein the modified amine curing agent is at least one of a modified alicyclic amine curing agent and a modified aliphatic amine curing agent.
6. The conductive epoxy adhesive for bonding floor cloth according to claim 1 or 2, wherein the polyamide curing agent is at least one of a curing agent XH429, a curing agent XH351, a curing agent V140, a curing agent Ancamide 910, and a curing agent Ancamide 2766.
7. The conductive epoxy adhesive for flooring adhesion according to claim 1 or 2, wherein the coupling agent is at least one of γ -aminopropyltriethoxysilane, γ -glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, and 3-methacryloxypropyltrimethoxysilane.
8. The conductive epoxy adhesive for floor cloth bonding according to claim 1 or 2, wherein the reactive diluent is one of monofunctional glycidyl ether and difunctional glycidyl ether;
the monofunctional glycidyl ether is one of benzyl glycidyl ether, n-butyl glycidyl ether and polyene phenol glycidyl ether;
the difunctional glycidyl ether is one of 1, 4-butanediol glycidyl ether, ethylene glycol diglycidyl ether and polyene phenol glycidyl ether.
9. The conductive epoxy adhesive for flooring adhesion according to claim 1 or 2, wherein the first epoxy resin is at least one of bisphenol a epoxy resin, hydrogenated bisphenol a epoxy resin, bisphenol F epoxy resin, and bisphenol S epoxy resin.
10. A method for preparing the conductive epoxy adhesive for floor cloth bonding of any one of the above claims 1 to 9, comprising the steps of:
s1, preparation of a component A: adding the first epoxy resin, the modified flexible epoxy resin, the first toughening agent, the reactive diluent, the coupling agent and the first auxiliary agent into a reaction kettle according to the mass ratio of 30-45 parts of the first epoxy resin, 10-20 parts of the modified flexible epoxy resin, 10-20 parts of the first toughening agent, 5-10 parts of the reactive diluent, 1-2 parts of the coupling agent, 1-2 parts of the first auxiliary agent and 55-80 parts of the conductive filler, mixing and dispersing at normal temperature, vacuumizing in the mixing and dispersing process, adding the conductive filler into the reaction kettle after mixing and dispersing for a certain time, mixing and dispersing, vacuumizing in the mixing and dispersing process, and defoaming after mixing and dispersing for a certain time, thereby preparing a component A;
s2, preparation of a component B: adding the modified amine curing agent, the polyamide curing agent, the second toughening agent and the second auxiliary agent into a reaction kettle according to the mass ratio of 40-60 parts of the modified amine curing agent, 20-30 parts of the polyamide curing agent, 10-20 parts of the second toughening agent, 1-2 parts of the second auxiliary agent and 20-30 parts of the second filler, mixing and dispersing at normal temperature, vacuumizing in the mixing and dispersing process, adding the second filler into the reaction kettle after mixing and dispersing for a certain time, mixing and dispersing, vacuumizing in the mixing and dispersing process, and defoaming after mixing and dispersing for a certain time to obtain a component B;
s3, the component A and the component B are used together according to the mass ratio of 100: 40-60, so that the conductive epoxy adhesive for bonding the floor cloth, which is disclosed by any one of the claims 1 to 9, is obtained.
CN202210931757.7A 2022-08-04 2022-08-04 Conductive epoxy adhesive for floor cloth bonding and preparation method thereof Pending CN115141589A (en)

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CN116355568A (en) * 2023-03-24 2023-06-30 核工业理化工程研究院 Adhesive sealant special for rubber ring and preparation method thereof

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CN111087958A (en) * 2019-12-20 2020-05-01 北京高盟新材料股份有限公司 Room-temperature fast-curing epoxy adhesive and preparation method thereof
CN111777977A (en) * 2020-07-22 2020-10-16 北京高盟新材料股份有限公司 Room-temperature fast-curing transparent epoxy adhesive for bonding engineering plastics and preparation method thereof
CN114292612A (en) * 2022-01-07 2022-04-08 北京高盟新材料股份有限公司 Single-component epoxy flexible adhesive and preparation method thereof
CN114316867A (en) * 2021-12-24 2022-04-12 南通高盟新材料有限公司 Weather-resistant room-temperature curing epoxy electronic pouring sealant and preparation method thereof

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CN109749680A (en) * 2017-11-06 2019-05-14 北京天山新材料技术有限公司 Floor cloth adhesive glue
CN111087958A (en) * 2019-12-20 2020-05-01 北京高盟新材料股份有限公司 Room-temperature fast-curing epoxy adhesive and preparation method thereof
CN111777977A (en) * 2020-07-22 2020-10-16 北京高盟新材料股份有限公司 Room-temperature fast-curing transparent epoxy adhesive for bonding engineering plastics and preparation method thereof
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