KR20210065014A - Low temperature adhesive composition and manufacturing method thereof - Google Patents

Abstract

The present disclosure relates to a low-temperature adhesive composition and a method for manufacturing the same, and more specifically, to a low-temperature adhesive composition which implements an adhesive layer maintaining adhesion even at low temperatures and a method for manufacturing the same.

Description

Low temperature adhesive composition and manufacturing method thereof

The present disclosure relates to a low-temperature pressure-sensitive adhesive composition, a tape using the same, and a method for manufacturing the same, and more particularly, to a low-temperature pressure-sensitive adhesive composition having an adhesive layer maintaining adhesion even at low temperatures, and a method for manufacturing the same.

Modern human life is living with electronic products with various functions. In particular, mobile phones and TVs are a part of life that goes beyond the necessities of modern people. Therefore, these mobile phones and TVs require more environmental factors than any other products.

Modern electronic product manufacturing is being put into production by applying adhesive processing to electronic parts with various functions for the highest productivity within the fastest time. At this time, the most used is an adhesive, which is usually implemented as a tape in the form of a film.

In spite of the innovative productivity improvement of adhesive-processed parts and materials, it is inevitable to detect unreacted toxic monomers and toluene, which are very harmful to the human body. Of course, an emulsion method for synthesizing a polymer in water rather than an atmosphere of an organic solvent was developed over 30 years ago, but the application field due to the limitations of its physical properties is very insignificant. In addition, a method using light (UV) has been recently proposed, but in reality, a manufacturing cost increase of 5 to 10 times or more compared to the existing oil-based products reveals the limit of diversification along with the local aspect of the application field.

It is practically very important to fundamentally remove toluene generated from various adhesive processing parts used in electronic products, especially mobile phones and TVs. In addition, it is very important to remove unreacted monomers that have a harmful effect on the human body.

In addition, in 2017, the coldest wave in North America for the first time in 100 years caused the sensible temperature to drop to minus 70°C, resulting in casualties, and at the same time, electronic equipment malfunctions and abnormalities were accompanied. This is one of the causes of product quality deterioration due to freeze-hardening of adhesive materials among materials included in electronic devices, and the need for developing adhesive materials with excellent low temperature resistance is required.

The present disclosure aims to develop an adhesive and an adhesive material that fundamentally eliminates the detection of toluene regulated in developed countries and does not cause product quality degradation even at low temperatures by maintaining adhesion even at -10°C or lower.

In the case of cold-resistant tapes, there are product groups made using silicone-based adhesives, but they have disadvantages such as lack of price competitiveness, weak adhesion, and difficulty in implementing BTX-free compared to acrylic tapes. Among the acrylic adhesive tapes, there are cold-resistant tapes, but BTX-free non-applied products account for a large proportion, and they have insufficient weather resistance to be applied to the mobile phone and display markets.

In the case of a polymer, it has a Tg value. If it is higher than the corresponding temperature, it has soft properties like a viscoelastic material, and at a temperature lower than Tg, it has a hard property like a solid. For example, the Tg of gum has a soft property at 36.5°C, which is about 29°C, which corresponds to the human body temperature, but exists as a solid solid when exhaled and exposed to a temperature lower than 29°C.

In the case of acrylic adhesive, it is synthesized by setting Tg at -40 to -45℃ normally, but adding a tackifying resin to improve adhesive strength. Since the softening point of the tackifier resin is high at 80~150℃, it is a cause of improving the total Tg of the adhesive. This causes the adhesive to harden easily when exposed to low temperatures, resulting in product quality degradation. When a low-molecular-weight adhesive is included in place of the tackifying resin, the effect of improving the adhesive strength is obtained and the total Tg can be maintained, which helps to have low-temperature resistance.

Pressure-sensitive adhesive (PSA) refers to a material that has adhesiveness at room temperature and is attached to an adherend with low pressure. In general, an adhesive product refers to a tape, etc., which is applied to various substrates.

As the industry develops, high-performance adhesive products are needed in each field, and they are used in various fields such as electrical and electronic insulating tapes, automotive tapes, medical tapes, label tapes, and building and civil engineering curing and waterproofing tapes, and the adhesive market is getting bigger

The characteristics of the adhesive tape may be expressed as adhesiveness, peeling force, cohesive force, and anchoring force. First, adhesion refers to initial adhesion, which means instantaneous adhesion, and refers to properties related to ease of attachment when attaching a tape. Second, peeling force is related to the magnitude of the viscoelastic strain energy at the interface of the adherend, and as the width of the tape increases, the resistance increases. Third, the cohesive force is a holding force and is affected by the force between branches, the degree of crosslinking, the structure and molecular weight of molecules, etc. Fourth, anchoring force refers to the bonding force between the support and the adhesive.

The following characteristics are required in order for the adhesive tape to adhere to the adherend and to come off cleanly without leaving the adhesive on the other adherend.

Tack > Adhesion > Cohesion > Keying strength

Adhesives can be classified by product type, use, and component. It is divided into emulsified, solvent, and solvent-free types according to the type of product, and emulsified pressure-sensitive adhesives are used by using monomers that do not mix with water so that the molecular structure exists in a colloidal form in aqueous solution through a polymer polymerization process. Water is the main raw material, and both rubber and acrylic are used. Solvent-type pressure-sensitive adhesives have been developed for the first time among pressure-sensitive adhesives and have been used in various ways until now, but there is a risk of environmental contamination due to solvents, and the raw materials include rubber, acrylic, resin, and the like. There are countless types of rubber, natural rubber, synthetic rubber, acrylic, resin and resin. Solvent-free adhesives are adhesives manufactured and used only with special rubber or acrylic monomers without the use of solvents, and although investment in facilities and concerns about environmental pollution are reduced, high technology and burden of raw materials are very disadvantageous.

It is divided into permanent type and re-peelable type by use. The permanent type is a type in which the cohesive force is constant but the adhesive strength changes over time, and the re-peelable type is known to have constant cohesive and adhesive strength even over time.

By component, it can be divided into rubber, vinyl, silicone, and acrylic. Rubber-based adhesives are mainly made of natural or synthetic rubber and tackifying resin, and have good adhesive strength, but because they contain unsaturated functional groups, they are weak to heat and UV rays and easily deteriorate. A vinyl-based pressure-sensitive adhesive is a copolymer of vinyl ether and acrylate, which is added to a solvent-free pressure-sensitive adhesive to improve adhesion. Silicone pressure-sensitive adhesives are made of high molecular weight polymethyl silane or polydimethyldiphenyl silane having a functional silanol (SiOH) group at the end of the molecular chain.

Acrylic adhesive is an adhesive whose use is increasing by replacing rubber adhesive, and can be used in various forms such as solvent, water-based, emulsion, hot melt, and solid reactive adhesive. It is a radical polymer containing acrylic acid ester as a main component or an oxidation-reduction polymer with a water-soluble catalyst. It has superior weather resistance, heat resistance, and oil resistance than adhesives of other components, and has the advantage of arbitrarily introducing a polar group into the polymer molecule. It has the great advantage of being able to arbitrarily control cohesive force, tackiness and adhesion by crosslinking, etc., and has little change in transparency and adhesion even when exposed to ultraviolet and oxygen in the atmosphere. Because it does not cause a reaction, its practical value is very high enough to be used for surgical tapes and food packaging.

Acrylic solution type adhesive has excellent weather resistance and oil resistance, and at the same time, copolymerization with other vinyl monomers is active, so it has the advantage of being able to introduce a polar group arbitrarily into a polymer molecule and making an adhesive suitable for the purpose relatively easily. However, since a crosslinking agent and an organic solvent are used as a medium, there is a smell during processing and a fire hazard. On the other hand, the drying speed is fast and the adhesion to the substrate is good during adhesion. Since the shelf life is about 5 months to 2 years, solution-type adhesives are widely used.

As the adhesive component in the acrylic pressure-sensitive adhesive, C ₄ to C ₁₀ acrylic acid alkyl esters having an alkyl group (eg, butyl acrylate, butyl methacrylate, hexyl acrylate, hexyl methacrylate, n-octyl acrylate, n -octyl methacrylate, isooctyl acrylate, isooctyl methacrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate, isononyl acrylate, isononyl methacrylate, etc.), and the Tg of the polymer is It is about -20 ~ -70℃. It has good adhesion but poor cohesiveness, so a cohesive component is required. The aggregation components include ethyl acrylate and vinyl acetate, and they play a role in increasing Tg and smoothing the synthesis reaction. This cohesive component not only increases cohesiveness, but also sometimes helps to improve various performances such as adhesion improvement, water resistance improvement, and transparency.

The inclusion of a functional group in the monomer is one of the good methods for improving the physical properties of the pressure-sensitive adhesive, and the functional groups include a monomer containing a carboxyl group (-COOH), a hydroxyl group (-OH) of acrylic acid, an acid amide (e.g., acrylic acid, methacrylic acid, 2-methacryloxy acetic acid, 3-methacryloxy propyl acid, 4-methacryloxy butyric acid, fumaric acid, maleic acid, maleic anhydride, 2-hydroxyethyl methacrylate as a hydroxyl group-containing monomer; 2-hydroxypropyl methacrylate, 4-hydroxybutyl methacrylate, 6-hydroxyhexyl methacrylate, 8-hydroxyoctyl methacrylate, 2-hydroxyethylene glycol methacrylate, which is a nitrogen-containing monomer. acrylamide, N-vinyl caprolactam, etc.). This not only performs crosslinking, but also improves cohesiveness or adhesion. In any case, a blending technique is required to balance the basic performance of the adhesive, such as tackiness, cohesiveness, and initial tack, and since the three physical properties have opposite tendencies, the degree of polymerization (Drgree of polymerization) and number average molecular weight (Mn: Number-average molecular weight), etc. to control the physical properties of the adhesive.

Since the monomer for the pressure-sensitive adhesive needs fluidity at room temperature and the Tg must be lowered, a copolymer of an acrylic acid alkyl ester having about _{C 2} to C _{10 alkyl group is used.} The acrylic pressure-sensitive adhesive is composed of a main monomer that imparts tackiness, a sub-monomer that imparts cohesiveness, and a functional group-containing monomer that imparts tackiness and forms a crosslinking point.

Research on acrylic adhesives generally uses binary or ternary monomers to measure various reaction conditions, such as the type and concentration of the initiator, the type and concentration of the solvent, the mixing ratio of the solvent and the monomer, the reaction rate, the reaction time, and the change in the concentration of the monomer. After polymerizing the adhesive by changing it, research on improving adhesive performance such as the effect on adhesive performance by measuring adhesive properties by cross-linking them has been common, but research on eco-friendly adhesives is being done little by little with recent environmental pollution. to be.

An object of the present disclosure is to provide a composition for low-temperature adhesive.

Another object of the present disclosure is to provide a method for preparing a low-temperature adhesive composition.

Another object of the present disclosure is to provide a tape coated with a low-temperature adhesive composition.

The technical problems of the present disclosure are not limited to the technical problems mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art from the following description.

The present disclosure relates to a low-temperature pressure-sensitive adhesive composition and a method for manufacturing the same, and more particularly, to a low-temperature pressure-sensitive adhesive composition and a method for manufacturing the same, which implements an adhesive layer maintaining adhesion even at low temperatures.

Hereinafter, the present disclosure will be described in more detail.

An example of the present disclosure relates to a low-temperature type pressure-sensitive adhesive composition comprising a pressure-sensitive adhesive and a curing agent.

In the present disclosure, the pressure-sensitive adhesive may include C ₄ to C ₁₀ acrylic acid alkyl esters having an alkyl group, an aggregation component, and a monomer functional group.

In the present disclosure, the adhesive can be implemented at a low temperature by containing the following monomers to lower the Tg (glass transition temperature) of the adhesive.

In the present disclosure, the acrylic acid alkyl esters are isooctyl acrylate (IOA), 2-ethylhexyl acrylate (2-EHA) and butyl acrylate (BA). It may be at least one selected from the group.

In the present disclosure, the acrylic acid alkyl esters are 30 to 70% by weight, 35 to 70% by weight, 40 to 70% by weight, 45 to 70% by weight, 50 to 70% by weight, 55 to 70% by weight based on the total weight of the monomer. %, 30 to 65% by weight, 35 to 65% by weight, 40 to 65% by weight, 45 to 65% by weight, 50 to 65% by weight, 55 to 65% by weight, for example, what is included in 60% by weight can

In the present disclosure, the aggregation component may be one or more selected from the group consisting of ethyl acrylate (Ethyl arylate; EA) and vinyl acetate (VA).

In the present disclosure, the agglomeration component is 10 to 40% by weight, 15 to 40% by weight, 20 to 40% by weight, 25 to 40% by weight, 30 to 40% by weight, for example, 35% by weight based on the total monomer weight. % may be included.

In the present disclosure, the monomer functional group is acrylic acid (Acrylic acid; AA), methacrylic acid (MAA) and beta-carboxyethyl acrylate (Beta-Carboxyethyl Acrylate; ß-CEA), 2-hydroxyethyl meta It may be at least one selected from the group consisting of acrylate (2-Hydroxyethyl methacrylate: 2-HEMA).

In the present disclosure, the monomer functional group may be included in an amount of 0.5 to 12.0% by weight based on the total weight of the monomer.

In the present disclosure, the curing agent may be at least one selected from the group consisting of isocyanate compounds, epoxy resins, melamine resins, urea resins, dialdehydes, and metal chelate compounds, but is not limited thereto.

In the present disclosure, the curing agent may be included in an amount of 0.1 to 10 parts by weight based on 100 parts by weight of the adhesive. If the content is less than 0.1 parts by weight, there is a fear that the durability reliability due to cohesive failure under high temperature and high humidity conditions may be reduced, and if it exceeds 10 parts by weight, there is a fear that fluidity may decrease due to compatibility deterioration.

In the present disclosure, the pressure-sensitive adhesive may further include a tackifying resin.

In the present disclosure, the pressure-sensitive adhesive may contain 0.1 to 30.0% by weight of the tackifying resin, for example, 20% by weight based on 100 parts by weight of the pressure-sensitive adhesive resin.

In the present disclosure, the tackifying resin may be at least one selected from the group consisting of rosin esters, phenolics, terpenes, and terpene phenolics, for example, , but may be a terpene phenol type, but is not limited thereto.

In the present disclosure, the adhesive resin may further include silicone oil. Silicone oil having a glass transition temperature of -80°C to -50°C is added to give the property of maintaining the fluidity of the pressure-sensitive adhesive at low temperatures.

In the present disclosure, the silicone oil may be included in an amount of 0.1 to 30 parts by weight based on 100 parts by weight of the adhesive resin. When the content exceeds 30 parts by weight, there is a fear that the cohesive force and adhesive force of the pressure-sensitive adhesive may be lowered.

In the present disclosure, the silicone oil may have a glass transition temperature of -80 to -50 °C, but is not limited thereto.

In the present disclosure, when the silicone oil is contained, it is possible to improve the adhesion at room temperature and implement the adhesion at low temperature.

In the present disclosure, the pressure-sensitive adhesive composition may be dissolved in a solvent and used.

In the present disclosure, the solvent may be a solvent excluding BTX. At this time, BTX is an abbreviation called by combining the initials of aromatic chemical products benzene (B), toluene (T), and xylene (X). This is because by excluding solvents corresponding to BTX (BTX) from solvents, the amount of carcinogens can be reduced and it can be used as an eco-friendly material.

In the present disclosure, the solvent is a C ₂ to C ₁₀ fatty acid ketone compound 5 to 40 wt %, C ₁ to C ₁₀ acetate compound 20 to 80 wt %, C ₁ to C ₁₀ alcohol compound 1 to 10 wt % and Normal/cyclohexane compound may contain 1 to 50% by weight, for example, a C ₁ to C ₁₀ acetate compound and a C ₂ to C ₁₀ fatty acid ketone compound are mixed in an 80 to 85: 15 to 20 weight ratio. It may be one, and preferably, it may be a mixture in a weight ratio of 80:20. This is to optimize the compatibility of the polymer and the synthesis conditions.

In an embodiment of the present disclosure, the solvent may be used by mixing ethyl acetate and acetone in a ratio of 80:20, but is not limited thereto.

In the present disclosure, the pressure-sensitive adhesive composition may be used in an amount of 25 to 45 parts by weight, 30 to 45 parts by weight, or 35 to 45 parts by weight, for example, 40 parts by weight based on 100 parts by weight of the solvent, The present invention is not limited thereto.

The adhesive strength of the pressure-sensitive adhesive composition of the present disclosure is 1,800 gf/in or more, 1,900 gf/in or more, 2,000 gf/in or more, 2,100 gf/in or more, 2,200 gf/in or more, 2,300 gf/in or more, 2,400 gf/in or more, may be, for example, may be 2,500 gf / in or more.

Cold resistance of the pressure-sensitive adhesive composition of the present disclosure may be 0 ℃ or less, -10 ℃ or less, -20 ℃ or less, for example, -30 ℃ or less.

In the present disclosure, the term “cold resistance” means that adhesion is maintained at a corresponding temperature, and when cold resistance is insufficient, the pressure-sensitive adhesive layer is solidified at the corresponding temperature and is easily detached from the adherend with low adhesive force.

The heat resistance of the pressure-sensitive adhesive composition of the present disclosure may be 120 °C or higher, 130 °C or higher, for example, 140 °C or higher.

In the present disclosure, the term “heat resistance” means that when a load of 500 g is adhered and maintained without sliding by attaching it in the range of 1 inch X 1 inch at the corresponding temperature, it means that there is heat resistance at the corresponding temperature.

A tape prepared by coating a pressure-sensitive adhesive comprising the pressure-sensitive adhesive composition of the present disclosure on a substrate for producing a tape may be obtained.

In the present disclosure, the substrate for manufacturing the tape may have a thickness of 1.4 to 100.0 μm, but is not limited thereto.

In the present disclosure, the tape may be prepared by applying an adhesive on both sides or one side of a base material for tape production.

In the present disclosure, the tape may be performed after treating the surface of the substrate with a primer before applying the adhesive to the substrate. Through such a primer treatment, the bonding force between the substrate and the pressure-sensitive adhesive may be improved.

In the present disclosure, the pressure-sensitive adhesive may be applied to the surface of the base material for tape production to a thickness of 3 to 70 μm, but is not limited thereto.

Another example of the present disclosure relates to a method of manufacturing a low-temperature type adhesive tape comprising the step of applying a pressure-sensitive adhesive composition on a substrate.

In the present disclosure, the pressure-sensitive adhesive composition may be used to prepare a coating solution by adding a solvent to adjust the viscosity to be suitable for coating operation.

In the present disclosure, the substrate may be a substrate having releasability.

In the present disclosure, the substrate having the release property is polyethylene terephthalate, polyethylene, polypropylene, polybutene, polybutadiene, polymethylpentene, polyvinyl chloride, vinyl chloride copolymer, polyurethane, polystyrene, polycarbonate, fluororesin , one type of substrate selected from the group consisting of a resin film such as , low-density polyethylene, triacetyl cellulose, or fine paper, coated paper, glassine paper, laminated paper, etc. can be used, for example, it has excellent elasticity and in terms of price. It may be an inexpensive polyethylene terephthalate film.

In the present disclosure, the thickness of the substrate is 5 to 200 μm, 10 to 200 μm, 15 to 200 μm, 20 to 200 μm, 5 to 150 μm, 10 to 150 μm, 15 to 150 μm, 20 to 150 μm, 5 to 100 μm, 10 to 100 μm, 15 to 100 μm, 20 to 100 μm, 5 to 75 μm, 10 to 75 μm, 15 to 75 μm, 20 to 75 μm, for example, 25 to 75 μm. have.

In the present disclosure, the pressure-sensitive adhesive composition is dried by a method used for conventional tape production such as a bar coating method, a reverse roll coating method, a knife coating method, a roll knife coating method, a gravure coating method, a doctor blade coating method, a slot die coating method, etc. And the thickness after curing is applied to be 3㎛ to 100㎛, and laminated with the core material to prepare a single-sided adhesive film.

In the present disclosure, the pressure-sensitive adhesive composition is coated on a substrate having different releasability, cured to form an adhesive layer, and laminated on the back surface of the prepared single-sided adhesive film to prepare a double-sided adhesive film.

In the present disclosure, the core material may be a synthetic resin film having a thickness of 1.4 to 100 μm, for example, 1.4 to 50 μm.

In the present disclosure, the synthetic resin film constituting the core material may be surface-treated on both surfaces by an oxidation method, an unevenness method, or the like, if necessary, for the purpose of improving adhesion with the pressure-sensitive adhesive layer applied on both surfaces thereof.

In the present disclosure, the oxidation method may be corona discharge treatment, cross acid treatment, plasma discharge treatment, ultraviolet irradiation treatment, primer coating, etc. For example, it may be a primer coating with the best adhesion to the substrate, but limited thereto it's not going to be

In the present disclosure, the roughening method may be a sand blasting method, a solvent treatment method, or the like, but is not limited thereto.

As used herein, the term "adhesive" refers to a material used to bond two objects to each other. It should be a polymer that is liquid at first and does not fall off when it solidifies later and does not break itself.

As used herein, the term “pressure-sensitive adhesive (PSA)” refers to an adhesive applied to the back of a cellophane tape or label, and is also referred to as a pressure-sensitive adhesive. It is different from adhesives in that it is characterized by instantaneous adhesion with very slight pressure, and complete curing is not achieved.

As used herein, the term "organic solvent:" is a liquid organic chemical substance capable of dissolving any substance, such as thinner or solvent. It is characterized by strong volatility, and may exist in the form of harmful gases in the air.

The technical solutions obtainable in the present disclosure are not limited to the above-mentioned solutions, and other solutions that are not mentioned are clearly to those of ordinary skill in the art to which the present disclosure belongs from the description below. can be understood

The present disclosure relates to a low-temperature adhesive tape and a method for manufacturing the same, and more particularly, to a low-temperature type adhesive tape having an adhesive layer that maintains adhesion even at low temperatures, and a manufacturing method thereof, and the adhesive tape according to the present disclosure relates to an automobile , can be widely applied to various industries such as electronics.

The effects obtainable in the present disclosure are not limited to the above-mentioned effects, and other effects not mentioned will be clearly understood by those of ordinary skill in the art to which the present disclosure belongs from the description below. .

Various aspects are now described with reference to the drawings, in which like reference numbers are used to refer to like elements collectively. In the following examples, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of one or more aspects. It will be evident, however, that such aspect(s) may be practiced without these specific details.
1 is a cross-sectional view of a tape prepared from a low-temperature adhesive composition according to an embodiment of the present disclosure.
2 is a cross-sectional view of a tape made of a low-temperature adhesive composition according to an embodiment of the present disclosure.
3 is a cross-sectional view of a tape made of the low-temperature adhesive composition according to an embodiment of the present disclosure.

Various embodiments and/or aspects are now disclosed with reference to the drawings. In the following description, for purposes of explanation, numerous specific details are set forth to provide a thorough understanding of one or more aspects. However, it will also be appreciated by one of ordinary skill in the art that such aspect(s) may be practiced without these specific details. The following description and accompanying drawings set forth in detail certain illustrative aspects of one or more aspects. These aspects are illustrative, however, and some of the various methods in principles of various aspects may be employed, and the descriptions set forth are intended to include all such aspects and their equivalents. Specifically, as used herein, “embodiment”, “example”, “aspect”, “exemplary”, etc. is not to be construed as an advantage or advantage of any aspect or design described over other aspects or designs. It may not be.

Hereinafter, the same or similar components are assigned the same reference numerals regardless of reference numerals, and overlapping descriptions thereof will be omitted. In addition, in describing the embodiments disclosed in the present specification, if it is determined that detailed descriptions of related known technologies may obscure the gist of the embodiments disclosed in the present specification, the detailed description thereof will be omitted. In addition, the accompanying drawings are only for easy understanding of the embodiments disclosed in the present specification, and the technical ideas disclosed in the present specification are not limited by the accompanying drawings.

Although the first, second, etc. are used to describe various elements or elements, these elements or elements are not limited by these terms, of course. These terms are only used to distinguish one element or component from another. Accordingly, it goes without saying that the first element or component mentioned below may be the second element or component within the spirit of the present disclosure.

Unless otherwise defined, all terms (including technical and scientific terms) used herein may be used with the meaning commonly understood by those of ordinary skill in the art to which this disclosure belongs. In addition, terms defined in a commonly used dictionary are not to be interpreted ideally or excessively unless clearly defined in particular.

In addition, the term “or” is intended to mean an inclusive “or” rather than an exclusive “or.” That is, unless otherwise specified or clear from context, "X employs A or B" is intended to mean one of the natural implicit substitutions. That is, X employs A; X employs B; or when X employs both A and B, "X employs A or B" may apply to either of these cases. It should also be understood that the term “and/or” as used herein refers to and includes all possible combinations of one or more of the listed related items.

Also, the terms "comprises" and/or "comprising" mean that the feature and/or element is present, but excludes the presence or addition of one or more other features, elements, and/or groups thereof. should be understood as not Also, unless otherwise specified or otherwise clear from context to refer to a singular form, the singular in the specification and claims should generally be construed to mean "one or more."

Preparation Example 1. Preparation of adhesive tape 1

62 g of 2-ethylhexyl acrylate (2-EHA) as an acrylic acid alkyl ester, 10 g of ethyl acrylate (Ethyl arylate; EA) as a coagulant component and 20 g of vinyl acetate (VA), and a monomer An acrylic PSA solid content was synthesized at 40% with 8 g of acrylic acid (AA) as a functional group, and then 1 g of an epoxy curing agent (2% solution) was mixed to prepare a pressure-sensitive adhesive composition.

Then, the pressure-sensitive adhesive composition was coated on the PET release film and dried to form an adhesive PSA layer having a thickness of 25 μm, and a PET film 25 μm was laminated thereon. A tape test piece was prepared by cross-linking reaction at a high temperature of 43° C. through an aging period of 48 hours.

Preparation Example 2. Preparation of adhesive tape 2

A tape test piece was prepared in the same manner as in Preparation Example 1, except that 7 g of the tackifying resin was additionally included.

Preparation Example 3. Preparation of adhesive tape 3

A tape test piece was prepared in the same manner as in Preparation Example 1 except that 10 g of the tackifying resin was additionally included.

Preparation Example 4. Preparation of adhesive tape 4

A tape test piece was prepared in the same manner as in Preparation Example 1, except that 10 g of the tackifying resin and 5 g of silicone oil were additionally included.

Preparation 5. Preparation of adhesive tape 5

A tape test piece was prepared in the same manner as in Preparation Example 1, except that 7 g of the tackifying resin and 5 g of silicone oil were additionally included.

Preparation Example 6. Preparation of adhesive tape 6

A tape test piece was prepared in the same manner as in Preparation Example 1, except that 7 g of the tackifying resin and 20 g of silicone oil were additionally included.

Production Example 7. Preparation of adhesive tape 7

A tape test piece was prepared in the same manner as in Preparation Example 1, except that the content of 2-EHA was adjusted to 80 g, and 7 g of the tackifying resin was additionally included.

Preparation 8. Preparation of adhesive tape 8

A tape test piece was prepared in the same manner as in Preparation Example 1, except that the content of 2-EHA was adjusted to 40 g and 7 g of tackifying resin was additionally included.

Preparation 9. Preparation of adhesive tape 9

62 g of butyl acrylate (BA) as an acrylic acid alkyl ester, 10 g of Ethyl arylate (EA) as a coagulant component and 20 g of vinyl acetate (VA), and acrylic acid (Acrylic acid) as a monomer functional group ; AA) 8 g of acrylic PSA solids were synthesized at 40%, and then 1 g of an epoxy curing agent (2% solution) and 7 g of a tackifying resin were mixed to prepare a pressure-sensitive adhesive composition.

Then, the pressure-sensitive adhesive composition was coated on the PET release film and dried to form an adhesive PSA layer having a thickness of 25 μm, and a PET film 25 μm was laminated thereon. A tape test piece was prepared by cross-linking reaction at a high temperature of 43° C. through an aging period of 48 hours.

Preparation 10. Preparation of adhesive tape 10

A tape test piece was prepared in the same manner as in Preparation Example 9 except that 80 g of butyl acrylate was used.

Preparation 11. Preparation of adhesive tape 11

A tape test piece was prepared in the same manner as in Preparation Example 9 except that 40 g of butyl acrylate was used.

Preparation 12. Preparation of adhesive tape 12

62 g of Isooctyl acrylate (IOA) as an acrylic acid alkyl ester, 10 g of Ethyl arylate (EA) as a coagulant component and 20 g of vinyl acetate (VA), and acrylic acid ( Acrylic acid; AA) 8 g of acrylic PSA solids were synthesized at 40%, and then 1 g of an epoxy curing agent (2% solution) and 7 g of a tackifying resin were mixed to prepare a pressure-sensitive adhesive composition.

Then, the pressure-sensitive adhesive composition was coated on the PET release film and dried to form an adhesive PSA layer having a thickness of 25 μm, and a PET film 25 μm was laminated thereon. A tape test piece was prepared by cross-linking reaction at a high temperature of 43° C. through an aging period of 48 hours.

Preparation 13. Preparation of adhesive tape 13

A tape test piece was prepared in the same manner as in Preparation Example 12 except that 80 g of isooctyl acrylate was used.

Preparation 14. Preparation of adhesive tape 14

A tape test piece was prepared in the same manner as in Preparation Example 12 except that 40 g of isooctyl acrylate was used.

Experimental Example 1. Measurement of adhesive force

For the test pieces prepared in Preparation Examples 1 to 14, the adhesive force was measured through the KS T 1028 test method. The unit is expressed in gf/inch. The KS T 1028 test method is a test method for adhesive tapes and adhesive sheets. A specimen of 1 inch in width and 250 mm in length is taken and adhered to a stainless steel plate (SUS 304) test piece with an area of 1 inch * 6 inch. It is a method of attaching a tape, reciprocating it once with a 2 kg roller, and measuring the adhesive force at a tensile speed (300±30 mm/min) by the 180° Peel Strength Test method after 30 minutes.

Preparation Example 1 Preparation 2 Preparation 3 Preparation 4 Preparation 5 Preparation 6 Preparation 7 adhesiveness
(gf/25mm) 1300 2100 2600 2400 2100 1800 2300 Preparation 8 Preparation 9 Preparation 10 Preparation 11 Preparation 12 Preparation 13 Preparation 14 adhesiveness
(gf/25mm) 1850 2000 2250 1600 2150 2150 1900

Experimental Example 2. Measurement of heat resistance

A measurement specimen having a width of 1 inch and a length of 150 mm was prepared using the adhesive tape prepared according to Preparation Example. Thereafter, the specimen was attached to the SUS by pressing and reciprocating twice with a hand roller of 2 kg in an area of 1 inch X 1 inch. Thereafter, after standing at room temperature for 30 minutes, a load of 500 g was applied in an oven at 50° C. and allowed to stand for 10 minutes. Thereafter, the temperature is increased by 10° C. every 10 minutes to measure the temperature at which the tape is pushed and further dropped. The temperature rise temperature is raised to 150 ℃ and maintained at 150 ℃ for 30 minutes. If the tape did not fall, the pushed distance was measured.

Preparation Example 1 Preparation 2 Preparation 3 Preparation 4 Preparation 5 Preparation 6 Preparation 7 heat resistance
(℃) 150 150 150 150 150 150 130 Preparation 8 Preparation 9 Preparation 10 Preparation 11 Preparation 12 Preparation 13 Preparation 14 Heat resistance (℃) 150 150 150 150 140 120 150

Experimental Example 3. Low-temperature adhesion measurement

A measurement specimen having a width of 1 inch and a length of 250 mm was prepared using the adhesive tape prepared according to Preparation Examples 1 to 14. Attach the adhesive tape to the stainless steel plate (SUS 304) test piece with an area of 1 inch * 6 inch, reciprocate it once with a 2 kg roller, and leave it for 30 minutes. After leaving it for 30 minutes in a low-temperature environment (in units of 5°C), it was immediately peeled off at a rate of 300±30 mm/min, and the measured value was recorded as the temperature at which adhesion is maintained to the stainless steel plate.

Preparation Example 1 Preparation 2 Preparation 3 Preparation 4 Preparation 5 Preparation 6 Preparation 7 low temperature adhesion
(℃) -40 -25 -10 -40 -55 -70 -30 Preparation 8 Preparation 9 Preparation 10 Preparation 11 Preparation 12 Preparation 13 Preparation 14 Low temperature adhesion (℃) 0 -15 -20 10 -30 -35 -5

sintering

Looking at Preparation Example 2 as a standard, Preparation Example 1 did not contain a tackifying resin, so it was confirmed that the low-temperature adhesion performance was increased, but the adhesive strength was significantly reduced. In Preparation Example 3, when the content of tackifying resin is increased, heat resistance of 150°C or higher is maintained and adhesive strength is improved, but it was confirmed that low-temperature adhesion performance is reduced. In Preparation Example 4, it was confirmed that the adhesive strength was improved when the content of the tackifying resin was increased and the silicone oil was added, but the low-temperature adhesion performance could also be improved. In Preparation Example 5, when a small amount of silicone oil is contained, the decrease in adhesive strength is not large, but it is confirmed that there is an improvement in low-temperature adhesion. In Preparation Example 6, when the silicone oil content was greatly increased, it was confirmed that the low-temperature adhesion was greatly improved, but the adhesive strength was reduced (maintaining heat resistance of 150°C or higher). In Preparation Example 7, it was confirmed that, when the content of 2-EHA was increased, adhesive strength and low-temperature adhesion performance were improved, but heat resistance performance was decreased. In Preparation Example 8, it was confirmed that when the content of 2-EHA was reduced, the adhesive strength and low-temperature adhesion performance were reduced, and the heat resistance performance was improved (there was no difference in data because the heat resistance performance was improved at 150℃ or higher).

In Preparation Example 9, when changing to BA instead of 2-EHA, it was confirmed that the adhesive strength and low-temperature adhesion performance were slightly reduced (the heat resistance performance is improved, but there is no difference in data because it is above 150℃). In Preparation Example 10, it was confirmed that the adhesive strength and low-temperature adhesion performance were improved compared to Preparation Example 9 due to the increase in BA content, and although the heat resistance performance was decreased, it was confirmed that there was no difference in data because the heat resistance performance of 150℃ or higher was realized. In Preparation Example 11, it was confirmed that the heat resistance performance was improved compared to Preparation Example 9 due to a decrease in the BA t flow rate, but the adhesive strength and low-temperature adhesion performance were decreased.

In Preparation Example 12, when IOA was used instead of 2-EHA, it was confirmed that the adhesive strength and low-temperature adhesion performance slightly increased, but the heat resistance performance decreased. In Preparation Example 13, when the IOA content was increased, it was confirmed that the low-temperature adhesion performance was improved compared to Preparation Example 12, and the adhesive strength was maintained at a similar level, but the heat resistance was reduced. In Preparation Example 14, when the IOA ?t flow rate was reduced, it was confirmed that the adhesive strength and low-temperature adhesion were decreased compared to Preparation Example 12, but the heat resistance performance was improved.

Objects and effects of the present disclosure, and technical configurations for achieving them will become clear with reference to the embodiments described below in detail in conjunction with the accompanying drawings. In describing the present disclosure, if it is determined that a detailed description of a well-known function or configuration may unnecessarily obscure the subject matter of the present disclosure, the detailed description thereof will be omitted. In addition, the terms described below are terms defined in consideration of functions in the present disclosure, which may vary according to intentions or customs of users and operators.

However, the present disclosure is not limited to the embodiments disclosed below and may be implemented in various different forms. Only the present embodiments are provided so that the present disclosure is complete, and to fully inform those of ordinary skill in the art to which the present disclosure belongs, the scope of the disclosure, and the present disclosure is only defined by the scope of the claims . Therefore, the definition should be made based on the content throughout this specification.

The description of the presented embodiments is provided to enable any person skilled in the art to make or use the present disclosure. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the scope of the present disclosure. Thus, the present disclosure is not to be limited to the embodiments presented herein, but is to be construed in the widest scope consistent with the principles and novel features presented herein.

The scope of the rights to the method in the claims of the present disclosure is generated by the functions and features described in each step, and unless the precedence of the order is specified in each step constituting the method, the claims It is not affected by the order of description of each step in For example, in a claim described as a method comprising steps A and B, even if step A is stated before step B, the scope of rights is not limited that step A must precede step B.

10: substrate layer
20: adhesive layer

Claims (14)

A pressure-sensitive adhesive comprising an alkyl group having C ₄ to C ₁₀ acrylic acid alkyl esters, an aggregation component, and a monomer functional group; and a curing agent;
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The acrylic acid alkyl esters are 1 selected from the group consisting of isooctyl acrylate (IOA), 2-ethylhexyl acrylate (2-EHA) and butyl acrylate (BA). more than a species,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The acrylic acid alkyl esters are included in an amount of 30 to 70% by weight based on the total weight of the monomers,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The aggregation component is at least one selected from the group consisting of ethyl acrylate (Ethyl arylate; EA) and vinyl acetate (VA),
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The aggregation component is included in an amount of 10 to 40% by weight based on the total weight of the monomer,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The monomer functional group is at least one selected from the group consisting of acrylic acid (Acrylic acid; AA), methacrylic acid (MAA) and beta-carboxyethyl acrylate (Beta-Carboxyethyl Acrylate; ß-CEA),
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The monomer functional group is included in an amount of 0.5 to 12.0% by weight based on the total weight of the monomer,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The curing agent is at least one selected from the group consisting of isocyanate compounds, epoxy resins, melamine resins, urea resins, dialdehydes and metal chelate compounds,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The curing agent is included in an amount of 0.1 to 10 parts by weight based on 100 parts by weight of the pressure-sensitive adhesive,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The composition further comprises a silicone oil,
Eco-friendly low-temperature adhesive composition. 11. The method of claim 10,
The silicone oil is contained in an amount of 0.1 to 30 parts by weight based on 100 parts by weight of the adhesive resin,
Eco-friendly low-temperature adhesive composition. 11. The method of claim 10,
The silicone oil will have a glass transition temperature of -80 ℃ to -50 ℃,
Eco-friendly low-temperature adhesive composition. The method of claim 1,
The composition further comprises a tackifying resin,
Eco-friendly low-temperature adhesive composition. 14. The method of claim 13,
The tackifying resin is at least one selected from the group consisting of rosin esters, phenolics, terpenes and terpene phenolics. that is,
Eco-friendly low-temperature adhesive composition.

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