CN111087950B - Adhesive, double-sided tape applying adhesive and preparation method of double-sided tape - Google Patents
Adhesive, double-sided tape applying adhesive and preparation method of double-sided tape Download PDFInfo
- Publication number
- CN111087950B CN111087950B CN201911336305.9A CN201911336305A CN111087950B CN 111087950 B CN111087950 B CN 111087950B CN 201911336305 A CN201911336305 A CN 201911336305A CN 111087950 B CN111087950 B CN 111087950B
- Authority
- CN
- China
- Prior art keywords
- adhesive
- coating
- double
- layer
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/005—Presence of polyester in the release coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention discloses an adhesive, a double-sided tape applying the adhesive and a preparation method of the double-sided tape, and relates to the technical field of double-sided tapes.
Description
Technical Field
The invention relates to the technical field of double-sided tapes, in particular to an adhesive, a double-sided tape using the adhesive and a preparation method of the double-sided tape.
Background
With the development of national economy and science and technology, the adhesive becomes an indispensable novel material in the development of high and new technology, and is widely applied to various departments of national economy and related fields of daily life. With the development of the Chinese industry, the application field of the adhesive is continuously expanded, and the adhesive is expanded from the industries mainly used for wood processing, clothing, light industry, building, packaging and the like to a plurality of fields such as new energy, mechanical manufacturing, aerospace, electronic and electric appliances, transportation, environmental protection, energy conservation, medical treatment, sanitation and the like, and becomes an indispensable important chemical product in national economy and people's life.
The adhesive tape is a special structure formed by combining a pressure-sensitive adhesive and various thin materials, is one of tools commonly used for fixing parts in daily life and work, and can be divided into a high-temperature adhesive tape, a double-sided adhesive tape, a conductive adhesive tape, a special adhesive tape, a pressure-sensitive adhesive tape, a die-cutting adhesive tape and the like according to functions. With the increasingly strict requirements on the thinning, water resistance, dust resistance and other performances of electronic products, the importance of the adhesive tape in the electronic products is more prominent. With the demand of thinning electronic products, the adhesive tape is also proposed to be thinner, strongly adhesive, resistant to heat and humidity aging and the like on the premise of meeting the physical property demand. The ultrathin double-sided adhesive tape generally comprises a release layer, a substrate layer and a modified polyacrylate pressure-sensitive adhesive layer, and is of a multilayer structure, the stability of the interlayer structure and the physical property of the modified polyacrylate pressure-sensitive adhesive layer directly influence the service performance of the adhesive tape, and the ultrathin design and the maintenance of the strong adhesive force of the ultrathin double-sided adhesive tape are difficult problems of the ultrathin adhesive tape.
Disclosure of Invention
In order to overcome the problem that the ultrathin adhesive tape in the prior art is not strong in adhesive force, the invention provides an adhesive, a double-sided adhesive tape using the adhesive and a preparation method of the double-sided adhesive tape.
The specific technical scheme is as follows:
the adhesive is prepared from the following raw materials in parts by weight:
preferably, the alkyl acrylate monomer polymer includes an alkyl acrylate monomer and an initiator, the alkyl acrylate monomer includes a viscoelastic monomer including at least two and not more than five of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, isooctyl acrylate, isononyl acrylate, 2-ethylhexyl acrylate, and a functional group monomer including at least one and not more than four of acrylic acid, methyl acrylate, methacrylic acid, methyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, vinyl acetate, hydroxyethyl methacrylate, VeoVa10, and styrene.
Preferably, the alkyl acrylate monomer has 2 to 15 carbon atoms in the alkyl group.
Preferably, the alkyl acrylate monomer has 4 to 10 carbon atoms in the alkyl group.
Preferably, the solvent is an organic solvent, and the organic solvent is ethyl acetate, toluene, xylene, butanone, methanol or diethyl ether.
Preferably, the tackifying resin is terpene resin, coumarone indene resin, petroleum C5 resin, petroleum C9 resin, petroleum C5/C9 resin, terpene phenol resin and the like, and hydrides, esters, polymers and polymerized rosins, rosin acids and rosin acid esters thereof, wherein at least one or more polymerized rosin resins are blended.
Preferably, the crosslinking agent is an isocyanate crosslinking agent, an epoxy crosslinking agent, a metal chelate, an aziridine, or an amino group.
The utility model provides a double-sided tape, includes substrate layer, sticky layer and leaves the type material layer, the substrate layer is the PET film, sticky layer sets up at least one face at the substrate layer, laminate on sticky layer surface from the type material layer, it is transparent polyester from the type membrane to leave the type material layer, the thickness of substrate layer is 0.5 ~ 25 mu m.
Preferably, the adhesive layer is arranged on the upper surface and the lower surface of the base material layer.
A preparation method of a double-sided adhesive tape comprises the following steps:
step 1: conveying the adhesive to a micro-concave coating head through a pump, coating the adhesive on a release material layer by the micro-concave coating head, then drying the adhesive in an oven, laminating the adhesive and a substrate layer through a composite roller, and rolling a coating line in a first rolling manner to obtain a first engineering coating semi-finished product;
step 2: conveying the adhesive to a micro-concave coating head through a pump, coating the adhesive on a release material layer by the micro-concave coating head, then drying the adhesive in an oven, laminating the adhesive with a first engineering coating semi-finished product through a composite roller, and rolling a coating line in a first rolling manner to obtain a PET double-sided tape semi-finished product;
and step 3: and (3) placing the semi-finished product of the PET double-sided tape into a circulating air oven at 40 ℃, and curing for 72 hours to obtain a finished product of the PET double-sided tape.
Compared with the prior art, the invention has the following beneficial effects:
the adhesive provided by the application comprises an alkyl acrylate monomer polymer, a solvent, tackifying resin and a cross-linking agent, wherein the acrylate adhesive polymer has the characteristics of high viscosity and high temperature and high humidity resistance of thin coating, and a PET double-sided tape comprises a base material layer, an adhesive layer and a release material layer, so that the adhesive has the characteristics of ultra-thin and high viscosity.
Drawings
FIG. 1 is a schematic structural view of a double-sided tape according to the present invention.
In the figure, 1 is a release material layer, 2 is an adhesive layer, and 3 is a base material layer.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention discloses an adhesive, a double-sided tape applying the adhesive and a preparation method thereof,
the adhesive is prepared from the following raw materials in parts by weight:
preferably, the alkyl acrylate monomer polymer includes an alkyl acrylate monomer and an initiator, the alkyl acrylate monomer includes a viscoelastic monomer and a functional group monomer, the viscoelastic monomer includes at least two of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, isooctyl acrylate, isononyl acrylate, and 2-ethylhexyl acrylate, and the specific ratio is not particularly limited, and the free radical polymerization is performed. The functional group monomer includes at least one of acrylic acid, methyl acrylate, methacrylic acid, methyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, vinyl acetate, hydroxyethyl methacrylate, VeoVa10, and styrene, and not more than four. The alkyl acrylate monomer preferably has an alkyl group having 2 to 15 carbon atoms, and includes a viscoelasticity-imparting monomer and a functional group-imparting monomer, and the viscoelasticity-imparting monomer may be methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, isooctyl acrylate, isononyl acrylate, 2-ethylhexyl acrylate, and the like, and the alkyl acrylate monomer preferably has 4 to 10 carbon atoms, and may be methyl acrylate, n-butyl acrylate, 2-ethylhexyl acrylate, and the like, from the viewpoint of adhesive properties.
The above-mentioned monomer having viscoelastic properties, preferably methyl acrylate, n-butyl acrylate or 2-ethylhexyl acrylate, is blended alone and/or in a copolymer thereof in an amount of 30% by mass or more, more preferably 60% by mass or more, particularly preferably 80% by mass or more, in order to achieve adhesive bonding properties.
Two or more of the functional group-containing monomers are selected and not more than four, the specific ratio is not particularly limited, and the amount of the functional group-containing monomers is limited to 5% by mass or more, preferably 10% by mass or more, and more preferably 15% by mass or more, which is effective for the adhesive, so as to achieve the characteristics such as cohesive strength, warpage resistance, and wet heat resistance of the adhesive.
Preferably, the solvent is an organic solvent, and the organic solvent is ethyl acetate, toluene, xylene, butanone, methanol or diethyl ether. According to the principle of the solvent polymerization characteristics, toluene or/and ethyl acetate is preferably used, the addition ratio is not particularly limited, and all solvents thereof account for 30 to 80 mass%, preferably 30 to 60 mass%, of the total mass.
The polymerization method of the acrylic pressure-sensitive adhesive contained in the raw material liquid of the adhesive layer is not particularly limited, and a known method can be used. In the case of solvent-based adhesives which are preferably used, the polymerization can be carried out using free-radical initiators, such as Benzoyl Peroxide (BPO), Azobisisobutyronitrile (AIBN), as initiators. In this case, the weight average molecular weight can be controlled by the mass% content of the initiator, the initiator addition process, the concentration of the polymerization monomer, the polymerization temperature profile, and the polymerization time, and the weight average molecular weight distribution measured by GPC (Gel Permeation Chromatography) is 10 to 150 ten thousand, more preferably 50 to 150 ten thousand, and particularly preferably 80 to 150 ten thousand.
The polymer is controlled by a solvent and a polymerization process, and is suitable for the viscosity of 3000-30000 mPa.s, and the optimal viscosity of 15000-30000 mPa.s.
Preferably, the tackifying resin is terpene resin, coumarone indene resin, petroleum C5 resin, petroleum C9 resin, petroleum C5/C9 resin, terpene phenol resin, etc., and hydrides, esters, polymers, polymerized rosins, rosin acids, rosin acid esters thereof, wherein at least one or more polymerized rosin resins are blended. The softening point of the polymerized rosin resin can be any temperature, preferably 60 to 180 ℃, more preferably 80 to 150 ℃, particularly preferably 100 to 140 ℃, and the mixing amount is 10 to 50 parts by weight (solid part) relative to 100 parts by weight of the main polymer (solid part), preferably 15 to 30% by weight (solid part).
Preferably, the crosslinking agent is an isocyanate-based crosslinking agent or an epoxy-based crosslinking agent or a metal chelate or an aziridine or an amino group. Appropriate cross-linking agents can be added into the solvent type modified polyacrylate pressure-sensitive adhesive for the adhesive layer, so that the stability and balance of the coating property and the dried adhesive property of the adhesive composition are realized. The crosslinking agent may be an isocyanate-based crosslinking agent, an epoxy-based crosslinking agent, a metal chelate, aziridine, an amino-based crosslinking agent, or the like, and preferably an isocyanate-based crosslinking agent and/or an epoxy-based crosslinking agent are used.
Wherein, a double-sided tape, as shown in fig. 1, include substrate layer 3, sticky layer 2 and leave type material layer 1, substrate layer 3 is the PET film, and sticky layer 2 sets up at least one face of substrate layer 3, from the laminating of type material layer 1 on sticky layer 2 surface, from type material layer 1 for transparent polyester release film, preferred, sticky layer 2 sets up the upper and lower surface at substrate layer 3.
The copolymer is prepared by introducing a novel monomer (VeoVa10, has a highly branched chain aliphatic structure, has a strong three-dimensional protection function on the self and adjacent monomers in the formed copolymer, so that the copolymer has excellent hydrolysis resistance, particularly alkali resistance and excellent ultraviolet irradiation resistance, and the highly branched side chain also provides very strong cohesive strength for the formed copolymer, and simultaneously has very good wettability and excellent leveling property, and can greatly improve the adhesive property, aging resistance, weather resistance and other properties of an adhesive layer) and various universal acrylate monomers, solvents, functional monomers, initiators, tackifying resins and the like, and different free radical polymerization processes are selected; the adhesive layer is formed by adhering polyacrylate pressure-sensitive adhesive to one or two surfaces of the base material layer 3 through a release film transfer coating process; and then, adhering a release film layer to the surface of the adhesive layer for isolation and protection, thereby forming the ultrathin PET double-sided adhesive tape. The thickness of the ultrathin PET adhesive tape can be adjusted by selecting base materials with different thicknesses and adhesive layers with different thicknesses, and preferably, the base material layer 3 is made of PET (polyethylene terephthalate); tensile strength, TD direction is not less than 170MPa, MD direction is not less than 170 MPa; elongation, T D direction is more than or equal to 40%, MD direction is more than or equal to 40%; the color may be black, white, transparent, etc.; the thickness may be 0.5 to 25 μm, preferably 1.5 to 6 μm.
The preparation method of the double-sided adhesive tape comprises the following steps:
step 1: conveying the adhesive to a micro-concave coating head through a pump, coating the adhesive on a release material layer 1 by the micro-concave coating head, then drying in an oven, laminating the adhesive with a substrate layer 3 through a composite roller, and rolling a coating line in a first rolling manner to obtain a first engineering coating semi-finished product;
step 2: conveying the adhesive to a micro-concave coating head through a pump, coating the adhesive on a release material layer 1 by the micro-concave coating head, then drying in an oven, laminating with a first engineering coating semi-finished product through a composite roller, and rolling by a first rolling of a coating line to obtain a PET double-sided tape semi-finished product;
and step 3: and (3) placing the semi-finished product of the PET double-sided tape into a circulating air oven at 40 ℃, and curing for 72 hours to obtain a finished product of the PET double-sided tape.
The double-sided adhesive tape may be produced by a known method for producing a double-sided adhesive tape. There may be a doctor blade coating, roll coating, gravure coating, slot extrusion coating, spray coating, die coating, etc. In the present invention, blade coating, slit extrusion coating, or dimple coating is preferable, and dimple coating is more preferable.
The solvent type modified polyacrylate pressure-sensitive adhesive of the adhesive layer is combined with efficiency and a coating process, the optimal coating viscosity is 10-100 mPa.s, so that the adhesive needs to be diluted, a diluting solvent can be an organic solvent such as ethyl acetate, toluene, butanone and butyl acetate, and the ethyl acetate is preferably used as the diluting solvent in consideration of coating processability, volatility of the solvent and environmental protection characteristics.
Comparative example 1 of adhesive:
4.45 parts by mass of acrylic acid, 0.2 part by mass of hydroxyethyl acrylate, 40 parts by mass of ethyl acrylate, 55 parts by mass of isooctyl acrylate and 100 parts by mass of toluene as a polymerization solvent were put into a three-necked flask, nitrogen gas was introduced below the liquid surface, and the temperature was raised in a water bath, and stirring was started while introducing nitrogen gas at a stirring speed of 100 to 200 revolutions per minute for 2 hours, and the temperature was maintained at 70 ℃ during introduction of nitrogen gas. Oxygen in the polymerization system was removed as much as possible, 0.05 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the exothermic reaction was started, the reaction mixture was heated to 73 ℃ and held at a cooling temperature for 30 hours, 0.05 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the reaction mixture was heated to 83 ℃ and held at a temperature for 1 hour, 0.25 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the reaction mixture was heated to 88 ℃ and held at a temperature for 6 hours, and when the reaction mixture was cooled to 70 ℃ or less, 50 parts by weight of ethyl acetate was added to obtain a polymer solution. The glass transition temperature of the obtained polymer is Tg-44 ℃, the solid content is 40%, the viscosity is 10000mPa.s, and the weight average molecular weight is 80 ten thousand.
To the polymer solution, 15 parts by weight of a tackified synthetic rosin resin having a softening point of 135 ℃ (manufactured by seikagawa chemical corporation) and 5 parts by weight of a C5 petroleum-based tackifying resin having a softening point of 100 ℃ (puggangbanlu chemical limited) were added, and 25 parts by weight of ethyl acetate was added to prepare an adhesive composition having a solid content of 40%, wherein the solvent-type modified polyacrylate pressure-sensitive adhesive had a viscosity of 8000mpa.s at 23 ± 2 ℃.
Before coating, 0.5 part by weight of an isocyanate-based crosslinking agent (manufactured by Tosoh chemical Co., Ltd.) was mixed with 100 parts by weight of the solid content of the composition, and the composition was diluted with ethyl acetate according to the coating process and the product design.
Preparation example 1 of adhesive:
4.45 parts by mass of acrylic acid, 0.2 part by mass of hydroxyethyl acrylate, 40 parts by mass of ethyl acrylate, 45 parts by mass of isooctyl acrylate, 10 parts by mass of VeoVa10 and 100 parts by mass of toluene as a polymerization solvent were put into a three-necked flask, nitrogen gas was introduced below the liquid surface, and the temperature of the three-necked flask was raised in a water bath, and stirring was started while introducing nitrogen gas at a stirring speed of 100 to 200 revolutions per minute and was continued for 2 hours, and the temperature was maintained at 70 ℃ during the introduction of nitrogen gas. Oxygen in the polymerization system was removed as much as possible, 0.05 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the exothermic reaction was started, the reaction mixture was heated to 73 ℃ and held at a cooling temperature for 30 hours, 0.05 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the reaction mixture was heated to 83 ℃ and held at a temperature for 1 hour, 0.25 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the reaction mixture was heated to 88 ℃ and held at a temperature for 6 hours, and when the reaction mixture was cooled to 70 ℃ or less, 50 parts by weight of ethyl acetate was added to obtain a polymer solution. The resulting polymer had a Tg of-40 deg.C, a solids content of 40%, a viscosity of 15000mPa.s and a weight average molecular weight of 100 ten thousand.
To the polymer solution, 5 parts by weight of a tackified synthetic rosin resin having a softening point of 135 ℃ (manufactured by seikagawa chemical corporation) and 15 parts by weight of a C5 petroleum-based tackifying resin having a softening point of 100 ℃ (puggangbanlu chemical corporation) were added per 100 parts by weight of the solid content thereof, and 30 parts by weight of ethyl acetate was added to prepare an adhesive composition having a solid content of 40%, wherein the solvent-type modified polyacrylate pressure-sensitive adhesive had a viscosity of 12000mpa.s at 23 ± 2 ℃.
Before coating, 0.5 part by weight of an isocyanate-based crosslinking agent (manufactured by Tosoh chemical Co., Ltd.) was mixed with 100 parts by weight of the solid content of the composition, and the composition was diluted with ethyl acetate according to the coating process and the product design.
Preparation example 2 of adhesive:
4.45 parts by mass of acrylic acid, 0.2 part by mass of hydroxyethyl acrylate, 35 parts by mass of ethyl acrylate, 45 parts by mass of isooctyl acrylate, 15 parts by mass of VeoVa10 and 100 parts by mass of toluene as a polymerization solvent were put into a three-necked flask, nitrogen gas was introduced below the liquid surface, and the temperature of the three-necked flask was raised in a water bath, and stirring was started while introducing nitrogen gas at a stirring speed of 100 to 200 revolutions per minute and was continued for 2 hours, and the temperature was maintained at 70 ℃ during the introduction of nitrogen gas. Oxygen in the polymerization system was removed as much as possible, 0.05 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the exothermic reaction was started, the reaction mixture was heated to 73 ℃ and held at a cooling temperature for 30 hours, 0.05 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the reaction mixture was heated to 83 ℃ and held at a temperature for 1 hour, 0.25 part by weight of AIBN (azobisisobutyronitrile) dissolved with a small amount of ethyl acetate was added, the reaction mixture was heated to 88 ℃ and held at a temperature for 6 hours, and when the reaction mixture was cooled to 70 ℃ or less, 50 parts by weight of ethyl acetate was added to obtain a polymer solution. The resulting polymer had a glass transition temperature of Tg-39 deg.C, a solids content of 40%, a viscosity of 25000mPa.s, and a weight average molecular weight of 130 ten thousand.
To the polymer solution, 5 parts by weight of a tackified synthetic rosin resin having a softening point of 135 ℃ (manufactured by seikagawa chemical corporation) and 15 parts by weight of a C5 petroleum-based tackifying resin having a softening point of 100 ℃ (puyang bandhu chemical limited) were added per 100 parts by weight of the solid content thereof, and 30 parts by weight of ethyl acetate was added to prepare an adhesive composition having a solid content of 40%, wherein the solvent-type modified polyacrylate pressure-sensitive adhesive had a viscosity of 20000mpa.s at 23 ± 2 ℃.
Before coating, 0.5 part by weight of an isocyanate-based crosslinking agent (manufactured by Tosoh chemical Co., Ltd.) was mixed with 100 parts by weight of the solid content of the composition, and the composition was diluted with ethyl acetate according to the coating process and the product design.
Preparation example 3 of adhesive:
to the polymer solution of preparation example 1 of the adhesive, 10 parts by weight of a tackified synthetic rosin resin having a softening point of 135 ℃ (manufactured by seikagawa chemical corporation) and 10 parts by weight of a C5 petroleum-based tackifying resin having a softening point of 100 ℃ (puggangband chemical corporation) were added per 100 parts by weight of the solid content thereof, and 30 parts by weight of ethyl acetate was added to prepare an adhesive composition having a solid content of 40%, wherein the solvent-type modified polyacrylate pressure-sensitive adhesive had a viscosity of 10000mpa.s at 23 ± 2 ℃.
Before coating, 0.5 part by weight of an isocyanate-based crosslinking agent (manufactured by Tosoh chemical Co., Ltd.) was mixed with 100 parts by weight of the solid content of the composition, and the composition was diluted with ethyl acetate according to the coating process and the product design.
Preparation example 4 of adhesive:
to a polymer solution of preparation example 2 of the adhesive, 10 parts by weight of a tackified synthetic rosin resin having a softening point of 135 ℃ (manufactured by seikagawa chemical corporation) and 10 parts by weight of a C5 petroleum-based tackifying resin having a softening point of 100 ℃ (puyang, kokushi, kokukoku corporation) were added, and 30 parts by weight of ethyl acetate was added to prepare an adhesive composition having a solid content of 40%, wherein the solvent-type modified polyacrylate pressure-sensitive adhesive had a viscosity of 20000mpa.s at 23 ± 2 ℃.
Before coating, 0.5 part by weight of an isocyanate-based crosslinking agent (manufactured by Tosoh chemical Co., Ltd.) was mixed with 100 parts by weight of the solid content of the composition, and the composition was diluted with ethyl acetate according to the coating process and the product design.
A method for preparing a double-sided adhesive tape,
comparative example 1: and (3) coating the adhesive obtained in the adhesive comparative example 1 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 4-micrometer adhesive layer, and compounding the adhesive layer with a 2-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. And (3) coating the adhesive obtained in the adhesive comparative example 1 on the release surface of the transparent PET release film, drying and drying at the highest temperature of 120 ℃, preparing a 4-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished product substrate to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 10 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Comparative example 2:
and (3) coating the adhesive obtained in the adhesive comparative example 1 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 1-micrometer adhesive layer, and compounding the adhesive layer with a 1.5-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive obtained in the adhesive comparative example 1 on the release surface of the transparent PET release film, drying and drying at the highest temperature of 120 ℃ to prepare a 1-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished product substrate to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 35 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Example 1:
and (2) coating the adhesive obtained in the adhesive preparation example 1 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 4-micrometer adhesive layer, and compounding the adhesive layer with a 2-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive obtained in the adhesive preparation 1 on the release surface of the transparent PET release film, drying at the highest temperature of 120 ℃, preparing a 4-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished base material to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 10 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Example 2:
and (3) coating the adhesive obtained in the adhesive preparation example 2 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 4-micrometer adhesive layer, and compounding the adhesive layer with a 2-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive prepared in the adhesive preparation 2 on the release surface of the transparent PET release film, drying at the highest temperature of 120 ℃, preparing a 4-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished base material to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 10 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Example 3:
and (3) coating the adhesive obtained in the adhesive preparation example 3 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 4-micrometer adhesive layer, and compounding the adhesive layer with a 2-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive prepared in the adhesive preparation 3 on the release surface of the transparent PET release film, drying at the highest temperature of 120 ℃, preparing a 4-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished base material to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 10 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Example 4:
and (3) coating the adhesive obtained in the adhesive preparation example 4 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 4-micrometer adhesive layer, and compounding the adhesive layer with a 2-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive prepared by the adhesive preparation 4 on the release surface of the transparent PET release film, drying at the highest temperature of 120 ℃, preparing a 4um adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished product substrate to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 10 um. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Example 5:
and (3) coating the adhesive obtained in the adhesive preparation example 3 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 1-micrometer adhesive layer, and compounding the adhesive layer with a 1.5-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive prepared in the adhesive preparation 3 on the release surface of the transparent PET release film, drying at the highest temperature of 120 ℃, preparing a 1-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished base material to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 3.5 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
Example 6:
and (3) coating the adhesive obtained in the adhesive preparation example 4 on the release surface of the transparent PET release film by adopting a micro-concave coating mode, drying and drying the release surface by coating equipment (with the highest temperature of 120 ℃), preparing a 1-micrometer adhesive layer, and compounding the adhesive layer with a 1.5-micrometer transparent PET base material to obtain a first engineering coating semi-finished product. Coating the adhesive prepared in the adhesive preparation step 4 on the release surface of the transparent PET release film, drying at the highest temperature of 120 ℃, preparing a 1-micron adhesive layer, and compounding the adhesive layer with the other composite surface of the first engineering coating semi-finished base material to obtain the double-sided PET adhesive tape semi-finished product with the total thickness of 3.5 microns. And (4) placing the double-sided adhesive tape into a circulating air oven at 40 ℃, curing for 72 hours to prepare the double-sided adhesive tape, and finishing all the evaluations.
The above results are shown in table 1 below:
wet heat aging resistance rating: 1, extremely poor, the retention of adhesive force is less than or equal to 30 percent; 2, poor, and retaining 30-60% of adhesive force; 3, good, keeping the adhesive force by 60-80%; 4, excellent, the adhesive force retention is more than or equal to 80 percent.
As shown in the above table, it is confirmed that the ultra-thin PET double-sided tape of the present invention has better adhesion in all the examples than the comparative examples, wherein example 4 is the best; the wet heat aging resistance is better than the comparative examples, and the best example is shown in example 4.
In conclusion, the ultrathin high-viscosity high-weatherability acrylate adhesive polymer disclosed by the invention has the characteristics of thin coating, high viscosity, high temperature and high humidity resistance.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (6)
1. An adhesive characterized by: the adhesive is prepared from the following raw materials in parts by weight:
the alkyl acrylate monomer polymer comprises an alkyl acrylate monomer and an initiator; the alkyl acrylate monomer comprises a viscoelastic monomer and a functional group monomer, wherein the viscoelastic monomer consists of ethyl acrylate and isooctyl acrylate, and the functional group monomer consists of acrylic acid, hydroxyethyl acrylate and VeoVa 10; the tackifying resin consists of tackifying synthetic rosin resin and C5 petroleum tackifying resin;
the adhesive is prepared by the following method:
putting an alkyl acrylate monomer and a solvent into a three-neck flask, introducing nitrogen below the liquid level, heating in a water bath, starting stirring while introducing the nitrogen, continuously stirring for 2 hours at a stirring speed of 100-200 revolutions per minute, starting temperature maintenance when the temperature reaches 70 ℃ in the process of introducing the nitrogen, adding an initiator dissolved by the solvent, starting an exothermic reaction, cooling and maintaining the temperature when the temperature is raised to 73 ℃, maintaining the temperature for 30 hours, heating to 83 ℃ when the initiator dissolved by the solvent is added, maintaining the temperature for 1 hour, adding the initiator dissolved by the solvent, heating to 88 ℃, maintaining the temperature for 6 hours, and cooling to below 70 ℃, adding the solvent to obtain a polymer solution;
adding tackifying resin and a solvent into the polymer solution to prepare an adhesive composition; before coating, the adhesive composition is mixed with a crosslinking agent.
2. An adhesive as defined in claim 1, wherein: the solvent is an organic solvent, and the organic solvent is ethyl acetate, toluene, xylene, butanone, methanol or diethyl ether.
3. An adhesive as defined in claim 1, wherein: the cross-linking agent is isocyanate cross-linking agent or epoxy cross-linking agent or metal chelate or aziridine or amino.
4. A double-sided tape using the adhesive according to any one of claims 1 to 3, wherein the double-sided tape comprises: include substrate layer, gluing layer and leave the type material layer, the substrate layer is the PET film, gluing layer sets up at least one face at the substrate layer, laminate on gluing layer surface from the type material layer, it is transparent polyester from the type membrane to leave the type material layer, the thickness of substrate layer is 0.5 ~ 25 mu m.
5. A double-sided adhesive tape according to claim 4, characterized in that: the adhesive layer is arranged on the upper surface and the lower surface of the base material layer.
6. The method for preparing a double-sided adhesive tape according to claim 5, wherein: the method comprises the following steps:
step 1: conveying the adhesive to a micro-concave coating head through a pump, coating the adhesive on a release material layer by the micro-concave coating head, then drying the adhesive in an oven, laminating the adhesive and a substrate layer through a composite roller, and rolling a coating line in a first rolling manner to obtain a first engineering coating semi-finished product;
step 2: conveying the adhesive to a micro-concave coating head through a pump, coating the adhesive on a release material layer by the micro-concave coating head, then drying the adhesive in an oven, laminating the adhesive with a first engineering coating semi-finished product through a composite roller, and rolling a coating line in a first rolling manner to obtain a PET double-sided tape semi-finished product;
and step 3: and (3) placing the semi-finished product of the PET double-sided tape into a circulating air oven at 40 ℃, and curing for 72 hours to obtain a finished product of the PET double-sided tape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911336305.9A CN111087950B (en) | 2019-12-23 | 2019-12-23 | Adhesive, double-sided tape applying adhesive and preparation method of double-sided tape |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911336305.9A CN111087950B (en) | 2019-12-23 | 2019-12-23 | Adhesive, double-sided tape applying adhesive and preparation method of double-sided tape |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111087950A CN111087950A (en) | 2020-05-01 |
| CN111087950B true CN111087950B (en) | 2021-11-16 |
Family
ID=70396269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911336305.9A Active CN111087950B (en) | 2019-12-23 | 2019-12-23 | Adhesive, double-sided tape applying adhesive and preparation method of double-sided tape |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111087950B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111944438A (en) * | 2020-07-24 | 2020-11-17 | 崴思新材料泰州有限公司 | Diamond-shaped ultrathin high-viscosity exhaust adhesive tape |
| CN111849380A (en) * | 2020-08-05 | 2020-10-30 | 苏州睿泰鑫材料科技有限公司 | Preparation method of ultrathin adhesive tape with controllable thickness |
| CN112852353A (en) * | 2021-01-14 | 2021-05-28 | 厘鑫胶粘科技(上海)有限公司 | Release-free paper double-sided adhesive tape and preparation method thereof |
| CN113249045A (en) * | 2021-04-21 | 2021-08-13 | 东莞市清鸿新材料科技有限公司 | Double-sided adhesive tape with three-prevention and high viscosity and preparation method thereof |
| CN114479694A (en) * | 2021-12-09 | 2022-05-13 | 苏州赛伍应用技术股份有限公司 | Ultrathin adhesive tape for wireless charging nanocrystalline and preparation method thereof |
| CN115247043A (en) * | 2022-08-25 | 2022-10-28 | 苏州赛伍应用技术股份有限公司 | Adhesive composition, insulating adhesive tape and preparation method thereof |
| CN115505344A (en) * | 2022-09-23 | 2022-12-23 | 江苏伊诺尔新材料科技有限公司 | High-temperature-resistance blue-shielding double-sided adhesive tape and preparation process thereof |
| CN115368844B (en) * | 2022-09-27 | 2024-02-13 | 苏州赛伍应用技术股份有限公司 | Pressure-sensitive adhesive tape for mica-based composite material and preparation method thereof |
| CN115820139A (en) * | 2022-12-14 | 2023-03-21 | 江苏伊诺尔新材料科技有限公司 | Magnetic conduction double sticky tape suitable for wireless field of charging |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104152077B (en) * | 2014-08-13 | 2016-05-25 | 隆昌羽玺新材料科技有限公司 | A kind of ultra-thin polyester two-sided tape and by glue and preparation method |
| CN105754506A (en) * | 2016-03-11 | 2016-07-13 | 苏州赛伍应用技术有限公司 | Positioning adhesive tape for photovoltaic modules |
| CN106590459A (en) * | 2016-12-23 | 2017-04-26 | 苏州赛伍应用技术有限公司 | High temperature-resistant adhesive tape used for photovoltaic assembly battery piece positioning, and production method thereof |
-
2019
- 2019-12-23 CN CN201911336305.9A patent/CN111087950B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111087950A (en) | 2020-05-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111087950B (en) | Adhesive, double-sided tape applying adhesive and preparation method of double-sided tape | |
| CN111154429B (en) | Polyacrylate pressure-sensitive adhesive | |
| CN211896779U (en) | Self-exhaust double-sided tape | |
| CN103031090B (en) | Acid-free OCA and adhesive belt and fabrication method of acid-free OCA and adhesive belt | |
| US11168236B2 (en) | Acrylic pressure-sensitive adhesive composition and pressure-sensitive adhesive sheet | |
| CN106519106A (en) | Super-transparent acrylate pressure-sensitive adhesive emulsion capable of being coated at high speed as well as preparation method and application thereof | |
| CN101974299A (en) | High temperature-resistant polyacrylate pressure-sensitive adhesive emulsion and preparation method and application thereof | |
| CN103725231B (en) | Adhesive material for adhesive tapes and preparation method thereof | |
| CN101798491A (en) | Pressure sensitive adhesive for protective film and preparation method thereof | |
| CN103788901A (en) | High temperature resistant pressure sensitive adhesive composition and preparation method thereof as well as double-sided adhesive tape | |
| CN103937197B (en) | A kind ofly prepare the polyurethane synthetic resin of seamless sticker and apply the seamless sticker that it is prepared | |
| CN102952503A (en) | High temperature resisting pressure-sensitive adhesive composition and high temperature resisting pressure-sensitive adhesive tape | |
| CN108285762B (en) | Acrylic acid adhesive and foam adhesive tape | |
| TW201923006A (en) | Adhesive sheet capable of maintaining the re-workability and further increasing the adhesive force subsequently | |
| CN109135588B (en) | Adhesive and application thereof | |
| CN103834320A (en) | Re-peel-off type special double-faced adhesive sheet for fixing flexible printed circuit board | |
| EP2447330B1 (en) | Clean removable adhesive sheet | |
| CN114214006B (en) | OCA optical glue with high filling property and OCA optical adhesive film | |
| CN101875829A (en) | Aqueous emulsion polyacrylate pressure-sensitive adhesive and preparation method thereof | |
| CN113024714A (en) | (meth) acrylic polymer having crosslinkable functional group at terminal position | |
| KR101233149B1 (en) | Adhesive Sheet with Emboss Release Liner | |
| TW201130863A (en) | Multimodal copolymers, their production and application in pressure-sensitive adhesive | |
| US20190161651A1 (en) | Pressure-sensitive adhesive sheet | |
| CN102101996A (en) | Pressure-sensitive adhesive used for cotton paper or non-woven fabrics and preparation method thereof | |
| US20200299553A1 (en) | Curable adhesive composition as well as adhesive tapes and products produced therefrom |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |