CN110628363A - Preparation method of adhesive and preparation method of adhesive tape - Google Patents
Preparation method of adhesive and preparation method of adhesive tape Download PDFInfo
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- CN110628363A CN110628363A CN201910929745.9A CN201910929745A CN110628363A CN 110628363 A CN110628363 A CN 110628363A CN 201910929745 A CN201910929745 A CN 201910929745A CN 110628363 A CN110628363 A CN 110628363A
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- 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
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- 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
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
- C09J133/12—Homopolymers or copolymers of methyl methacrylate
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- 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
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- 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
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- 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
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- 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
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a preparation method of an adhesive and a preparation method of an adhesive tape thereof, wherein a reasonable formula design is adopted, a precise coating mode is utilized to form a film, the performance that common UV (ultraviolet) viscosity reducing adhesive cannot be balanced in a harsh environment can be realized, and the adhesive not only has the common characteristics of high adhesion in the initial stage and extremely low adhesion after UV in the aspect of performance, but also can keep the excellent performance of stable performance under harsh conditions such as high temperature, high humidity, low temperature, cold and hot shock and the like; or a synthetic mechanism of solvent type free radical polymerization is adopted, a film is formed by a precise coating mode, the uniform and thin thickness of the UV type OCA which is difficult to realize can be realized, the UV type OCA has the advantages of high adhesive force, high temperature and high humidity resistance, low temperature resistance and cold and heat shock resistance in the aspect of performance, the reworking performance is excellent, the excellent performance which is difficult to balance of other OCA adhesives is considered, the used raw material acrylate monomers are all monomers with low industrial price, and no special monomer is available.
Description
Technical Field
The invention belongs to the technical field of adhesive materials, and relates to a preparation method of an adhesive and a preparation method of an adhesive tape.
Background
With the rapid development of science and technology, the electronic industry is updated very rapidly. The demand of UV visbreaking protective films in various fields such as wafer cutting, semiconductor chips, OCA (optical clear adhesive) bonding and positioning is increasing or decreasing. Such tapes are intended to be stable in position initially, and to be easily removed after the cutting process and UV irradiation without leaving any residue, so that the tape is required to have a high adhesion initially and a property of rapidly reducing the adhesion after UV irradiation. The principle for realizing the process is that after UV, double bonds of a large number of oligomers in the adhesive tape are subjected to crosslinking reaction, and Tg is rapidly increased to lose viscosity. For a commercially available UV visbreaking tape with a 15 μm thickness, an initial adhesion of 18N/25mm and a post-UV adhesion of 0.1N/25mm will become common requirements. However, some of the existing domestic UV visbreaking tapes can only maintain 20N within one month, and in order to meet the acid and alkali resistance, the optimal formula can only achieve 10N in the initial stage under the condition that the UV is reduced to 0.1N after the UV is met. Therefore, the improvement of the performance of the UV visbreaking adhesive tape has a domestic rising space. In addition, another problem is that the main resin of the UV anti-adhesive tape is mainly purchased, is not independently developed, and is easily hampered by some foreign suppliers besides the problem of high price. In addition to the requirement for initial and post-UV adhesion of UV adhesive tapes, weatherability will also be an important trend. For example, 24 months 1 and 2018, the lowest temperature of harbin reaches-33 ℃; the humidity of 23 Risu district in 4 and 4 months in 2019 can reach 85RH percent, the different environments can cause great influence on the performance of the adhesive tape, some UV visbreaking adhesive tapes can completely lose effectiveness after changing the district, and the problem of weather resistance is also an important subject.
In addition, the application field of OCA (transparent optical adhesive tape) is mostly on the cover plate and the back cover of the mobile phone. In the field of rupture membranes, it is required that the higher the adhesion of the OCA, the better, so as to prevent splashing caused by screen cracking, resulting in unnecessary damage. However, in actual production, 100% success of the application is difficult to achieve, and rework may be required. The high-adhesion OCA is easy to remain adhesive, and further the waste adhesive tape (reworked adhesive tape) needs to be further removed, so that the process is complicated, the efficiency is reduced, and the cost is increased. Most of the traditional OCAs are polymerized in a UV mode, the light transmittance and the properties of cold and heat shock are good, and in addition, the method has the advantages of no solvent and low VOC (volatile organic compounds). However, the method of UV preparation of solvent-free OCA cannot avoid the disadvantage of large thickness tolerances in thin coating due to equipment reasons. For example, an OCA of 25 μm, the practical tolerance may be up to + -5 μm. The solvent-based OCA can exert advantages, and the thickness tolerance can still keep +/-1 mu m under the condition that the thickness is very thin by precisely coating the solvent-based OCA. This is more in line with the new trend of faster, lighter and thinner requirements of current technological development. At present, research is also carried out on solvent type reworkable OCA, the initial adhesive force of the OCA adhesive tape can reach 1900g/25mm, and the reworking performance is excellent. However, the method for testing the reworkability (reworkability) is as follows: and sticking the adhesive tape on a mobile phone cover plate, and standing for 2 hours at room temperature. The reworking performance is judged by tearing the solvent-based OCA manually, and the reworking performance is judged according to the tearing difficulty, so that the requirement of the market on reworking is more strict at present, the reworking performance is required to be tested under the condition of 80 ℃ for 1 hour under the pressure of 7kg, the requirement of hot tearing is also required to be carried out under the condition of 70 ℃ to check the reworking performance, and under the strict condition, the common reworking OCA cannot meet the requirement, so that the solvent-based OCA with more excellent performance needs to be developed.
Therefore, there is a need for an adhesive and tape thereof.
Disclosure of Invention
The invention aims to provide a preparation method of an adhesive and a preparation method of an adhesive tape, and solves the technical problems.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the adhesive comprises the following steps:
(1) preparation of mixed monomers: according to parts by weight, mixing and stirring 0-5 parts of methyl methacrylate, 0-15 parts of isobornyl acrylate, 2.5-12.5 parts of acrylic acid and 69-84 parts of n-butyl acrylate uniformly to obtain a polymerization monomer;
(2) adding the polymerization monomer into a four-neck flask, adding 150-230 parts of solvent, introducing nitrogen under a water bath condition, adding azodiisobutyronitrile with the concentration of 0.1%, and starting to react for 3 hours;
(3) heating to 78 deg.C within 1 hr, adding azodiisobutyronitrile with concentration of 0.1%, and maintaining for 2 hr;
(4) and adding 170-250 parts of solvent for dilution, cooling to room temperature, and discharging to obtain the adhesive.
As a preferred embodiment of the present invention, step (2) is replaced with: adding the polymerization monomer into a four-neck flask, adding 150-230 parts of solvent, introducing nitrogen under the condition of water bath, adding azodiisobutyronitrile with the concentration of 0.1%, and starting to react for 3 hours.
In a preferred embodiment of the present invention, in step (1), the components include 1 to 3 parts of methyl methacrylate, 12 to 15 parts of isobornyl acrylate, 2.5 to 12.5 parts of acrylic acid, and 69 to 84 parts of n-butyl acrylate.
As a preferred embodiment of the present invention, the nitrogen gas is introduced into the step (2) for 1 hour at a nitrogen rate of 500ml/min at a temperature of 63-67 ℃.
As a preferred embodiment of the present invention, the solvent is ethyl acetate.
As a preferred embodiment of the present invention, the solid content of the adhesive in the step (4) is 20%.
The application also provides a preparation method of the adhesive tape, which comprises the following steps: firstly, taking 100g of the adhesive obtained in any one of claims 1 and 3-6, adding 10-50 g of ethyl acetate, 0.3g of epoxy curing agent, 8g of epoxy acrylic resin and 2g of photoinitiator, uniformly stirring, standing and defoaming; secondly, uniformly coating the defoamed adhesive on a 50-micron PET substrate, putting the PET substrate into a 120-DEG C oven for drying for 3min, taking out the PET substrate, measuring the thickness of the adhesive layer to be 15 microns, and then attaching the adhesive layer to a 75-micron PET release film to obtain a semi-product of the adhesive tape; and finally, putting the semi-finished product of the adhesive tape into a 60 ℃ oven, and curing for 2 days to obtain the finished product of the UV visbreaking adhesive tape.
The application also provides another preparation method of the adhesive tape: firstly, taking 100g of the adhesive obtained in any one of claims 2-6, adding 10-50 g of ethyl acetate and 0.3g of epoxy curing agent, uniformly stirring, standing and defoaming; secondly, uniformly coating the defoamed adhesive on a 50-micron PET substrate, putting the PET substrate into a 120-DEG C oven for drying for 3min, taking out the PET substrate to obtain a glue layer with the thickness of 25 microns, and attaching the glue layer to a 75-micron PET release film to obtain a semi-product of the adhesive tape; finally, putting the adhesive tape semi-product into a 60 ℃ oven, curing for 2 days to obtain a finished product OCA adhesive tape:
the invention discloses a preparation method of two adhesives, which comprises the following steps: a method for preparing weather-resistant UV (ultraviolet) viscosity-reducing adhesive main body resin through free radical polymerization is mainly applied to a UV viscosity-reducing adhesive tape under a severe temperature and humidity environment, related acrylate monomers are all low-cost industrialized monomers, Methyl Methacrylate (MMA), isobornyl acrylate (IBOA), Acrylic Acid (AA), n-Butyl Acrylate (BA) and the like, the weather-resistant UV viscosity-reducing adhesive main body resin adopts a synthetic mechanism of solvent type free radical polymerization, through reasonable formula design, a film is formed by utilizing a precise coating mode, the performance that general UV viscosity-reducing adhesive cannot be balanced in the severe environment can be realized, the general characteristics of high adhesion at the initial stage and extremely low adhesion after UV in the aspect of performance are provided, the excellent performance of stable performance can be still maintained under severe conditions of high temperature, high humidity, low temperature, cold and hot shock and the like, the used raw material acrylate monomers are all low-cost industrialized monomers, the adhesive tape has no special monomer, the initial adhesive force of the adhesive tape is more than 20N/25mm, the adhesive force can be rapidly reduced to be less than 10g/25mm after UV illumination, and stable adhesive tape performance can be ensured under the conditions of-40 ℃, 85 ℃/85 RH% and-40-80 ℃ cold and hot impact; the other method for preparing the solvent-type OCA (transparent optical adhesive tape) by free radical polymerization is characterized in that related acrylate monomers are all low-price industrialized monomers, Methyl Methacrylate (MMA), isobornyl acrylate (IBOA), Acrylic Acid (AA), n-Butyl Acrylate (BA) and the like, an OCA adhesive adopts a synthesis mechanism of solvent-type free radical polymerization, a precise coating mode is used for film forming, the uniform and thin thickness of the UV-type OCA which is difficult to realize can be realized, the performance has the advantages of high adhesion, high temperature and high humidity resistance, low temperature resistance and cold and heat shock resistance, the reworkability is excellent, the excellent performance which is difficult to balance of other OCA adhesives is considered, the used raw material acrylate monomers are all low-price industrialized monomers, no special monomers are available, the reworkability is excellent, and even if the OCA is treated under the condition of 80 ℃ and 7kg, can still be reworked, still ensures good reworkability when being hot-torn at 70 ℃, and can ensure high adhesive force performance of more than 16N under the conditions of cold and hot impact at 40 ℃ below zero, 85 ℃/85RH percent and 40 ℃ below zero to 80 ℃.
Detailed Description
A preparation method of weather-resistant UV visbreaking adhesive main body resin comprises the following steps:
step 1, preparation of mixed monomers: according to parts by weight, 0-5 parts of methyl methacrylate, 0-15 parts of isobornyl acrylate, 2.5-12.5 parts of acrylic acid and 69-84 parts of n-butyl acrylate are mixed and stirred uniformly to obtain a polymerized monomer; step 2, adding a polymerization monomer into a four-neck flask, adding 150-230 parts of ethyl acetate (EtAc) serving as a solvent, introducing nitrogen, heating by using a water bath kettle (the time is 1 hour, the nitrogen rate is 500ml/min, and the temperature is 63-67 ℃), then adding 0.1% of Azobisisobutyronitrile (AIBN), and starting to react for 3 hours; step 3, heating to 78 ℃ within 1 hour, adding 0.1% AIBN, and then preserving heat for 2 hours; step 4, adding 170-250 parts of EtAc diluent solvent, cooling to room temperature, and discharging to obtain the weather-resistant UV visbreaking adhesive main body resin; step 5, taking 100g of the weather-resistant UV visbreaking adhesive main body resin, adding 10-50 g of ethyl acetate (EtAc), 0.3g of epoxy curing agent NE-5X, 8g of epoxy acrylic resin CN159 (Sandoma, Guangzhou chemical Co., Ltd.), and 2g of photoinitiator 184, then uniformly stirring, standing and defoaming; step 6, uniformly coating the defoamed adhesive on a PET substrate with the thickness of 50 micrometers, putting the PET substrate into a drying oven with the temperature of 120 ℃ for drying for 3min, taking out the PET substrate, measuring the thickness of the adhesive layer to be 15 micrometers, and attaching a PET release film with the thickness of 75 micrometers to obtain a semi-product of the adhesive tape; and 7, putting the semi-finished product into a 60 ℃ oven, curing for 2 days to obtain a finished product of the UV visbreaking adhesive tape for testing.
In the above steps: in the step 1, 1-3 parts of methyl methacrylate, 12-15 parts of isobornyl acrylate, 2.5-12.5 parts of acrylic acid and 69-84 parts of n-butyl acrylate are preferably selected. The solid content of the main resin in the step 4 can be adjusted according to the dilution solvent, and is preferably 20%.
A preparation method of a reworkable solvent-based OCA comprises the following steps:
step 1, preparation of mixed monomers: according to parts by weight, 0-5 parts of methyl methacrylate, 0-15 parts of isobornyl acrylate, 2.5-12.5 parts of acrylic acid and 69-84 parts of n-butyl acrylate are mixed and stirred uniformly to obtain a polymerized monomer; step 2, adding a polymerization monomer into a four-neck flask, adding 150-230 parts of ethyl acetate (EtAc) serving as a solvent, introducing nitrogen, heating by using a water bath kettle (the time is 1 hour, the nitrogen rate is 500ml/min, and the temperature is 63-67 ℃), then adding 0.1% of Azobisisobutyronitrile (AIBN), and starting to react for 3 hours; step 3, heating to 78 ℃ within 1 hour, adding 0.1% AIBN, and then preserving heat for 2 hours; step 4, adding 170-250 parts of EtAc diluent solvent, cooling to room temperature, and discharging to obtain the solvent OCA; step 5, taking 100g of the solvent OCA, adding 10-50 g of ethyl acetate (EtAc) and 0.3g of epoxy curing agent NE-5X, uniformly stirring, standing and defoaming; step 6, uniformly coating the defoamed adhesive on a PET substrate with the thickness of 50 micrometers, putting the PET substrate into a drying oven with the temperature of 120 ℃ for drying for 3min, taking out the PET substrate, measuring the thickness of the adhesive layer to be 25 micrometers, and attaching a PET release film with the thickness of 75 micrometers to obtain a semi-product of the adhesive tape; and 7, putting the semi-finished product into a 60 ℃ oven, curing for 2 days to obtain a finished product OCA tape for testing.
In the above steps: 1-3 parts of methyl methacrylate, 12-15 parts of isobornyl acrylate, 2.5-12.5 parts of acrylic acid and 69-84 parts of n-butyl acrylate which are optimized in the step 1; further, the solid content of the solvent-type OCA in the step 4 can be adjusted according to the dilution solvent, and is preferably 20 percent
The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
Step 1, preparation of mixed monomers: according to the weight portion, 2 portions of isobornyl acrylate, 12.5 portions of acrylic acid and 80.5 portions of n-butyl acrylate are evenly stirred at normal temperature to obtain the mixed monomer.
And 2, adding the mixed monomer into a four-neck flask, adding 170 parts of ethyl acetate (EtAc) serving as a solvent, introducing nitrogen, simultaneously heating by using a water bath kettle (the time is 1 hour, the nitrogen rate is 500ml/min, and the temperature is 63-67 ℃), then adding 0.1% of Azobisisobutyronitrile (AIBN), defining the initial heat release as the initial time of the reaction, and controlling the reaction temperature within a set range for 3 hours.
And 3, heating to 78 ℃ in a temperature gradient manner for 1 hour, adding 0.1 percent of AIBN, and preserving heat for 2 hours.
And 4, adding 227 parts of EtAc diluent solvent, cooling to room temperature, and discharging to obtain the weather-resistant UV viscosity-reducing adhesive main body resin.
Step 5, taking 100g of the weather-resistant UV visbreaking adhesive main body resin, adding 10-50 g of ethyl acetate (EtAc), 0.3g of epoxy curing agent NE-5X, 8g of epoxy acrylic resin CN159 (Sandoma, Guangzhou chemical Co., Ltd.) and 2g of photoinitiator 184, then uniformly stirring, standing and defoaming
And 6, uniformly coating the defoamed adhesive on a PET (polyethylene terephthalate) substrate with the thickness of 50 micrometers, drying in a drying oven with the temperature of 120 ℃ for 3min, taking out the adhesive, measuring the thickness of the adhesive to be 15 micrometers, and attaching a PET release film with the thickness of 75 micrometers to obtain a semi-product of the adhesive tape.
And 7, putting the semi-finished product into a 60 ℃ oven, curing for 2 days to obtain a finished product of the UV visbreaking adhesive tape for testing.
Example 2
Example 1 was repeated except that:
in step 1), 4 parts of isobornyl acrylate, 12.5 parts of acrylic acid and 78.5 parts of n-butyl acrylate.
In step 2), 160 parts of EtAc were added.
In step 4), 237 parts of EtAc were added.
Example 3
Example 1 was repeated except that:
in the step 1), 15 parts of isobornyl acrylate, 10 parts of acrylic acid and 75 parts of n-butyl acrylate.
In step 2), 160 parts of EtAc were added.
In step 4), 237 parts of EtAc were added.
Example 4
Example 1 was repeated except that:
in step 1), methyl methacrylate is 1 part, isobornyl acrylate is 15 parts, acrylic acid is 2.5 parts, and n-butyl acrylate is 81.5 parts.
In step 2), 160 parts of EtAc were added.
In step 4), 237 parts of EtAc were added.
Example 5
Example 1 was repeated except that:
in the step 1), 2 parts of methyl methacrylate, 2 parts of acrylic acid, 71 parts of n-butyl acrylate and 25 parts of methyl acrylate.
Example 6
Example 1 was repeated except that:
in step 1), 2 parts of methyl methacrylate, 2 parts of isobornyl acrylate, 12.5 parts of acrylic acid, 58.5 parts of n-butyl acrylate and 25 parts of methyl acrylate.
In the step 2), 180 parts of EtAc is added.
In step 4), 217 parts of EtAc was added.
Example 7
Example 1 was repeated except that:
in step 1), 3 parts of methyl methacrylate, 10 parts of isobornyl acrylate, 2.5 parts of acrylic acid and 84.5 parts of n-butyl acrylate.
In step 2), 150 parts of EtAc was added.
In step 4), 247 parts of EtAc were added.
Example 8
Example 1 was repeated except that:
in step 1), methyl methacrylate is 4 parts, acrylic acid is 2.5 parts, n-butyl acrylate is 53.5 parts, and methyl acrylate is 40 parts.
In the step 2), 180 parts of EtAc is added.
In step 4), 217 parts of EtAc was added.
The comparative test of the relevant performance of the UV visbreaking adhesive tape prepared by the above examples has the following results:
table 1 test results of each example
Note: abbreviations and symbols in the table are summarized: 2-EHA: isooctyl acrylate; MMA: methyl methacrylate; IBOA: isobornyl methacrylate; AA: acrylic acid; BA: n-butyl acrylate; a: methyl acrylate; AIBN: azobisisobutyronitrile; EtAc: ethyl acetate; 5B: no shedding.
Example 9
Step 1, preparation of mixed monomers: according to the weight portion, 2 portions of isobornyl acrylate, 12.5 portions of acrylic acid and 80.5 portions of n-butyl acrylate are evenly stirred at normal temperature to obtain the mixed monomer.
And 2, adding the mixed monomer into a four-neck flask, adding 170 parts of ethyl acetate (EtAc) serving as a solvent, introducing nitrogen, simultaneously heating by using a water bath kettle (the time is 1 hour, the nitrogen rate is 500ml/min, and the temperature is 63-67 ℃), then adding 0.1% of Azobisisobutyronitrile (AIBN), defining the initial heat release as the initial time of the reaction, and controlling the reaction temperature within a set range for 3 hours.
And 3, heating to 78 ℃ in a temperature gradient manner for 1 hour, adding 0.1 percent of AIBN, and preserving heat for 2 hours.
And 4, adding 227 parts of EtAc diluent solvent, cooling to room temperature, and discharging to obtain the solvent OCA.
And 5, taking 100g of the solvent OCA, adding 10-50 g of ethyl acetate (EtAc) and 0.3g of epoxy curing agent NE-5X, uniformly stirring, standing and defoaming.
And 6, uniformly coating the defoamed adhesive on a PET (polyethylene terephthalate) substrate with the thickness of 50 micrometers, drying in a drying oven with the temperature of 120 ℃ for 3min, taking out the adhesive, measuring the thickness of the adhesive to be 25 micrometers, and attaching a PET release film with the thickness of 75 micrometers to obtain a semi-product of the adhesive tape.
And 7, putting the semi-finished product into a 60 ℃ oven, curing for 2 days to obtain a finished product OCA tape for testing.
Example 10
Example 1 was repeated except that:
in step 1), 4 parts of isobornyl acrylate, 12.5 parts of acrylic acid and 78.5 parts of n-butyl acrylate.
In step 2), 160 parts of EtAc were added.
In step 4), 237 parts of EtAc were added.
Example 11
Example 1 was repeated except that:
in the step 1), 15 parts of isobornyl acrylate, 10 parts of acrylic acid and 75 parts of n-butyl acrylate.
In step 2), 160 parts of EtAc were added.
In step 4), 237 parts of EtAc were added.
Example 12
Example 1 was repeated except that:
in step 1), methyl methacrylate is 1 part, isobornyl acrylate is 15 parts, acrylic acid is 2.5 parts, and n-butyl acrylate is 81.5 parts.
In step 2), 160 parts of EtAc were added.
In step 4), 237 parts of EtAc were added.
Example 13
Example 1 was repeated except that:
in the step 1), 2 parts of methyl methacrylate, 2 parts of acrylic acid, 71 parts of n-butyl acrylate and 25 parts of methyl acrylate.
Example 14
Example 1 was repeated except that:
in step 1), 2 parts of methyl methacrylate, 2 parts of isobornyl acrylate, 12.5 parts of acrylic acid, 58.5 parts of n-butyl acrylate and 25 parts of methyl acrylate.
In the step 2), 180 parts of EtAc is added.
In step 4), 217 parts of EtAc was added.
Example 15
Example 1 was repeated except that:
in step 1), 3 parts of methyl methacrylate, 10 parts of isobornyl acrylate, 2.5 parts of acrylic acid and 84.5 parts of n-butyl acrylate.
In step 2), 150 parts of EtAc was added.
In step 4), 247 parts of EtAc were added.
Example 16
Example 1 was repeated except that:
in step 1), methyl methacrylate is 4 parts, acrylic acid is 2.5 parts, n-butyl acrylate is 53.5 parts, and methyl acrylate is 40 parts.
In the step 2), 180 parts of EtAc is added.
In step 4), 217 parts of EtAc was added.
The comparative test of the relevant performance of the OCA adhesive tape prepared by the above examples has the following results:
TABLE-test results under different examples
Note: abbreviations and symbols in the table are summarized: 2-EHA: isooctyl acrylate; MMA: methyl methacrylate; IBOA: isobornyl methacrylate; AA: acrylic acid; BA: n-butyl acrylate; MA: methyl acrylate; AIBN: azobisisobutyronitrile; EtAc: ethyl acetate; o: excellent; and (delta): generally; x: and (4) poor.
In conclusion, the super-adhesive and the preparation method of the adhesive tape have the beneficial effects that: the adhesive force before UV is more than 20N/25mm, and the adhesive force after UV can be reduced to be less than 0.1N/25 mm; 2. the performance is kept stable under the conditions of high temperature, cold and hot impact, low temperature and high humidity; 3, the OCA still keeps excellent reworking performance at high temperature after high-temperature defoaming; the OCA can still maintain good OCA performance under the conditions of high temperature, high humidity, low temperature and cold and hot impact.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (8)
1. The preparation method of the adhesive is characterized by comprising the following steps:
(1) preparing mixed monomers, namely mixing and uniformly stirring 0 ~ 5 parts of methyl methacrylate, 0 ~ 15 parts of isobornyl acrylate, 2.5 ~ 12.5.5 parts of acrylic acid and 69 ~ 84 parts of n-butyl acrylate according to parts by weight to obtain a polymerized monomer;
(2) adding the polymerization monomer into a four-neck flask, adding 150 ~ 230 parts of solvent, introducing nitrogen under the condition of water bath, adding 0.1% azobisisobutyronitrile, and starting to react for 3 hours;
(3) heating to 78 deg.C within 1 hr, adding azodiisobutyronitrile with concentration of 0.1%, and maintaining for 2 hr;
(4) and adding 170 ~ 250 parts of solvent to dilute, cooling to room temperature, and discharging to obtain the adhesive.
2. The method for preparing the adhesive according to claim 1, wherein the step (2) is replaced by adding the polymerized monomers into a four-neck flask, adding 150 ~ 230 parts of solvent, introducing nitrogen under the condition of water bath, adding azobisisobutyronitrile with the concentration of 0.1%, and starting the reaction for 3 hours.
3. The process according to claim 1 or 2, wherein in the step (1), the methyl methacrylate is 1 ~ 3 parts, isobornyl acrylate is 12 ~ 15 parts, acrylic acid is 2.5 ~ 12.5.5 parts, and n-butyl acrylate is 69 ~ 84 parts.
4. The process according to claim 1 or 2, wherein the nitrogen gas is introduced in the step (2) at a rate of 500ml/min for 1 hour and at a temperature of 63 ~ 67 ℃.
5. The method for preparing an adhesive according to claim 1 or 2, wherein: the solvent is ethyl acetate.
6. The method for preparing an adhesive according to claim 1 or 2, wherein: the solid content of the adhesive in the step (4) is 20%.
7. A preparation method of the adhesive tape is characterized by comprising the following steps:
firstly, taking 100g of the adhesive obtained in any one of claims 1 and 3-6, adding 10 ~ 50g of ethyl acetate, 0.3g of epoxy curing agent, 8g of epoxy acrylic resin and 2g of photoinitiator, then uniformly stirring, standing and defoaming;
secondly, uniformly coating the defoamed adhesive on a 50-micron PET substrate, putting the PET substrate into a 120-DEG C oven for drying for 3min, taking out the PET substrate, measuring the thickness of the adhesive layer to be 15 microns, and then attaching the adhesive layer to a 75-micron PET release film to obtain a semi-product of the adhesive tape;
and finally, putting the semi-finished product of the adhesive tape into a 60 ℃ oven, and curing for 2 days to obtain the finished product of the UV visbreaking adhesive tape.
8. A preparation method of the adhesive tape is characterized by comprising the following steps:
firstly, taking 100g of the adhesive obtained in any one of claims 2-6, adding 10 ~ 50g of ethyl acetate and 0.3g of epoxy curing agent, uniformly stirring, standing and defoaming;
secondly, uniformly coating the defoamed adhesive on a 50-micron PET substrate, putting the PET substrate into a 120-DEG C oven for drying for 3min, taking out the PET substrate to obtain a glue layer with the thickness of 25 microns, and attaching the glue layer to a 75-micron PET release film to obtain a semi-product of the adhesive tape;
and finally, putting the semi-product of the adhesive tape into a 60 ℃ oven, and curing for 2 days to obtain a finished product OCA adhesive tape.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113429907A (en) * | 2021-07-27 | 2021-09-24 | 江苏斯迪克新材料科技股份有限公司 | Preparation method of high-temperature-resistant low-transfer protective film |
| CN115197663A (en) * | 2022-08-15 | 2022-10-18 | 芊惠半导体科技(苏州)有限公司 | UV (ultraviolet) viscosity reducing adhesive for wafer, preparation method of UV viscosity reducing adhesive and UV viscosity reducing adhesive tape for wafer |
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| US20170290125A1 (en) * | 2016-03-29 | 2017-10-05 | Asustek Computer Inc. | Lighting structure with patterns |
| CN107353854A (en) * | 2017-07-14 | 2017-11-17 | 东莞市纳利光学材料有限公司 | A kind of OCA optical cements and OCA optical adhesive films |
| CN109096441A (en) * | 2018-06-11 | 2018-12-28 | 广州慧谷工程材料有限公司 | A kind of OCA resin combination, OCA adhesive tape and preparation method thereof |
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| US20170290125A1 (en) * | 2016-03-29 | 2017-10-05 | Asustek Computer Inc. | Lighting structure with patterns |
| CN107353854A (en) * | 2017-07-14 | 2017-11-17 | 东莞市纳利光学材料有限公司 | A kind of OCA optical cements and OCA optical adhesive films |
| CN109096441A (en) * | 2018-06-11 | 2018-12-28 | 广州慧谷工程材料有限公司 | A kind of OCA resin combination, OCA adhesive tape and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113429907A (en) * | 2021-07-27 | 2021-09-24 | 江苏斯迪克新材料科技股份有限公司 | Preparation method of high-temperature-resistant low-transfer protective film |
| CN115197663A (en) * | 2022-08-15 | 2022-10-18 | 芊惠半导体科技(苏州)有限公司 | UV (ultraviolet) viscosity reducing adhesive for wafer, preparation method of UV viscosity reducing adhesive and UV viscosity reducing adhesive tape for wafer |
| CN115197663B (en) * | 2022-08-15 | 2024-06-21 | 芊惠半导体科技(苏州)有限公司 | UV (ultraviolet) adhesive reducing tape for wafer, preparation method of UV adhesive reducing tape and UV adhesive reducing tape for wafer |
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Application publication date: 20191231 |