CN110016295B - Optical adhesive for repairing cracks of touch screen and application thereof - Google Patents
Optical adhesive for repairing cracks of touch screen and application thereof Download PDFInfo
- Publication number
- CN110016295B CN110016295B CN201910279862.5A CN201910279862A CN110016295B CN 110016295 B CN110016295 B CN 110016295B CN 201910279862 A CN201910279862 A CN 201910279862A CN 110016295 B CN110016295 B CN 110016295B
- Authority
- CN
- China
- Prior art keywords
- mixture
- minutes
- touch screen
- acrylate
- mixed solution
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/487—Polyethers containing cyclic groups
- C08G18/4883—Polyethers containing cyclic groups containing cyclic groups having at least one oxygen atom in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention provides an optical adhesive for repairing cracks of a touch screen and application thereof, which is prepared by mixing an ultraviolet light initiator with monomers such as glycidyl methacrylate, ethoxylated trimethylolpropane triacrylate and the like to prepare a first mixture, adding an emulsifier into deionized water to obtain a mixed solution, then mixing acrylic ester, toluene diisocyanate, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate, isobornyl methacrylate and the like serving as raw materials with the mixed solution to prepare prepolymer emulsion, and then adding ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether, dibutyltin dilaurate, a copolymer of 2-methyl methacrylate and butyl acrylate to prepare a second mixture, and finally slowly adding the first mixture into the second mixture under a light-shielding condition to obtain the optical adhesive for repairing the cracks of the touch screen. The original appearance of the touch screen is restored after the repair, crack traces can not be seen visually, the light transmittance is over 99.5 percent, the viscosity is high, and the curing shrinkage rate is low.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an optical adhesive for repairing cracks of a touch screen and application thereof.
Background
In recent years, with the widespread use of electronic devices such as mobile phones, touch panels have been developed very rapidly. The touch screen is relatively fragile, and is very easy to be damaged by cracks and the like due to collision in daily use. It is now common practice to replace a new touch screen, which requires specialized equipment by a professional, time consuming, and costly. Moreover, the crack degree of the touch screen is not serious in many times, and the direct replacement undoubtedly causes resource waste.
Compared with the common adhesive, the special adhesive for cementing the transparent optical element, also called as optical adhesive, has higher requirement, needs to be colorless and transparent, has the light transmittance of more than 90 percent, has good cementing strength, can be cured at room temperature or intermediate temperature, and has the characteristics of small curing shrinkage and the like. It is common to use silicone, acrylic resins, unsaturated polyesters, polyurethanes, epoxies, etc. for cementing optical components, and it is often necessary to add a certain amount of a treating agent to improve the optical properties or reduce the cure shrinkage during formulation.
The existing optical cement product cannot meet the high standard requirement of crack repair of the touch screen.
Disclosure of Invention
The invention aims to provide an optical adhesive for repairing cracks of a touch screen and application thereof, which can meet the high standard requirement of repairing cracks of the touch screen.
In order to achieve the purpose, the invention is realized by the following scheme:
a preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5-6: 7-8, mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water of which the weight is 40-50 times that of the emulsifier, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 10-15 minutes, adding acrylate and toluene diisocyanate, carrying out ultrasonic oscillation for 10-12 minutes, then adding the mixture into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 800-1000 r/min for 25-30 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 55-65 ℃, reacting for 2-3 hours, adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 70-80 ℃, and reacting for 3-4 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Preferably, in the step (1), the ultraviolet light initiator is selected from any one or more of benzils (diphenylethanone, α -dimethoxy- α -phenylacetophenone), alkylbenzophenones (α, α -diethoxyacetophenone, α -hydroxyalkylphenone, α -aminoalkylphenone), acylphosphorus oxides (aroylphosphine oxide, bisbenzoylphenylphosphine oxide), benzophenones (benzophenone, 2, 4-dihydroxybenzophenone, michler's ketone), diaryliodonium salts, triaryliodonium salts, alkyliodonium salts, cumeneferrocene hexafluorophosphate; they are compounds which can decompose free radicals or cations under ultraviolet light (wavelength of 250-400 nm).
Preferably, in the step (2), the emulsifier is sodium dodecyl sulfate or polyethylene glycol nonyl benzyl ether.
Preferably, in the step (3), the mass ratio of the silica hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 10-15: 8-10: 10-12: 20-30: 10-12: 12-15: 3-5: 4 to 7.
Preferably, in the step (3), the sequential slow addition means that the feeding is completed within 20-30 minutes.
Preferably, in the step (3), the silica hollow nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, carrying out ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 180-200 ℃, reacting for 12-24 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 180-200 mg: 18mL of: 50 mg.
Further preferably, the specific method of centrifugation is: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
Further preferably, the silica nano solid sphere is prepared by
The method comprises the following steps: under the environment of 30 ℃, 100mL of absolute ethyl alcohol, 3mL of secondary distilled water and 5mL of ammonia water solution with the mass concentration of 25-28% are placed in a three-neck flask, placed in a magnetic stirrer (1200 rpm) and stirred for 10 minutes, then 4mL of tetraethyl orthosilicate is added dropwise (the solution is completely dripped in 30 minutes), and after stirring is continued for 4-5 hours, the volume ratio of the mixture is 1: and (3) centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water of 1 for 3-4 times (10000 r/min, 5 min/time) to obtain the product.
More preferably, the particle size of the silicon dioxide nanometer solid sphere is 170-220 nm.
Preferably, in the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the methyl 2-methacrylate and the butyl acrylate is 1: 3-4: 0.002 to 0.005: 25-30: 2 to 3.
Preferably, in the step (4), the defoaming agent is mixed in a mass ratio of 1: 1.5-2.5 of a mixture of polydimethylsiloxane and polyoxypropylene polyoxyethylene glycerol ether, and the omission of any component can affect various performances of the obtained optical cement, so that the repair effect is poor.
Preferably, in the step (4), the mass ratio of the leveling agent is 1: 2-3, omitting any component which can affect various performances of the obtained optical cement, and causing the repairing effect to be poor.
Preferably, in the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.3-0.4: 0.001 to 0.002: 0.001 to 0.002.
Preferably, in the step (5), the slow adding is completed within 20-30 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
The optical cement is applied to touch screen crack repair.
Preferably, the specific method of the application is as follows: cleaning cracks of the touch screen, extruding the optical cement into the cracks, erasing redundant optical cement overflowing the cracks, and directly irradiating for 8-10 minutes in the sun or for 30-50 seconds under an ultraviolet lamp.
Further preferably, the specific method for cleaning the cracks of the touch screen is as follows: and (4) penetrating the crack by using a fine needle, removing any loose particles, repeatedly blowing for 2-3 minutes by using a hair drier, and wiping the periphery of the crack by using clean non-woven fabric.
The invention has the beneficial effects that:
the method comprises the steps of mixing an ultraviolet initiator with monomers such as glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate to prepare a first mixture, adding an emulsifier into deionized water to obtain a mixed solution, mixing the mixed solution with raw materials such as acrylate, toluene diisocyanate, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate to prepare a prepolymer emulsion, adding a copolymer of ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether, dibutyltin dilaurate, 2-methyl methacrylate and butyl acrylate to prepare a second mixture, and slowly adding the first mixture into the second mixture in a dark condition to obtain the optical adhesive for repairing cracks of the touch screen. The original appearance of the touch screen is restored after the repair, crack traces can not be seen visually, the light transmittance is over 99.5 percent, the viscosity is high, and the curing shrinkage rate is low.
When the prepolymer emulsion is prepared, the hollow silicon dioxide nanospheres are added into cyclohexane, have a hollow structure, have aggregation and loading effects, are beneficial to aggregation of all raw materials to the surfaces of the hollow silicon dioxide nanospheres, are fully expanded and fully react to form a prepolymer, part of the prepolymer is loaded in the hollow structure, and active groups extend out of the hollow structure, so that the subsequent further rapid reaction is facilitated.
The raw materials of the monomer and the prepolymer are continuously screened by the applicant, and have synergistic effect, so that the repair performance of the product is improved. When the second mixture is prepared, the copolymer of the 2-methyl methacrylate and the butyl acrylate is added after the heating reaction is carried out for a period of time, which is more beneficial to the full mixing reaction with other raw materials and the improvement of the repair performance of the product. When in use, no special bubble removing step is needed, the feasibility is strong, and the professional requirement is not high.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5: 7, mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 40 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 10 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 10 minutes, then adding the mixture into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 800r/min for 25 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 55 ℃, reacting for 2 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 70 ℃, and reacting for 3 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is diphenylethanone.
In the step (2), the emulsifier is sodium dodecyl sulfate.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 10: 8: 10: 20: 10: 12: 3: 4.
in the step (3), the slow addition in sequence means that the feeding is completed within 20 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, carrying out ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 180 ℃, reacting for 12 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 180 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: under the environment of 30 ℃, 100mL of absolute ethyl alcohol, 3mL of secondary distilled water and 5mL of ammonia water solution with the mass concentration of 25% are put into a three-neck flask, placed into a magnetic stirrer (1200 rpm) and stirred for 10 minutes, then 4mL of tetraethyl orthosilicate is added dropwise (the dropwise addition is finished in 30 minutes), and after stirring is continued for 4 hours, the mixture is stirred for 4 hours, and then the mixture is stirred by using a stirring device with the volume ratio of 1: centrifuging the mixed solution of anhydrous ethanol and secondary distilled water of 1 for 3 times (10000 r/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 170 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 3: 0.002: 25: 2.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 1.5 mixture of polydimethylsiloxane and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 2 and an alkyl modified organosiloxane.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.3: 0.001: 0.001. the slow addition was completed in 20 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Example 2
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 6: 8, mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 50 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 15 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 12 minutes, then adding the silicon dioxide hollow nanospheres into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 1000r/min for 30 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 65 ℃, reacting for 3 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 80 ℃, and reacting for 4 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is alpha, alpha-diethoxyacetophenone.
In the step (2), the emulsifier is polyethylene glycol nonyl benzyl ether.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 15: 10: 12: 30: 12: 15: 5: 7.
in the step (3), the sequential slow addition means that the feeding is completed within 30 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, performing ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 200 ℃, reacting for 24 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 200 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: placing 100mL of absolute ethyl alcohol, 3mL of secondary distilled water and 5mL of ammonia water solution with the mass concentration of 28% into a three-neck flask, placing the three-neck flask into a magnetic stirrer (1200 rpm) and stirring for 10 minutes, then dropwise adding 4mL of tetraethyl orthosilicate (dropwise adding up in 30 minutes), then continuously stirring for 5 hours, and then using a volume ratio of 1: 1 the mixed solution of absolute ethyl alcohol and secondary distilled water is centrifuged for 4 times (10000)Rotating/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 220 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 4: 0.005: 30: 3.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 2.5 mixture of polydimethylsiloxane and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 3 and an alkyl modified organosiloxane.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.4: 0.002: 0.002. the slow addition was completed in 30 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Example 3
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5: 8, mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 40 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 15 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 10 minutes, then adding the silicon dioxide hollow nanospheres into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 1000r/min for 25 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 65 ℃, reacting for 2 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 80 ℃, and reacting for 3 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is alpha-amine alkyl benzophenone.
In the step (2), the emulsifier is sodium dodecyl sulfate.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 15: 8: 12: 20: 12: 12: 5: 4.
in the step (3), the sequential slow addition means that the feeding is completed within 30 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, carrying out ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 180 ℃, reacting for 24 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 180 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: at the temperature of 30 ℃, 100mL of absolute ethyl alcohol, 3mL of redistilled water and 5mL of ammonia water solution with the mass concentration of 28 percent are put into a three-neck flask, placed into a magnetic stirrer (1200 revolutions per minute) and stirred for 10 minutes, and then 4mL of normal pressure is added dropwiseTetraethyl silicate (dripping off within 30 minutes), after which stirring was continued for 4 hours using a volume ratio of 1: centrifuging the mixed solution of anhydrous ethanol and secondary distilled water of 1 for 4 times (10000 r/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 170 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 4: 0.002: 30: 2.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 2.5 mixture of polydimethylsiloxane and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 2 and an alkyl modified organosiloxane.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.4: 0.001: 0.002. the slow addition was completed in 20 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Example 4
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 6: 7, mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 50 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 10 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 12 minutes, then adding the silicon dioxide hollow nanospheres into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 800r/min for 30 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 55 ℃, reacting for 3 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 70 ℃, and reacting for 4 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is diaryl iodonium salt.
In the step (2), the emulsifier is polyethylene glycol nonyl benzyl ether.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 10: 10: 10: 30: 10: 15: 3: 7.
in the step (3), the slow addition in sequence means that the feeding is completed within 20 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, performing ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 200 ℃, reacting for 12 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 200 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: at the temperature of 30 ℃, 100mL of anhydrousPutting ethanol, 3mL of redistilled water and 5mL of ammonia water solution with the mass concentration of 25% into a three-neck flask, placing the three-neck flask into a magnetic stirrer (1200 rpm) to stir for 10 minutes, then dropwise adding 4mL of tetraethyl orthosilicate (the solution is completely dripped in 30 minutes), and after stirring for 5 hours continuously, using a solution with the volume ratio of 1: centrifuging the mixed solution of anhydrous ethanol and secondary distilled water of 1 for 3 times (10000 r/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 220 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 3: 0.005: 25: 3.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 1.5 mixture of polydimethylsiloxane and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 3 and an alkyl modified organosiloxane.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.3: 0.002: 0.001. the slow addition was completed in 30 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Example 5
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5.5: 7.5 mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 45 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 12 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 11 minutes, then adding the silicon dioxide hollow nanospheres into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 900r/min for 28 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 60 ℃, reacting for 2 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 75 ℃, and reacting for 3 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is cumen ferrocenyl hexafluorophosphate.
In the step (2), the emulsifier is sodium dodecyl sulfate.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 12: 9: 11: 25: 11: 13: 4: 6.
in the step (3), the slow addition in sequence means that the feeding is completed within 25 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, performing ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 190 ℃, reacting for 18 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 190 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: placing 100mL of absolute ethyl alcohol, 3mL of secondary distilled water and 5mL of ammonia water solution with the mass concentration of 27% into a three-neck flask, placing the three-neck flask into a magnetic stirrer (1200 rpm), stirring for 10 minutes, then dropwise adding 4mL of tetraethyl orthosilicate (dropwise adding within 30 minutes), stirring for 4 hours continuously, and then using a volume ratio of 1: centrifuging the mixed solution of anhydrous ethanol and secondary distilled water of 1 for 3 times (10000 r/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 200 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 3.5: 0.004: 28: 3.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 2 and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 2.5 mixtures of polysiloxanes and alkyl-modified organosiloxanes.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.35: 0.001: 0.002. the slow addition was completed in 25 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Comparative example 1
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 13 mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 45 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 12 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 11 minutes, then adding the silicon dioxide hollow nanospheres into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 900r/min for 28 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 60 ℃, reacting for 2 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 75 ℃, and reacting for 3 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is cumen ferrocenyl hexafluorophosphate.
In the step (2), the emulsifier is sodium dodecyl sulfate.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 12: 9: 11: 25: 11: 13: 4: 6.
in the step (3), the slow addition in sequence means that the feeding is completed within 25 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, performing ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 190 ℃, reacting for 18 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 190 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: placing 100mL of absolute ethyl alcohol, 3mL of secondary distilled water and 5mL of ammonia water solution with the mass concentration of 27% into a three-neck flask, placing the three-neck flask into a magnetic stirrer (1200 rpm), stirring for 10 minutes, then dropwise adding 4mL of tetraethyl orthosilicate (dropwise adding within 30 minutes), stirring for 4 hours continuously, and then using a volume ratio of 1: centrifuging the mixed solution of anhydrous ethanol and secondary distilled water of 1 for 3 times (10000 r/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 200 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 3.5: 0.004: 28: 3.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 2 and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 2.5 mixtures of polysiloxanes and alkyl-modified organosiloxanes.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.35: 0.001: 0.002. the slow addition was completed in 25 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Comparative example 2
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5.5: 7.5 mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 45 times, and uniformly mixing to obtain a mixed solution;
(3) adding acrylate and toluene diisocyanate into cyclohexane, carrying out ultrasonic oscillation for 11 minutes, then adding the mixture into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 900r/min for 28 minutes to obtain emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 60 ℃, reacting for 2 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 75 ℃, and reacting for 3 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is cumen ferrocenyl hexafluorophosphate.
In the step (2), the emulsifier is sodium dodecyl sulfate.
In the step (3), the mass ratio of cyclohexane, acrylic ester, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 12: 9: 11: 25: 11: 13: 4: 6.
in the step (3), the slow addition in sequence means that the feeding is completed within 25 minutes.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 3.5: 0.004: 28: 3.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 2 and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 2.5 mixtures of polysiloxanes and alkyl-modified organosiloxanes.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.35: 0.001: 0.002. the slow addition was completed in 25 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Comparative example 3
A preparation process of optical cement for repairing cracks of a touch screen comprises the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5.5: 7.5 mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water with the weight of 45 times, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 12 minutes, adding acrylic ester and toluene diisocyanate, carrying out ultrasonic oscillation for 11 minutes, then adding the mixture into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate and tetrahydrofuran acrylate, and stirring at the rotating speed of 900r/min for 28 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 60 ℃, reacting for 2 hours, then adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 75 ℃, and reacting for 3 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
Wherein, in the step (1), the ultraviolet initiator is cumen ferrocenyl hexafluorophosphate.
In the step (2), the emulsifier is sodium dodecyl sulfate.
In the step (3), the mass ratio of the silicon dioxide hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate and tetrahydrofuran acrylate is 1: 12: 9: 11: 25: 11: 13: 10.
in the step (3), the slow addition in sequence means that the feeding is completed within 25 minutes.
In the step (3), the hollow silica nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, performing ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 190 ℃, reacting for 18 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 190 mg: 18mL of: 50 mg. The specific method of centrifugation is as follows: the liquid fraction was removed by centrifugation and the volume ratio was again used as 1: 1, centrifuging the mixed solution of the absolute ethyl alcohol and the secondary distilled water for 3 times, centrifuging the secondary distilled water for 3 times, wherein the centrifugation speed is 7000 r/min, and the centrifugation time is 5 minutes each time.
The silica nano solid sphere is prepared by
The method comprises the following steps: placing 100mL of absolute ethyl alcohol, 3mL of secondary distilled water and 5mL of ammonia water solution with the mass concentration of 27% into a three-neck flask, placing the three-neck flask into a magnetic stirrer (1200 rpm), stirring for 10 minutes, then dropwise adding 4mL of tetraethyl orthosilicate (dropwise adding within 30 minutes), stirring for 4 hours continuously, and then using a volume ratio of 1: centrifuging the mixed solution of anhydrous ethanol and secondary distilled water of 1 for 3 times (10000 r/min, 5 min/time). The particle size of the silicon dioxide nanometer solid sphere is 200 nm.
In the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion and the copolymer of the 2-methyl methacrylate and the butyl acrylate is 1: 3.5: 0.004: 28: 3.
in the step (4), the defoaming agent is prepared by mixing the following components in a mass ratio of 1: 2 and polyoxypropylene polyoxyethylene glyceryl ether. The mass ratio of the leveling agent is 1: 2.5 mixtures of polysiloxanes and alkyl-modified organosiloxanes.
In the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.35: 0.001: 0.002. the slow addition was completed in 25 minutes.
The optical adhesive for repairing the cracks of the touch screen is obtained by the preparation process.
Test examples
The optical adhesives of the embodiments 1-5 and the comparative examples 1-3 are respectively used for repairing the mobile phone touch screen with the equivalent crack condition, and the specific method comprises the following steps: cleaning cracks of the touch screen, extruding optical cement into the cracks, erasing redundant optical cement overflowing the cracks, and irradiating for 40 seconds under ultraviolet rays with the wavelength of 320-420 nm. The specific method for cleaning the cracks of the touch screen comprises the following steps: the fine needle is used for penetrating into the crack to remove any loose particles, the electric hair drier is used for blowing repeatedly for 3 minutes, and then the clean non-woven fabric is used for wiping the periphery of the crack. The viscosity and the repair curing shrinkage rate of the optical cement and the light transmittance after repair are measured, and the results are shown in table 1.
TABLE 1 comparison of crack repair Performance for touch screens
| Viscosity (cps) | Curing shrinkage (%) | Light transmittance (%) | |
| Example 1 | 3000 | 0.3 | 99.5 |
| Example 2 | 3100 | 0.3 | 99.6 |
| Example 3 | 3200 | 0.2 | 99.7 |
| Example 4 | 3200 | 0.2 | 99.7 |
| Example 5 | 3200 | 0.2 | 99.8 |
| Comparative example 1 | 2300 | 1.1 | 94.3 |
| Comparative example 2 | 1800 | 2.2 | 91.1 |
| Comparative example 3 | 2700 | 0.8 | 97.2 |
As can be seen from Table 1, the optical adhesives of examples 1 to 5 have high adhesiveness, low curing shrinkage and high light transmittance for repairing touch screens, and have excellent repairing effects. Comparative example 1 omitting glycidyl methacrylate in step (1), comparative example 2 omitting the silica hollow nanospheres in step (3), and comparative example 3 omitting isobornyl methacrylate in step (3), the repairing effect was remarkably deteriorated.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation process of optical cement for repairing cracks of a touch screen is characterized by comprising the following specific steps:
(1) under the condition of keeping out of the sun, mixing an ultraviolet initiator, glycidyl methacrylate and ethoxylated trimethylolpropane triacrylate according to the mass ratio of 1: 5-6: 7-8, mixing and stirring to obtain a first mixture for later use;
(2) adding an emulsifier into deionized water of which the weight is 40-50 times that of the emulsifier, and uniformly mixing to obtain a mixed solution;
(3) adding the silicon dioxide hollow nanospheres into cyclohexane, carrying out ultrasonic oscillation for 10-15 minutes, adding acrylate and toluene diisocyanate, carrying out ultrasonic oscillation for 10-12 minutes, then adding the mixture into the mixed solution obtained in the step (2), then sequentially and slowly adding triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate, and stirring at the rotating speed of 800-1000 r/min for 25-30 minutes to obtain an emulsion;
(4) mixing ethylene glycol dimethacrylate, polypropylene glycol glycidyl ether and dibutyltin dilaurate, slowly adding the mixture into the emulsion obtained in the step (3), heating to 55-65 ℃, reacting for 2-3 hours, adding a copolymer of 2-methyl methacrylate and butyl acrylate, heating to 70-80 ℃, and reacting for 3-4 hours to obtain a second mixture;
(5) and (3) slowly adding the first mixture obtained in the step (1) into the second mixture in a dark condition, adding a defoaming agent and a flatting agent while stirring, and filtering to obtain the optical adhesive for repairing the cracks of the touch screen.
2. The process of claim 1, wherein in step (1), the UV initiator is selected from one or more of benzil, alkylbenzene, acylphosphorus oxide, benzophenone, diaryliodonium salt, triaryliodonium salt, alkyl iodonium salt, cumeneferrocene hexafluorophosphate.
3. The process according to claim 1, wherein in the step (2), the emulsifier is sodium dodecyl sulfate or polyethylene glycol nonyl benzyl ether.
4. The preparation process according to claim 1, wherein in the step (3), the mass ratio of the silica hollow nanospheres, cyclohexane, acrylate, toluene diisocyanate, mixed solution, triethylene glycol diacrylate, polyether acrylate, tetrahydrofuran acrylate and isobornyl methacrylate is 1: 10-15: 8-10: 10-12: 20-30: 10-12: 12-15: 3-5: 4 to 7.
5. The preparation process according to claim 1, wherein in the step (3), the sequential slow addition is completed within 20-30 minutes.
6. The preparation process according to claim 1, wherein in the step (3), the silica hollow nanospheres are prepared by the following method: weighing ferrous acetate in an oxygen-free glove box, adding secondary distilled water, adding silicon dioxide nano solid spheres after the ferrous acetate is completely dissolved, carrying out ultrasonic treatment for 10 minutes, putting the mixture into a 20mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven preheated to 180-200 ℃, reacting for 12-24 hours, and centrifuging to obtain the product; the mass-volume ratio of the ferrous acetate, the secondary distilled water and the silicon dioxide nanometer solid spheres is 180-200 mg: 18mL of: 50 mg.
7. The production process according to claim 1, wherein in the step (4), the mass ratio of the ethylene glycol dimethacrylate, the polypropylene glycol glycidyl ether, the dibutyltin dilaurate, the emulsion, and the copolymer of methyl 2-methacrylate and butyl acrylate is 1: 3-4: 0.002 to 0.005: 25-30: 2 to 3.
8. The preparation process according to claim 1, wherein in the step (5), the mass ratio of the first mixture to the second mixture to the defoaming agent to the leveling agent is 1: 0.3-0.4: 0.001 to 0.002: 0.001 to 0.002.
9. An optical adhesive for repairing cracks of a touch screen is obtained by the preparation process of any one of claims 1-8.
10. Use of the optical cement of claim 9 in touch screen crack repair.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910279862.5A CN110016295B (en) | 2019-04-09 | 2019-04-09 | Optical adhesive for repairing cracks of touch screen and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910279862.5A CN110016295B (en) | 2019-04-09 | 2019-04-09 | Optical adhesive for repairing cracks of touch screen and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110016295A CN110016295A (en) | 2019-07-16 |
| CN110016295B true CN110016295B (en) | 2021-04-16 |
Family
ID=67190789
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910279862.5A Active CN110016295B (en) | 2019-04-09 | 2019-04-09 | Optical adhesive for repairing cracks of touch screen and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110016295B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110577811B (en) * | 2019-09-29 | 2021-01-05 | 苏州鑫河镜业有限公司 | Preparation process of high-strength stable OCA (optically clear adhesive) |
| CN113075235B (en) * | 2021-03-29 | 2024-03-26 | 重庆烯宇新材料科技有限公司 | Touch screen silk-screen silver paste defect maintenance method |
| CN115627115B (en) * | 2022-11-14 | 2023-11-17 | 福耀玻璃工业集团股份有限公司 | Coating, substrate with coating and preparation method of substrate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046315B (en) * | 2014-06-11 | 2015-11-18 | 深圳职业技术学院 | UV-light dual cure conductive adhesive and preparation method thereof |
| US9850329B2 (en) * | 2015-06-29 | 2017-12-26 | Fina Technology, Inc. | Farnesene-based polymers and liquid optically clear adhesive compositions incorporating the same |
| CN105754545B (en) * | 2016-04-26 | 2019-04-09 | 深圳职业技术学院 | A kind of display ultraviolet light mixing cured adhesive and preparation method thereof |
| CN108478816A (en) * | 2018-04-24 | 2018-09-04 | 上海交通大学医学院附属瑞金医院 | The silicon dioxide hollow nanosphere of Fe2O3 doping, composite material, preparation method and application |
-
2019
- 2019-04-09 CN CN201910279862.5A patent/CN110016295B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110016295A (en) | 2019-07-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110016295B (en) | Optical adhesive for repairing cracks of touch screen and application thereof | |
| CN103031105A (en) | Ultraviolet curing liquid optical clear adhesive and preparation method thereof | |
| KR20140113938A (en) | Ultraviolet curde optic binder | |
| CN105765024A (en) | Photocurable adhesive composition, adhesive sheet and laminate | |
| CN102888161B (en) | Environment-friendly water-based high adhesion force PET precoated shet coating composition and preparation, purposes | |
| CN1255467C (en) | Protective film composition for cylindrical shock insulator of liquid crystal display element | |
| CN110713818B (en) | Ultraviolet/moisture dual fast-curing polysiloxane adhesive composition | |
| KR20130139329A (en) | Sealant composition, method for preventing liquid crystal contamination, liquid crystal panel and display device | |
| CN102816551A (en) | Ultraviolet (UV)-moisture double-curing liquid optical transparent adhesive and preparation method thereof | |
| CN114350266B (en) | Liquid optical cement and preparation method and application method thereof | |
| WO2021230371A1 (en) | Photo/moisture-curable resin composition, adhesive for electronic component, cured body and electronic component | |
| CN109943203A (en) | Photovoltaic back bi-component repair coating and preparation method thereof, application method and application | |
| JP2024026609A (en) | Curable resin composition and cured product | |
| CN103275617A (en) | Preparation method and application of organosilicon photo-diffusion particle | |
| WO2020149377A1 (en) | Curable resin composition and cured body | |
| CN108003623B (en) | Single-component silicone rubber for acrylic bonding and preparation method thereof | |
| CN109735159A (en) | Photovoltaic back bi-component repairing putty and preparation method thereof, application method and application | |
| TW202037624A (en) | Photo/moisture curable resin composition and cured body | |
| CN106589731A (en) | Method for preparing IPN structure PMMA-PU high-transparency composite board through ultrasonic assistance | |
| CN109868095A (en) | In-situ polymerization type has organic silicon-acrylate adhesive preparation method of light diffusion function and products thereof and application | |
| CN107674626B (en) | High-thixotropic transparent marble adhesive and preparation method thereof | |
| CN106634772B (en) | Organic silicon modified wood floor glue and preparation method thereof | |
| TW202208480A (en) | Photo/moisture curable resin composition and cured body | |
| TW202134309A (en) | Photo/moisture curable resin composition, adhesive for electronic components, method for producing electronic component, and cured body | |
| WO2022114186A1 (en) | Moisture-curable resin composition and adhesive for electronic appliance |
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 | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: An Optical Adhesive for Touchscreen Crack Repair and Its Application Effective date of registration: 20230818 Granted publication date: 20210416 Pledgee: South Taihu New Area sub branch of Huzhou Wuxing Rural Commercial Bank Co.,Ltd. Pledgor: ZHEJIANG GUONENG TECHNOLOGY Co.,Ltd. Registration number: Y2023980052842 |