CN110003841B - Application method of ultraviolet light curing adhesive and electronic product - Google Patents
Application method of ultraviolet light curing adhesive and electronic product Download PDFInfo
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- CN110003841B CN110003841B CN201910304506.4A CN201910304506A CN110003841B CN 110003841 B CN110003841 B CN 110003841B CN 201910304506 A CN201910304506 A CN 201910304506A CN 110003841 B CN110003841 B CN 110003841B
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- 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
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- C08G18/40—High-molecular-weight compounds
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- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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- 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
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- C08G18/4825—Polyethers containing two hydroxy groups
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- 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
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
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- 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
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- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
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- 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
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- 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
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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
- 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
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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Abstract
An application method of an ultraviolet light curing adhesive and an electronic product are provided, wherein the ultraviolet light curing adhesive comprises the following raw materials: 30-50% of polyfunctional polyurethane acrylate prepolymer; 40-60% of an active diluent; 2-7% of a photoinitiator; 0-3% of a silane coupling agent; 0-3% of fumed silica; 1-8% of temperature change powder; 0.001-0.1% of fluorescent powder, wherein the polyfunctional group polyurethane acrylate prepolymer comprises the following raw materials of dihydric alcohol polymer: diisocyanate: the molar ratio of the hydroxyl-containing acrylate is 1: 1.4-1.7: 1.9-2.1, and the catalyst accounts for 0.1-1 per mill of the weight of the polyfunctional group polyurethane acrylate prepolymer, so that the prepolymer has the following four characteristics: 1) the glue is fragile, and the screwdriver can be simply punctured; 2) the glue curing speed is high; 3) the anti-counterfeiting effect is certain, and a third party cannot easily imitate the anti-counterfeiting effect; 4) cannot be completely removed by using a tool such as tweezers.
Description
Technical Field
The invention relates to the technical field of structural bonding, in particular to a using method of an ultraviolet curing adhesive and an electronic product.
Background
In the electronic product field, the guarantee after purchasing the product many times only needs just can realize through breakable sticker on the mainboard, and most merchants see just can provide the guarantee after the breakable sticker of matter guarantor, but the breakable sticker of present electronic product generally is the breakable subsides of paper, has two technical problems: 1) the existing paper fragile sticker is easily obtained from other parties, can be used in a private fit mode, and is easily used as a means for deceiving free warranty by some consumers; 2) in the production process, most workers use manual lamination or clamp the lamination by using tweezers, and after the structural design of the mobile phone is thinner and thinner, the manual lamination is very easy to damage, and the production efficiency is low.
In view of the above, the inventor intends to develop a novel fragile anti-counterfeiting glue to replace the fragile sticker. As is well known, the ultraviolet curing adhesive has some remarkable characteristics of good compatibility, high curing speed, high strength, environmental protection and the like, so that the ultraviolet curing adhesive is widely applied to the fields of optics, electronic and electric appliances, digital optical disks and the like, and the production automation degree is high, so that the ultraviolet curing adhesive becomes a first choice for solving the second problem; but it also has certain limitation, and at present, the adhesive force of current ultraviolet curing gluing agent at home and abroad is strong and is not fragile, does not possess anti-fake ability simultaneously, and its performance that is applicable to the breakable anti-fake glue who replaces breakable sticker should possess following four requirements: 1) the glue is fragile, and the screwdriver can be simply punctured; 2) the glue curing speed is high; 3) the anti-counterfeiting effect is certain, and a third party cannot easily imitate the anti-counterfeiting effect; 4) cannot be completely removed by a tool such as tweezers, so as to prevent the adhesive from being adhered back after being removed by a user (consumer). In order to meet the performance requirements, new ultraviolet curing glue is further developed by the people.
Disclosure of Invention
The invention aims to provide the ultraviolet curing adhesive which is fragile, high in curing speed, anti-counterfeiting and incapable of being completely taken down.
The second purpose of the invention is to provide a preparation method of the ultraviolet curing adhesive.
The third purpose of the invention is to provide a using method of the ultraviolet light curing adhesive.
The fourth objective of the present invention is to provide an electronic product, wherein the electronic product uses the above ultraviolet light curing adhesive to cover the quality assurance screw, so that the setting of the warranty is very simple, and the anti-counterfeit effect is greatly improved.
In order to achieve the above purpose, the solution of the invention is: an ultraviolet light curing adhesive is prepared from the following raw materials in percentage by weight:
30-50% of polyfunctional polyurethane acrylate prepolymer;
40-60% of an active diluent;
2-7% of a photoinitiator;
0-3% of a silane coupling agent;
0-3% of fumed silica;
1-8% of temperature change powder;
0.001 to 0.1 percent of fluorescent powder.
Further, the raw materials of the multifunctional polyurethane acrylate prepolymer comprise a dihydric alcohol polymer, diisocyanate, a catalyst and hydroxyl-containing acrylate, wherein the weight ratio of the dihydric alcohol polymer: diisocyanate: the molar ratio of the hydroxyl-containing acrylate is 1: 1.4-1.7: 1.9-2.1, and the catalyst accounts for 0.1-1 per mill of the weight of the polyfunctional group polyurethane acrylate prepolymer.
Further, the molecular weight of the glycol polymer is 1000-6000.
Further, the diol polymer is one or more of polyethylene glycol (PEG), poly-1, 4-butylene glycol adipate (PBA), poly-ethylene glycol adipate glycol (PEA), polypropylene oxide glycol (PPG), polytetrahydrofuran ether glycol (PTMG), poly-1, 4-butylene glycol adipate (PBA), and poly-1, 6-hexanediol adipate (PHA).
Further, the diisocyanate is one or more of hexamethylene diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, xylylene diisocyanate and dicyclohexylmethane diisocyanate.
Further, the hydroxyl-containing acrylate is one or more of hydroxypropyl methacrylate (HPMA), hydroxyethyl acrylate (HEA), hydroxypropyl acrylate (HPA), trimethylolpropane diacrylate (TMPDA), hydroxyethyl methacrylate (HEMA), pentaerythritol triacrylate (PETA).
Further, the catalyst is organic bismuth.
Further, 1-8 wt% of optically variable powder is added into the raw materials.
Further, 1-8 wt% of fragrant powder is added into the raw materials.
Further, 0.1-5 wt% of pearl powder is added into the raw materials.
Further, the reactive diluent is one or a mixture of more of ethylene glycol dimethacrylate, cyclohexane dimethanol diacrylate, pentaerythritol triacrylate, isobornyl acrylate, dicyclopentadiene methacrylate and N, N-dimethylacrylamide.
Further, the photoinitiator is one or a mixture of more of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl benzophenone, bis (2, 4, 6-trimethylbenzoyl) phenyl phosphorus oxide, alpha' -dimethylbenzyl ketal, benzophenone, isopropyl thioxanthone, methyl o-benzoylbenzoate and 2,4, 6-trimethylbenzoyl diphenyl phosphorus oxide.
The preparation method of the ultraviolet curing adhesive comprises the following steps:
weighing raw materials, by weight, 40-60% of an active diluent, 2-7% of a photoinitiator, 0-3% of a silane coupling agent, 0-3% of fumed silica, 1-8% of a temperature-change powder and 0.001-0.1% of a fluorescent powder, adding the raw materials into a stirrer, controlling the temperature at 25-35 ℃, vacuumizing until the vacuum degree is-0.08-0.05 MPa, and stirring for 0.5-1 hour at 200-500 r/min until no particles exist; and adding 30-50% of polyfunctional group polyurethane acrylate prepolymer into a stirrer, controlling the temperature at 25-35 ℃, vacuumizing to the vacuum degree of-0.08-0.05 MPa, stirring for 0.5-1 hour at 200-500 r/min, uniformly stirring, and sealing and packaging in a dark place.
Further, the preparation process of the multifunctional group polyurethane acrylate prepolymer comprises the following steps: vacuumizing and dehydrating the dihydric alcohol polymer for 2-3 hours at the temperature of 110-120 ℃; then adding diisocyanate, and fully stirring for 0.5-1 hour in vacuum at the temperature of 50-70 ℃; then adding a catalyst, controlling the temperature at 70-80 ℃ and carrying out vacuum reaction for 2-4 hours; then adding hydroxyl-containing acrylate, fully stirring in vacuum at the temperature of 60-80 ℃, continuously reacting for 2-3 hours, sampling every 30min to determine the NCO value, and discharging for later use when the measured value is zero; wherein the ratio of glycol polymer: diisocyanate: the molar ratio of the hydroxyl-containing acrylate is 1: 1.4-1.7: 1.9-2.1, and the catalyst accounts for 0.1-1 per mill of the weight of the polyfunctional group polyurethane acrylate prepolymer.
The use method of the ultraviolet light curing adhesive is characterized by comprising the following steps: covering a layer of ultraviolet curing glue on a quality-guaranteed screw screwed in an electronic product, and then irradiating under a 365nm ultraviolet lamp for 300 mj-500 mj, and curing within 3 seconds.
Furthermore, the thickness of the covered layer of ultraviolet curing glue is 0.3-0.5 mm.
An electronic product, wherein at least one layer of any one layer of the ultraviolet light curing adhesive after curing is covered on a quality-guaranteed screw screwed tightly.
Furthermore, the thickness of the ultraviolet curing adhesive is 0.3-0.5 mm.
After the scheme is adopted, the ultraviolet curing glue can be completely cured under the energy of 300mJ, when the ultraviolet curing glue is used for protecting the quality-guaranteed screw of an electronic product, the ultraviolet curing glue has the effects of frangibility and anti-counterfeiting, and the ultraviolet curing glue has strong bonding force with metal and is not easy to take down in a whole block; compared with other polyurethane acrylate prepolymers, the proportion of hydroxyl groups to isocyanate groups is closer to 1:1 in the formula design of the patent of our formulation, the synthesized molecular weight is larger, more active groups are arranged on a molecular chain, and the bonding strength is higher. On the other hand, the synthesized polyfunctional group urethane acrylate prepolymer has high functionality, and the prepared glue is high in crosslinking density after being cured and is fragile due to small elongation at break; meanwhile, the multifunctional polyurethane acrylate contains more carbamate groups with lone pair electrons, and can form more hydrogen bonds with hydroxyl on the surface of a metal substrate, so that the bonding strength with metal (quality assurance screws) is high, and therefore, if the cured ultraviolet curing adhesive is tried to be picked off, the ultraviolet curing adhesive is easy to break and break, integrity is not maintained any more, and the adhesive is difficult to be attached back naturally; meanwhile, the anti-counterfeiting material is added in the production of the ultraviolet light curing adhesive, so that the ultraviolet light curing adhesive has an anti-counterfeiting effect, and a user (consumer) cannot easily find a substitute product to disguise the product into an undetached model; therefore, the problems that the fragile paster in the prior art is extremely easy to obtain and the fragile paster is easy to separate and replace are solved. The ultraviolet curing adhesive has the characteristics of anti-counterfeiting, frangibility, low curing energy, difficult simulation, high strength, poor toughness and incapability of taking off the whole piece, is particularly suitable for replacing the traditional frangibility sticker for large-scale production and use, and has remarkable significance in industrial innovation of the industry.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1:
firstly, preparing a polyfunctional group urethane acrylate prepolymer: adding 200 g (0.2mol) of poly adipic acid-1, 6-hexanediol ester (Mn is 1000) into a reactor, vacuumizing and dehydrating at the temperature of 110 ℃ for 2 hours, cooling to 65 ℃, adding 73.5 g (0.28mol) of dicyclohexylmethane diisocyanate, stirring in vacuum for 0.5 hour, then adding 0.2 g of organic bismuth, reacting at the temperature of 75 ℃ for 2.5 hours, adding 54.8g (0.38mol) of hydroxypropyl methacrylate, continuing stirring in vacuum at the temperature of 75 ℃ for 2 hours, sampling every 30min to determine the NCO value, and discharging for later use when the determined value is zero;
secondly, preparing ultraviolet curing glue: accurately weighing 14g of cyclohexane dimethanol diacrylate ester as each raw material according to the weight percentage; 46g of dicyclopentadiene methacrylate; 3g of photoinitiator benzophenone; 2g of photoinitiator alpha, alpha' -dimethyl benzil ketal; 1g of fumed silica, 4g of temperature change powder and 0.01g of fluorescent powder; adding the weighed raw materials into a double-planetary power mixing stirrer, controlling the temperature at 25 ℃, vacuumizing until the vacuum degree is-0.08 MPa, and stirring at 500 revolutions per minute for 1 hour until no particles exist; and adding 30g of the multifunctional group polyurethane acrylate prepolymer, controlling the temperature at 25 ℃, vacuumizing to the vacuum degree of-0.08 MPa, stirring for 1 hour at 500 r/min, uniformly stirring to obtain the ultraviolet curing adhesive, and sealing and packaging in a dark place to obtain a sample I.
Example 2:
firstly, preparing a polyfunctional group urethane acrylate prepolymer: adding 300 g (0.1mol) of poly adipic acid-1, 6-hexanediol ester (Mn is 3000) into a reactor, vacuumizing and dehydrating at the temperature of 120 ℃ for 3 hours, cooling to 70 ℃, adding 26.1 g of toluene diisocyanate (0.15mol), stirring in vacuum for 1 hour, then adding 0.036 g of organic bismuth, reacting at the temperature of 80 ℃ for 4 hours, then adding 28.8g (0.2mol) of hydroxypropyl methacrylate, continuing to stir in vacuum at the temperature of 80 ℃ for 3 hours, sampling every 30min to determine the NCO value, and discharging for later use until the measured value is zero;
secondly, preparing ultraviolet curing glue: accurately weighing 14g of pentaerythritol triacrylate; 36g of N, N-dimethylacrylamide; 3g of photoinitiator benzophenone; 2g of photoinitiator alpha, alpha' -dimethylbenzylketal; 2g of fumed silica, 5g of temperature change powder and 0.1g of fluorescent powder; adding the weighed raw materials into a double-planetary power mixing stirrer, controlling the temperature at 35 ℃, vacuumizing until the vacuum degree is-0.05 MPa, and stirring at 400 revolutions per minute for 1 hour until no particles exist; and adding 40g of the multifunctional group polyurethane acrylate prepolymer, controlling the temperature at 35 ℃, vacuumizing to the vacuum degree of-0.05 MPa, stirring for 1 hour at 500 revolutions per minute, uniformly stirring to obtain the ultraviolet curing adhesive, and sealing and packaging to obtain a second sample.
Example 3:
firstly, preparing a polyfunctional group urethane acrylate prepolymer: adding 300 g (0.05mol) of poly adipic acid-1, 6-hexanediol ester (Mn is 6000) into a reactor, vacuumizing and dehydrating for 2 hours at the temperature of 110 ℃, cooling to 50 ℃, adding 22.3 g (0.085mol) of dicyclohexylmethane diisocyanate, stirring for 0.5 hour in vacuum, then adding 0.2 g of organic bismuth, reacting for 2 hours at the temperature of 70 ℃, adding 15.1g (0.105mol) of hydroxypropyl acrylate, continuing to stir for reaction for 2 hours at the temperature of 60 ℃, sampling every 30min to determine the NCO value, and discharging for later use when the determined value is zero;
secondly, preparing ultraviolet curing glue: accurately weighing 18g of ethylene glycol dimethacrylate as each raw material according to the weight percentage; 22g of N, N-dimethylacrylamide; 3g of photoinitiator benzophenone; 2g of photoinitiator alpha, alpha' -dimethylbenzylketal; silane coupling agent KH 5601 g, gas-phase silicon dioxide 3g, temperature-change powder 8g and fluorescent powder 0.01 g; adding the weighed raw materials into a double-planetary power mixing stirrer, controlling the temperature at 25 ℃, vacuumizing until the vacuum degree is-0.06 MPa, and stirring for 1 hour at 200 revolutions per minute until no particles exist; and adding 50g of the multifunctional group polyurethane acrylate prepolymer, controlling the temperature at 25 ℃, vacuumizing to the vacuum degree of-0.05 MPa, stirring for 1 hour at 200 r/min, uniformly stirring to obtain the ultraviolet curing adhesive, and sealing and packaging in a dark place to obtain a third sample.
Example 4:
firstly, preparing a polyfunctional group urethane acrylate prepolymer: adding 200 g (0.2mol) of polyoxypropylene diol (Mn is 1000) into a reactor, vacuumizing and dehydrating at the temperature of 110 ℃ for 2 hours, cooling to 70 ℃, adding 47.1 g (0.28mol) of hexamethylene diisocyanate, stirring in vacuum for 0.5 hour, then adding 3.01 g of organic bismuth, reacting at the temperature of 75 ℃ for 2.5 hours, adding 113.3g (0.38mol) of pentaerythritol triacrylate, continuing to stir in vacuum at the temperature of 75 ℃ for 2 hours, sampling every 30min to determine the NCO value, and discharging for later use until the determined value is zero;
secondly, preparing ultraviolet curing glue: accurately weighing 22g of pentaerythritol triacrylate; 38g of isobornyl acrylate; 3g of photoinitiator benzophenone; 2g of photoinitiator alpha, alpha' -dimethylbenzylketal; 1g of fumed silica, 1g of temperature-change powder, 0.01g of fluorescent powder, 8g of optically variable powder and 3g of pearl powder; adding the weighed raw materials into a double-planetary power mixing stirrer, controlling the temperature at 25 ℃, vacuumizing until the vacuum degree is-0.07 MPa, and stirring at 500 revolutions per minute for 1 hour until no particles exist; and adding 30g of the multifunctional group polyurethane acrylate prepolymer, controlling the temperature at 25 ℃, vacuumizing to the vacuum degree of-0.07 MPa, stirring for 1 hour at 500 r/min, uniformly stirring to obtain the ultraviolet curing adhesive, and sealing and packaging in a dark place to obtain a sample IV.
Example 5:
firstly, preparing a polyfunctional group urethane acrylate prepolymer: adding 300 g (0.1mol) of polyoxypropylene diol (Mn is 3000) into a reactor, vacuumizing and dehydrating at the temperature of 110 ℃ for 2 hours, cooling to 65 ℃, adding 39.4 g (0.15mol) of dicyclohexylmethane diisocyanate, stirring in vacuum for 0.5 hour, then adding 0.2 g of organic bismuth, reacting at the temperature of 75 ℃ for 2.5 hours, adding 59.7g (0.2mol) of pentaerythritol triacrylate, continuing to stir in vacuum at the temperature of 75 ℃ for 2 hours, sampling every 30min to determine the NCO value, and discharging for later use when the determined value is zero;
secondly, preparing ultraviolet curing glue: accurately weighing 26g of isobornyl acrylate serving as each raw material according to the weight percentage; 24g of N, N-dimethylacrylamide; 3g of photoinitiator benzophenone; 2g of photoinitiator alpha, alpha' -dimethylbenzylketal; 1g of fumed silica, 4g of temperature-change powder, 0.01g of fluorescent powder and 8g of incense powder; adding the weighed raw materials into a double-planetary power mixing stirrer, controlling the temperature at 25 ℃, vacuumizing until the vacuum degree is-0.08 MPa, and stirring at 500 revolutions per minute for 1 hour until no particles exist; and adding 40g of the multifunctional group polyurethane acrylate prepolymer, controlling the temperature at 25 ℃, vacuumizing until the vacuum degree is-0.07 MPa, stirring for 1 hour at 500 revolutions per minute, uniformly stirring to obtain the ultraviolet curing adhesive, and sealing and packaging in a dark place to obtain a fifth sample.
Example 6:
firstly, preparing a polyfunctional group urethane acrylate prepolymer: adding 300 g (0.05mol) of polytetrahydrofuran ether glycol (PTMG) (Mn ═ 6000) into a reactor, vacuumizing and dehydrating at the temperature of 110 ℃ for 3 hours, cooling to 50 ℃, adding 22.3(0.085mol) of dicyclohexylmethane diisocyanate, stirring in vacuum for 0.5 hour, then adding 0.2 g of organic bismuth, reacting at the temperature of 80 ℃ for 2 hours, adding 31.3g (0.105mol) of pentaerythritol triacrylate, continuing stirring in vacuum at the temperature of 80 ℃ for reacting for 2 hours, sampling every 30min to determine the NCO value, and discharging for later use until the determined value is zero;
secondly, preparing ultraviolet curing glue: accurately weighing 30g of dicyclopentadiene methacrylate; 10g of cyclohexanedimethanol diacrylate; 3g of photoinitiator benzophenone; 2g of photoinitiator alpha, alpha' -dimethylbenzylketal; 1g of fumed silica, 4g of temperature change powder and 0.01g of fluorescent powder; adding the weighed raw materials into a double-planetary power mixing stirrer, controlling the temperature at 25 ℃, vacuumizing until the vacuum degree is-0.08 MPa, and stirring at 500 revolutions per minute for 1 hour until no particles exist; and adding 50g of the multifunctional group polyurethane acrylate prepolymer, controlling the temperature at 25 ℃, vacuumizing to the vacuum degree of-0.08 MPa, stirring for 1 hour at 500 revolutions per minute, uniformly stirring to obtain the ultraviolet curing adhesive, and sealing and packaging in a dark place to obtain a sample six.
The silane coupling agent can be one or a mixture of any two of KH551, KH560 and KH 570.
The fumed silica is one or more of R972 of winning company, MA100 of Mitsubishi company and N20 of Wacker company.
The performance test is carried out on the samples obtained by the six embodiments, and related tests are carried out through a viscometer, a universal tester, a shore durometer, a screw hole simulation experiment and an anti-counterfeiting experiment test, and the method specifically comprises the following steps:
and (3) viscosity testing: testing at 25 ℃ by adopting a Bohler fly plate viscometer with a 52# rotor at 10rpm, and recording viscosity data obtained by the test;
and (3) testing the shear strength: during testing, the first sample is coated on a stainless steel sheet and pressed by the stainless steel sheet. Controlling the thickness of a 0.13mm copper wire, controlling the area to be 12.7 x 25.4mm, and curing by using an LED ultraviolet lamp; after cooling, the two sheets are pulled apart in opposite directions by using a universal testing machine, and the measured force value is recorded by strength (MPa); samples two through six were tested in the same manner and recorded.
And (3) hardness testing: and (3) curing a sample I with the thickness of 5mm by using an LED ultraviolet lamp, testing by using a Shore hardness tester, recording the hardness data of the sample I, and testing and recording samples II to six in the same manner.
Screw hole simulation experiment test: spotting a sample I with the thickness of about 0.3mm on a screw hole with the diameter of 2.5mm, curing the sample I into a rubber block by using an LED ultraviolet lamp at 300mJ, and observing whether the rubber block can be easily punctured by using a screwdriver or not so as to screw out the screw; and (3) dotting a sample I with the thickness of about 0.3mm on a screw hole with the diameter of 2.5mm, curing the sample I into a rubber block by using an LED ultraviolet lamp at 300mJ, prying the cured rubber block from the edge carefully and wingedly by using tweezers, and observing whether the whole block can be taken down. Samples two through six were tested in the same manner and observed.
Anti-counterfeiting experimental test: dropping a sample I with the thickness of about 0.5mm on a screw hole with the diameter of 2.5mm, curing the sample I into a rubber block by using an LED ultraviolet lamp at 300mJ, blowing the cured rubber block for five seconds by using a 100-DEG hot air gun, and observing whether the color of the rubber block changes; and meanwhile, the cured glue is placed under a 365nm ultraviolet lamp to observe whether the glue block is blue or not. Samples two through six were tested in the same manner and observed.
The test results are shown in table one:
watch 1
The viscosity and the shear strength of the adhesive are within a reasonable range, and according to the test data in the table I, the viscosity of the samples I to VI is between 2000-9000cps, the shear strength is more than 2.5Mpa, and the bonding and shear strength within the proper range are determined, so that the cured adhesive is not easy to fall off, and the cured adhesive is not too viscous to be beneficial to fully paving the screw before short curing time;
in the test data, the hardness of the samples I to six is less than 95A, so that the samples can be punctured by a screwdriver with lower hardness;
as can be seen from the screw hole simulation experiment, the screw driver can easily puncture the rubber blocks of the first sample to the sixth sample, so that the screw is screwed out; prying the cured rubber blocks of the first sample to the sixth sample by using tweezers from the edge carefully and wingedly, and not tilting the whole rubber block for taking down;
the anti-counterfeiting effect is further observed, the glue blocks of the samples I to VI are heated by the hot air gun to become red after being cured, and the glue blocks become blue under an ultraviolet lamp, so that the double anti-counterfeiting effect is realized, and the authenticity of the glue blocks can be identified by after-sales service personnel.
The ultraviolet curing adhesive has the advantages of proper viscosity, high strength after curing, frangibility, incapability of being pried down in a whole block, dual anti-counterfeiting function, capability of meeting the requirements of customers and capability of replacing frangibility stickers.
The temperature change powder added in practical application can be one or a mixture of more of colorless color change or colorless color change.
The optically variable powder can be one or a mixture of several optically variable powders which change color under sunlight or ultraviolet lamps.
The fragrance-feeling powder can comprise one or a mixture of more of fruit fragrance-feeling powder or flower fragrance-feeling powder.
The fluorescent powder is one or a mixture of several kinds of fluorescent powder which develops color under each ultraviolet lamp.
The pearl powder is one or a mixture of several kinds of pearl powders which show different colors under different angles.
The patent can realize multiple anti-counterfeiting means by using one or a mixture of a plurality of temperature-changing powder, light-changing powder, fluorescent powder, aroma-sensing powder and pearl powder.
The above description is only an embodiment of the present invention, and is not intended to limit the design of the present invention, and all equivalent changes made according to the design key of the present invention fall within the protection scope of the present invention.
Claims (17)
1. A method for using ultraviolet light curing glue is characterized in that: covering a layer of ultraviolet curing glue on a quality-guaranteed screw screwed in an electronic product, and then irradiating under a 365nm ultraviolet lamp for 300 mj-500 mj, and curing within 3 seconds; the ultraviolet light curing adhesive is prepared from the following raw materials in percentage by weight: 30-50% of polyfunctional polyurethane acrylate prepolymer; 40-60% of an active diluent; 2-7% of a photoinitiator; 0-3% of a silane coupling agent; 0-3% of fumed silica; 1-8% of temperature change powder; 0.001 to 0.1 percent of fluorescent powder.
2. The method for using the UV curable adhesive according to claim 1, wherein: the raw materials of the multifunctional group polyurethane acrylate prepolymer comprise a dihydric alcohol polymer, diisocyanate, a catalyst and hydroxyl-containing acrylate, wherein the weight ratio of the dihydric alcohol polymer: diisocyanate: the molar ratio of the hydroxyl-containing acrylate is 1: 1.4-1.7: 1.9-2.1, and the catalyst accounts for 0.1-1 per mill of the weight of the polyfunctional group polyurethane acrylate prepolymer.
3. The method of claim 2, wherein the method comprises the following steps: the molecular weight of the dihydric alcohol polymer is 1000-6000.
4. The method of claim 3, wherein the method comprises the following steps: the dihydric alcohol polymer is one or more of polyethylene glycol, poly adipic acid-1, 4-butanediol ester, poly adipic acid glycol ester glycol, polypropylene oxide glycol, polytetrahydrofuran ether glycol, poly adipic acid-1, 4-butanediol ester and poly adipic acid-1, 6-hexanediol ester.
5. The method of claim 2, wherein the method comprises the following steps: the diisocyanate is one or more of hexamethylene diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, xylylene diisocyanate and dicyclohexylmethane diisocyanate.
6. The method of claim 2, wherein the method comprises the following steps: the hydroxyl-containing acrylate is one or more of hydroxypropyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, trimethylolpropane diacrylate, hydroxyethyl methacrylate and pentaerythritol triacrylate.
7. The method of claim 2, wherein the method comprises the following steps: the catalyst is organic bismuth.
8. The method for using the UV curable adhesive according to claim 1, wherein: the raw materials are also added with 1-8 wt% of optically variable powder.
9. The method for using the UV curable adhesive according to claim 1, wherein: 1-8 wt% of fragrant powder is also added into the raw materials.
10. The method for using the UV curable adhesive according to claim 1, wherein: 0.1-5 wt% of pearl powder is also added into the raw materials.
11. The method for using the UV curable adhesive according to claim 1, wherein: the active diluent is one or a mixture of more of ethylene glycol dimethacrylate, cyclohexane dimethanol diacrylate, pentaerythritol triacrylate, isobornyl acrylate, dicyclopentadiene methacrylate and N, N-dimethylacrylamide.
12. The method for using the UV curable adhesive according to claim 1, wherein: the photoinitiator is one or a mixture of more of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl benzophenone, bis (2, 4, 6-trimethylbenzoyl) phenyl phosphorus oxide, alpha' -dimethylbenzoyl ketal, benzophenone, isopropyl thioxanthone, methyl o-benzoylbenzoate and 2,4, 6-trimethylbenzoyl diphenyl phosphorus oxide.
13. The method for using the UV-curable adhesive according to any one of claims 1 to 12, wherein the method for preparing the UV-curable adhesive comprises the following steps:
weighing raw materials, by weight, 40-60% of an active diluent, 2-7% of a photoinitiator, 0-3% of a silane coupling agent, 0-3% of fumed silica, 1-8% of a temperature-change powder and 0.001-0.1% of a fluorescent powder, adding the raw materials into a stirrer, controlling the temperature at 25-35 ℃, vacuumizing until the vacuum degree is-0.08-0.05 MPa, and stirring for 0.5-1 hour at 200-500 r/min until no particles exist; and adding 30-50% of polyfunctional group polyurethane acrylate prepolymer into a stirrer, controlling the temperature at 25-35 ℃, vacuumizing to the vacuum degree of-0.08-0.05 MPa, stirring for 0.5-1 hour at 200-500 r/min, uniformly stirring, and sealing and packaging in a dark place.
14. The method for using the UV curable adhesive according to claim 13, wherein the preparation process of the multifunctional urethane acrylate prepolymer comprises the following steps: vacuumizing and dehydrating the dihydric alcohol polymer for 2-3 hours at the temperature of 110-120 ℃; then adding diisocyanate, and fully stirring for 0.5-1 hour in vacuum at the temperature of 50-70 ℃; then adding a catalyst, controlling the temperature at 70-80 ℃ and carrying out vacuum reaction for 2-4 hours; then adding hydroxyl-containing acrylate, fully stirring in vacuum at the temperature of 60-80 ℃, continuously reacting for 2-3 hours, sampling every 30min to determine the NCO value, and discharging for later use when the measured value is zero; wherein the ratio of glycol polymer: diisocyanate: the molar ratio of the hydroxyl-containing acrylate is 1: 1.4-1.7: 1.9-2.1, and the catalyst accounts for 0.1-1 per mill of the weight of the polyfunctional group polyurethane acrylate prepolymer.
15. The method for using the UV curable adhesive according to claim 1, wherein: the thickness of the covered layer of ultraviolet curing glue is 0.3-0.5 mm.
16. An electronic product, characterized in that: the method for using the ultraviolet curing adhesive of any one of claims 1 to 12 on the quality-guaranteed screw screwed by the screw is used for covering at least one layer of cured ultraviolet curing adhesive.
17. The electronic product of claim 16, wherein the thickness of the ultraviolet-curable adhesive is 0.3 to 0.5 mm.
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| CN110591632A (en) * | 2019-09-09 | 2019-12-20 | 烟台德邦科技有限公司 | Black ultraviolet light curing adhesive and preparation method thereof |
| CN112807246B (en) * | 2019-11-15 | 2023-01-13 | 万华化学集团股份有限公司 | Ultraviolet-curing optically variable nail polish and preparation method thereof |
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| CN112679692A (en) * | 2020-12-23 | 2021-04-20 | 四川大学 | Fluorescent anti-counterfeiting material and preparation method and application thereof |
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| JP2003064325A (en) * | 2001-08-28 | 2003-03-05 | Oji Paper Co Ltd | Re-releasable adhesive sheet having buffering function |
| CN102321437B (en) * | 2011-07-25 | 2014-07-16 | 珠海保税区天然宝杰数码科技材料有限公司 | Novel UV (ultraviolet)-curable decoration adhesive |
| CN102708755A (en) * | 2011-12-31 | 2012-10-03 | 明尼苏达矿业制造特殊材料（上海）有限公司 | Anti-counterfeiting label with ultraviolet-cured glue film |
| CN103408716A (en) * | 2013-05-02 | 2013-11-27 | 鑫洲科技有限公司 | (Methyl) acrylic modified polyurethane resin, and ultraviolet curable insulating coating containing same and nano-material |
| CN105860916B (en) * | 2016-05-11 | 2018-08-24 | 烟台德邦科技有限公司 | A kind of high temperature resistant ultraviolet cured adhesive and preparation method thereof |
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