CN109762509B - UV (ultraviolet) viscosity reducing adhesive and application thereof - Google Patents
UV (ultraviolet) viscosity reducing adhesive and application thereof Download PDFInfo
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Abstract
The invention relates to UV (ultraviolet) viscosity-reducing adhesive and application thereof. The UV viscosity reducing adhesive comprises, by weight, 50-100 parts of a component A and 50-100 parts of a component B; the component A comprises, by weight, 10-40 parts of cured resin, 20-40 parts of polyfunctional active monomer, 10-30 parts of polyfunctional oligomer and 1-10 parts of photoinitiator; and the component B is at least one selected from the group consisting of isocyanate-containing curing agents and mercapto-containing curing agents.
Description
Technical Field
The invention relates to UV (ultraviolet) viscosity-reducing adhesive and application thereof.
Background
In the thinning and polishing of glass for mobile phones, high-temperature paraffin is generally selected by the industry to be firstly bonded and fixed on a ceramic plate, then thinning and polishing are carried out by a probe, and the process needs that the glass is fixed on a ceramic substrate and bears certain shearing force. And then polishing in alkali liquor, after thinning and polishing are finished, melting paraffin at high temperature to enable the glass to be removed from the substrate, and because a certain amount of residual paraffin exists on the contact surface of the glass and the paraffin, the residual paraffin can be removed by cleaning with a solvent, so that the environment is not protected, a large amount of labor is used, pollution discharge is increased, and the labor cost is lowered.
Document CN103923572A discloses a method for producing UV-reduced films by adding a photocurable monomer in an acrylic system. The peel strength of the UV visbroken film produced in this way at 180 ℃ before light irradiation is only 1.4N/25mm, which is not enough to provide the adhesive strength of the material before light irradiation. The document CN104496853A discloses that the thermal reaction synthesis method requires special resin synthesis equipment, the reaction time is long, and after the reaction process is fixed, the initial adhesion and the adhesion after UV tack reduction cannot be adjusted according to the adhesion required by different substrates. Meanwhile, in the prior art of UV viscosity reduction, solvent components exist, and the solvent needs to be removed before curing, so that the method is inconvenient, can generate a large amount of VOC, and is not environment-friendly. The presence of solvents also affects the range of applications of the anti-tack adhesive, and in many closed application scenarios, the solvent cannot escape without sufficient environment, and this type of anti-tack adhesive cannot be used.
Disclosure of Invention
The invention relates to UV (ultraviolet) viscosity reducing adhesive. The UV viscosity reducing adhesive comprises 50-100 parts of a component A and 50-100 parts of a component B in parts by weight, based on the total weight parts of the component A and the component B;
the component A comprises 10-40 parts of cured resin, 20-40 parts of polyfunctional active monomer, 10-30 parts of polyfunctional oligomer and 1-10 parts of photoinitiator by weight, based on the total weight parts of the cured resin, the polyfunctional active monomer, the polyfunctional oligomer and the photoinitiator;
wherein the cured resin contains hydroxyl groups and acrylate groups;
the polyfunctional reactive monomer is selected from the group consisting of pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, trimethylolpropane triacrylate, ethoxylated trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, 2-hydroxyethyl methacrylate, acrylamide, 1, 6-hexanediol dimethacrylate, 1, 6-hexanediol diacrylate, ethylene glycol diacrylate, triethylene glycol diacrylate, tripropylene glycol diacrylate, p-neopentyl glycol diacrylate, trimethylolpropane triacrylate, trimethylolpentane trimethacrylate, trimethylolpropane pentaerythritol triacrylate, propoxylated neopentyl glycol diacrylate, trimethylolpropane triacrylate, and mixtures thereof, At least one member selected from the group consisting of ethoxylated 1, 6-hexanediol diacrylate and tris (2-acryloxyethyl) isocyanurate;
the multifunctional oligomer is at least one selected from the group consisting of an aliphatic urethane acrylate oligomer, an aromatic polyacrylate oligomer, a pure acrylate oligomer, an epoxy acrylate oligomer, and a polyester acrylate oligomer;
and the component B is at least one selected from the group consisting of isocyanate-containing curing agents and mercapto-containing curing agents.
According to one aspect of the invention, the cured resin is obtained by reacting a mixture comprising hydroxyalkyl acrylate, isocyanate and glycol.
According to one aspect of the present invention, the hydroxyalkyl acrylate is at least one selected from the group consisting of hydroxyethyl acrylate and hydroxyethyl methacrylate.
According to an aspect of the present invention, the isocyanate is at least one selected from the group consisting of isophorone diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate, and dicyclohexylmethane diisocyanate.
According to an aspect of the present invention, the glycol is at least one selected from the group consisting of polyester glycol, polyether glycol and alkyl glycol.
According to one aspect of the invention, the molar ratio of the hydroxyalkyl acrylate, the isocyanate and the diol in the mixture is 0.3 to 1.2: 0.5-1: 0.3-1.2.
According to one aspect of the invention, the reaction temperature is 40-90 ℃, preferably 60-80 ℃; the reaction time is from 0.5 to 5 hours, preferably from 1 to 3 hours.
According to one aspect of the invention, the glycol has a molecular weight of 100 to 5000.
According to one aspect of the present invention, the isocyanate-containing curing agent has an NCO content of 10 to 25% by weight.
According to one aspect of the present invention, the mercapto group content of the mercapto group-containing curing agent is 2 to 15 wt%.
According to an aspect of the present invention, the isocyanate-containing curing agent is at least one selected from the group consisting of isophorone diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, and polyisocyanate (such as hexamethylene diisocyanate trimer).
According to an aspect of the present invention, the mercapto group-containing curing agent is at least one selected from the group consisting of pentaerythritol tetrakis (3-mercaptopropionate), pentaerythritol tris (3-mercaptopropionate), and pentaerythritol bis (3-mercaptopropionate).
According to one aspect of the invention, the photoinitiator is selected from the group consisting of 1-hydroxycyclohexyl phenyl ketone, 2,4,6- (trimethylbenzoyl) diphenyl phosphine oxide, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone and ethyl 2,4, 6-trimethylbenzoylphenylphosphonate, benzoin ether, dimethyl benzil ketal, alpha hydroxy ketone, acyl phosphorous oxide and benzophenone.
According to one aspect of the invention, the a-side and the B-side are present in a form independent of each other, such as separate packages or mechanical mixtures with each other.
According to one aspect of the invention, the component B also comprises 0-10 parts of defoaming agent, leveling agent and antioxidant. The antifoaming agent may be one or more selected from Xinyue KS-66, bike BYK011, Mitig TSA750S, Dow Corning DC62, Digao Airex900 and bike BYK 067. The leveling agent can be one or more than two of Dow Corning DC56, Xinyue KP-324, Yingchuang Deliosai Glide 432, Bik BYK361N, Yingchuang Deliosai Glide 410, Bik BKY333 and Effeka efka-3580. The antioxidant can be one or more selected from bisphenol A, antioxidant RD, antioxidant AW, antioxidant 264 and antioxidant 445.
The invention also provides application of the UV viscosity reducing adhesive. The UV viscosity reducing adhesive is used for thinning and polishing treatment of glass for the mobile phone.
The invention has the beneficial effects that:
the invention adopts two-component curing UV viscosity-reducing adhesive.
1. The glue has high initial viscosity after being thermally cured, and is convenient to process and operate.
2. The peel force after UV irradiation is low and the glue can be easily removed without residual glue. The UV visbreaking process time is short.
3. The operation process is simple, and manpower and material resources are saved.
4. No solvent, environmental protection and can meet a plurality of application scenes.
5. The cured resin can participate in thermosetting and photocuring, so that the initial bonding force after thermosetting is ensured, and the high crosslinking density of the whole body after UV post-curing is ensured, and better viscosity reduction is realized.
Detailed Description
The invention is described in detail below, but it is to be understood that the scope of the invention is not limited thereto, but rather by the appended claims.
All publications, patent applications, patents, and other references mentioned in this specification are herein incorporated by reference in their entirety. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In case of conflict, the present specification, including definitions, will control.
In the context of the present specification, anything or things which are not mentioned, except where explicitly stated, are directly applicable to those known in the art without any changes. Moreover, any embodiment described herein may be freely combined with one or more other embodiments described herein, and the technical solutions or concepts resulting therefrom are considered part of the original disclosure or original disclosure of the invention, and should not be considered as new matters not disclosed or contemplated herein, unless a person skilled in the art would consider such a combination to be clearly unreasonable.
The UV viscosity-reducing adhesive is an A, B bi-component system, wherein the A, B component is packaged and stored separately at ordinary times, and the A, B component is mixed uniformly before use.
The performance of the UV viscosity reducing adhesive is tested by the following method:
uniformly coating the UV anti-sticking adhesive on the surface of the ceramic substrate, adhering a glass cover plate, and pre-curing in an oven at 80 ℃ for 30 min; then soaking the mixture in 2 weight percent NaOH solution for 4 hours at the temperature of 50 ℃; after taking out, the glass was removed from the surface of the ceramic substrate by UV irradiation (1000mJ, irradiation time 10s or less) to observe whether or not the adhesive remains.
The detection items are as follows:
initial adhesion (adhesion before UV detackification): after thermosetting at 80 ℃ for 30min, detecting the bonding strength by using a pulling machine, wherein the formula is as follows: the bonding strength is the maximum tensile force per bonding area (unit MPa).
Alkali resistance: soaking the thermosetting material in 2 wt% NaOH solution for 4 hours at 50 ℃, taking out and observing the falling-off condition of the glue (1 → 5): 1-no change at all; 5-the glue falls off completely.
Bonding force after visbreaking: after UV curing (energy 1000mj), the adhesion strength was measured using a tensile machine, and the formula is: the bonding strength is the maximum tensile force per bonding area (unit MPa).
The residual gum rate: after UV tack reduction, the glue was peeled off, the substrate surface was observed with a microscope and rated according to the amount of residual glue (1 → 5): 1-complete residual glue; 5-the residual glue is spread over the surface.
[ example 1 ]
Synthesis of cured resin: 1.2mol of hydroxyethyl methacrylate, 0.7mol of IPDI and 0.3mol of polyethylene glycol adipate (with the molecular weight of 5000) react for 1-3 hours at the temperature of 60-80 ℃ to obtain the cured resin A1。
The component A comprises: cured resin A110g of trimethylolpropane triacrylate, 40g of trimethylolpropane triacrylate, 20g of an aliphatic urethane acrylate oligomer-sartomer CN8011 (functionality 6), 6g of alpha hydroxy ketone.
And B component: 50g of Bayer HDI aliphatic isocyanate 7790(NCO content 17%).
The preparation method comprises the following steps: and (3) sequentially putting the cured resin and the active monomer raw materials into a stirring cylinder, stirring for half an hour, filtering to obtain a component A, and respectively putting the component A and the component B into different containers to obtain a final product.
[ example 2 ]
Synthesis of cured resin: 0.3mol of hydroxyethyl acrylate, 0.5mol of IPDI and 0.8mol of polyethylene glycol (molecular weight 200) are reacted for 1 to 3 hours at the temperature of between 60 and 80 ℃ to obtain the cured resin A2。
The component A comprises: cured resin A240g of pentaerythritol tetraacrylate 20g, 30g of aliphatic urethane acrylate oligomer-sartomer CN8011 (functionality of 6), 5g of alpha-hydroxyketone and 5g of acylphosphine oxide.
And B component: 99 g of basf HB175(NCO content 16.5%), 0.5 g of defoamer dygaairex 910, 0.5 g of leveling agent BYK 333.
The preparation method comprises the following steps: curing resin A2Sequentially adding the active monomer raw materials and the active monomer raw materials into a stirring cylinder, stirring for half an hour, filtering to obtain a component A, and respectively filling the component A and the component B into different containers to obtain a final product.
[ example 3 ]
Synthesis of cured resin: 1.2mol of hydroxyethyl acrylate, 1.0mol of IPDI and 1.0mol of pentanediol react for 1-3 hours at the temperature of 60-80 ℃ to obtain the cured resin A3。
The component A comprises: cured resin A320g of dipentaerythritol hexaacrylate, 30g of aliphatic urethane acrylate oligomer-sartomera CN8011 (functionality of 6)10g and 1g of 2,4,6- (trimethylbenzoyl) diphenyl phosphorus oxide.
And B component: 60g of Bayer HDI aliphatic isocyanate 7790(NCO content 17%).
The preparation method comprises the following steps: curing resin A3Sequentially adding the active monomer raw materials and the active monomer raw materials into a stirring cylinder, stirring at medium speed for half an hour, filtering to obtain a component A, and respectively filling the component A and the component B into different containers to obtain a final product.
[ example 4 ]
Synthesis of cured resin: 0.8mol of hydroxyethyl methacrylate, 0.9mol of HDI and 1.2mol of polytetrahydrofuran (molecular weight of 1000) are reacted for 1 to 3 hours at the temperature of 60 to 80 ℃ to obtain the cured resin A4。
The component A comprises: cured resin A430g of ethoxylated 1, 6-hexanediol diacrylate, 30g of epoxy acrylate oligomer-sartomer CN2204 (functionality of 4) and 8g of 1-hydroxycyclohexyl phenyl ketone.
And B component: BasfHB175(NCO content 16.5%) 75 g.
The preparation method comprises the following steps: curing resin A4Sequentially adding the active monomer raw materials and the active monomer raw materials into a stirring cylinder, stirring at medium speed for half an hour, filtering to obtain a component A, and respectively filling the component A and the component B into different containers to obtain a final product.
[ COMPARATIVE EXAMPLE 1 ]
The component A comprises: 30g of ethoxylated 1, 6-hexanediol diacrylate, 30g of epoxy acrylate oligomer-sartomer CN2204 (functionality of 4) and 6g of 1-hydroxycyclohexyl phenyl ketone.
And B component: BasfHB175(NCO content 16.5%) 60 g.
The preparation method comprises the following steps: and sequentially putting the raw materials of each component into a stirring cylinder, stirring for 2 hours at medium speed, and filtering to respectively prepare a component A and a component B.
[ COMPARATIVE EXAMPLE 2 ]
Paraffin wax: alkali-resistant paraffin wax of Japanese ALCOWAX
The test results of the compositions prepared in examples 1 to 4 and comparative examples 1 to 2 under the respective test methods were as follows:
| detecting items | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Initial adhesion | 1.2mpa | 1.5mpa | 1.3mpa | 1.3mpa | 0.4mpa | 2.0mpa |
| Alkali resistance | 1 | 1 | 1 | 1 | 3 | 2 |
| Post UV adhesion | 0.1mpa | 0.1mpa | 0.1mpa | 0.1mpa | 0.1mpa | 2.0mpa |
| Condition of adhesive residue | 1 | 1 | 1 | 1 | 1 | 5 |
From the above data, it can be seen that all 4 examples have good initial adhesion, good alkali resistance, and good protection of the substrate, and can be easily peeled off after UV without adhesive residue. In contrast, comparative example 1 had no self-made resin, resulting in low initial adhesion and poor alkali resistance; on the other hand, comparative example 2 is not satisfactory in that UV visbreaking is not possible and complicated high-temperature (150 ℃ C.) visbreaking is required.
Claims (11)
1. The UV viscosity-reducing adhesive comprises 50-100 parts of a component A and 50-100 parts of a component B in parts by weight, based on the total parts by weight of the component A and the component B;
the component A comprises 10-40 parts of cured resin, 20-40 parts of polyfunctional active monomer, 10-30 parts of polyfunctional oligomer and 1-10 parts of photoinitiator by weight, based on the total weight parts of the cured resin, the polyfunctional active monomer, the polyfunctional oligomer and the photoinitiator;
wherein the cured resin contains hydroxyl groups and acrylate groups; the curing resin is obtained by reacting a mixture containing hydroxyalkyl acrylate, isocyanate and dihydric alcohol;
the hydroxyalkyl acrylate is at least one selected from the group consisting of hydroxyethyl acrylate and hydroxyethyl methacrylate;
the isocyanate is at least one selected from the group consisting of isophorone diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate, and dicyclohexylmethane diisocyanate;
the diol is at least one selected from the group consisting of polyester diol, polyether diol and alkyl diol;
the multifunctional active monomer is selected from pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, trimethylolpropane triacrylate, ethoxylated trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, 2-hydroxyethyl methacrylate, acrylamide, 1, 6-hexanediol dimethacrylate, 1, 6-hexanediol diacrylate, at least one member selected from the group consisting of ethylene glycol diacrylate, triethylene glycol diacrylate, tripropylene glycol diacrylate, p-neopentyl glycol diacrylate, trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, trimethylolpropane pentaerythritol triacrylate, propoxylated neopentyl glycol diacrylate, ethoxylated 1, 6-hexanediol diacrylate, and tris (2-acryloxyethyl) isocyanurate;
the multifunctional oligomer is at least one selected from the group consisting of an aliphatic urethane acrylate oligomer, an aromatic polyacrylate oligomer, an epoxy acrylate oligomer, and a polyester acrylate oligomer;
and the component B is at least one selected from the group consisting of isocyanate-containing curing agents and mercapto-containing curing agents.
2. The UV viscosity-reducing adhesive according to claim 1, wherein the reaction temperature is 40-90 ℃; the reaction time is 0.5-5 hours.
3. The UV viscosity-reducing adhesive according to claim 2, wherein the reaction temperature is 60-80 ℃; the reaction time is 1-3 hours.
4. The UV deglued adhesive according to claim 1, wherein the molecular weight of the diol is 100-5000.
5. The UV anti-adhesive according to claim 1, wherein the isocyanate-containing curing agent has an NCO content of 10 to 25% by weight, and the mercapto-containing curing agent has a mercapto content of 2 to 15% by weight.
6. The UV vis-broken adhesive according to claim 1, wherein the isocyanate-containing curing agent is at least one selected from the group consisting of isophorone diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, and polyisocyanate;
the mercapto group-containing curing agent is at least one selected from the group consisting of pentaerythritol tetrakis (3-mercaptopropionate), pentaerythritol tris (3-mercaptopropionate), and pentaerythritol bis (3-mercaptopropionate).
7. The UV deglued adhesive according to claim 6, wherein the polyisocyanate is hexamethylene diisocyanate trimer.
8. The UV anti-adhesive according to claim 1, the photoinitiator is at least one selected from the group consisting of 1-hydroxycyclohexyl phenyl ketone, 2,4,6- (trimethylbenzoyl) diphenyl phosphorus oxide, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone and ethyl 2,4, 6-trimethylbenzoylphenylphosphonate, benzoin ether, dimethyl benzil ketal, alpha hydroxy ketone, acyl phosphorus oxide and benzophenone.
9. The UV deglued adhesive according to claim 1, wherein the A-component and the B-component are present independently of each other.
10. The UV tack-reducing adhesive of claim 9, wherein the mutually independent forms are mutually independent packages or mechanical mixtures.
11. The use of the UV detackifier according to any one of claims 1-10 in the thinning and polishing of glass for a cellular phone.
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| CN110330919A (en) * | 2019-07-03 | 2019-10-15 | 昆山博益鑫成高分子材料有限公司 | A kind of UV visbreaking glue |
| CN110738933A (en) * | 2019-10-25 | 2020-01-31 | Oppo广东移动通信有限公司 | Display screen assembly, manufacturing method thereof and electronic equipment |
| CN110903790A (en) * | 2019-11-22 | 2020-03-24 | 苏州高泰电子技术股份有限公司 | UV (ultraviolet) viscosity-reducing composition and UV viscosity-reducing adhesive tape with same |
| CN111440574B (en) * | 2019-12-27 | 2021-10-26 | 宁波激智科技股份有限公司 | Adhesive composition and anti-adhesive tape applied to cutting optical filter |
| CN112625496A (en) * | 2020-12-31 | 2021-04-09 | 和运创新印刷包装有限责任公司 | Solvent-free ultraviolet curing gravure printing ink |
| CN113897168A (en) * | 2021-10-26 | 2022-01-07 | 湖北大学 | UV (ultraviolet) viscosity-reducing glue solution, single-side UV viscosity-reducing protective film and preparation method |
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| CN108441135A (en) * | 2018-02-02 | 2018-08-24 | 苏州城邦达力材料科技有限公司 | A kind of UV visbreakings composition, UV visbreaking films and preparation method thereof |
| CN108611010A (en) * | 2018-03-30 | 2018-10-02 | 东莞市澳中电子材料有限公司 | A kind of two-sided UV Protection glues band of easy-clear and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108441135A (en) * | 2018-02-02 | 2018-08-24 | 苏州城邦达力材料科技有限公司 | A kind of UV visbreakings composition, UV visbreaking films and preparation method thereof |
| CN108611010A (en) * | 2018-03-30 | 2018-10-02 | 东莞市澳中电子材料有限公司 | A kind of two-sided UV Protection glues band of easy-clear and preparation method thereof |
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