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Deeply curable UV-to-black adhesive

A deep curing and adhesive technology, applied in the direction of adhesives, adhesive additives, adhesive types, etc., can solve the problems that affect the strength and curing effect of the glue body, the proportion of dyes should not be too much, and the color will fade.

Active Publication Date: 2021-09-14
SHUNDE POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are also plans in the industry to use photochromic dyes to realize the curing of adhesives, such as the Chinese patent application with publication number CN112126401A, the title of which is "a color-changing UV-curable adhesives and their preparation methods and applications”, which uses thermochromic pigments, but mainly monomeric dyes are blended with traditional UV glue formulas. After UV irradiation, acid is generated, and a On the one hand, the UV glue is cured and the dye turns black at the same time, but these monomeric dyes have no double bond structure and cannot participate in the free radical reaction in the glue. They are physically blended with other components, so on the one hand, the dye addition ratio should not be too high. Too much, otherwise it will affect the strength and curing effect of the glue body. At the same time, due to the physical blending, the dye glue is easy to precipitate after long-term use after curing, especially under high temperature and high humidity, which will cause the color to gradually fade

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1 Preparation of fluoran-based acrylate monomer

[0031] 2-Bromo-3-methyl-6-N,N-bisbutylamino-fluoran (CAS: 117342-26-4) and 2-(methacrylate)ethyl 4-aminobenzoic acid (CAS: 130291 -82-6) Add to solvent A, then add catalyst A, the reaction temperature rises to 80°C, and the reaction time is 2 hours to obtain fluoran acrylate monomers, which are photochromic fluoran containing double bonds Acrylate monomer, its molecular structure formula is as follows:

[0032]

[0033] Wherein 2-bromo-3-methyl-6-N, N-bisbutylamino-fluorane, 2-(methacrylic acid) ethyl ester 4-aminobenzoic acid, the mass ratio of solvent A and catalyst A is: 1: 1:10:0.01; the solvent A is formamide; the catalyst A is triethylamine.

[0034] Step 2 Preparation of deep-curable UV blackening adhesive

[0035] Mix and stir the fluoran acrylate monomer, photoacid generator, amine compound, acrylic resin, diluent, crosslinking agent, photoinitiator, silane coupling agent and filler synthesized in ste...

Embodiment 2

[0038] Step 1 Preparation of fluoran-based acrylate monomer

[0039]2-Bromo-3-methyl-6-N,N-bisbutylamino-fluoran (CAS: 117342-26-4) and 2-(methacrylate)ethyl 4-aminobenzoic acid (CAS: 130291 -82-6) Add to solvent A, then add catalyst A, the reaction temperature rises to 100°C, and the reaction time is 6 hours to obtain fluoran acrylate monomers, which are photochromic fluoran containing double bonds Acrylate monomer; its molecular formula is as follows:

[0040]

[0041] Wherein 2-bromo-3-methyl-6-N, N-bisbutylamino-fluorane, 2-(methacrylic acid) ethyl ester 4-aminobenzoic acid, the mass ratio of solvent A and catalyst A is: 1: 3:30:0.03; the solvent A is: nitrogen methyl pyrrolidone; the catalyst A is sodium hydroxide.

[0042] Step 2 Preparation of deep-curable UV blackening adhesive

[0043] Stir the fluoran acrylate monomer, photoacid generator, amine compound, acrylic resin, diluent, crosslinking agent, photoinitiator, silane coupling agent and filler synthesized in...

Embodiment 3

[0046] Step 1 Preparation of fluoran-based acrylate monomer

[0047] 2-Bromo-3-methyl-6-N,N-bisbutylamino-fluoran (CAS: 117342-26-4) and 2-(methacrylate)ethyl 4-aminobenzoic acid (CAS: 130291 -82-6) Add to solvent A, then add catalyst A, the reaction temperature rises to 80°C, and the reaction time is 3 hours, and the fluoran acrylate monomer, which is the color-changing fluoran acrylate containing double bonds, can be obtained Monomer, its molecular formula is as follows:

[0048]

[0049] Wherein 2-bromo-3-methyl-6-N, N-bisbutylamino-fluorane, 2-(methacrylic acid) ethyl ester 4-aminobenzoic acid, the mass ratio of solvent A and catalyst A is: 1: 2:20:0.02; the solvent A is dimethyl sulfoxide; the catalyst A is potassium hydroxide.

[0050] Step 2 Preparation of deep-curable UV blackening adhesive

[0051] Stir the fluoran acrylate monomer, photoacid generator, amine compound, acrylic resin, diluent, crosslinking agent, photoinitiator, silane coupling agent and filler s...

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Abstract

The invention relates to a deeply curable UV-to-black adhesive, which is characterized by comprising a fluorane acrylate monomer, a photoacid generator, an amine compound, acrylic resin, a diluent, a cross-linking agent, a photoinitiator, a silane coupling agent and a filler, wherein the weight ratio of the fluorane acrylate monomer to the photoacid generator to the amine compound to the acrylic resin to the diluent to the cross-linking agent to the photoinitiator to the silane coupling agent to the filler is 1: (1-2): (0.1-2): (10-100): (2-20): (1-10): (0.1-4): (0.005-0.02): (0.1-5). The adhesive has the advantages that the adhesive shows a transparent or faint yellow transparent effect before curing, deep irradiation of UV light is guaranteed, then a UV initiator in the adhesive generates free radicals to initiate curing of active functional groups in the adhesive, meanwhile, the photoacid generator is added into an adhesive system, the UV light initiates the photoacid generator to generate acid, and dye is promoted to be changed into black, so that the deep curing of the UV adhesive is finally realized, and the black effect is presented.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a deep-curable UV blackening adhesive. Background technique [0002] As an important part of adhesives, UV adhesives occupy an important position, especially in the field of transparent optics. UV adhesive has the characteristics of rapid curing at room temperature, so UV adhesives are selected in many fields that require rapid room temperature curing. [0003] However, UV adhesives have a fatal shortcoming. The curing of glue depends on UV irradiation, so the glue is required to be able to pass through UV light. For some scenes that require black shading effect or black appearance effect, it is difficult to use UV glue, because it requires To achieve UV glue with shading or black appearance, it is necessary to add carbon black or black pigment to it. Once it is added, it will make it difficult for UV light to reach the bottom, so that the glue can only be cured on the...

Claims

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Application Information

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IPC IPC(8): C09J175/14C09J167/06C09J163/10C09J11/04C09J11/06
CPCC09J175/14C09J167/06C09J163/10C09J11/04C09J11/06C08K2003/2227C08L67/06C08L63/10C08K7/18C08K3/36C08K5/375C08K3/34C08K3/22
Inventor 刘锋霍应鹏陈燕舞肖瑞雄洪丹刘明宇
Owner SHUNDE POLYTECHNIC
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