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Photocuring resin containing polyethoxy bisthiophenyl fluorene structure and preparation method thereof

A technology of ethoxybisphenylthiofluorene and curing resin, which is applied in the field of structural photocurable resin containing polyethoxybisphenylthiofluorene and its preparation, can solve the problem that the refractive index cannot reach more than 1.55 and the refractive index cannot Reach 1.58, poor heat resistance and yellowing resistance, etc., achieve high refractive index, excellent self-healing performance, and good self-healing performance

Active Publication Date: 2015-11-18
东莞市贝特利新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, ethoxy (meth)acrylate with bisphenol A structure has a low refractive index and cannot reach above 1.55, and has poor heat resistance and yellowing resistance; ethoxy (meth)acrylate with ortho-benzene structure, For acrylates with phenoxybenzylethoxy structure, the refractive index cannot reach more than 1.58; for the (meth)acrylic resin of polyoxybisphenoxyfluorene, the highest refractive index can only reach 1.62, which is used in products Poor self-healing performance; high-refractive-index acrylate containing halogen (Br), which is likely to cause environmental concerns; adding inorganic nano-powder blending method to increase the refractive index can even reach more than 1.67, but the product has poor transparency and stable storage sex is not guaranteed
[0004] The patent document with the patent application number 201310450262.3 discloses a preparation method of phenoxybenzyl acrylate, but the refractive index of the phenoxybenzyl acrylate is only 1.565, which cannot meet higher industrial demands, and as mentioned above , and its self-healing performance is also poor

Method used

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  • Photocuring resin containing polyethoxy bisthiophenyl fluorene structure and preparation method thereof
  • Photocuring resin containing polyethoxy bisthiophenyl fluorene structure and preparation method thereof
  • Photocuring resin containing polyethoxy bisthiophenyl fluorene structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 11.76 g of 9.9-(4-phenylthio-2-hydroxyethoxy) bisfluorene, 4.68 g of acrylic acid, and 49.32 g of toluene to a 100 ml four-neck flask equipped with a mechanical stirrer, a condenser and a water separator. 0.43g of ethylsulfonic acid, 0.016g of p-hydroxyanisole, and 0.32g of ethyl hypophosphite were reacted at 115-120°C for 5 hours under reflux to generate 0.88-0.98g of water, and continued to reflux for 1 hour without changing the amount of water.

[0049] After the reaction, the reaction mixture was washed with 10wt% NH 4 NO 3 Solution washing once, 5wt% KOH aqueous solution alkali washing once until the pH value is about 8, then washing three times with distilled water, and finally drying with 2.5wt% anhydrous magnesium sulfate, adding a polymerization inhibitor para-hydroxyl to the dried solution Anisole 0.01g, under certain temperature conditions, the vacuum degree is 0.093~0.095MPa, and the solvent toluene is distilled off under reduced pressure to obtain a co...

Embodiment 2

[0052] Add 11.76 g of 9.9-(4-phenylthio-2-hydroxyethoxy) bisfluorene, 5.59 g of methacrylic acid, and 52.05 g of toluene to a 100 ml four-neck flask equipped with a mechanical stirrer, a condenser and a water separator g, 0.37g of trifluoromethanesulfonic acid, 0.017g of 2,6-di-tert-butyl-p-cresol, and 0.35g of ethyl phosphite. After the reaction was refluxed at 115-120°C for 3 hours, 0.93-1.03g of water was generated. Continue to reflux for 1h, and the water volume will not change.

[0053] After the reaction, the reaction mixture was washed once with 10wt% NaCl solution, once with 5wt% NaOH aqueous solution until the pH value was about 8, then washed three times with distilled water, and finally dried with 2.5wt% anhydrous magnesium sulfate. Add 0.01g of polymerization inhibitor tert-butyl-p-cresol in the solution of the above-mentioned solution, under certain temperature condition, vacuum degree is 0.093~0.095MPa, underpressure distillation removes solvent toluene, obtains ...

Embodiment 3

[0056] Add 13.61 g of 9.9-(4-phenylthio-hydroxydiethoxy) bisfluorene, 4.68 g of acrylic acid, 54.87 g of toluene, and 0.27g of methyl sulfonic acid, 0.018g of p-hydroxyanisole, and 0.36g of ethyl hypophosphite. During the reaction, nitrogen protection was always passed. After reflux reaction at 115-120°C for 4 hours, 1.05-1.15g of water was generated, and the reflux was continued for 1 hour. The amount of water no longer changes.

[0057] After the reaction finished, the reaction mixture was washed once with 10wt% NaCl solution, once with 5wt% KOH aqueous solution until the pH value was about 7, then washed three times with distilled water, and finally dried with 2.5wt% anhydrous magnesium sulfate, and then applied to Add 0.01 g of polymerization inhibitor p-hydroxyanisole to the solution after drying, and under certain temperature conditions, the vacuum degree is 0.093 ~ 0.095 MPa, and the solvent toluene is removed with a rotary evaporator to obtain a colorless and transpare...

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Abstract

The invention relates to the technical field of a resin and a preparation method thereof, particularly a photocuring resin containing polyethoxy bisthiophenyl fluorene structure and a preparation method thereof. The preparation method comprises the following steps: adding 9.9-(4-thiophenyl-hydroxypolyethoxy)bis fluorene and (methyl)acrylic acid into an organic solvent, and carrying out esterification reaction by using an organic acid as a catalyst in the presence of a polymerization inhibitor and a reducer; and after the reaction finishes, carrying out salt washing, neutralization, water washing, drying and reduced pressure distillation to remove the solvent, thereby obtaining the 9.9-(4-thiophenyl-(methyl)acryloyloxypolyethoxy)bis fluorene. The polyethoxy acrylate resin containing bisthiophenyl fluorene structure is a colorless or light yellow transparent photocuring resin, has favorable heat resistance and transparency, and has different refractive index gradients.

Description

technical field [0001] The invention relates to the technical field of resins and resin preparation methods, in particular to a light-curable resin containing polyethoxy bisphenylthiofluorene structure and a preparation method thereof. Background technique [0002] In the prior art, polymers or copolymers containing polyethoxy (meth)acrylate in the molecule are widely used in optical materials due to their excellent transparency, high refractive index, high temperature resistance, self-healing properties, etc. Optical lens resins, optical coatings such as brightness enhancement films (in the backlight modules of LCD TVs and mobile phone displays, increase the brightness of the screen and reduce energy consumption), and high temperature resistant optical adhesives and other industries. [0003] At present, ethoxy (meth)acrylate with bisphenol A structure has a low refractive index and cannot reach above 1.55, and has poor heat resistance and yellowing resistance; ethoxy (meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/12C07C319/20C08G65/00
Inventor 周传玉陶林华黄思富谢梓华
Owner 东莞市贝特利新材料有限公司
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