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Dendritic fluorescein sodium-iodonium salt visible light initiator and preparation method and application thereof

A technology of sodium fluorescein and visible light, applied in the field of photoinitiation, can solve the problems of single function, high volatility, weak anti-migration ability, etc., and achieve the effect of strong penetrating ability, high initiation efficiency and cheap light source

Active Publication Date: 2019-10-11
CHANGSHU INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although there are many types of small-molecule initiators and their development is relatively mature, small-molecule visible light initiators have disadvantages such as heavy odor, high volatility, weak anti-migration ability, poor environmental compatibility, poor resin compatibility, and single function.

Method used

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  • Dendritic fluorescein sodium-iodonium salt visible light initiator and preparation method and application thereof
  • Dendritic fluorescein sodium-iodonium salt visible light initiator and preparation method and application thereof
  • Dendritic fluorescein sodium-iodonium salt visible light initiator and preparation method and application thereof

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preparation example Construction

[0031] The preparation method of dendritic fluorescein sodium-iodonium salt visible light initiator of the present invention comprises the steps:

[0032] (1) The end group of the intermediate is a dendrimer (PAE (=) of 8 acrylates 8 ) synthesis: mix trimethylolpropane triacrylate, ethylenediamine, and anhydrous methanol, heat to 30°C, react for 6 hours, wash with anhydrous methanol to obtain a colorless and transparent viscous liquid, and react The formula is as follows:

[0033]

[0034] (2) Dendrimers with 8 primary amino groups at the end of the intermediate (PAE(NH 2 ) 8 ) synthesis: the PAE (=) 8 Mix with ethylenediamine, heat to 30°C, react for 24 hours, distill under reduced pressure, wash with ethyl acetate to obtain light yellow transparent viscous liquid, the reaction formula is as follows:

[0035]

[0036] (3) Synthesis of intermediate diphenyliodonium chloride: mix benzene, acetic anhydride, and potassium iodate, react in a brine ice bath, add acetic an...

Embodiment 1

[0042] Embodiment 1: the preparation of visible light initiator

[0043] (1) The end group of the intermediate is a dendrimer (PAE (=) of 8 acrylates 8 )Synthesis:

[0044] Mix 60g of trimethylolpropane triacrylate, 2.4g of ethylenediamine, and 30mL of anhydrous methanol, heat to 30°C, react for 6 hours, wash with anhydrous methanol, and obtain a colorless and transparent viscous liquid.

[0045] (2) Dendrimers with 8 primary amino groups at the end of the intermediate (PAE(NH 2 ) 8 )Synthesis:

[0046] 4.665g PAE(=) 8 Mix with 108g of ethylenediamine, heat to 30-50°C, react for 24 hours, distill under reduced pressure, wash with ethyl acetate to obtain light yellow transparent viscous liquid.

[0047] (3) Synthesis of intermediate diphenyliodonium chloride salt:

[0048] Mix 9mL of benzene, 10mL of acetic anhydride, and 10.7g of potassium iodate, and slowly drop in a mixture of 7mL of concentrated sulfuric acid and 10mL of acetic anhydride in a brine ice bath (about -5°C)...

Embodiment 2

[0055] Embodiment 2: PAE-FS (IPh 2 ) 2 Visible Light Initiated Unsaturated Resins

[0056] PAE-FS (IPh 2 ) 2 Visible Light Initiated Epoxy Acrylates:

[0057] Get 1.3g epoxy acrylate and 0.7g reactive diluent TMPTA, stir and mix, add the various visible photoinitiators (PAE-FS of the present invention (IPh 2 ) 2 Photoinitiator, FS(IPh 2 ) 2 Photoinitiator and FS+10% by weight of the combined photoinitiator (i.e. FS+10%Vc) formed by the co-initiator vitamin C), mix with a mixer, be coated on a glass sheet into an approximately 0.1mm thick film, place Curing under 500W LED lamp radiation, record the curing time. The results are shown in Table 1.

[0058] Table 1 Initiator triggers epoxy acrylate curing time

[0059]

[0060]

[0061] PAE-FS (IPh 2 ) 2 Visible Light Initiated Hyperbranched Polyester Acrylates:

[0062] Get 1.3g hyperbranched polyester acrylate and 0.7g reactive diluent TMPTA, stir and mix uniformly, add various visible photoinitiators (PAE-FS (...

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Abstract

The invention discloses a dendritic fluorescein sodium-iodonium salt visible light initiator and a preparation method and application thereof. By combination of chromophore fluorescein sodium and iodonium salt, an electron transfer type visible light initiator system is obtained; by introduction of the electron transfer type visible light initiator system into a dendritic compound, visible light initiating efficiency is remarkably improved. The light initiator has advantages of environmental friendliness, high compatibility, low energy consumption and the like and used for initiating unsaturated resin curing. A macromolecular light initiator is achieved, and by application of specific dendritic fluorescein sodium-iodonium salt to unsaturated resin curing-polymerization, appearance, hardness, glossiness and flexibility of obtained coatings are all excellent.

Description

technical field [0001] The invention relates to photoinitiation technology, in particular to a dendritic fluorescein sodium-iodonium salt visible light initiator and a preparation method and application thereof. Background technique [0002] Photocuring technology has become an integral part of the field of polymer science and technology. Photoinitiation not only consumes less energy, but also has high polymerization efficiency and is environmentally friendly. It has now become a key component of photocuring technology. [0003] Since the energy of ultraviolet light is much higher than that of visible light, the development of ultraviolet photoinitiators is more mature. However, there are many problems caused by ultraviolet light that cannot be ignored. When ultraviolet light acts on the human body, it will cause headaches, dizziness, eye irritation, dermatitis, and even skin cancer. Compared with ultraviolet light, visible light can directly use sunlight [0004] Sunligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09D163/10C09D167/06C09D7/65
CPCC08G83/003C08G83/004C09D163/10C09D167/06C08F2/48C08F283/105C08F283/01
Inventor 宁春花周弟吉汪冲程彦霖董洁
Owner CHANGSHU INSTITUTE OF TECHNOLOGY
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