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Photosensitive resin composition and application thereof

A photosensitive resin and composition technology, applied in the field of photoinitiators, can solve the problems of cured products such as amine odor, easy yellowing, increased use of reagents and operating procedures, etc., to reduce the use of chemicals, simplify the production process, and achieve good efficiencies elicited

Active Publication Date: 2021-07-23
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Now there are many kinds of AQ derivatives as photoinitiators, but they all need to be used in conjunction with onium salt cationic photoinitiators or tertiary amine co-initiators, which increases the use of reagents and operating procedures on the one hand, and the other On the one hand, there will also be problems of amine odor and easy yellowing of cured products

Method used

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  • Photosensitive resin composition and application thereof
  • Photosensitive resin composition and application thereof
  • Photosensitive resin composition and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1: the synthesis of photoinitiator Q3

[0058] The synthetic route of photoinitiator Q3 is as figure 1 shown.

[0059] Step 1: Add 150mL of acetone into a round bottom flask, add 3.32g (24.0mmol) of potassium carbonate, 12ml of bromopropylene (138.0mmol) and 720.6mg (3.0mmol) of 1,4-dihydroxyanthraquinone to fully dissolve them. The reaction system was sealed and protected from light, and stirred under reflux at 58° C. for 20 h. Monitor the reactant 1,4-dihydroxyanthraquinone by TLC plate After consumption, 150mlH 2 O was added to the reaction system and extracted with ether (3 x 60ml). After completion, the organic phases were combined and washed with H 2 O and washed with saturated brine. After the organic phase was dried and concentrated, it was purified by silica gel column (eluent: petroleum ether / ethyl acetate=4 / 1), and the yellow solid product (Q2) was obtained 676.5 mg after removal of the solvent, with a yield of 80%.

[0060] Step 2: Under arg...

Embodiment 2

[0063] Embodiment 2: performance detection of Q3

[0064] 1. UV-visible absorption test: preparation 2.2×10 -5 The mol / L acetonitrile solution of Q3 synthesized by the present invention was tested for ultraviolet-visible absorption by a TU1901 ultraviolet-visible spectrophotometer of the Lambda Company of Japan. UV-Vis absorption spectrum such as image 3 shown by image 3 It can be seen that the maximum ultraviolet absorption of the photoinitiator extends to around 550nm, indicating that the photoinitiator of the present invention can be used as a visible light photoinitiator.

[0065] 2. Photolysis test: preparation 2.813×10 -4 Add 2mL of mol / L Q3 acetonitrile solution to a 1cm×1cm×3cm quartz cuvette. Using OmniCure S1000 UV / visible point light source irradiation (LED@405nm), fix the distance between the UV / visible light point light source fiber and the cuvette, and measure the radiation power at the cuvette with a blue light irradiation meter to be 45mw / cm 2 . The UV ...

Embodiment 3

[0067] Embodiment 3: Q3 tests the polymerization kinetics of acrylate monomer

[0068] First weigh 200.0 mg of trimethylolpropane triacrylate (TMPTA), add 2.0 mg of Q3 photoinitiator prepared in Example 1, and stir evenly. Obtain a real-time infrared test sample, wherein the photoinitiator content is 1wt%. The sample was smeared on the KBr salt sheet and irradiated by OmniCure S1000 UV / visible light point light source. The radiation energy density measured by the blue light irradiation meter (405nm detection head) was 45mw / cm 2 , the radiation curing time is 900s, and the conversion rate of the acrylate double bond is monitored in real time by Nicolet6700 Fourier Transform Infrared Spectrometer of Thermo Fisher Scientific Co., Ltd. of the United States. Acrylate double bond peak area interval is taken as 1650cm -1 -1550cm -1 .

[0069] Such as Figure 6 Shown is the real-time conversion curve for photoinitiator-induced TMPTA curing. Among them, the final conversion rate ...

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Abstract

The invention discloses photosensitive resin and application thereof in photocuring, and belongs to the technical field of photoinitiators. According to the invention, the single-component photoinitiator disclosed by the invention can initiate free radical polymerization under the condition that other auxiliary initiators are not added. In the photocuring exploration of trimethylolpropane triacrylate, the single-component photoinitiator shows good initiation efficiency, and the double-component photosensitive resin can simplify the production process of the photocuring technology and reduce the use of chemicals, and has very high practical application value in the aspects of cost saving and environment protection.

Description

technical field [0001] The invention relates to a two-component photosensitive resin composition and its application in photocuring, belonging to the technical field of photoinitiators. Background technique [0002] Photocuring technology refers to a radiation processing technology in which liquid resin is cured by polymerization reaction under the irradiation of a specific wavelength of emission light source. Due to its "5E" advantages of energy saving, economy, environmental protection, high efficiency and wide adaptability, Therefore, it is widely used in coatings, inks, photoresists, adhesives, additive manufacturing and other fields. [0003] The current mature light curing process is often completed by relying on traditional high-pressure mercury lamps or other types of ultraviolet lamps. From the perspective of environmental pollution, these light sources often produce ozone, mercury pollution, and ultraviolet pollution, which are harmful to the human body. The devel...

Claims

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Application Information

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IPC IPC(8): G03F7/027C08F122/14C08F2/48C09D4/02C09D11/101B33Y70/00
CPCG03F7/027C08F122/14C08F2/48C09D4/00C09D11/101B33Y70/00
Inventor 刘仁朱乙皮峻逸王景泉
Owner JIANGNAN UNIV