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COLLOID AND POLYMER SCIENCE · 2020 ·Vol. 298 ·期 10 ·1285-1291 · IF 1.536

Preparation of poly(methyl methacrylate) microspheres via photopolymerization initiated by LED light source

Xie Chuanbao,Leng Kangwei,Sheng Jie,Wang Xuemei,Li Qianmin,Song Liang,Liu Lei,Sun Hejing,Huang Xiaowen,Wang Zhongwei,Yu Qing

Poly(methyl methacrylate) (PMMA) microspheres were synthesized through visible light–induced photopolymerization of methyl methacrylate (MMA). 2,4,6-Trimethylbenzoyldipenylphosphine oxide (TPO), polyvinylpyrrolidone (PVP), and light-emitting diodes (LEDs) were used as the photoinitiator, stabilizer, and light source, respectively. No other additive was involved. The effect of LEDs, TPO, and PVP was discussed. Results showed that PMMA microspheres with the size of 0.5–0.8 μm could be obtained when LED@385 nm was the light source, and the content of TPO and PVP was 2 wt% and 30 wt% of MMA. Moreover, the possible formation pathway of PMMA microspheres was proposed based on the investigation of reaction time and addition method of PVP. Graphical abstract

研究领域: 材料科学 · 化学工程
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JOURNAL OF APPLIED POLYMER SCIENCE · 2018 ·Vol. 135 ·期 37 ·46686 · IF 1.901

Binary phase solid-state photopolymerization behavior of acrylate cryogels under different light sources

Safdar Ali,Farooq Khurum Shehzad,Inamullah Maitlo,Sultan Valiev,Ghulam Muhyodin,Jun Nie

Two types of cryogels were obtained using 2-hydroxyethyl acrylate (HEA) and 2-hydroxyethyl methacrylate (HEMA) by homogeneous mixing with poly(ethylene glycol) diacrylate (PEGDA) as crosslinker at subzero temperature followed by photopolymerization with two different light initiation sources (high-pressure Hg arc lamp and UV-LED).The solution was frozen unidirectionally at −60 °C before polymerization and finally photopolymerized at the same temperature. The cryogels were characterized using photo-DSC, UV–vis and Fourier transform infrared spectroscopy, and scanning electron microscopy techniques. The cryogels cured with an LED light showed a higher polymerization rate and better morphological characteristics than ones cured with a high-pressure Hg arc. The water intake ratio of HEA/PEGDA was higher than HEMA/PEGDA for both curing sources. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135 , 46686.

研究领域: 材料科学 · 高分子化学
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NEW JOURNAL OF CHEMISTRY · 2023 ·Vol. 47 ·期 11 ·5330-5337 · IF 3.3

New functionalized thioxanthone derivatives as type I photoinitiators for polymerization under UV-Vis LEDs

Yu Wang,Rao Chen,Dongmei Liu,Chaofei Peng,Junwei Wang,Xiaoqing Dong

The development of effective Vis-sensitive photoinitiators for light-emitting diode (LED) polymerization is still an emerging challenge as LEDs are being developed into the predominant light sources. In this work, a series of new functionalized photoinitiators, containing thioxanthones and oxime-esters as functional groups, was designed and straightforwardly synthesized in two steps. The structures of the photoinitiators were studied using 1H NMR, 13C NMR, and high-resolution mass spectrometry. The conclusion of the photophysical properties indicated that the long wavelength absorptions from 360 nm to 405 nm made the investigated thioxanthone derivatives quite appealing as a valuable photoinitiator under UV-Vis LEDs. The structure–reactivity relationship was also studied in detail through real-time FTIR spectroscopy. A possible photolysis mechanism was expected based on further photolysis and online 1H NMR activities. With a proper molecular design, the new functionalized photoinitiators were synthesised straightforwardly and they displayed more advanced initiation abilities than their parent thioxanthone.

CAS / MDL: 147-93-3
研究领域: 材料化学 · 光化学 · 有机合成
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ACS Applied Polymer Materials · 2024 · IF 4.4

Silicone-Modified Flavonols for Organosilicon Photopolymerization

Dawei Zhao,Yimei Liu,Yating Zhang,Shitao Liu,Xiwang Zhang,Tao Wang

Organosilicon polymers exhibit excellent biocompatibility and stable chemical properties, and the use of photopolymerization in synthesizing silicone polymers is increasing due to its environmental and energy-saving benefits. However, most photoinitiators cannot be dissolved in a sufficient quantity in silicone prepolymers and have wavelengths that do not align with eco-friendly LED light sources, posing challenges in the photopolymerization of silicone prepolymers. This study focuses on the synthesis of two flavonol photoinitiators, HF-MDT and HF-MTQ, incorporating poly(sesquisiloxanes). The results for photopolymerization demonstrated that they have good compatibility with methacrylate-containing poly(sesquicarbazone) prepolymer, enabling the initiation of photopolymerization under 365 or 460 nm LEDs when combined with co-initiators triethanolamine/iodonium salt (TEOA/ONI). Films cured with HF-MDT and HF-MTQ exhibited enhanced migratory stability and hydrophilicity, making these photoinitiators suitable for various applications, such as silicone coating manufacturing, medical devices, and food packaging. Through fluorescence burst experiments, cyclic voltammetry experiments, and electron paramagnetic resonance experiments, the interaction mechanisms of flavonol photoinitiators with co-initiators were elucidated, providing insights into their photoinitiation activities under LED light sources.

研究领域: 材料科学 · 化学工程 · 生物医学工程
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TALANTA · 2017 · IF 4.162

A LED-based fiber-optic sensor integrated with lab-on-valve manifold for colorimetric determination of free chlorine in water

Yan Xiong,Jun Tan,Shenwen Fang,Chengjie Wang,Qing Wang,Jiayi Wu,Jie Chen,Ming Duan

In this work, a colorimetric methodology was developed for free chlorine determination by constructing a fiber-optic sensor (FOS) which was designed by using a small LED as light source and two silica fibers as light transmission elements. Then the FOS was integrated with the sequential injection lab-on-valve (SI-LOV) manifold to fabricate a FOS-SI-LOV system for free chlorine detection. The colorimetric determination was based on the reaction between N , N -diethyl- p -phenylenediamine (DPD) reagent and free chlorine, which would produce a chromophore showing maximum absorbance at 511 and 551   nm and detected by a micro spectrometer detector. By choosing a green LED with emission wavelength at 520   nm as light source, the chlorine concentration could be simply evaluated according to Beer's law. The developed FOS-SI-LOV system showed improved performances of wide linear range (10–400   μg   L −1 ), low detection limit (3.5   μg   L −1 , 3σ), fast analysis (6.85   s) and excellent repeatability (0.0083 RSD, n=8) for chlorine determination. The proposed FOS-SI-LOV system has been applied to on-line and real-time chlorine determination in different water samples with excellent selectivity. Furthermore, this FOS-SI-LOV methodology provided a colorimetric and fluorescence detection platform for other hazardous species monitoring in water environment based on Beer's law and Stern-Volmer relationship, respectively.

研究领域: 分析化学 · 环境科学
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PROGRESS IN ORGANIC COATINGS · 2020 · IF 4.469

Carbazolyl α-diketones as novel photoinitiators in photopolymerization under LEDs

Xiaoyu Ma,Ding Cao,Xiaotong Hu,Jun Nie,Tao Wang

Novel photoinitiators (α-DKs) bearing α-dicarbonyl groups as initiating group and aromatic groups as chromophore group were synthesized and developed as visible light type I photoinitiators with high performance for radical photopolymerization of acrylate. α-DKs exhibit good absorption at 405 nm and higher initiation efficiency compared with commercial initiator camphorquinone (CQ) under LED sources. Meanwhile, α-DKs were found to efficiently photosensitize bis (4-methylphenyl) hexafluorophosphate (ION) and initiate both free radical polymerization and cationic polymerization.

研究领域: 材料化学 · 光化学
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EUROPEAN POLYMER JOURNAL · 2022 · IF 5.546

Large-molecular-weight acyldiphenylphosphine oxides as low-mobility type I photoinitiator for radical polymerization

Yinping Wu,Jiasheng Ke,Changxiang Dai,Jiuwu Wang,Chenguang Huang,Yue Situ,Hong Huang

In recent years, the light source for photopolymerization technology is evolving from energy-hungry mercury lamps to the safer light-emitting diodes (LEDs), and it is urgent to develop new photoinitiator adapted to the photopolymerization system with LED light source. Some acyldiphenylphosphine oxide photoinitiators have been designed and developed for LED light source, but their application is severely limited in the fields of food packing, medical equipment, environmentally-friendly product etc. due to their high mobility in photocured polymers. In this study, eight acyldiphenylphosphine oxide molecules (DAPO-1 ∼ DAPO-8) were synthesized by introducing large molecular weight groups and their UV–visible absorption, photodegradation quantum yield, photopolymerization properties, mobility and solubility in monomer were determined. Thereinto, photoinitiators show lower mobility than TPO, the photoinitiator commonly used in industry, as well as good solubility in monomers and excellent photopolymerization performance. Therefore, they can serve as potential substitutes for commercial TPO, especially in the application of low-migration photocurable system.

研究领域: 材料科学 · 聚合物化学
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MICROSYSTEM TECHNOLOGIES-MICRO-AND NANOSYSTEMS-INFORMATION STORAGE AND PROCESSING SYSTEMS · 2024 · IF 1.6

Active integrated fabrication method and evaluation of polymer with microneedles LED light source integration

Zhang Xiaoning,Han Qingxin,Hu Xiaoqing,Zhang Lei,Kang Xiaoya,Li Ming,Gao Qiang,Liu Fengyi,Sun Jingyao,Zhu Jingxian,Zhuang Jian

This article proposes a new process for fabricating a polymer microneedles (MNs) patch integrated with an LED light source (LED-HEMA/MN, LH-MN) using ultraviolet (UV) curing technology. Hydroxyethyl methacrylate (HEMA) is used as the base material, with a focus on studying the active integrated fabrication process of the MNs patch. The study also investigates the morphology, size, mechanical properties, ex vivo skin penetration performance, operating temperature, and performance optimization of the LH-MN. The experimental results show that the LH-MN fabricated using the optimal process has a good appearance, high molding rate, short production cycle, and excellent mechanical properties. It can effectively penetrate the skin without the risk of thermal injury. In addition, the MNs patch (LED-HEMA/HEA-MN, LHH-MN) prepared by optimizing and modifying with hydroxyethyl acrylate (HEA) possesses good flexibility and mechanical properties. It can adapt to different shapes and locations of the affected area, greatly enhancing the practicality of the MNs.

CAS / MDL: 818-61-1
研究领域: 生物医学工程 · 材料科学 · 医学
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MICROCHEMICAL JOURNAL · 2025 · IF 5.1

LED-based photothermal device for rapid uric acid detection

Miao Ma,Qing Wang,Qianqian Su,Weizhe Liu,Hui Xia,Caixia Zhou,Mengtian Li,Fang Yang,Fujian Xu

Blood uric acid (UA) levels are closely associated with various diseases. This study presents a novel UA photothermal detection system. UA reacts with uricase to generate hydrogen peroxide, which then oxidizes 3,3′,5,5′-tetramethylbenzidine (TMB) into oxidized TMB (oxTMB) in the presence of copper ions as the catalyst. Crucially, instead of expensive laser, Light Emitting Diode (LED) was applied to offer the irradiation on oxTMB, inducing a temperature increase. The increment of temperature measured by a handheld household thermometer exhibits a linear correlation with the concentration of UA in the samples. This method demonstrates enhanced detection sensitivity and excellent anti-interference capabilities. It has been successfully applied to precisely determine UA levels in volunteer blood samples. The sensing platform achieves portable UA detection in human blood within 3 min, featuring a linear response range of 50–400 μM, a detection limit (LOD) of 14.4 μM. This work establishes a novel miniaturized LED-based photothermal (LED-PT) uric acid detection device, holding significant potential for rapid, portable UA monitoring in healthcare and clinical diagnostics.

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