Triethylamine fluorescence sensor based on L-type nanometer zeolite rare earth beta-ketone complex hybrid material and preparation method and application thereof
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A fluorescence sensor and triethylamine technology, applied in the field of fluorescence sensors, can solve the problems of expensive instruments or components, long detection time, etc., and achieve the effects of simple detection, simple preparation method and mild conditions
Inactive Publication Date: 2017-08-25
SUN YAT SEN UNIV
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However, these methods have disadvantages such as expensive instruments or components, and long detection time.
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Embodiment 1
[0033] Example 1: Synthesis of ligand β-diketone (HPPO):
[0034] in N 2 Under the effect of protection, add 3-acetylphenanthrene (0.2202g, 1mmol) into LDA lithium diisopropylamide (2M, 1ml), stir at -40°C for 3h, raise the temperature to 0°C, add methyl pentafluoropropionate Esters (130μl, 1.2mmol), stirred for 3h, quenched with water, extracted with 30ml of dichloromethane, dried over anhydrous sodium sulfate, overnight. After the filtrate obtained by filtration was spin-dried, it was recrystallized with anhydrous ether and dichloromethane to obtain yellow needle-like crystals (HPPO).
Embodiment 2
[0035] Example 2: Synthesis of ligand β-diketone (HBFPD):
[0036] in N 2 Under the effect of protection, 2-acetylfluorene (0.2083g, 1mmol) was added to LDA (2M, 1ml), stirred at -40°C for 3h, heated to 0°C, added biphenyl-4-carboxylic acid methyl ester (0.2547g , 1.2mmol), stirred for 3h, quenched with water, extracted with 30ml of dichloromethane, dried over anhydrous sodium sulfate, overnight. After the filtrate was spin-dried, it was recrystallized from anhydrous ether and dichloromethane to obtain a yellow solid (HBFPD).
Embodiment 3
[0037] Embodiment 3: Nano L-type zeolite rare earth europium β-diketone complex hybrid material Eu(HPPO) n Synthesis of @K-NZL:
[0038] Nano L-type zeolite (0.1g) K-NZL and EuCl 3 • xH 2 O ethanol solution (0.1M, 2.5 ml) was mixed, refluxed at 80°C for 24 h and then centrifuged to obtain a white powder. After drying at 50°C, Eu@K-NZL (0.1g) and β-diketone (HPPO, 0.2g) were obtained Mix and grind, heat in vacuum at 100°C for 2 h, wash with dichloromethane for 3 times, and dry to obtain light yellow powder Eu(HPPO) n @K-NZL. Among them, rare earth ions accounted for 9.90% of the total mass of the fluorescent sensor, and β-diketone ligands accounted for 3.40% of the total mass of the fluorescent sensor.
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Abstract
The invention discloses a triethylamine fluorescence sensor based on an L-type nanometer zeolite rare earth beta-ketone complex hybrid material and a preparation method and application thereof. The triethylamine fluorescence sensor is composed of L-type nanometer zeolite and a rare earth beta-ketone complex, wherein the rare earth beta-ketone complex is a rare earth complex prepared from europium and / or terbium and beta-ketone ligands, and the structure formulas of the beta-ketone ligands are shown in a formula (I), a formula (II) and a formula (III); the preparation method of the L-type nanometer zeolite rare earth beta-ketone complex hybrid material is simple, the condition is mild, the performance of the hybrid material is stable, when triethylamine and the L-type nanometer zeolite rare earth beta-ketone complex hybrid material react with each other, the changes of fluorescence intensity of a luminescent material can be caused, and triethylamine can be distinguished and detected by utilizing the changes. The sensor has very weak sensitivity to other organic volatile substances, can be applied to specific triethylamine distinguishing and mixture detection with other gas, and has great application prospects in the field of triethylamine gas detection. The formula (I), the formula (II) and the formula (III) are shown in the descriptions.
Description
technical field [0001] The invention belongs to the technical field of fluorescence sensors, and more specifically relates to a triethylamine fluorescence sensor based on a nano L-type zeolite rare earth β-diketone complex hybrid material and a preparation method and application thereof. Background technique [0002] Triethylamine is an important aliphatic amine in organic amines, and it is a colorless and transparent liquid with strong amine odor volatility. With the rapid development of industry, the usage of triethylamine is also increasing rapidly. A large amount of triethylamine enters the environment, which will not only damage the environment, but also threaten human health. Human inhalation of highly irritating triethylamine can cause pulmonary edema and even death. Therefore, it is urgent to find a simple and rapid method for detecting triethylamine in the environment. At present, the main methods for detecting triethylamine are gas chromatography and semiconduct...
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