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Solventhermal synthesis method for L-tartaric acid rare earth complexes

A rare earth complex, tartaric acid technology, applied in the preparation of organic compounds, chemical instruments and methods, carboxylate preparation and other directions, can solve the problem that the rare earth complex of tartrate has not been reported in the literature, etc., and achieves convenient operation, concise process flow, The effect of good thermal stability

Inactive Publication Date: 2010-12-22
ZHEJIANG NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Some synthetic methods of tartrate rare earth complexes have been reported in the literature at present, but the tartrate rare earth complexes synthesized by solvothermal have not been reported in the literature

Method used

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  • Solventhermal synthesis method for L-tartaric acid rare earth complexes
  • Solventhermal synthesis method for L-tartaric acid rare earth complexes
  • Solventhermal synthesis method for L-tartaric acid rare earth complexes

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Experimental program
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Effect test

Embodiment 1

[0038] Put 0.3g of cerium oxide and 0.3g of L-tartaric acid into a 20ml reaction kettle, add 2ml of ethanol, and mix evenly with 16ml of water.

[0039] Crystallize at a constant temperature of 140°C for 3 days and then cool to room temperature at a rate of 5°C per hour to obtain millimeter-sized cerium L-tartrate crystals. The molecular formula of the synthesized product L-cerium tartrate is: [Ce 2 (L-TAR) 3 (H 2 O) 4 ]·H 2 O, the space group is P2(1)2(1)2(1), and the unit cell parameter is a=7.9273(3) b=15.5871(6) c=17.5573(6) α=β=γ=90°, V=2169.44(14) Z=4, Dc=2.494g / cm 3 , which has a structure like figure 1 , figure 2 As shown, under the excitation of excitation light with a wavelength of 250nm, fluorescence with a wavelength of 355nm is emitted.

Embodiment 2

[0041] Put 0.3g of dysprosium oxide and 0.3g of L-tartaric acid into a 20ml reaction kettle, add 2ml of ethanol and 16ml of water and mix evenly. Crystallize at a constant temperature of 140°C for 3 days and then cool to room temperature at a rate of 5°C per hour to obtain millimeter-sized L-dysprosium tartrate complex crystals. The molecular formula of the synthesized product L-dysprosium tartrate is: [Dy 2 (L-TAR) 3 (H 2 O) 2 ]·3H 2 O, the space group is P1, and the unit cell parameter is a=5.9841(2) b=7.3983(2) c=13.2347(5) α=102.7500(10)°, β=101.669(2)°, γ=90.682(2)°, V=558.69(3) Z=1, Dc=2.554g / cm 3 , which has a structure like image 3 , Figure 4 As shown, under the excitation of the excitation light with the wavelength of 265nm, the fluorescence with the wavelength of 480nm can be emitted.

Embodiment 3

[0043] Put 0.3g of europium oxide and 0.3g of L-tartaric acid into a 20ml reaction kettle, add 2ml of ethanol and 16ml of water and mix evenly. Crystallize at a constant temperature of 140°C for 3 days and then cool down to room temperature at a rate of 5°C per hour to obtain millimeter-sized europium-tartrate complex crystals. In the method for solvothermally synthesizing chiral microporous fluorescent material L-europium tartrate of the present invention, L-europium tartrate, it is characterized in that, the molecular formula of the product L-europium tartrate synthesized is: [Eu 2 (L-TAR) 3 (H 2 O) 2 ]·3H 2 O, the space group is P1, and the unit cell parameter is a=6.0211(1) b=7.4575(1) c=13.2224(2) α=102.666(1)°, β=101.384(1)°, γ=90.894(1)°, V=566.795(15) Z=1, Dc=2.456g / cm3 , which has a structure like Figure 5 , Figure 6 As shown, under the excitation of the excitation light with the wavelength of 260mm, the fluorescence with the wavelength of 560nm can be ...

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Abstract

The invention provides a solventhermal synthesis method for L-tartaric acid rare earth complexes, which belongs to the field of synthesis of chiral compounds. The method has the advantages of controlling the particle sizes and shapes of products by changing the proportion of raw materials, crystallization temperature and temperature reduction rates, along with simple process flow and convenient operation. The synthesized L-tartaric acid rare earth complexes have high thermal stability, keep stable under alkaline condition and can be used for photoactivation materials or chiral resolving agents.

Description

technical field [0001] The invention relates to a synthesis method of a chiral material L-tartrate rare earth complex. It belongs to the field of synthesis of chiral compounds. Background technique [0002] Organometallic complexes have abundant and tunable crystal structures, and the synthesis and study of organometallic complexes is an active field. Tartaric acid, also known as 2,3-dihydroxysuccinic acid, is a simple and common α-hydroxy diacid, widely used in chemical and food industries; it has two mutually symmetrical chiral carbon , has three optical isomers, namely: D-tartaric acid (L-tartaric acid), L-tartaric acid (L-tartaric acid), meso-tartaric acid (meso-tartaric acid). Tartaric acid and its derivatives are not only commonly used chiral synthesis raw materials and chiral resolution agents, but also added to food as antioxidants. Some tartrates have important physical properties such as piezoelectricity and ferroelectricity and can be used in the electronics in...

Claims

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Application Information

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IPC IPC(8): C07C59/255C07C51/347
Inventor 吕耀康王晓娟陈静苏虹冯云龙
Owner ZHEJIANG NORMAL UNIVERSITY
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