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O-cumaric acid LEuH complex and synthesis method thereof

A synthesis method, o-coumaric acid technology, applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the problems of large error and low detection sensitivity, and achieve the effect of improving sensitivity and enhancing fluorescence performance

Inactive Publication Date: 2014-10-29
BEIJING NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, due to the low content of o-coumaric acid in flue-cured tobacco leaves, when detecting its fluorescence, there are problems of low detection sensitivity and large errors.

Method used

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  • O-cumaric acid LEuH complex and synthesis method thereof
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  • O-cumaric acid LEuH complex and synthesis method thereof

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preparation example Construction

[0038] The synthetic method of above-mentioned o-coumaric acid-LEuH complex can comprise the following steps:

[0039] 1) Synthesis of LEuH:

[0040] Eu(NO 3 ) 3 ·6H 2 O, NaNO 3 , Hexamethylenetetramine was dissolved in water to obtain an aqueous solution, in which Eu(NO 3 ) 3 ·6H 2 O, NaNO 3 , the molar ratio of hexamethylenetetramine is: 1: (10-15): (0.5-1.5); preferably Eu(NO3) 3 ·6H 2 O, NaNO 3 1. Hexamethylenetetramine is dissolved in degassed water, and degassed water refers to the water that got rid of the dissolved gas in the water, which can be obtained by boiling distilled water for 10 minutes, and the degassed water amount is preferably 60-120ml / mmolEu(NO 3 ) 3 ·6H 2 O.

[0041] N was introduced into the above aqueous solution 2 , into N 2 The time is preferably 3-10 minutes, and then the hydrothermal reaction is carried out. The preferred reaction temperature is 70-100°C; the preferred reaction time is 12-18h. After the reaction is completed, filter ...

Embodiment 1

[0052] 0.446g (1mmol) Eu(NO3) 3 ·6H 2 O, 0.846g (10mmol) NaNO 3 , 0.07g (0.5mmol) hexamethylenetetramine is dissolved in 65ml degassed water, obtains aqueous solution, this aqueous solution is transferred in the reactor and feeds N into this aqueous solution 2 3min, then hydrothermal reaction at 70°C for 18 hours. After the reaction, the obtained product was suction filtered, washed with deionized water and then suction filtered twice, and then vacuum-dried at 40° C. for 24 hours to obtain 0.196 g of white powder LEuH. 80% yield based on LEuH.

[0053] Add 0.207g (1.26mmol) of o-coumaric acid and 0.054g (1.26mmol) of NaOH into 10mL of deionized water, and ultrasonically dissolve the o-coumaric acid to obtain a clear aqueous solution of o-coumaric acid sodium salt.

[0054] Disperse 0.10 g (0.42 mmol) of LEuH in 140 ml of deionized water, mix it with the aqueous solution of o-coumaric acid sodium salt prepared above, transfer it to a reaction kettle, and conduct a hydrother...

Embodiment 2

[0056] 0.446g (1mmol) Eu(NO 3 ) 3 ·6H 2 O, 1.10g (13mmol) NaNO 3 , 0.14g (1mmol) hexamethylenetetramine is dissolved in 80ml degassed water, obtains an aqueous solution, this aqueous solution is transferred in the reactor and feeds N in this aqueous solution 2 5min, then 90°C hydrothermal reaction for 14 hours. After the reaction, the obtained product was suction filtered, washed with deionized water and then suction filtered three times, then vacuum dried at 60° C. for 20 hours to obtain 0.240 g of white powder LEuH. Based on LEuH, the yield was 98%.

[0057] Add 0.207g (1.26mmol) of o-coumaric acid and 0.081g (1.9mmol) of NaOH into 15mL of deionized water, and ultrasonically dissolve the o-coumaric acid to obtain a clear aqueous solution of o-coumaric acid sodium salt.

[0058] Disperse 0.05g (0.21mmol) of LEuH in 100ml of deionized water and mix it with the aqueous solution of o-coumaric acid sodium salt prepared above, and transfer it to a reaction kettle for hydrothe...

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Abstract

The invention discloses an O-cumaric acid LEuH complex and a synthesis method thereof. The O-cumaric acid LEuH complex is as shown in the following chemical formula: Eu(OH)2.4(C9H7O3)0.6.0.77H2O. The O-cumaric acid LEuH complex is synthesized from O-cumaric acid and a layered europium hydroxide LEuH by using an ion exchange method. Compared with an O-cumaric acid monomer, the complex is remarkably improved in fluorescence property, so that the sensitivity of fluorescence detection is improved, and the complex has the potential to be applied to detection on O-cumaric acid in flue-cured tobacco.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to an o-coumaric acid-LEuH complex and a synthesis method thereof. Background technique [0002] O-coumaric acid (trans 2-hydroxycinnamic acid) is an organic phenolic acid often present in flue-cured tobacco leaves, and its content is one of the important indicators of the quality of tobacco leaves. O-coumaric acid has certain fluorescence, therefore, the content difference of o-coumaric acid in different flue-cured tobacco leaves can be compared according to the fluorescence parameters of o-coumaric acid in flue-cured tobacco leaves, so as to determine the quality of flue-cured tobacco leaves. [0003] However, due to the low content of o-coumaric acid in flue-cured tobacco leaves, when detecting its fluorescence, there are problems of low detection sensitivity and large errors. [0004] Therefore, on the premise that the content of o-coumaric acid cannot be increased, how to incr...

Claims

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Application Information

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IPC IPC(8): C09K11/78C09K11/06G01N21/64
Inventor 马淑兰谷庆阳苏飞飞马腾
Owner BEIJING NORMAL UNIVERSITY
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