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3-hydroxy-2-naphthoic acid/1-perfluorooctane sulfonate/LYH complex and synthetic method thereof

A synthesis method and octanesulfonic acid technology are applied in the field of 3-hydroxy-2-naphthoic acid/1-octanesulfonic acid/LYH complex and its synthesis, and can solve the problem of fluorescence of 3-hydroxy-2-naphthoic acid sodium salt Low emission intensity, etc.

Inactive Publication Date: 2017-03-15
BEIJING NORMAL UNIVERSITY +1
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  • Claims
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Problems solved by technology

[0005] The embodiment of the present invention discloses a 3-hydroxy-2-naphthoic acid / 1-octanesulfonic acid / LYH complex and its synthesis method, which is used to solve the problem of low fluorescence emission intensity of 3-hydroxy-2-naphthoic acid sodium salt The problem

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  • 3-hydroxy-2-naphthoic acid/1-perfluorooctane sulfonate/LYH complex and synthetic method thereof
  • 3-hydroxy-2-naphthoic acid/1-perfluorooctane sulfonate/LYH complex and synthetic method thereof
  • 3-hydroxy-2-naphthoic acid/1-perfluorooctane sulfonate/LYH complex and synthetic method thereof

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preparation example Construction

[0033] The present invention also provides a synthesis method of the above-mentioned complex, which may include the following steps:

[0034] a) With sodium hydroxide or potassium hydroxide as alkaline reagent, 1-octane sodium sulfonate, alkaline reagent and 3-hydroxyl-2-naphthoic acid are dissolved in water to obtain a mixed solution, wherein, 3-hydroxyl-2- The molar ratio of naphthoic acid and alkaline reagent is 1: (1-2); the molar ratio of 3-hydroxy-2-naphthoic acid and 1-octane sodium sulfonate is 1: (3-5);

[0035] Since the LYH layer is positively charged, there are exchangeable anions between the layers, which are easy to combine with anionic compounds. Therefore, it is necessary to deprotonate 3-hydroxy-2-naphthoic acid to form an anionic compound so that it can be inserted into the LYH layer between. Specifically, sodium hydroxide or potassium hydroxide can be used as an alkaline reagent to react with 3-hydroxyl-2-naphthoic acid, thereby deprotonating 3-hydroxyl-2-n...

Embodiment 1

[0042] Example 1NO 3 Synthesis and structure characterization of -LYH

[0043] Synthesized by homogeneous precipitation method, specifically as follows: 0.3383g (1mmol) Y(NO 3 ) 3 ·6H 2 O, 1.10g (13mmol) NaNO 3 , 0.14g (1mmol) hexamethylenetetramine (HMT) was dissolved in 80mL exhaust water, transferred to the reactor and passed N 2 5 minutes, then hydrothermal reaction at 90°C for 12 hours; after the reaction, the product obtained was filtered with suction, washed with deionized water and then filtered with suction, repeated 3 times, and dried in vacuum for 24 hours to obtain white powder NO 3 -LYH 0.177g. With Y(NO 3 ) 3 ·6H 2 Based on O, the yield was 96.2%.

[0044] The elemental analyzer (model: Vario EL) produced by German Elementar Company was adopted to measure the NO synthesized in the embodiment of the present invention 1. 3 -C, H, N content of LYH; Adopt the plasma inductively coupled atomic emission spectrometer (ICP) (model: SPECTROARCOSEOP) that German ...

Embodiment 2

[0048] Synthesis and structural characterization of embodiment 2 complex

[0049] 0.0607g (0.3225mmol) of 3-hydroxy-2-naphthoic acid, 0.0129g (0.3225mmol) of sodium hydroxide and 0.2267g (0.9675mmol) of sodium 1-octanesulfonate were added to 8ml of deionized water, Ultrasound dissolves 3-hydroxy-2-naphthoic acid, sodium hydroxide and sodium 1-octanesulfonate to obtain a mixed solution containing sodium 3-hydroxy-2-naphthoate and sodium 1-octanesulfonate;

[0050] 0.07912g (0.43mmol) of NO 3 -LYH was dispersed in 130ml of deionized water, added to the mixed solution, mixed evenly, transferred to a reaction kettle, and hydrothermally reacted at 70°C for 24 hours. After the reaction, filter under reduced pressure, then wash the product with deionized water, repeat 3 times, and then dry it in vacuum at 40°C for 24 hours to obtain 3-hydroxy-2-naphthoic acid / 1-octanesulfonic acid / LYH complex 0.1011g, with NO 3 -LYH as the benchmark, the yield was 91.4%.

[0051] Elemental analy...

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Abstract

The embodiment of the invention discloses a 3-hydroxy-2-naphthoic acid / 1-perfluorooctane sulfonate / LYH complex and a synthetic method thereof. The 3-hydroxy-2-naphthoic acid / 1-perfluorooctane sulfonate / LYH complex has the following chemical formula: Y(OH)2.5(Cl1H7O3)xC8H17O3S)y.zH2O, wherein x is equal to 0.07 to 0.13, y is equal to 0.36 to 0.37, and z is equal to 1 to 2. The synthetic method comprises the following steps: combining NO3-LYH with deprotonated 3-hydroxy-2-naphthoic acid (namely 3-hydroxy-2-naphthoate ion) and 1-octanesulfonate ion, so as to obtain the 3-hydroxy-2-naphthoic acid / 1-perfluorooctane sulfonate / LYH complex. The fluorescence emission intensity of the complex is obviously higher than that of 3-hydroxy-2-naphthoic acid sodium salt, so that the detection limit in the process of detecting 3-hydroxy-2-naphthoic acid by adopting fluorescent spectrometry can be reduced.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a 3-hydroxy-2-naphthoic acid / 1-octanesulfonic acid / LYH complex and a synthesis method thereof. Background technique [0002] 3-Hydroxy-2-naphthoic acid (structural formula is ) is an important intermediate of dyes and organic pigments, widely used in the printing and dyeing industry and other fields, such as for the synthesis of naphthol AS and other naphthols. In the process of producing dyes and organic pigments with 3-hydroxy-2-naphthoic acid as an intermediate, industrial wastewater containing 3-hydroxy-2-naphthoic acid will be produced. In order to prevent 3-hydroxy-2-naphthalene in industrial wastewater Formic acid pollutes the environment and needs to be recycled, degraded and other harmless treatments. Before treatment, it is necessary to detect the content of 3-hydroxy-2-naphthoic acid in the wastewater. [0003] Since the sodium salt of 3-hydroxy-2-naphthoic acid ha...

Claims

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Application Information

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IPC IPC(8): C09K11/06C09K11/78
CPCC09K11/06C09K11/7701C09K2211/1011
Inventor 马淑兰苏飞飞谢林霞李新新
Owner BEIJING NORMAL UNIVERSITY
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