Purifying method of laser dye cumarin-4

A technology of laser dye and purification method, which is applied in the field of purification of laser dye coumarin-4, which can solve the problems of poor economy, low purity of laser dye coumarin-4, and short dye life, so as to prolong life and improve purity , Improve the effect of economy

Inactive Publication Date: 2010-05-26
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] Due to the defects in the purification process, the purity of the prepared ...

Method used

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  • Purifying method of laser dye cumarin-4

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Embodiment 1

[0022] 0.1 mol of resorcinol was dissolved in 0.1 mol of newly distilled ethyl acetoacetate to make a solution, and this solution was added dropwise to 100ml of concentrated sulfuric acid cooled to 0°C in an ice-salt bath with stirring, The reaction temperature is controlled below 10°C, and the dropwise addition is completed in 2 hours; continue to stir for half an hour, and then inject the reaction mixture into a 1000g ice-water mixture. 3×5ml Wash the precipitate with cooling water, filter it with suction and dry it in an oven to obtain the crude product of laser dye coumarin-4, and then purify:

[0023] (1). The laser dye coumarin-4 crude product is dissolved in a 5% sodium hydroxide aqueous solution at a temperature of 30°C, then the solution is cooled to room temperature, and the filtered filtrate is used for subsequent use;

[0024] (2). Adding dilute sulfuric acid to the filtrate at a temperature of 0 to -5°C to adjust the pH to 6, and washing, suction filtering, and dr...

Embodiment 2

[0029] The preparation of the crude product of laser dye coumarin-4 is the same as embodiment 1, and its purification steps are:

[0030] (1). The laser dye coumarin-4 crude product is dissolved in a 5% sodium hydroxide aqueous solution at a temperature of 40° C., then the solution is cooled to room temperature, and the filtered filtrate is set aside;

[0031] (2). Adding dilute sulfuric acid to the filtrate at a temperature of 0 to -5°C to adjust the pH to 6, and washing, suction filtering, and drying the filtered precipitate to obtain the light gray laser dye coumarin-4;

[0032] (3). Add the light gray laser dye coumarin-4 to 95% ethanol, heat and reflux until the light gray laser dye coumarin-4 is completely dissolved, and then add activated carbon to reflux for decolorization;

[0033] (4). Activated carbon is filtered out of the decolorized solution, the filtrate is left standing in a cold water bath, and the precipitated crystals are filtered and dried to obtain white l...

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Abstract

The invention belongs to the field of laser dye, particularly to a purifying method of laser dye cumarin-4, which comprises the following steps of: 1. washing a crude product of the laser dye cumarin-4 with a sodium hydroxide aqueous solution; 2. adding dilute sulphuric acid into the alkali laser dye cumarin-4 and processing to obtain light gray laser dye cumarin-4; 3. completely dissolving the product in ethanol, and discoloring with active carbon; 4. crystallizing the ethanol solution, and drying to obtain white laser dye cumarin-4; and 5. recrystallizing the product to finish the purifying process. After conducting alkali washing, repeated recrystallization and active carbon discoloring on the crude product of the laser dye cumarin-4, the impurities contained in the crude product of the laser dye cumarin-4 can be effectively removed, the purity of the laser dye cumarin-4 is effectively improved, the life of the laser dye cumarin-4 in use is prolonged, and the economic performance for preparing the laser dye cumarin-4 is markedly improved.

Description

technical field [0001] The invention belongs to the field of laser dyes, in particular to a method for purifying laser dye coumarin-4. Background technique [0002] With the rapid development of laser spectroscopy and laser chemistry, tunable dye lasers are needed to achieve laser radiation in any band in the near-ultraviolet, visible and infrared spectral regions in the study of isotope separation and directional synthesis chemical reactions. . In order to obtain high-efficiency tunable lasers and high-resolution laser spectra, in addition to using the knowledge of physical optics to improve the optical system, it is a simple and easy method to use various laser dyes that can produce different laser spectra. [0003] Molecular formula of laser dye coumarin-4: C 10 h 8 o 3 , 7-hydroxy-4-methylcoumarin, as shown in formula (I), is a kind of Ideal laser dyes in the wavelength band, [0004] [0005] It has the characteristics of high conversion rate and wide tuning r...

Claims

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Application Information

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IPC IPC(8): C09B57/02C09B67/54
Inventor 张淑珍
Owner TIANJIN CHEM REAGENT RES INST
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