CN101712811A - Purifying method of laser dye cumarin-4 - Google Patents
Purifying method of laser dye cumarin-4 Download PDFInfo
- Publication number
- CN101712811A CN101712811A CN 200810152007 CN200810152007A CN101712811A CN 101712811 A CN101712811 A CN 101712811A CN 200810152007 CN200810152007 CN 200810152007 CN 200810152007 A CN200810152007 A CN 200810152007A CN 101712811 A CN101712811 A CN 101712811A
- Authority
- CN
- China
- Prior art keywords
- cumarin
- laser dye
- laser
- dye
- light gray
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Lasers (AREA)
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
The invention belongs to the laser dyes field, especially a kind of purification process of laser dye cumarin-4.
Background technology
Along with developing rapidly of laser spectroscopy and laser chemistry, in the microcosmic course research work of separation of isotopes, directed synthetic chemistry reaction, need tunable dye lasers to be implemented on any wave band of near ultraviolet, visible light and infrared spectral region and carry out laser radiation.For obtaining high efficiency tunable laser and high-resolution laser spectrum, except that utilizing physical optics knowledge to improve the optical system, be a kind of letter and the easy method of row by means of the various laser dyess that can produce different laser spectrums.
Laser dye cumarin-4 molecular formula: C
10H
8O
3, the 7-hydroxy-4-methylcoumarin, shown in (I), be a kind of
Ideal laser dyes comparatively in the wave band,
It has high-conversion rate, than the characteristics of wide tunable range.
The preparation method who is now adopted is with Resorcinol and the thick product of methyl aceto acetate reaction synthetic laser dyestuff coumarin-4, will be met the laser dye cumarin-4 of purity requirement behind the thick product process of the synthetic laser dye cumarin-4 purifying then.
Because the defective that purifying process exists, the purity of the laser dye cumarin-4 of feasible preparation is lower, and the dyestuff life-span in use is shorter, and economy is relatively poor.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and make that laser dye cumarin-4 purity is higher, the purification process of the laser dye cumarin-4 of long service life and better economy.
The utility model solves its technical problem and is achieved through the following technical solutions:
A kind of purification process of laser dye cumarin-4 is characterized in that: the step of purification process comprises:
(1). the thick product of laser dye cumarin-4 is dissolved in concentration under 30～40 ℃ temperature condition be in 5% the aqueous sodium hydroxide solution, then solution is cooled to room temperature, and filtrate filtered is standby;
Adding the dilute sulphuric acid adjust pH under (2) 0～-5 ℃ the temperature condition in above-mentioned filtrate is 6, and the throw out that leaches obtains the light gray laser dye cumarin-4 through washing, suction filtration, oven dry;
(3). the light gray laser dye cumarin-4 is added in 95% ethanol, and reflux to light gray laser dye cumarin-4 all dissolves, and adds the gac reflux decolour then;
(4). the solution filtering gac after the decolouring, filtrate is left standstill in cooling bath, the crystallization of separating out after filtration, drying, obtain white laser dyestuff coumarin-4 crystal;
(5). white laser dyestuff coumarin-4 crystal through 2～4 recrystallizations, is promptly finished the purifying of laser dye cumarin-4.
And the temperature of oven dry is 80 ℃～120 ℃ in the described step (2).
And the drying temperature in the described step (4) is 60 ℃～80 ℃, and pressure is 500mmHg～700mmHg.
Advantage of the present utility model and beneficial effect are:
The present invention is by carrying out alkali cleaning to the thick product of laser dye cumarin-4, repeatedly after the art breading that recrystallization and gac fade, can effectively remove the impurity that is contained in the thick product of laser dye cumarin-4, improve the purity of laser dye cumarin-4 effectively, prolong its life-span in use, significantly improve the economy of laser dye cumarin-4 preparation.
Embodiment
The utility model is described in further detail below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection domain of the present utility model with this.
Embodiment 1:
0.1 molar Resorcinol is dissolved in the 0.1 molar new distillatory methyl aceto acetate makes solution, this solution under agitation is added drop-wise in the 100ml vitriol oil that is cooled to 0 ℃ in the cryosel bath, temperature of reaction is controlled at below 10 ℃, dropwises in 2 hours; Continue to stir half an hour, will reflect that subsequently mixture is injected in the 1000g mixture of ice and water, product is particulate state and separates out filtering precipitate at this moment, with
3 * 5mlThe water coolant washing precipitate, the rearmounted oven drying of suction filtration promptly gets the crude product of laser dye cumarin-4, then purifying:
(1). the thick product of laser dye cumarin-4 is dissolved in concentration under 30 temperature condition be in 5% the aqueous sodium hydroxide solution, then solution is cooled to room temperature, and filtrate filtered is standby;
(2) adding the dilute sulphuric acid adjust pH under the temperature condition of .0～-5 ℃ in above-mentioned filtrate is 6, and the throw out that leaches obtains the light gray laser dye cumarin-4 through washing, suction filtration, oven dry;
(3). the light gray laser dye cumarin-4 is added in 95% ethanol, and reflux to light gray laser dye cumarin-4 all dissolves, and adds the gac reflux decolour then;
(4). the solution filtering gac after the decolouring, filtrate is left standstill in cooling bath, the crystallization of separating out after filtration, drying, obtain white laser dyestuff coumarin-4 crystal;
(5). white laser dyestuff coumarin-4 crystal through 2 recrystallizations, is promptly finished the purifying of laser dye cumarin-4.
Embodiment 2:
The preparation of the crude product of laser dye cumarin-4 is with embodiment 1, and its purification step is:
(1). the thick product of laser dye cumarin-4 is dissolved in concentration under 40 ℃ temperature condition be in 5% the aqueous sodium hydroxide solution, then solution is cooled to room temperature, and filtrate filtered is standby;
(2) adding the dilute sulphuric acid adjust pH under the temperature condition of .0～-5 ℃ in above-mentioned filtrate is 6, and the throw out that leaches obtains the light gray laser dye cumarin-4 through washing, suction filtration, oven dry;
(3). the light gray laser dye cumarin-4 is added in 95% ethanol, and reflux to light gray laser dye cumarin-4 all dissolves, and adds the gac reflux decolour then;
(4). the solution filtering gac after the decolouring, filtrate is left standstill in cooling bath, the crystallization of separating out after filtration, drying, obtain white laser dyestuff coumarin-4 crystal;
(5). white laser dyestuff coumarin-4 crystal through 4 recrystallizations, is promptly finished the purifying of laser dye cumarin-4.
Claims (3)
1. the purification process of a laser dye cumarin-4, it is characterized in that: the step of purification process comprises:
(1). the thick product of laser dye cumarin-4 is dissolved in concentration under 30～40 ℃ temperature condition be in 5% the aqueous sodium hydroxide solution, then solution is cooled to room temperature, and filtrate filtered is standby;
Adding the dilute sulphuric acid adjust pH under (2) 0～-5 ℃ the temperature condition in above-mentioned filtrate is 6, and the throw out that leaches obtains the light gray laser dye cumarin-4 through washing, suction filtration, oven dry;
(3). the light gray laser dye cumarin-4 is added in 95% ethanol, and reflux to light gray laser dye cumarin-4 all dissolves, and adds the gac reflux decolour then;
(4). the solution filtering gac after the decolouring, filtrate is left standstill in cooling bath, the crystallization of separating out after filtration, drying, obtain white laser dyestuff coumarin-4 crystal;
(5). white laser dyestuff coumarin-4 crystal through 2～4 recrystallizations, is promptly finished the purifying of laser dye cumarin-4.
2. the preparation method of laser dye cumarin-4 according to claim 1 is characterized in that: the temperature of oven dry is 80 ℃～120 ℃ in the described step (2).
3. the preparation method of laser dye cumarin-4 according to claim 1, it is characterized in that: the drying temperature in the described step (4) is 60 ℃～80 ℃, and pressure is 500mmHg～700mmHg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810152007 CN101712811A (en) | 2008-10-06 | 2008-10-06 | Purifying method of laser dye cumarin-4 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810152007 CN101712811A (en) | 2008-10-06 | 2008-10-06 | Purifying method of laser dye cumarin-4 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101712811A true CN101712811A (en) | 2010-05-26 |
Family
ID=42416833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200810152007 Pending CN101712811A (en) | 2008-10-06 | 2008-10-06 | Purifying method of laser dye cumarin-4 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101712811A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955490A (en) * | 2010-09-07 | 2011-01-26 | 浙江大学 | Method purifying angelica dahuricae |
| CN103013178A (en) * | 2012-12-27 | 2013-04-03 | 中国科学院上海硅酸盐研究所 | Method for purifying ruthenium complex crude product through recrystallization method |
| CN103073923A (en) * | 2012-12-27 | 2013-05-01 | 中国科学院上海硅酸盐研究所 | Purification method for ruthenium complex photosensitive dye raw product and ruthenium complex photosensitive dye product |
| CN103146226A (en) * | 2012-12-27 | 2013-06-12 | 中国科学院上海硅酸盐研究所 | Ruthenium complex dye crude product purification method with column chromatography |
| CN103373976A (en) * | 2013-07-25 | 2013-10-30 | 兰亚朝 | Refining method of armillarisin |
| CN116987401A (en) * | 2022-04-25 | 2023-11-03 | 中国科学院化学研究所 | Organic single crystal dye laser, and preparation method and application thereof |
-
2008
- 2008-10-06 CN CN 200810152007 patent/CN101712811A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955490A (en) * | 2010-09-07 | 2011-01-26 | 浙江大学 | Method purifying angelica dahuricae |
| CN103013178A (en) * | 2012-12-27 | 2013-04-03 | 中国科学院上海硅酸盐研究所 | Method for purifying ruthenium complex crude product through recrystallization method |
| CN103073923A (en) * | 2012-12-27 | 2013-05-01 | 中国科学院上海硅酸盐研究所 | Purification method for ruthenium complex photosensitive dye raw product and ruthenium complex photosensitive dye product |
| CN103146226A (en) * | 2012-12-27 | 2013-06-12 | 中国科学院上海硅酸盐研究所 | Ruthenium complex dye crude product purification method with column chromatography |
| CN103013178B (en) * | 2012-12-27 | 2014-07-16 | 中国科学院上海硅酸盐研究所 | Method for purifying ruthenium complex crude product through recrystallization method |
| CN103146226B (en) * | 2012-12-27 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Ruthenium complex dye crude product purification method with column chromatography |
| CN103373976A (en) * | 2013-07-25 | 2013-10-30 | 兰亚朝 | Refining method of armillarisin |
| CN116987401A (en) * | 2022-04-25 | 2023-11-03 | 中国科学院化学研究所 | Organic single crystal dye laser, and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101712811A (en) | Purifying method of laser dye cumarin-4 | |
| CN102911036A (en) | Method for obtaining high pure dicarboxylic acid | |
| CN104119243B (en) | A kind of energy-saving clean production method of iminodiethanoic acid | |
| CN101717365B (en) | Method for purification of torasemide and preparation of big crystal form | |
| CN103342671B (en) | A kind of method utilizing acetylizad saponification liquor to prepare L-Methionine | |
| CN101648878A (en) | Preparation method of dimethyldiallylammonium chloride with low salt | |
| CN101962367B (en) | Method for purifying bendamustine hydrochloride | |
| CN108822169A (en) | The heavy aurantiamarin that alcohol extracting prepares the method for crystallising of heavy aurantiamarin and is prepared | |
| CN102304077A (en) | Method for purifying tryptophan | |
| CN102153560A (en) | Rectification method of allopurinol | |
| JP5760089B2 (en) | Preparation of 5-sulfoisophthalic acid monolithium salt with low sulfuric acid ester concentration using acetic acid washing | |
| CN101723925B (en) | Preparation method of 7-hydroxy-4-methylcoumarin | |
| CN103274432B (en) | A kind of method of hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization | |
| CN102690312A (en) | Purification method for lanolin cholesterol | |
| CN101712810A (en) | Preparation method of laser dye 7-diethylamino-4-methylcoumarin | |
| CN102627643A (en) | Refining method for ganciclovir | |
| CN107488129A (en) | A kind of method that L valines are purified in the valine compound from L | |
| CN105601687A (en) | Refinement method of erythromycin thiocyanate | |
| CN101712666A (en) | Preparation method of laser dye 7-amino-4-methylcoumarin | |
| CN101955415B (en) | Method for preparing 2-hydroxyl biphenyl compound | |
| CN102936213A (en) | Clean preparation method of 1, 8-dinitro-3, 6-naphthalenedisulfonic acid | |
| CN109678858B (en) | Preparation method of folic acid | |
| CN102731352B (en) | Preparation method of 4-methylthio benzaldehyde | |
| WO2016078584A1 (en) | Emtricitabine purification method | |
| CN109694317B (en) | Process for producing high-purity glycolic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100526 |