CN105001116A - Preparation of highly sensitive 2,4-dinitrophenylhydrazine - Google Patents
Preparation of highly sensitive 2,4-dinitrophenylhydrazine Download PDFInfo
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- CN105001116A CN105001116A CN201410163895.0A CN201410163895A CN105001116A CN 105001116 A CN105001116 A CN 105001116A CN 201410163895 A CN201410163895 A CN 201410163895A CN 105001116 A CN105001116 A CN 105001116A
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- dinitrophenylhydrazine
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- necked flask
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Abstract
The invention relates to a preparation method of 2,4-dinitrophenylhydrazine, and concretely relates to a preparation method of highly sensitive 2,4-dinitrophenylhydrazine. The purpose of the invention is to solve the problems of high impurity content, low sensitivity and unable meeting of detection needs of a tiny amount of aldehyde ketone of 2,4-dinitrophenylhydrazine prepared through present 2,4-dinitrophenylhydrazine preparation methods, and high preparation cost of the present preparation methods. The method concretely comprises the following steps: adding 2,4-dinitrochlorobenzene, 1.6-1.7 times ethanol with the concentration of 95% and active carbon into a flask with three necks and with the capacity of 20L; pouring the obtained filtrate into a flask with three necks and with the capacity of 20L, and adding a hydrazine hydrate solution having a same amount to 2,4-dinitrochlorobenzene; continuously refluxing for 1-2h, and stopping refluxing when red crystals precipitate; and washing the red crystals by hot ethanol 1-3 times, and drying the washed crystals at 60-80DEG C. The preparation method can be used in the field of chemical reagents.
Description
Technical field
The present invention relates to a kind of preparation method of 2.4-dinitrophenylhydrazine, be specifically related to a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine, belong to chemical reagent field.
Background technology
2.4-dinitrophenylhydrazine is a kind of powder of red crystalline, be slightly soluble in water and ethanol, be dissolved in acid, inflammable, strong shock can be blasted, and is mainly used in explosive manufacture, the developer of spectrphotometric method for measuring aldehyde, ketone, the developer of tlc determination aldehyde, ketone, is also used as the ultraviolet derivative reagent of aldehyde and ketone, for organic synthesis and explosive manufacture.In acidic medium, carbonyl compound and 2.4-dinitrophenylhydrazine reaction, generate 2.4-dinitrophenylhydrazone, in garnet in basic solution, can be used for spectrophotometry or visual colorimetry mensuration carbonyl compound.Develop into again the mensuration reagent of carbohydrate, vitamins, carbonylic acid in recent years, its range of application is more and more wider, and demand is increasing.The synthetic method of existing conventional 2.4-dinitrophenylhydrazine is: carry out reaction by hydrazine hydrate and 2.4-dinitrochlorobenzene and prepare.But 2.4-dinitrophenylhydrazine foreign matter content prepared by this method is higher, sensitivity is low, can not meet the needs measuring micro-aldehyde ketone, and preparation cost is higher.
Summary of the invention
In view of this, main purpose of the present invention is the preparation method providing a kind of highly sensitive 2.4-dinitrophenylhydrazine, 2.4-dinitrophenylhydrazine foreign matter content prepared by existing 2.4-dinitrophenylhydrazine preparation method can be solved higher, sensitivity is low, the needs measuring micro-aldehyde ketone can not be met, and the problem that preparation cost is higher.
For achieving the above object, the technical scheme that the present invention takes is: concrete steps of the present invention are as follows:
Step one, at capacity be add 2.4-dinitrochlorobenzene in the there-necked flask of 20 liters, 1.6-1.7 concentration be doubly 95% ethanol and gac;
Step 2, heated and boiled is carried out to there-necked flask, after the solid in there-necked flask all dissolves, solution is filtered;
Step 3, the filtrate of step 3 kind poured in the there-necked flask of 20 liters, there-necked flask is connected with reflux, carries out total reflux;
Step 4, in the there-necked flask of 20 liters, add the hydrazine hydrate solution with 2.4-dinitrochlorobenzene equivalent;
Step 5, continuation backflow one to two hour, separate out red colored crystalline, stop backflow;
Step 6, make the temperature in the there-necked flask of 20 liters be down to 55 DEG C, leach crystallisate;
In step 7, use hot ethanol washing step six, crystallisate one to three time, dry under being placed in 60-80 DEG C of temperature.
Compared with prior art, the present invention has following beneficial effect: the present invention, by improving the consumption of hydrazine hydrate, improves the productive rate of 2.4-dinitrophenylhydrazine; The present invention, by changing feed rate, first quick and back slow, had both saved the time, and had not made again reaction too strong; Invention increases crystallization and generate temperature and wash temperature, more impurity is stayed in solution and washings, reduces the foreign matter content of product, improve the sensitivity of product; Productive rate of the present invention can reach 98% ~ 100%.The present invention is while the sensitivity of raising product, and meet the needs measuring micro-aldehyde ketone, the preparation cost reducing product is higher.
Embodiment
Embodiment one: described in present embodiment, a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine realizes as follows:
Step one, at capacity be add 2.4-dinitrochlorobenzene in the there-necked flask of 20 liters, 1.6-1.7 concentration be doubly 95% ethanol and gac;
Step 2, heated and boiled is carried out to there-necked flask, after the solid in there-necked flask all dissolves, solution is filtered;
Step 3, the filtrate of step 3 kind poured in the there-necked flask of 20 liters, there-necked flask is connected with reflux, carries out total reflux;
Step 4, in the there-necked flask of 20 liters, add the hydrazine hydrate solution with 2.4-dinitrochlorobenzene equivalent;
Step 5, continuation backflow one to two hour, separate out red colored crystalline, stop backflow;
Step 6, make the temperature in the there-necked flask of 20 liters be down to 55 DEG C, leach crystallisate;
In step 7, use hot ethanol washing step six, crystallisate one to three time, dry under being placed in 60-80 DEG C of temperature.
Present embodiment reaction principle is:
+2NH
2NH
2.H
2O→
+ NH
2.NH
2.HCL+H
2O。
Embodiment two: in the step 4 of a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine described in present embodiment, the concentration of hydrazine hydrate solution is 50%.Other composition and annexation identical with embodiment one.
Embodiment three: in the step 4 of a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine described in present embodiment, the Adding Way of hydrazine hydrate solution is:
Steps A, in the there-necked flasks of 20 liters, add the hydrazine hydrate solution of hydrazine hydrate solution total amount 15%;
Step B, the hydrazine hydrate solution of remainder slowly to be added in the there-necked flask of 20 liters.Other composition and annexation identical with embodiment one or two.
Embodiment four: be the concentration adding 1.6 times in the there-necked flask of 20 liters at capacity in the step one of a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine described in present embodiment be the ethanol of 95%.Other composition and annexation identical with embodiment one.
Embodiment five: with crystallisate in absolute ethanol washing step 6 twice time in the step 7 of a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine described in present embodiment, dry under being placed in 60-80 DEG C of temperature.Other composition and annexation identical with embodiment one.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., be all included within protection scope of the present invention.
Claims (5)
1. a preparation method for highly sensitive 2.4-dinitrophenylhydrazine, is characterized in that: the preparation method of described a kind of highly sensitive 2.4-dinitrophenylhydrazine realizes as follows:
Step one, at capacity be add 2.4-dinitrochlorobenzene in the there-necked flask of 20 liters, 1.6-1.7 concentration be doubly 95% ethanol and gac;
Step 2, heated and boiled is carried out to there-necked flask, after the solid in there-necked flask all dissolves, solution is filtered;
Step 3, the filtrate of step 3 kind poured in the there-necked flask of 20 liters, there-necked flask is connected with reflux, carries out total reflux;
Step 4, in the there-necked flask of 20 liters, add the hydrazine hydrate solution with 2.4-dinitrochlorobenzene equivalent;
Step 5, continuation backflow one to two hour, separate out red colored crystalline, stop backflow;
Step 6, make the temperature in the there-necked flask of 20 liters be down to 55 DEG C, leach crystallisate;
In step 7, use hot ethanol washing step six, crystallisate one to three time, dry under being placed in 60-80 DEG C of temperature.
2. the preparation method of a kind of highly sensitive 2.4-dinitrophenylhydrazine according to claim 1, is characterized in that: in step 4, the concentration of hydrazine hydrate solution is 50%.
3. a kind of preparation method of highly sensitive 2.4-dinitrophenylhydrazine according to claim 1 or 2, is characterized in that: in step 4, the Adding Way of hydrazine hydrate solution is:
Steps A, in the there-necked flasks of 20 liters, add the hydrazine hydrate solution of hydrazine hydrate solution total amount 15%;
Step B, the hydrazine hydrate solution of remainder slowly to be added in the there-necked flask of 20 liters.
4. the preparation method of a kind of highly sensitive 2.4-dinitrophenylhydrazine according to claim 1, is characterized in that: be the concentration adding 1.6 times in the there-necked flask of 20 liters at capacity in step one be the ethanol of 95%.
5. the preparation method of a kind of highly sensitive 2.4-dinitrophenylhydrazine according to claim 1, is characterized in that: with crystallisate in absolute ethanol washing step 6 twice time in step 7, dry under being placed in 60-80 DEG C of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410163895.0A CN105001116A (en) | 2014-04-23 | 2014-04-23 | Preparation of highly sensitive 2,4-dinitrophenylhydrazine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410163895.0A CN105001116A (en) | 2014-04-23 | 2014-04-23 | Preparation of highly sensitive 2,4-dinitrophenylhydrazine |
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| CN105001116A true CN105001116A (en) | 2015-10-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410163895.0A Pending CN105001116A (en) | 2014-04-23 | 2014-04-23 | Preparation of highly sensitive 2,4-dinitrophenylhydrazine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033025A (en) * | 2017-06-07 | 2017-08-11 | 李博强 | A kind of preparation method of 2,4,6 trinitrophenyl-hydrazine |
| CN107188825A (en) * | 2017-06-07 | 2017-09-22 | 李博强 | A kind of preparation method of 2,4 dinitro benzene hydrazine hydrochloride |
-
2014
- 2014-04-23 CN CN201410163895.0A patent/CN105001116A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033025A (en) * | 2017-06-07 | 2017-08-11 | 李博强 | A kind of preparation method of 2,4,6 trinitrophenyl-hydrazine |
| CN107188825A (en) * | 2017-06-07 | 2017-09-22 | 李博强 | A kind of preparation method of 2,4 dinitro benzene hydrazine hydrochloride |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20151028 |
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| WD01 | Invention patent application deemed withdrawn after publication |