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Preparation of highly sensitive 2,4-dinitrophenylhydrazine

A dinitrophenylhydrazine, high-sensitivity technology, applied in the field of chemical reagents, can solve the problems of inability to measure trace amounts of aldehydes and ketones, high preparation cost, and high impurity content, and achieves increasing crystallization temperature and washing temperature, reducing preparation cost, The effect of reducing the impurity content

Inactive Publication Date: 2015-10-28
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of this, the main purpose of the present invention is to provide a kind of preparation method of high-sensitivity 2.4-dinitrophenylhydrazine, can solve the 2.4-dinitrophenylhydrazine impurity content prepared by existing 2.4-dinitrophenylhydrazine preparation method High, low sensitivity, can not meet the needs of the determination of trace aldehydes and ketones, and the problem of high preparation cost

Method used

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Experimental program
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specific Embodiment approach 1

[0015] Specific embodiment one: the preparation method of a kind of high sensitivity 2.4-dinitrophenylhydrazine described in this embodiment is realized through the following steps:

[0016] Step 1, adding 2.4-dinitrochlorobenzene, 1.6-1.7 times the concentration of 95% ethanol and activated carbon in a three-necked flask with a capacity of 20 liters;

[0017] Step 2, heat and boil the three-necked bottle, and filter the solution after all the solids in the three-necked bottle are dissolved;

[0018] Step 3, pour the filtrate of step 3 into a 20-liter three-necked bottle, and the three-necked bottle is connected to the reflux device for full reflux;

[0019] Step 4, add the hydrazine hydrate solution equivalent to 2.4-dinitrochlorobenzene in the there-necked bottle of 20 liters;

[0020] Step 5, continue to reflux for one to two hours, and red crystals are precipitated, and the reflux is stopped;

[0021] Step 6, the temperature in the 20-liter three-neck flask is reduced to...

specific Embodiment approach 2

[0025] Specific embodiment 2: The concentration of the hydrazine hydrate solution in step 4 of the preparation method of a high-sensitivity 2.4-dinitrophenylhydrazine described in this embodiment is 50%. Other components and connections are the same as those in the first embodiment.

specific Embodiment approach 3

[0026] Specific embodiment three: the adding method of hydrazine hydrate solution in the step four of the preparation method of a kind of highly sensitive 2.4-dinitrophenylhydrazine described in this embodiment is:

[0027] Step A, add the hydrazine hydrate solution of hydrazine hydrate solution total amount 15% in the there-necked bottle of 20 liters;

[0028] Step B, slowly add the remaining hydrazine hydrate solution into a 20-liter three-necked flask. Other compositions and connections are the same as those in Embodiment 1 or 2.

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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 [0001] The invention relates to a preparation method of 2.4-dinitrophenylhydrazine, in particular to a preparation method of high-sensitivity 2.4-dinitrophenylhydrazine, belonging to the field of chemical reagents. Background technique [0002] 2.4-Dinitrophenylhydrazine is a red crystalline powder, slightly soluble in water and ethanol, soluble in acid, flammable, will explode when hit by strong impact, mainly used in the manufacture of explosives, photometric determination of aldehydes and ketones Chromogenic reagent, used for the determination of aldehydes and ketones by thin-layer chromatography, and also used as a UV derivatization reagent for aldehydes and ketones, used in organic synthesis and explosives manufacturing. In acidic medium, carbonyl compounds react with 2.4-dinitrophenylhydrazine to generate 2.4-dinitrophenylhydrazone, which is dark red in alkaline solution, and can be used for the determination of carbonyl compounds by spectrophotometry o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/22
Inventor 张贵珠贾伟青
Owner TIANJIN GUANGFU TECH DEV
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