CN103787889A - Method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration - Google Patents
Method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration Download PDFInfo
- Publication number
- CN103787889A CN103787889A CN201410035073.4A CN201410035073A CN103787889A CN 103787889 A CN103787889 A CN 103787889A CN 201410035073 A CN201410035073 A CN 201410035073A CN 103787889 A CN103787889 A CN 103787889A
- Authority
- CN
- China
- Prior art keywords
- dinitrophenol
- phenol
- heating
- sulfuric acid
- preparing
- 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
Abstract
A method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration relates to the technical field of chemical industry. The method comprises the steps of firstly, putting sulfuric acid which meets the standard into a reaction kettle and quickly heating to 110 DEG C; secondarily, adding phenol into the reaction kettle and heating to 130-140 DEG C, preserving heat for 180 minutes, and then cooling to 20 DEG C; thirdly, adding nitric acid into the reaction kettle and heating to 40-50 DEG C, standing for 24 hours, then heating to 90 DEG C, and reacting for 40 minutes at the constant temperature; fourthly naturally cooling to 20 DEG C, filtering, crystalizing and drying to obtain the finished product of the 2,4-dinitrophenol, and finally packaging and warehousing the finished product of the 2,4-dinitrophenol. The method disclosed by the invention has the following beneficial effects that the preparation process for the 2,4-dinitrophenol is advanced, the price of the raw materials is low, the preparation method is convenient and simple, and easy to operate, and the purity of the 2,4-dinitrophenol is high, and the 2,4-dinitrophenol is safe and reliable.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to a kind of nitrated method of preparing 2,4-DNP of phenol sulfonation.
Background technology
2,4-DNP, outward appearance is light yellow monoclinic crystal, 113 ℃ of fusing points, relative density 1.683, is dissolved in hot water, ethanol, ether, acetone, toluene, benzene, chloroform and pyridine, is insoluble to cold water, can volatilize with water vapour, heating sublimation.After suction, can cause the symptoms such as hidrosis, collapse, granular leukopenia.Have stronger toxicity, its rare aqueous solution is colourless in the time of acidity, is yellow when alkalescence, can be used as one-color indicator, and for the preparation of dyestuff, medicine and the intermediate as organic synthesis.Still can be used for wood preservation for photographic developer indicator.Traditional 2,4-DNP composition is comparatively complicated, and preparation technology is numerous and diverse unordered.
Summary of the invention
It is a kind of environment friendly and pollution-free that technical problem to be solved by this invention is to provide, and prepares the nitrated method of preparing 2,4-DNP of simple phenol sulfonation.
Technical problem to be solved by this invention realizes by the following technical solutions:
The nitrated method of preparing 2,4-DNP of phenol sulfonation, is characterized in that: comprise following processing step,
A, choose standard compliant sulfuric acid and put into reactor and sulfuric acid be heated to 110 ℃ rapidly.
B. choose phenol and add in the sulfuric acid in step a, again temperature is added to 130-140 ℃ and constant temperature 180min.
C. the solution in step b is cooled to 20 ℃, adds nitric acid and temperature to rise to 40-50 ℃ of standing 24h to inside.
D. the mixture in step c is heated to again to 90 ℃ and isothermal reaction 40min.
E. the mixture that in steps d, reaction finishes is naturally cooled to 20 ℃, start to filter.
F. the mixture after filtering is dropped into and in exquisite still, carry out after crystallization the then dry 2,4-DNP finished product packing warehouse-in that obtains.
The invention has the beneficial effects as follows: the technique advanced person of the prepared 2,4-DNP of the present invention, cost of material is cheap, easy to prepare simple, convenient operation, the 2,4-DNP purity of preparation is high, safe and reliable.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
The nitrated method of preparing 2,4-DNP of phenol sulfonation, comprises following processing step,
A, choose standard compliant sulfuric acid and put into reactor and sulfuric acid be heated to 110 ℃ rapidly.
B. choose phenol and add in the sulfuric acid in step a, again temperature is added to 130-140 ℃ and constant temperature 180min.
C. the solution in step b is cooled to 20 ℃, adds nitric acid and temperature to rise to 40-50 ℃ of standing 24h to inside.
D. the mixture in step c is heated to again to 90 ℃ and isothermal reaction 40min.
E. the mixture that in steps d, reaction finishes is naturally cooled to 20 ℃, start to filter.
F. the mixture after filtering is dropped into and in exquisite still, carry out after crystallization the then dry 2,4-DNP finished product packing warehouse-in that obtains.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (1)
1. the nitrated method of preparing 2,4-DNP of phenol sulfonation, is characterized in that: comprise following processing step,
A, choose standard compliant sulfuric acid and put into reactor and sulfuric acid be heated to 110 ℃ rapidly.
B. choose phenol and add in the sulfuric acid in step a, again temperature is added to 130-140 ℃ and constant temperature 180min.
C. the solution in step b is cooled to 20 ℃, adds nitric acid and temperature to rise to 40-50 ℃ of standing 24h to inside.
D. the mixture in step c is heated to again to 90 ℃ and isothermal reaction 40min.
E. the mixture that in steps d, reaction finishes is naturally cooled to 20 ℃, start to filter.
F. the mixture after filtering is dropped into and in exquisite still, carry out after crystallization the then dry 2,4-DNP finished product packing warehouse-in that obtains.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410035073.4A CN103787889A (en) | 2014-01-23 | 2014-01-23 | Method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410035073.4A CN103787889A (en) | 2014-01-23 | 2014-01-23 | Method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103787889A true CN103787889A (en) | 2014-05-14 |
Family
ID=50664004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410035073.4A Pending CN103787889A (en) | 2014-01-23 | 2014-01-23 | Method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103787889A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086434A (en) * | 2014-06-10 | 2014-10-08 | 蚌埠团结日用化学有限公司 | Method for preparing 2,4-dinitrophenol from phenol by nitration |
| CN108164422A (en) * | 2017-12-28 | 2018-06-15 | 大连泰瑞海铭化工集团有限公司 | The production method of o-sec-butyl -4,6- dinitrophenol |
-
2014
- 2014-01-23 CN CN201410035073.4A patent/CN103787889A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 裴华: "2，4-二硝基苯酚的性质用途合成方法", 《百度文库》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086434A (en) * | 2014-06-10 | 2014-10-08 | 蚌埠团结日用化学有限公司 | Method for preparing 2,4-dinitrophenol from phenol by nitration |
| CN108164422A (en) * | 2017-12-28 | 2018-06-15 | 大连泰瑞海铭化工集团有限公司 | The production method of o-sec-butyl -4,6- dinitrophenol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dewar et al. | 624. New heteroaromatic compounds. Part I. 9-Aza-10-boraphenanthrene | |
| CN103787889A (en) | Method for preparing 2,4-dinitrophenol by phenol sulfonation and nitration | |
| CN104194257B (en) | A kind of fiberglass reinforced moulding compound of heat resistant type Environmental protection phenol formaldehyde resin | |
| CN106187929A (en) | The production method of metamitron | |
| CN104045565A (en) | Preparation method of 2,4-dinitrophenol | |
| CN102344478B (en) | Crystal of 17 alpha-acetoxyl group-11 beta-(4-N, N-dimethylamino phenyl)-19-norpregna-4, 9- diene-3, 20- ketone and preparation method thereof | |
| CN104086434A (en) | Method for preparing 2,4-dinitrophenol from phenol by nitration | |
| CN104230739B (en) | N, the technique of N, N-thricyclohexyl-1,3,5-benzamide is produced with trimesic acid | |
| CN102531973B (en) | Method for preparing fatty acid ester sulfonate powder | |
| CN104086448A (en) | Synthesis method of o-amino pheylmethyl ether | |
| CN104276605B (en) | A kind of preparation method of monoclinic phase molybdenum trioxide | |
| CN104447506B (en) | The preparation method of the alkyl carbazole of 2 acetyl group 9 | |
| CN108546248B (en) | Preparation method of 1, 2-dihydro-3, 6-pyridazine dione | |
| CN103980201B (en) | A kind of preparation method of the full substituted pyrazolecarboxylic containing sulfuryl | |
| CN105622408A (en) | Method for preparing bi (2-micristin) calcium urea compound | |
| CN105622679A (en) | Preparation method of edible tannic acid | |
| CN108727167B (en) | Preparation method of anoplophora chinensis gathering pheromone | |
| CN104151192A (en) | Improved method of preparation technology of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl acrylate methyl sulfate | |
| CN106946711A (en) | A kind of hexanitro Stilbene synthetic method | |
| CN103848432A (en) | Method used for synthesizing flame retardant zinc borate | |
| US3182039A (en) | Fluorinated polymers containing hydrazide groups | |
| CN104031001B (en) | Cook different foods in one pot and prepare the method for 2-[N-(2,4,5-trimethoxy-benzene methylamino) is amino]-4-ethoxycarbonyl-1,3-thiazoles | |
| CN106588785A (en) | Preparation method of acetylpyrazine | |
| US3347941A (en) | Triphenyl methane free radicals and their preparation | |
| CN104478708B (en) | One step prepares the method for salicylic acid compounds |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140514 |