CN105777550B - The method that one kind being continuously synthesizing to 2,4- dinitroanisol - Google Patents
The method that one kind being continuously synthesizing to 2,4- dinitroanisol Download PDFInfo
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- CN105777550B CN105777550B CN201610317074.7A CN201610317074A CN105777550B CN 105777550 B CN105777550 B CN 105777550B CN 201610317074 A CN201610317074 A CN 201610317074A CN 105777550 B CN105777550 B CN 105777550B
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- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
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Abstract
The invention discloses one kind to be continuously synthesizing to 2, the method of 4- dinitroanisol, it is related to chemical raw material synthesis field, it mainly include that five processes are packed in synthesis, Methanol Recovery, washing, drying and film-making, the present invention uses continuous synthetic method, and solvent high-efficiency recycling is polluted small, at low cost, process safety is reliable, steady.90% or more total yield of products, 99.2% or more purity.
Description
Technical field
The present invention relates to chemical raw material synthesis fields, and in particular to one kind is continuously synthesizing to the side of 2,4- dinitroanisol
Method.
Background technique
2,4- dinitroanisols (DNAN) are a kind of castexplosive carriers of function admirable reported recently.Molecular formula is
C7H6N3O5, density 1.341g/cm3, a kind of fulvescent are slightly soluble in water, are dissolved in most of organic to light yellow crystalline solid
Solvent, including methanol, ethyl alcohol, there are also ether.
2015, Zhejiang Dibang Chemical Co., Ltd. declared and authorizes " a conjunction for one kind 2,4- dinitroanisol
At technique " invention patent mandate, Patent No. CN201310325839.8.The 2,4- dinitroanisol mentioned in the patent
Synthetic method is composite inorganic alkali soluble to be obtained methanol lye in methanol, then carbinol base drop is added in CDB and synthesize instead
It answers, reaction solution decrease temperature crystalline is filtered, washed to obtain product dna N.The patent of invention is a kind of method for being interrupted synthetic DNA N.
Currently, domestic in relation to there are two types of DNAN industrial synthetic methods.The first is to be mixed using chlorobenzene as raw material with nitre sulphur
Acid nitrifies and 1- chlorine 2,4-dinitrochlorobenzene (CDB) intermediate is made at 40 DEG C.CDB after product purification processes with methanol solution
Alkali, which reacts, is made the reaction solution containing DNAN；Be for second using CDB as raw material, in methanol solution, by methanol solution aqueous slkali into
DNAN reaction solution is made in row nucleophilic displacement of fluorine.Two methods are interruption synthetic method, and reaction solution containing DNAN obtained passes through solid-liquid
After separation, the liquid phase of the alcohol and water containing first carries out Methanol Recovery processing, and the DNAN of solid phase and a small amount of impurity can be by continuous washings
Obtain product dna N.The above-mentioned interruption production method that the producer of domestic production DNAN is all made of, the production of the product are not yet realized
Serialization.
Summary of the invention
It can not continuous caused high cost, week it is an object of the invention to solve 2,4- dinitroanisol (DNAN) product
The problems such as phase is long, wastewater flow rate is larger provides a kind of 2,4- dinitro continuous, synthesis cycle is short, production cost is low, wastewater flow rate is small
Base methyl phenyl ethers anisole (DNAN) industrial preparative method.
To achieve the goals above, the technical scheme adopted by the invention is as follows: provided one kind is continuously synthesizing to 2,4- bis-
The method of Nitroanisole, including following processing steps:
(1) 2,4-dinitrochlorobenzene continuously enters synthesis reactor with methanol liquid alkaline mixed liquor by a certain percentage and reacts synthesizing liquid
2,4- dinitroanisol, reaction solution carries lifting system by synthesis reactor and continuously enters aging machine and further synthesize；
(2) reaction solution promotes bucket by aging machine and continuously enters in evaporator, and a large amount of first alcohol and water continuous evaporation is continuous
Into in methanol rectifying tower, the methanol of recoverable, rectifying column and evaporator atmospheric operation are formed by rectifying；Water and 2,4-
Dinitroanisol and sodium chloride then continuously enter in rinsing maching from the evaporator other end；
(3) hot water are carried out by three concatenated washing kettles continuously to wash, mode of washing is countercurrent washing, washes into
Enter wastewater disposal basin；
(4) after the moisture in drying machine heated-air drying control product, product is continuously entered in pelleter；
(5) sheet 2,4- dinitroanisol are formed, product continuously enters hopper, automatic weighing, packaging.
Preferably, step (1) chinese raw materials feeds intake situation are as follows: 2,4-dinitrochlorobenzene: liquid alkaline: methanol quality ratio is
1:(0.65~0.72): (5~8), wherein the mass fraction of liquid alkaline is 30%.
Preferably, synthesis reactor in the step (1), aging machine reaction temperature be 62~67 DEG C, pressure is normal pressure.
Preferably, evaporator in the step (2), the pressure in rectifying column are normal pressure.
Preferably, the temperature of hot wash-water is 95~98 DEG C in washing process in the step (3), and slurry amount is 2,
2~4 times of 4- dinitroanisol volume.
Preferably, it is 1# washing kettle that countercurrent washing regime, which is 2,4- dinitroanisol flow direction of material, in the step (3)
→ 2# washing kettle → 3# washing kettle, hot wash-water flow direction are then 3# washing kettle → 2# washing kettle → 1# washing kettle.
Preferably, heated-air drying temperature is 110~120 DEG C in the step (4).
Using technical solution of the present invention, using continuous synthetic method, small, at low cost, mistake is polluted in solvent high-efficiency recycling
Journey is safe and reliable, steady.90% or more total yield of products, 99.2% or more purity.
Detailed description of the invention:
Fig. 1 is that this is continuously synthesizing to DNAN general flow chart.
Specific embodiment
2,4- dinitro is continuously synthesizing to below by specific embodiment and in conjunction with one kind in the attached drawing narration present invention
The method of methyl phenyl ethers anisole (DNAN).Unless stated otherwise, technological means used in the present invention is that those skilled in the art institute is public
The method known.In addition, embodiment is interpreted as illustrative, to be not intended to limit the present invention range, essence of the invention and model
It encloses and is limited only by the claims that follow.To those skilled in the art, in the premise without departing substantially from spirit and scope of the present invention
Under, protection model of the invention is also belonged to the various changes or change of material component and dosage progress in these embodiments
It encloses.
Embodiment 1:
(1) it is by the 2,4-dinitrochlorobenzene (CDB) of 65 DEG C of molten states, 20 DEG C of methanol and 20 DEG C of mass fractions
30% liquid alkaline solution is that 1:0.69:6 is continuously added into reactor in mass ratio, and keeping temperature constant in reactor is 65
℃；
(2) synthesis reaction solution continuously enters in evaporator, and methanol enters rectifying column from evaporator gaseous phase outlet, from rectifying column
Top is continuously entered containing 2,4- dinitroanisol (DNAN), sodium-chloride water solution from evaporator liquid-phase outlet into returnable bottle
In sink；
(3) washed through 95 DEG C of hot water in sink, into separator in settle and separate, at isolated wastewater collection is unified
Reason, product 2,4- dinitroanisol (DNAN) are dried after collecting, weigh, analyze test；
It is tested by analysis, obtains sheet 2, the total recovery of 4- dinitroanisol (DNAN) is 91%, and purity is
99.4%, fusing point is 96.2 DEG C.
Embodiment 2:
(1) 2,4-dinitrochlorobenzene (CDB) of methanol, liquid alkaline, molten state is continuously conveyed respectively to corresponding raw material height
In the slot of position；
(2) lye, methanol and 2,4-dinitrochlorobenzene (CDB) are continuously added to instead for 1:0.72:5 from head tank in mass ratio
It answers in kettle, reaction kettle set temperature is 65 DEG C, and normal pressure, reaction solution continuously enters aging machine by reaction kettle lifting system, curing
Machine set temperature is 65 DEG C, normal pressure；
(3) mixed material in aging machine continuously enters evaporator by lifting system, and evaporator uses autoclave self-loopa
Mode, the reaction solution after methanol removal continuously enter First washing kettle from evaporator side, and methanol, the water of evaporator evaporation steam
Vapour continuously enters methanol rectifying tower, and tower operates under normal pressure, and top gaseous phase enters first by condensation, one reflux, one extraction
Alcohol recycles storage tank；
(4) washing unit is mainly composed in series by three washing kettles with separator, and material and washing water are gone here and there in adverse current
Connection washing, hot wash-water use 96 DEG C of hot water of hot water storgae, and hot wash-water flow direction is then washed for 3# washing kettle → 2# washing kettle → 1#
Wash kettle → liquid medicine separator → effluent settling chamber；2,4- dinitroanisols (DNAN) flow direction of material is 1# washing kettle → 2# washing
Kettle → 3# washing kettle → liquid medicine separator → drying unit；
(5) 2,4- dinitroanisol (DNAN) continuously enter in hot-air drier, by steam contact drying, dry temperature
Degree is 110 DEG C, and drier bottom blasts air, is taken away the moisture in material using air, 2, the 4- dinitrobenzene after drying
Methyl ether (DNAN) continuously enters pelleter；
(6) lead to cold water in the roller interlayer of pelleter, solidify 2, the 4- dinitroanisol (DNAN) of roller surface, quilt
Scraper, which scrapes, is made sheet, falls into hopper, and dress automobile is sent after automatic weighing, barrelling, is transported to DNAN warehouse for finished product.
It is tested by analysis, obtains sheet 2, the total recovery of 4- dinitroanisol (DNAN) is 92%, and purity is
99.3%, fusing point is 96.0 DEG C.
Embodiment 3:
(1) 2,4-dinitrochlorobenzene (CDB) of methanol, liquid alkaline, molten state is continuously conveyed respectively to corresponding raw material height
In the slot of position；
(2) lye, methanol and 2,4-dinitrochlorobenzene (CDB) are continuously added to instead for 1:0.72:8 from head tank in mass ratio
It answers in kettle, reaction kettle set temperature is 62 DEG C, and normal pressure, reaction solution continuously enters aging machine by reaction kettle lifting system, curing
Machine set temperature is 62 DEG C, normal pressure；
(3) mixed material in aging machine continuously enters evaporator by lifting system, and evaporator uses autoclave self-loopa
Mode, the reaction solution after methanol removal continuously enter First washing kettle from evaporator side, and methanol, the water of evaporator evaporation steam
Vapour continuously enters methanol rectifying tower, and tower operates under normal pressure, and top gaseous phase enters first by condensation, one reflux, one extraction
Alcohol recycles storage tank；
(4) washing unit is mainly composed in series by three washing kettles with separator, and material and washing water are gone here and there in adverse current
Connection washing, hot wash-water use 98 DEG C of hot water of hot water storgae, and hot wash-water flow direction is then washed for 3# washing kettle → 2# washing kettle → 1#
Wash kettle → liquid medicine separator → effluent settling chamber；2,4- dinitroanisols (DNAN) flow direction of material is 1# washing kettle → 2# washing
Kettle → 3# washing kettle → liquid medicine separator → drying unit；
(5) 2,4- dinitroanisol (DNAN) continuously enter in hot-air drier, by steam contact drying, dry temperature
Degree is 115 DEG C, and drier bottom blasts air, is taken away the moisture in material using air, 2, the 4- dinitrobenzene after drying
Methyl ether (DNAN) continuously enters pelleter；
(6) lead to cold water in the roller interlayer of pelleter, solidify 2, the 4- dinitroanisol (DNAN) of roller surface, quilt
Scraper, which scrapes, is made sheet, falls into hopper, and dress automobile is sent after automatic weighing, barrelling, is transported to DNAN warehouse for finished product.
It is tested by analysis, obtains sheet 2, the total recovery of 4- dinitroanisol (DNAN) is 93%, and purity is
99.5%, fusing point is 96.1 DEG C.
Embodiment 4:
(1) 2,4-dinitrochlorobenzene (CDB) of methanol, liquid alkaline, molten state is continuously conveyed respectively to corresponding raw material height
In the slot of position；
(2) lye, methanol and 2,4-dinitrochlorobenzene (CDB) are continuously added to instead for 1:0.70:7 from head tank in mass ratio
It answers in kettle, reaction kettle set temperature is 67 DEG C, and normal pressure, reaction solution continuously enters aging machine by reaction kettle lifting system, curing
Machine set temperature is 67 DEG C, normal pressure；
(3) mixed material in aging machine continuously enters evaporator by lifting system, and evaporator uses autoclave self-loopa
Mode, the reaction solution after methanol removal continuously enter First washing kettle from evaporator side, and methanol, the water of evaporator evaporation steam
Vapour continuously enters methanol rectifying tower, and tower operates under normal pressure, and top gaseous phase enters first by condensation, one reflux, one extraction
Alcohol recycles storage tank；
(4) washing unit is mainly composed in series by three washing kettles with separator, and material and washing water are gone here and there in adverse current
Connection washing, hot wash-water use 96 DEG C of hot water of hot water storgae, and hot wash-water flow direction is then washed for 3# washing kettle → 2# washing kettle → 1#
Wash kettle → liquid medicine separator → effluent settling chamber；2,4- dinitroanisols (DNAN) flow direction of material is 1# washing kettle → 2# washing
Kettle → 3# washing kettle → liquid medicine separator → drying unit；
(5) 2,4- dinitroanisol (DNAN) continuously enter in hot-air drier, by steam contact drying, dry temperature
Degree is 120 DEG C, and drier bottom blasts air, is taken away the moisture in material using air, 2, the 4- dinitrobenzene after drying
Methyl ether (DNAN) continuously enters pelleter；
(6) lead to cold water in the roller interlayer of pelleter, solidify 2, the 4- dinitroanisol (DNAN) of roller surface, quilt
Scraper, which scrapes, is made sheet, falls into hopper, and dress automobile is sent after automatic weighing, barrelling, is transported to DNAN warehouse for finished product.
It is tested by analysis, obtains sheet 2, the total recovery of 4- dinitroanisol (DNAN) is 92%, and purity is
99.3%, fusing point is 96.0 DEG C.
Obviously present invention specific implementation is not subject to the restrictions described above, as long as using method concept and skill of the invention
The improvement for the various unsubstantialities that art scheme carries out, or not improved the conception and technical scheme of the invention are directly applied to it
Its occasion, it is within the scope of the present invention.
Claims (6)
1. the method that one kind is continuously synthesizing to 2,4- dinitroanisol, which is characterized in that include the following steps:
(1) 2,4-dinitrochlorobenzene and methanol liquid alkaline mixed liquor continuously enter 2 that synthesis reactor reacts synthesizing liquid by a certain percentage,
4- dinitroanisol, reaction solution continuously enter aging machine by the included lifting system of synthesis reactor and further synthesize；
(2) reaction solution promotes bucket by aging machine and continuously enters in evaporator, and a large amount of first alcohol and water continuous evaporation continuously enters
In methanol rectifying tower, the methanol of recoverable, rectifying column and evaporator atmospheric operation are formed by rectifying；Water and 2,4- dinitro
Base methyl phenyl ethers anisole and sodium chloride then continuously enter in rinsing maching from the evaporator other end；
(3) it carries out hot water by three concatenated washing kettles continuously to wash, mode of washing is countercurrent washing, and washes enters useless
Pond；
(4) after the moisture in drying machine heated-air drying control product, product is continuously entered in pelleter；
(5) sheet 2,4- dinitroanisol are formed, product continuously enters hopper, automatic weighing, packaging.
2. the method that one kind according to claim 1 is continuously synthesizing to 2,4- dinitroanisol, it is characterised in that: described
Step (1) chinese raw materials feeds intake situation are as follows: 2,4-dinitrochlorobenzene: liquid alkaline: methanol quality ratio is 1:(0.65~0.72): (5~
8), wherein the mass fraction of liquid alkaline is 30%.
3. the method that one kind according to claim 1 is continuously synthesizing to 2,4- dinitroanisol, it is characterised in that: described
Synthesis reactor in step (1), aging machine reaction temperature be 62~67 DEG C, pressure is normal pressure.
4. the method that one kind according to claim 1 is continuously synthesizing to 2,4- dinitroanisol, it is characterised in that: described
The temperature of hot wash-water is 95~98 DEG C in washing process in step (3), and slurry amount is 2,4- dinitroanisol volume
2~4 times.
5. the method that one kind according to claim 1 is continuously synthesizing to 2,4- dinitroanisol, it is characterised in that: described
It is 1# washing kettle → 2# washing kettle → 3# washing that countercurrent washing regime, which is 2,4- dinitroanisol flow direction of material, in step (3)
Kettle, hot wash-water flow direction are then 3# washing kettle → 2# washing kettle → 1# washing kettle.
6. the method that one kind according to claim 1 is continuously synthesizing to 2,4- dinitroanisol, it is characterised in that: described
Heated-air drying temperature is 110~120 DEG C in step (4).
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| CN102391126A (en) * | 2011-10-17 | 2012-03-28 | 山东昌邑灶户盐化有限公司 | Method for producing 2, 4-dinitrobenzene methyl ether and 2, 4- dinitrophenol simultaneously |
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| WO2015031598A3 (en) * | 2013-08-30 | 2015-05-14 | Yale University | Therapeutic dnp derivatives and methods using same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040133046A1 (en) * | 2003-01-07 | 2004-07-08 | Highsmith Thomas K. | Continuous process for preparing alkoxynitroarenes |
| CN101464550B (en) * | 2007-12-19 | 2012-05-02 | 鸿富锦精密工业（深圳）有限公司 | device and method for disassembling lens module |
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| CN102391126A (en) * | 2011-10-17 | 2012-03-28 | 山东昌邑灶户盐化有限公司 | Method for producing 2, 4-dinitrobenzene methyl ether and 2, 4- dinitrophenol simultaneously |
| CN103396318A (en) * | 2013-07-30 | 2013-11-20 | 浙江迪邦化工有限公司 | Synthetic process for 2,4-dinitroanisole |
| WO2015031598A3 (en) * | 2013-08-30 | 2015-05-14 | Yale University | Therapeutic dnp derivatives and methods using same |
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