CN106336359A - Device for continuously producing nitroanisole through nitrochlorobenzene and production method - Google Patents
Device for continuously producing nitroanisole through nitrochlorobenzene and production method Download PDFInfo
- Publication number
- CN106336359A CN106336359A CN201610866504.0A CN201610866504A CN106336359A CN 106336359 A CN106336359 A CN 106336359A CN 201610866504 A CN201610866504 A CN 201610866504A CN 106336359 A CN106336359 A CN 106336359A
- Authority
- CN
- China
- Prior art keywords
- kettle
- methoxylation
- level
- methanol
- sodium methoxide
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a device for continuously producing nitroanisole through nitrochlorobenzene and a production method. The device comprises a wash water storage tank, a wash water metering pump, a methyl alcohol storage tank, a methyl alcohol metering pump, a spiral conveyer, a first-order sodium methoxide solution preparation kettle, a second-order sodium methoxide solution preparation kettle, a sodium methoxide solution storage tank, a methyl alcohol metering pump, a nitrochlorobenzene storage tank, a nitrochlorobenzene metering pump, a first-order methoxylation kettle, a second-order methoxylation kettle, a third-order methoxylation kettle, a dealcoholization tower metering pump, a dealcoholization tower, a cooler, a separator, a nitroanisole storage tank and a waste water tank. The device and the method have the advantages of high degree of automation, high simpleness in operation, high production efficiency, cleanliness and environmental friendliness.
Description
Technical field
The invention belongs to chemical production field, continuously produce the device of Nitroanisole particularly to a kind of chloronitrobenzene,
And the method using this device production Nitroanisole.
Background technology
Base methyl phenyl ethers anisole (predominantly ortho-nitroanisole and paranitroanisole) is the weight of the industry such as dyestuff, medicine, spice
Want intermediate.The preparation of ortho-nitroanisole and paranitroanisole is generally respectively with o-nitrochlorobenzene and paranitrochlorobenzene at present
For raw material, the sodium methoxide solution through being formulated with sodium hydroxide, methanol is by methoxylation, dealcoholysis, washing, stratification etc.
Operation is obtained.
Domestic production Nitroanisole is all produced using batch process at present, and the production of this product not yet realizes serialization,
Method of having a rest produces there is automaticity low, complex operation, low production efficiency, and Con trolling index fluctuation is big, the problems such as working environment difference.
Content of the invention
Technical problem solved by the invention is device and the production providing chloronitrobenzene continuously to produce Nitroanisole
Method.
The technical solution realizing the object of the invention is: a kind of chloronitrobenzene continuously produces the device of Nitroanisole,
Prepare including washing water storage tank, washings dosing pump, methanol storage tank, methanol dosing pump, conveying worm, one-level sodium methoxide solution
Kettle, secondary methanol sodium solution prepare kettle, sodium methoxide solution storage tank, Feldalat NM dosing pump, chloronitrobenzene storage tank, chloronitrobenzene metering
Pump, one-level methoxylation kettle, two grades of methoxylation kettles, three-level methoxylation kettle, dealcoholysis tower dosing pump, dealcoholysis tower, cooler, point
From device, Nitroanisole storage tank, wastewater trough；
Described one-level sodium methoxide solution preparation kettle is identical with secondary methanol sodium solution preparation kettle structure, described one-level methoxylation
Kettle, two grades of methoxylation kettles, three-level methoxylation kettle structure all sames；
Described one-level sodium methoxide solution is prepared kettle top and is provided with methanol charging aperture, flaky sodium hydrate input port, one-level Feldalat NM
Solution is prepared kettle side wall and is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export；
Described one-level methoxylation kettle top is provided with Feldalat NM charging aperture, chloronitrobenzene charging aperture, one-level methoxylation kettle side wall
It is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, one-level methoxylation bottom portion is provided with methoxylation
Kettle drain；
Described separator is provided with separator material inlet, light liquid outlet, heavy liquid exit；
Described washing water storage tank is connected with washings dosing pump by pipeline, and washings dosing pump passes through pipeline and three-level methoxyl group
Change kettle charging aperture to connect, methanol storage tank is connected with methanol dosing pump by pipeline, methanol dosing pump passes through pipeline and one-level methanol
Sodium solution prepares the methanol charging aperture connection of kettle, and conveying worm passes through pipeline and one-level sodium methoxide solution prepares the lamellar hydrogen of kettle
Sodium oxide input port connects, and the Feldalat NM mixture export that one-level sodium methoxide solution prepares kettle is molten with secondary methanol sodium by pipeline
Liquid prepares the Feldalat NM mixed liquor inlet communication of kettle, and the Feldalat NM mixture export that secondary methanol sodium solution prepares kettle passes through pipeline
Connect with sodium methoxide solution storage tank, sodium methoxide solution storage tank is connected with Feldalat NM dosing pump by pipeline, Feldalat NM dosing pump with
The Feldalat NM charging aperture connection of one-level methoxylation kettle, chloronitrobenzene storage tank is connected with chloronitrobenzene dosing pump by pipeline, nitre
Base chlorobenzene dosing pump is connected with the chloronitrobenzene charging aperture of one-level methoxylation by pipeline, the methoxyl group of one-level methoxylation kettle
Change the methoxylation kettle mixed liquor inlet communication that kettle mixture export passes through pipeline and two grades of methoxylation kettles, two grades of methoxylations
The methoxylation kettle mixture export of kettle passes through the methoxylation kettle mixed liquor inlet communication of pipeline and three-level methoxylation kettle, and three
The methoxylation kettle drain of level methoxylation kettle is connected with dealcoholysis tower dosing pump by pipeline, and dealcoholysis tower dosing pump passes through pipeline
Connect with dealcoholysis tower, dealcoholysis top of tower is connected with methanol storage tank by pipeline, and dealcoholysis bottom of towe is connected with cooler by pipeline, cold
But device is connected with the separator material inlet of separator by pipeline, and the light liquid outlet of separator is by pipeline with wastewater trough even
Logical, the heavy liquid exit of separator is connected with Nitroanisole storage tank by pipeline.
Preferably, described one-level sodium methoxide solution preparation kettle includes internal low head, internal straight barrel, upper cover, outside
Lower envelope, outside straight barrel, dasher, shaft, actuating device, described actuating device is fixed on upper cover by support,
Dasher is two-layer blade, is connected with actuating device by shaft, straight tube body sidewall is provided with Feldalat NM mixed liquor and enters
Mouth, Feldalat NM mixture export, are provided with discharging weir, the upper end on discharging weir inside the straight barrel of Feldalat NM mixture export side
Open wide, the lower end on discharging weir connects with inside straight barrel, the upper cover that described sodium methoxide solution prepares kettle is provided with hydroxide flake
Sodium adds mouth, methanol charging aperture；
Preferably, described one-level methoxylation kettle includes low head, straight barrel, upper cover, guide shell, agitator, shaft, changes
Hot coil and actuating device, described actuating device is fixed on upper cover by support, and guide shell is fixed on straight barrel by support
Interior, guide shell inwall is provided with radial direction baffle plate, and agitator is connected with actuating device by shaft, and paddle device is suspended in guide shell
Interior, it is provided with heat exchange coil between straight barrel and guide shell, the side wall of straight barrel is provided with methoxylation kettle mixed liquor import, methoxy
Base kettle mixture export, is provided with discharging weir inside the straight barrel of methoxylation kettle mixture export side, discharging weir upper
Portion is opened wide, and the bottom on discharging weir connects with inside straight barrel, and the upper cover of described one-level methoxylation kettle is provided with sodium methoxide solution
Charging aperture, chloronitrobenzene charging aperture, wherein, sodium methoxide solution charging aperture is connected with sodium methoxide solution feed conduit one end, methanol
The sodium solution feed conduit other end is placed in guide shell, and chloronitrobenzene charging aperture is connected with chloronitrobenzene feed conduit one end, nitre
The base methyl phenyl ethers anisole feed conduit other end is placed in guide shell；
Preferably, described separator is the density contrast using two kinds of liquid, designs according to law of connected vessels, the shell of separator
Body is made up of front side board, left plate, right plate, the back side panel with radian, base plate, top board, is provided with dividing plate in shell separator, every
Plate is fixed with front side board, base plate sealing, and dividing plate leaves gap with the back side panel with radian, and dividing plate is divided into inside shell separator
Feed zone and sub-material area, feed zone is connected by gap with sub-material area, is provided with mixed liquor import on the front side board of feed zone,
The front side board in sub-material area is provided with light liquid outlet and heavy liquid exit, and light liquid outlet is higher than heavy liquid exit, heavy liquid exit and mozzle
Sidepiece connects, and mozzle lower end connects with shell separator, and mozzle upper end, lower end are all unlimited.
A kind of Nitroanisole production method of the device continuously producing Nitroanisole based on chloronitrobenzene, including following
Step:
Step 1, one-level sodium methoxide solution prepare kettle, secondary methanol sodium solution prepare kettle in compounding methanol sodium solution: by spiral shell
Rotation conveyer is prepared in kettle to one-level sodium methoxide solution and is added quantitative flaky sodium hydrate, starts stirring, then methanol storage tank
In methanol one-level sodium methoxide solution put into by dosing pump prepare in kettle, after flaky sodium hydrate all dissolves, by setting
Ratio continuously adds flaky sodium hydrate and methanol, compounding methanol sodium solution, and sodium methoxide solution continuously flow to sodium methoxide solution storage
Groove.
Step 2, one-level methoxylation kettle, two grades of methoxylation kettles, three-level methoxylation kettle put into kettle effectively hold
Long-pending 70% methanol, starts stirring, is warming up to design temperature, continuously adds sodium methoxide solution and chloronitrobenzene in proportion, carry out first
Oxygen glycosylation reaction, when two grades of methoxylation kettles have reactant liquor to flow into three-level methoxylation kettle, by the washing in washing water storage tank
Water is continuously added to three-level methoxylation kettle by washings dosing pump, and in three-level methoxylation kettle, reactant liquor is measured with dealcoholysis tower
It is pumped into dealcoholysis tower.
Step 3, reactant liquor carry out separating in dealcoholysis tower, and wherein, the extraction of dealcoholysis column overhead methanol flows into methanol storage tank, uses
Prepare in sodium methoxide solution, flow into separator after the kettle material cooled device cooling of methanol storage tank, separator is continuously divided
From the Nitroanisole after separating flows into Nitroanisole storage tank, and waste water flows into waste water tank.
Preferably, in sodium methoxide solution process for preparation in step 1, flaky sodium hydrate, piece are added using conveying worm
Alkali dosage is controlled by the motor speed of converter adjustable screw conveyer.
Preferably, in step 1, chloronitrobenzene can be o-nitrochlorobenzene or paranitrochlorobenzene or o-nitrochlorobenzene
Mixture with paranitrochlorobenzene arbitrary proportion.
Preferably, in sodium methoxide solution process for preparation in step 1, methanol with the mol ratio of sodium hydroxide is: 8～15:1,
Sodium methoxide solution prepares temperature: 30～50 DEG C.
Preferably, during methoxylation in step 2, sodium methoxide solution (in terms of sodium hydroxide) and chloronitrobenzene mole
Than for: 1.1～1.2:1, reaction pressure is: 0.30～0.40mpa, and reaction temperature is: 95～100 DEG C.
Preferably, in step 3, dealcoholysis column overhead temperatures are: 65～70 DEG C, bottom temperature is 100～120 DEG C, dealcoholysis tower tower
Top extraction methanol specific gravity control is at 0.792～0.796(20 DEG C) between.
Compared with prior art, its remarkable advantage is the present invention: 1) produces and realizes serialization, equipment volume is little, cost
Low, device is compact, and floor space is little；2) continuous prodution, Automated condtrol, production efficiency is high, reduces production cost；3) adopt
With the airtight production of serialization, production environment cleaning；4) one-level methoxylation kettle, two grades of methoxylation kettles, three-level methoxylation kettles
Interior setting guide shell, the effect of guide shell: the mixing efficiency of liquid can be improved, on the one hand improve the stirring journey to liquid
Degree, strengthens the direct mechanical shearing effect to liquid for the agitator；On the other hand all liq in device is made all can to pass through guide shell
Interior strong mixed zone, decreases the chance that liquid walks short circuit.Guide shell inwall is provided with radial direction baffle plate and can effectively stop kettle
The circular motion of interior liquid；5) separator utilizes linker and fluid density difference principle it is achieved that the continuous AUTOMATIC ZONING of material,
Layered velocity is fast, and layered effect is good；6) continuous prodution realizes technological parameter stably, and equipment safety performance improves, and accomplishes essence
Safety.
Below in conjunction with the accompanying drawings the present invention is described in further detail.
Brief description
Fig. 1 continuously produces the structural representation of the device of Nitroanisole for chloronitrobenzene of the present invention.
Fig. 2 is that the one-level sodium methoxide solution of the present invention prepares kettle structural representation.
Fig. 3 is the one-level methoxylation kettle structural representation of the present invention.
Fig. 4 is the separator overlooking the structure diagram of the present invention.
Fig. 5 is the separator side structure schematic view of the present invention.
Specific embodiment
In conjunction with Fig. 1-Fig. 5, a kind of chloronitrobenzene of the present invention continuously produces the device of Nitroanisole, including washings storage
Groove 1, washings dosing pump 2, methanol storage tank 3, methanol dosing pump 4, conveying worm 5, one-level Feldalat NM meter solution prepare kettle 6,
Secondary methanol sodium solution prepares kettle 7, sodium methoxide solution storage tank 8, Feldalat NM dosing pump 9, chloronitrobenzene storage tank 10, chloronitrobenzene meter
Amount pump 11,12, two grades of methoxylation kettles 13 of one-level methoxylation kettle, three-level methoxylation kettle 14, dealcoholysis tower dosing pump 15, dealcoholysis
Tower 16, cooler 17, separator 18, Nitroanisole storage tank 19, wastewater trough 20；
Described one-level sodium methoxide solution preparation kettle 6 is identical with secondary methanol sodium solution preparation kettle 7 structure, described one-level methoxylation
12, two grades of methoxylation kettles 13 of kettle, three-level methoxylation kettle 14 structure all same；
Described one-level sodium methoxide solution is prepared kettle 6 top and is provided with methanol charging aperture, flaky sodium hydrate input port, one-level Feldalat NM
Solution is prepared kettle 6 side wall and is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export；
Described one-level methoxylation kettle 12 top is provided with Feldalat NM charging aperture, chloronitrobenzene charging aperture, one-level methoxylation kettle 12
Side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, and one-level methoxylation kettle 12 bottom is provided with first
Epoxide kettle drain；
Described separator 18 is provided with separator material inlet, light liquid outlet, heavy liquid exit；
Described washing water storage tank 1 is connected with washings dosing pump 2 by pipeline, and washings dosing pump 2 passes through pipeline and three-level first
Epoxide kettle 14 charging aperture connects, and methanol storage tank 2 connects with methanol dosing pump 4 by pipeline, methanol dosing pump 4 by pipeline and
One-level sodium methoxide solution prepares the methanol charging aperture connection of kettle 6, and conveying worm 5 is passed through pipeline and prepared with one-level sodium methoxide solution
Kettle 6 flaky sodium hydrate input port connection, one-level sodium methoxide solution prepare kettle 6 Feldalat NM mixture export pass through pipeline with
Secondary methanol sodium solution prepares the Feldalat NM mixed liquor inlet communication of kettle 7, and secondary methanol sodium solution prepares the Feldalat NM mixing of kettle 7
Liquid outlet is connected with sodium methoxide solution storage tank 8 by pipeline, and sodium methoxide solution storage tank 8 passes through pipeline with Feldalat NM dosing pump 9 even
Logical, Feldalat NM dosing pump 9 connect with the Feldalat NM charging aperture of one-level methoxylation kettle 12, chloronitrobenzene storage tank 10 by pipeline and
Chloronitrobenzene dosing pump 11 connects, and chloronitrobenzene dosing pump 11 passes through the chloronitrobenzene charging of pipeline and one-level methoxylation 12
Mouth connection, the methoxylation kettle mixture export of one-level methoxylation kettle 12 passes through the methoxy of pipeline and two grades of methoxylation kettles 13
Base kettle mixed liquor inlet communication, the methoxylation kettle mixture export of two grades of methoxylation kettles 13 passes through pipeline and three-level methoxy
The methoxylation kettle mixed liquor inlet communication of base kettle 14, the methoxylation kettle drain of three-level methoxylation kettle 14 passes through pipeline
Connect with dealcoholysis tower dosing pump 15, dealcoholysis tower dosing pump 15 is connected with dealcoholysis tower 16 by pipeline, pipe is passed through at dealcoholysis tower 16 top
Road is connected with methanol storage tank 3, and dealcoholysis tower 16 bottom is connected with cooler 17 by pipeline, and cooler 17 passes through pipeline and separator 18
Separator material inlet connection, separator 18 light liquid outlet connected with wastewater trough 20 by pipeline, the heavy-fluid of separator 18
Outlet is connected with Nitroanisole storage tank 19 by pipeline.
One-level sodium methoxide solution is prepared kettle 6 and is included internal low head 22, internal straight barrel 23, upper cover 27, outer subordinate envelope
21st, outside straight barrel 24, dasher 31, shaft 30, actuating device 26, described actuating device 26 is fixed on by support
Upper cover 27, dasher 31 is two-layer blade, is connected with actuating device 26 by shaft 30, straight barrel 23 side wall sets
There are Feldalat NM mixed liquor import, Feldalat NM mixture export, be provided with inside the straight barrel 23 of Feldalat NM mixture export side
Discharging weir 29, the open upper end on discharging weir 29, the lower end on discharging weir 29 is internal with straight barrel 23 to be connected, and described sodium methoxide solution is joined
The upper cover 27 of kettle 6 processed is provided with flaky sodium hydrate and adds mouth, methanol charging aperture；
One-level methoxylation kettle 12 includes low head 33, straight barrel 35, upper cover 39, guide shell 34, agitator 43, shaft
42nd, heat exchange coil 36 and actuating device 38, described actuating device 38 is fixed on upper cover 39 by support, and guide shell 34 passes through to prop up
Frame is fixed in straight barrel 35, and guide shell 34 inwall is provided with radial direction baffle plate 45, and agitator 43 passes through shaft 42 and actuating device
38 connections, paddle device 43 is suspended in guide shell 34, is provided with heat exchange coil 36, straight barrel between straight barrel 35 and guide shell 34
35 side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, goes out in methoxylation kettle mixed liquor
It is provided with discharging weir 40, the opened upper end on discharging weir 40, in the bottom on discharging weir 40 and straight barrel 35 inside the straight barrel of mouth side
Portion connects, and the upper cover 39 of described one-level methoxylation kettle 12 is provided with sodium methoxide solution charging aperture, chloronitrobenzene charging aperture, its
In, sodium methoxide solution charging aperture is connected with sodium methoxide solution feed conduit one end, and the sodium methoxide solution feed conduit other end is placed in
In guide shell 35, chloronitrobenzene charging aperture is connected with chloronitrobenzene feed conduit one end, the Nitroanisole feed conduit other end
It is placed in 35 in guide shell；
Separator 18 is the density contrast using two kinds of liquid, designs according to law of connected vessels, the housing of separator 18 is by front
Side plate 48, left plate 49, right plate 52, the back side panel 51 with radian, base plate 55, top board 54 form, and set in separator 18 housing
There is dividing plate 50, dividing plate 50 is fixed with front side board 48, base plate 55 sealing, and dividing plate 50 leaves gap with the back side panel 51 with radian, every
Separator 18 enclosure interior is divided into feed zone and sub-material area by plate 50, and feed zone is connected by gap with sub-material area, in feed zone
Front side board 48 be provided with mixed liquor import 47, light liquid outlet 46 and heavy liquid exit 45 is provided with the front side board 48 in sub-material area,
Light liquid outlet 46 is higher than heavy liquid exit 45, and heavy liquid exit 45 connects with mozzle 53 sidepiece, mozzle 53 lower end and separator 18
Connection in housing, mozzle 53 upper end, lower end are all unlimited.
A kind of Nitroanisole production method of the device continuously producing Nitroanisole based on chloronitrobenzene, including following
Step:
Step 1, one-level sodium methoxide solution prepare kettle 6, secondary methanol sodium solution prepare kettle 7 in compounding methanol sodium solution: pass through
Conveying worm 5 is prepared in kettle 6 to one-level sodium methoxide solution and is added quantitative flaky sodium hydrate, starts stirring, then methanol
Methanol in storage tank 3 puts into one-level sodium methoxide solution by dosing pump 4 and prepares in kettle 6, after flaky sodium hydrate all dissolves,
Continuously add flaky sodium hydrate and methanol, compounding methanol sodium solution by setting ratio, sodium methoxide solution continuously flow to Feldalat NM
Solution storage tank 8.
Step 2, in 12, two grades of methoxylation kettles 13 of one-level methoxylation kettle, three-level methoxylation kettle 14 put into kettle
The methanol of dischargeable capacity 70%, starts stirring, is warming up to design temperature, continuously adds sodium methoxide solution and chloronitrobenzene in proportion,
Carry out methoxylation, when two grades of methoxylation kettles 13 have reactant liquor to flow into three-level methoxylation kettle 14, washings are store
Washings in groove 1 are continuously added to three-level methoxylation kettle 14 by washings dosing pump 2, anti-in three-level methoxylation kettle 14
Liquid dealcoholysis tower dosing pump 15 is answered to send into dealcoholysis tower 16.
Step 3, reactant liquor carry out separating in dealcoholysis tower 16, and wherein, the extraction of dealcoholysis tower 16 tower top methanol flows into methanol storage
Groove 3, prepares for sodium methoxide solution, flows into separator 18, separator after the cooled device of kettle material 17 cooling of methanol storage tank 3
18 are continuously separated, and the Nitroanisole after separating flows into Nitroanisole storage tank, and waste water flows into waste water tank.
In sodium methoxide solution process for preparation in step 1, flaky sodium hydrate, piece alkali dosage are added using conveying worm
Controlled by the motor speed of converter adjustable screw conveyer 5.
In step 1, chloronitrobenzene can be o-nitrochlorobenzene or paranitrochlorobenzene or o-nitrochlorobenzene and to nitre
The mixture of base chlorobenzene arbitrary proportion.
In sodium methoxide solution process for preparation in step 1, methanol with the mol ratio of sodium hydroxide is: 8～15:1, Feldalat NM is molten
Liquid prepares temperature: 30～50 DEG C.
During methoxylation in step 2, sodium methoxide solution with the mol ratio of chloronitrobenzene is in terms of sodium hydroxide: 1.1
～1.2:1, reaction pressure is: 0.30～0.40mpa, and reaction temperature is: 95～100 DEG C.
In step 3, dealcoholysis tower 16 tower top temperature is: 65～70 DEG C, bottom temperature is 100～120 DEG C, dealcoholysis tower 16 tower top
Extraction methanol specific gravity control is at 0.792～0.796(20 DEG C) between.
With reference to embodiment the present invention is done with further detailed description:
Embodiment 1
A kind of chloronitrobenzene continuously produces the device of Nitroanisole, including washing water storage tank 1, washings dosing pump 2, methanol storage
Groove 3, methanol dosing pump 4, conveying worm 5, one-level Feldalat NM meter solution prepare kettle 6, secondary methanol sodium solution prepares kettle 7, first
Sodium alkoxide solution storage tank 8, Feldalat NM dosing pump 9, chloronitrobenzene storage tank 10, chloronitrobenzene dosing pump 11, one-level methoxylation kettle 12,
Two grades of methoxylation kettles 13, three-level methoxylation kettle 14, dealcoholysis tower dosing pump 15, dealcoholysis tower 16, cooler 17, separator 18,
Nitroanisole storage tank 19, wastewater trough 20；
Described one-level sodium methoxide solution preparation kettle 6 is identical with secondary methanol sodium solution preparation kettle 7 structure, described one-level methoxylation
12, two grades of methoxylation kettles 13 of kettle, three-level methoxylation kettle 14 structure all same；
Described one-level sodium methoxide solution is prepared kettle 6 top and is provided with methanol charging aperture, flaky sodium hydrate input port, one-level Feldalat NM
Solution is prepared kettle 6 side wall and is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export；
Described one-level methoxylation kettle 12 top is provided with Feldalat NM charging aperture, chloronitrobenzene charging aperture, one-level methoxylation kettle 12
Side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, and one-level methoxylation kettle 12 bottom is provided with first
Epoxide kettle drain；
Described separator 18 is provided with separator material inlet, light liquid outlet, heavy liquid exit；
Described washing water storage tank 1 is connected with washings dosing pump 2 by pipeline, and washings dosing pump 2 passes through pipeline and three-level first
Epoxide kettle 14 charging aperture connects, and methanol storage tank 2 connects with methanol dosing pump 4 by pipeline, methanol dosing pump 4 by pipeline and
One-level sodium methoxide solution prepares the methanol charging aperture connection of kettle 6, and conveying worm 5 is passed through pipeline and prepared with one-level sodium methoxide solution
Kettle 6 flaky sodium hydrate input port connection, one-level sodium methoxide solution prepare kettle 6 Feldalat NM mixture export pass through pipeline with
Secondary methanol sodium solution prepares the Feldalat NM mixed liquor inlet communication of kettle 7, and secondary methanol sodium solution prepares the Feldalat NM mixing of kettle 7
Liquid outlet is connected with sodium methoxide solution storage tank 8 by pipeline, and sodium methoxide solution storage tank 8 passes through pipeline with Feldalat NM dosing pump 9 even
Logical, Feldalat NM dosing pump 9 connect with the Feldalat NM charging aperture of one-level methoxylation kettle 12, chloronitrobenzene storage tank 10 by pipeline and
Chloronitrobenzene dosing pump 11 connects, and chloronitrobenzene dosing pump 11 passes through the chloronitrobenzene charging of pipeline and one-level methoxylation 12
Mouth connection, the methoxylation kettle mixture export of one-level methoxylation kettle 12 passes through the methoxy of pipeline and two grades of methoxylation kettles 13
Base kettle mixed liquor inlet communication, the methoxylation kettle mixture export of two grades of methoxylation kettles 13 passes through pipeline and three-level methoxy
The methoxylation kettle mixed liquor inlet communication of base kettle 14, the methoxylation kettle drain of three-level methoxylation kettle 14 passes through pipeline
Connect with dealcoholysis tower dosing pump 15, dealcoholysis tower dosing pump 15 is connected with dealcoholysis tower 16 by pipeline, pipe is passed through at dealcoholysis tower 16 top
Road is connected with methanol storage tank 3, and dealcoholysis tower 16 bottom is connected with cooler 17 by pipeline, and cooler 17 passes through pipeline and separator 18
Separator material inlet connection, separator 18 light liquid outlet connected with wastewater trough 20 by pipeline, the heavy-fluid of separator 18
Outlet is connected with Nitroanisole storage tank 19 by pipeline.
One-level sodium methoxide solution is prepared kettle 6 and is included internal low head 22, internal straight barrel 23, upper cover 27, outer subordinate envelope
21st, outside straight barrel 24, dasher 31, shaft 30, actuating device 26, described actuating device 26 is fixed on by support
Upper cover 27, dasher 31 is two-layer blade, is connected with actuating device 26 by shaft 30, straight barrel 23 side wall sets
There are Feldalat NM mixed liquor import, Feldalat NM mixture export, be provided with inside the straight barrel 23 of Feldalat NM mixture export side
Discharging weir 29, the open upper end on discharging weir 29, the lower end on discharging weir 29 is internal with straight barrel 23 to be connected, and described sodium methoxide solution is joined
The upper cover 27 of kettle 6 processed is provided with flaky sodium hydrate and adds mouth, methanol charging aperture；
One-level methoxylation kettle 12 includes low head 33, straight barrel 35, upper cover 39, guide shell 34, agitator 43, shaft
42nd, heat exchange coil 36 and actuating device 38, described actuating device 38 is fixed on upper cover 39 by support, and guide shell 34 passes through to prop up
Frame is fixed in straight barrel 35, and guide shell 34 inwall is provided with radial direction baffle plate 45, and agitator 43 passes through shaft 42 and actuating device
38 connections, paddle device 43 is suspended in guide shell 34, is provided with heat exchange coil 36, straight barrel between straight barrel 35 and guide shell 34
35 side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, goes out in methoxylation kettle mixed liquor
It is provided with discharging weir 40, the opened upper end on discharging weir 40, in the bottom on discharging weir 40 and straight barrel 35 inside the straight barrel of mouth side
Portion connects, and the upper cover 39 of described one-level methoxylation kettle 12 is provided with sodium methoxide solution charging aperture, chloronitrobenzene charging aperture, its
In, sodium methoxide solution charging aperture is connected with sodium methoxide solution feed conduit one end, and the sodium methoxide solution feed conduit other end is placed in
In guide shell 35, chloronitrobenzene charging aperture is connected with chloronitrobenzene feed conduit one end, the Nitroanisole feed conduit other end
It is placed in 35 in guide shell；
Separator 18 is the density contrast using two kinds of liquid, designs according to law of connected vessels, the housing of separator 18 is by front
Side plate 48, left plate 49, right plate 52, the back side panel 51 with radian, base plate 55, top board 54 form, and set in separator 18 housing
There is dividing plate 50, dividing plate 50 is fixed with front side board 48, base plate 55 sealing, and dividing plate 50 leaves gap with the back side panel 51 with radian, every
Separator 18 enclosure interior is divided into feed zone and sub-material area by plate 50, and feed zone is connected by gap with sub-material area, in feed zone
Front side board 48 be provided with mixed liquor import 47, light liquid outlet 46 and heavy liquid exit 45 is provided with the front side board 48 in sub-material area,
Light liquid outlet 46 is higher than heavy liquid exit 45, and heavy liquid exit 45 connects with mozzle 53 sidepiece, mozzle 53 lower end and separator 18
Connection in housing, mozzle 53 upper end, lower end are all unlimited.
A kind of Nitroanisole production method of the device continuously producing Nitroanisole based on chloronitrobenzene, including following
Step:
Step 1, one-level sodium methoxide solution prepare kettle 6, secondary methanol sodium solution prepare kettle 7 in compounding methanol sodium solution: pass through
Conveying worm 5 is prepared in kettle 6 to one-level sodium methoxide solution and is added quantitative flaky sodium hydrate, starts stirring, then methanol
Methanol in storage tank 3 puts into one-level sodium methoxide solution by dosing pump 4 and prepares in kettle 6, after flaky sodium hydrate all dissolves,
Continuously add flaky sodium hydrate and methanol by mol ratio 12:1 of methanol and sodium hydroxide, sodium methoxide solution prepares kettle temperature degree control
At 35～40 DEG C, sodium methoxide solution continuously flow to sodium methoxide solution storage tank 8 to system.Step 2, in 12, two grades of one-level methoxylation kettle
Put into the methanol of kettle dischargeable capacity 70% in methoxylation kettle 13, three-level methoxylation kettle 14, start stirring, be warming up to 70 DEG C,
Continuously add sodium methoxide solution and adjacent nitro by sodium methoxide solution (in terms of sodium hydroxide) and o-nitrochlorobenzene mol ratio 1.1:1
Chlorobenzene, carries out methoxylation, when two grades of methoxylation kettles 13 have reactant liquor to flow into three-level methoxylation kettle 14, will wash
Washings in water storage tank 1 are continuously added to three-level methoxylation kettle 14 by washings dosing pump 2, and 1:2(neighbour's nitre pressed by washings
Base methyl phenyl ethers anisole and the volume ratio of washings) ratio adds, one-level methoxylation kettle 12, two grades of methoxylation kettles 13, three-level methoxies
Base kettle 14 reaction temperature all controls at 70～120 DEG C, and reaction pressure rises to 0.1～0.5mpa, three-level methoxylation kettle naturally
In 14, reactant liquor sends into dealcoholysis tower 16 with dealcoholysis tower feed pump 15.Step 3, reactant liquor carry out separating in dealcoholysis tower 16, wherein,
Control dealcoholysis tower 16 tower top temperature: 65～70 DEG C, dealcoholysis tower 16 column bottom temperature: 100～120 DEG C, dealcoholysis tower 16 overhead extraction first
Alcohol specific gravity control is at 0.792～0.796(20 DEG C) between, the extraction of dealcoholysis tower 16 tower top methanol flows into methanol storage tank 3, for methanol
Sodium solution is prepared, and flows into separator 18, separator 18 is continuously divided after the cooled device of kettle material 17 cooling of methanol storage tank 3
From the Nitroanisole after separating flows into Nitroanisole storage tank 19, and waste water flows into waste water tank 20.
Embodiment 2
A kind of chloronitrobenzene continuously produces the device of Nitroanisole, including washing water storage tank 1, washings dosing pump 2, methanol storage
Groove 3, methanol dosing pump 4, conveying worm 5, one-level Feldalat NM meter solution prepare kettle 6, secondary methanol sodium solution prepares kettle 7, first
Sodium alkoxide solution storage tank 8, Feldalat NM dosing pump 9, chloronitrobenzene storage tank 10, chloronitrobenzene dosing pump 11, one-level methoxylation kettle 12,
Two grades of methoxylation kettles 13, three-level methoxylation kettle 14, dealcoholysis tower dosing pump 15, dealcoholysis tower 16, cooler 17, separator 18,
Nitroanisole storage tank 19, wastewater trough 20；
Described one-level sodium methoxide solution preparation kettle 6 is identical with secondary methanol sodium solution preparation kettle 7 structure, described one-level methoxylation
12, two grades of methoxylation kettles 13 of kettle, three-level methoxylation kettle 14 structure all same；
Described one-level sodium methoxide solution is prepared kettle 6 top and is provided with methanol charging aperture, flaky sodium hydrate input port, one-level Feldalat NM
Solution is prepared kettle 6 side wall and is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export；
Described one-level methoxylation kettle 12 top is provided with Feldalat NM charging aperture, chloronitrobenzene charging aperture, one-level methoxylation kettle 12
Side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, and one-level methoxylation kettle 12 bottom is provided with first
Epoxide kettle drain；
Described separator 18 is provided with separator material inlet, light liquid outlet, heavy liquid exit；
Described washing water storage tank 1 is connected with washings dosing pump 2 by pipeline, and washings dosing pump 2 passes through pipeline and three-level first
Epoxide kettle 14 charging aperture connects, and methanol storage tank 2 connects with methanol dosing pump 4 by pipeline, methanol dosing pump 4 by pipeline and
One-level sodium methoxide solution prepares the methanol charging aperture connection of kettle 6, and conveying worm 5 is passed through pipeline and prepared with one-level sodium methoxide solution
Kettle 6 flaky sodium hydrate input port connection, one-level sodium methoxide solution prepare kettle 6 Feldalat NM mixture export pass through pipeline with
Secondary methanol sodium solution prepares the Feldalat NM mixed liquor inlet communication of kettle 7, and secondary methanol sodium solution prepares the Feldalat NM mixing of kettle 7
Liquid outlet is connected with sodium methoxide solution storage tank 8 by pipeline, and sodium methoxide solution storage tank 8 passes through pipeline with Feldalat NM dosing pump 9 even
Logical, Feldalat NM dosing pump 9 connect with the Feldalat NM charging aperture of one-level methoxylation kettle 12, chloronitrobenzene storage tank 10 by pipeline and
Chloronitrobenzene dosing pump 11 connects, and chloronitrobenzene dosing pump 11 passes through the chloronitrobenzene charging of pipeline and one-level methoxylation 12
Mouth connection, the methoxylation kettle mixture export of one-level methoxylation kettle 12 passes through the methoxy of pipeline and two grades of methoxylation kettles 13
Base kettle mixed liquor inlet communication, the methoxylation kettle mixture export of two grades of methoxylation kettles 13 passes through pipeline and three-level methoxy
The methoxylation kettle mixed liquor inlet communication of base kettle 14, the methoxylation kettle drain of three-level methoxylation kettle 14 passes through pipeline
Connect with dealcoholysis tower dosing pump 15, dealcoholysis tower dosing pump 15 is connected with dealcoholysis tower 16 by pipeline, pipe is passed through at dealcoholysis tower 16 top
Road is connected with methanol storage tank 3, and dealcoholysis tower 16 bottom is connected with cooler 17 by pipeline, and cooler 17 passes through pipeline and separator 18
Separator material inlet connection, separator 18 light liquid outlet connected with wastewater trough 20 by pipeline, the heavy-fluid of separator 18
Outlet is connected with Nitroanisole storage tank 19 by pipeline.
One-level sodium methoxide solution is prepared kettle 6 and is included internal low head 22, internal straight barrel 23, upper cover 27, outer subordinate envelope
21st, outside straight barrel 24, dasher 31, shaft 30, actuating device 26, described actuating device 26 is fixed on by support
Upper cover 27, dasher 31 is two-layer blade, is connected with actuating device 26 by shaft 30, straight barrel 23 side wall sets
There are Feldalat NM mixed liquor import, Feldalat NM mixture export, be provided with inside the straight barrel 23 of Feldalat NM mixture export side
Discharging weir 29, the open upper end on discharging weir 29, the lower end on discharging weir 29 is internal with straight barrel 23 to be connected, and described sodium methoxide solution is joined
The upper cover 27 of kettle 6 processed is provided with flaky sodium hydrate and adds mouth, methanol charging aperture；
One-level methoxylation kettle 12 includes low head 33, straight barrel 35, upper cover 39, guide shell 34, agitator 43, shaft
42nd, heat exchange coil 36 and actuating device 38, described actuating device 38 is fixed on upper cover 39 by support, and guide shell 34 passes through to prop up
Frame is fixed in straight barrel 35, and guide shell 34 inwall is provided with radial direction baffle plate 45, and agitator 43 passes through shaft 42 and actuating device
38 connections, paddle device 43 is suspended in guide shell 34, is provided with heat exchange coil 36, straight barrel between straight barrel 35 and guide shell 34
35 side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, goes out in methoxylation kettle mixed liquor
It is provided with discharging weir 40, the opened upper end on discharging weir 40, in the bottom on discharging weir 40 and straight barrel 35 inside the straight barrel of mouth side
Portion connects, and the upper cover 39 of described one-level methoxylation kettle 12 is provided with sodium methoxide solution charging aperture, chloronitrobenzene charging aperture, its
In, sodium methoxide solution charging aperture is connected with sodium methoxide solution feed conduit one end, and the sodium methoxide solution feed conduit other end is placed in
In guide shell 35, chloronitrobenzene charging aperture is connected with chloronitrobenzene feed conduit one end, the Nitroanisole feed conduit other end
It is placed in 35 in guide shell；
Separator 18 is the density contrast using two kinds of liquid, designs according to law of connected vessels, the housing of separator 18 is by front
Side plate 48, left plate 49, right plate 52, the back side panel 51 with radian, base plate 55, top board 54 form, and set in separator 18 housing
There is dividing plate 50, dividing plate 50 is fixed with front side board 48, base plate 55 sealing, and dividing plate 50 leaves gap with the back side panel 51 with radian, every
Separator 18 enclosure interior is divided into feed zone and sub-material area by plate 50, and feed zone is connected by gap with sub-material area, in feed zone
Front side board 48 be provided with mixed liquor import 47, light liquid outlet 46 and heavy liquid exit 45 is provided with the front side board 48 in sub-material area,
Light liquid outlet 46 is higher than heavy liquid exit 45, and heavy liquid exit 45 connects with mozzle 53 sidepiece, mozzle 53 lower end and separator 18
Connection in housing, mozzle 53 upper end, lower end are all unlimited.
A kind of Nitroanisole production method of the device continuously producing Nitroanisole based on chloronitrobenzene, including following
Step:
Step 1, one-level sodium methoxide solution prepare kettle 6, secondary methanol sodium solution prepare kettle 7 in compounding methanol sodium solution: pass through
Conveying worm 5 is prepared in kettle 6 to one-level sodium methoxide solution and is added quantitative flaky sodium hydrate, starts stirring, then methanol
Methanol in storage tank 3 puts into one-level sodium methoxide solution by dosing pump 4 and prepares in kettle 6, after flaky sodium hydrate all dissolves,
Continuously add flaky sodium hydrate and methanol by mol ratio 15:1 of methanol and sodium hydroxide, sodium methoxide solution prepares kettle temperature degree control
At 35～40 DEG C, sodium methoxide solution continuously flow to sodium methoxide solution storage tank 8 to system.Step 2, in 12, two grades of one-level methoxylation kettle
Put into the methanol of kettle dischargeable capacity 70% in methoxylation kettle 13, three-level methoxylation kettle 14, start stirring, be warming up to 70 DEG C,
By sodium methoxide solution, (in terms of sodium hydroxide, paranitrochlorobenzene mol ratio 1.25:1 continuously adds sodium methoxide solution and to nitroxyl chloride
Benzene carries out methoxylation, when two grades of methoxylation kettles 13 have reactant liquor to flow into three-level methoxylation kettle 14, by washings
Washings in storage tank 1 are continuously added to three-level methoxylation kettle 14 by washings dosing pump 2, and washings press 1:2.5(to nitre
Base methyl phenyl ethers anisole and the volume ratio of washings) ratio adds, one-level methoxylation kettle 12, two grades of methoxylation kettles 13, three-level methoxies
Base kettle 14 reaction temperature all controls at 70～120 DEG C, and reaction pressure rises to 0.1～0.5mpa, three-level methoxylation kettle naturally
In 14, reactant liquor sends into dealcoholysis tower 16 with dealcoholysis tower feed pump 15.Step 3, reactant liquor carry out separating in dealcoholysis tower 16, wherein,
Control dealcoholysis tower 16 tower top temperature: 65～70 DEG C, dealcoholysis tower 16 column bottom temperature: 100～120 DEG C, dealcoholysis tower 16 overhead extraction first
Alcohol specific gravity control is at 0.792～0.796(20 DEG C) between, the extraction of dealcoholysis tower 16 tower top methanol flows into methanol storage tank 3, for methanol
Sodium solution is prepared, and flows into separator 18, separator 18 is continuously divided after the cooled device of kettle material 17 cooling of methanol storage tank 3
From the paranitroanisole after separating flows into paranitroanisole storage tank 19, and waste water flows into waste water tank 20.
Embodiment 3
A kind of chloronitrobenzene continuously produces the device of Nitroanisole, including washing water storage tank 1, washings dosing pump 2, methanol storage
Groove 3, methanol dosing pump 4, conveying worm 5, one-level Feldalat NM meter solution prepare kettle 6, secondary methanol sodium solution prepares kettle 7, first
Sodium alkoxide solution storage tank 8, Feldalat NM dosing pump 9, chloronitrobenzene storage tank 10, chloronitrobenzene dosing pump 11, one-level methoxylation kettle 12,
Two grades of methoxylation kettles 13, three-level methoxylation kettle 14, dealcoholysis tower dosing pump 15, dealcoholysis tower 16, cooler 17, separator 18,
Nitroanisole storage tank 19, wastewater trough 20；
Described one-level sodium methoxide solution preparation kettle 6 is identical with secondary methanol sodium solution preparation kettle 7 structure, described one-level methoxylation
12, two grades of methoxylation kettles 13 of kettle, three-level methoxylation kettle 14 structure all same；
Described one-level sodium methoxide solution is prepared kettle 6 top and is provided with methanol charging aperture, flaky sodium hydrate input port, one-level Feldalat NM
Solution is prepared kettle 6 side wall and is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export；
Described one-level methoxylation kettle 12 top is provided with Feldalat NM charging aperture, chloronitrobenzene charging aperture, one-level methoxylation kettle 12
Side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, and one-level methoxylation kettle 12 bottom is provided with first
Epoxide kettle drain；
Described separator 18 is provided with separator material inlet, light liquid outlet, heavy liquid exit；
Described washing water storage tank 1 is connected with washings dosing pump 2 by pipeline, and washings dosing pump 2 passes through pipeline and three-level first
Epoxide kettle 14 charging aperture connects, and methanol storage tank 2 connects with methanol dosing pump 4 by pipeline, methanol dosing pump 4 by pipeline and
One-level sodium methoxide solution prepares the methanol charging aperture connection of kettle 6, and conveying worm 5 is passed through pipeline and prepared with one-level sodium methoxide solution
Kettle 6 flaky sodium hydrate input port connection, one-level sodium methoxide solution prepare kettle 6 Feldalat NM mixture export pass through pipeline with
Secondary methanol sodium solution prepares the Feldalat NM mixed liquor inlet communication of kettle 7, and secondary methanol sodium solution prepares the Feldalat NM mixing of kettle 7
Liquid outlet is connected with sodium methoxide solution storage tank 8 by pipeline, and sodium methoxide solution storage tank 8 passes through pipeline with Feldalat NM dosing pump 9 even
Logical, Feldalat NM dosing pump 9 connect with the Feldalat NM charging aperture of one-level methoxylation kettle 12, chloronitrobenzene storage tank 10 by pipeline and
Chloronitrobenzene dosing pump 11 connects, and chloronitrobenzene dosing pump 11 passes through the chloronitrobenzene charging of pipeline and one-level methoxylation 12
Mouth connection, the methoxylation kettle mixture export of one-level methoxylation kettle 12 passes through the methoxy of pipeline and two grades of methoxylation kettles 13
Base kettle mixed liquor inlet communication, the methoxylation kettle mixture export of two grades of methoxylation kettles 13 passes through pipeline and three-level methoxy
The methoxylation kettle mixed liquor inlet communication of base kettle 14, the methoxylation kettle drain of three-level methoxylation kettle 14 passes through pipeline
Connect with dealcoholysis tower dosing pump 15, dealcoholysis tower dosing pump 15 is connected with dealcoholysis tower 16 by pipeline, pipe is passed through at dealcoholysis tower 16 top
Road is connected with methanol storage tank 3, and dealcoholysis tower 16 bottom is connected with cooler 17 by pipeline, and cooler 17 passes through pipeline and separator 18
Separator material inlet connection, separator 18 light liquid outlet connected with wastewater trough 20 by pipeline, the heavy-fluid of separator 18
Outlet is connected with Nitroanisole storage tank 19 by pipeline.
One-level sodium methoxide solution is prepared kettle 6 and is included internal low head 22, internal straight barrel 23, upper cover 27, outer subordinate envelope
21st, outside straight barrel 24, dasher 31, shaft 30, actuating device 26, described actuating device 26 is fixed on by support
Upper cover 27, dasher 31 is two-layer blade, is connected with actuating device 26 by shaft 30, straight barrel 23 side wall sets
There are Feldalat NM mixed liquor import, Feldalat NM mixture export, be provided with inside the straight barrel 23 of Feldalat NM mixture export side
Discharging weir 29, the open upper end on discharging weir 29, the lower end on discharging weir 29 is internal with straight barrel 23 to be connected, and described sodium methoxide solution is joined
The upper cover 27 of kettle 6 processed is provided with flaky sodium hydrate and adds mouth, methanol charging aperture；
One-level methoxylation kettle 12 includes low head 33, straight barrel 35, upper cover 39, guide shell 34, agitator 43, shaft
42nd, heat exchange coil 36 and actuating device 38, described actuating device 38 is fixed on upper cover 39 by support, and guide shell 34 passes through to prop up
Frame is fixed in straight barrel 35, and guide shell 34 inwall is provided with radial direction baffle plate 45, and agitator 43 passes through shaft 42 and actuating device
38 connections, paddle device 43 is suspended in guide shell 34, is provided with heat exchange coil 36, straight barrel between straight barrel 35 and guide shell 34
35 side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, goes out in methoxylation kettle mixed liquor
It is provided with discharging weir 40, the opened upper end on discharging weir 40, in the bottom on discharging weir 40 and straight barrel 35 inside the straight barrel of mouth side
Portion connects, and the upper cover 39 of described one-level methoxylation kettle 12 is provided with sodium methoxide solution charging aperture, chloronitrobenzene charging aperture, its
In, sodium methoxide solution charging aperture is connected with sodium methoxide solution feed conduit one end, and the sodium methoxide solution feed conduit other end is placed in
In guide shell 35, chloronitrobenzene charging aperture is connected with chloronitrobenzene feed conduit one end, the Nitroanisole feed conduit other end
It is placed in 35 in guide shell；
Separator 18 is the density contrast using two kinds of liquid, designs according to law of connected vessels, the housing of separator 18 is by front
Side plate 48, left plate 49, right plate 52, the back side panel 51 with radian, base plate 55, top board 54 form, and set in separator 18 housing
There is dividing plate 50, dividing plate 50 is fixed with front side board 48, base plate 55 sealing, and dividing plate 50 leaves gap with the back side panel 51 with radian, every
Separator 18 enclosure interior is divided into feed zone and sub-material area by plate 50, and feed zone is connected by gap with sub-material area, in feed zone
Front side board 48 be provided with mixed liquor import 47, light liquid outlet 46 and heavy liquid exit 45 is provided with the front side board 48 in sub-material area,
Light liquid outlet 46 is higher than heavy liquid exit 45, and heavy liquid exit 45 connects with mozzle 53 sidepiece, mozzle 53 lower end and separator 18
Connection in housing, mozzle 53 upper end, lower end are all unlimited.
A kind of Nitroanisole production method of the device continuously producing Nitroanisole based on chloronitrobenzene, including following
Step:
Step 1, one-level sodium methoxide solution prepare kettle 6, secondary methanol sodium solution prepare kettle 7 in compounding methanol sodium solution: pass through
Conveying worm 5 is prepared in kettle 6 to one-level sodium methoxide solution and is added quantitative flaky sodium hydrate, starts stirring, then methanol
Methanol in storage tank 3 puts into one-level sodium methoxide solution by dosing pump 4 and prepares in kettle 6, after flaky sodium hydrate all dissolves,
Continuously add flaky sodium hydrate and methanol by mol ratio 13:1 of methanol and sodium hydroxide, sodium methoxide solution prepares kettle temperature degree control
At 35～40 DEG C, sodium methoxide solution continuously flow to sodium methoxide solution storage tank 8 to system.Step 2, in 12, two grades of one-level methoxylation kettle
Put into the methanol of kettle dischargeable capacity 70% in methoxylation kettle 13, three-level methoxylation kettle 14, start stirring, be warming up to 70 DEG C,
Continuously throw by mixture mol ratio 1.30:1 of sodium methoxide solution (in terms of sodium hydroxide) and o-nitrochlorobenzene and paranitrochlorobenzene
Plus sodium methoxide solution carries out methoxylation with o-nitrochlorobenzene and paranitrochlorobenzene mixture, treat two grades of methoxylation kettles 13
When having reactant liquor to flow into three-level methoxylation kettle 14, the washings in washing water storage tank 1 are passed through washings dosing pump 2 to three-level
Methoxylation kettle 14 is continuously added to, and washings are in the volume ratio of 1:3(Nitroanisole and washings) ratio adds, one-level methoxy
12, two grades of methoxylation kettles 13 of base kettle, three-level methoxylation kettle 14 reaction temperature all control at 70～120 DEG C, reaction pressure
Naturally rise to 0.1～0.5mpa, in three-level methoxylation kettle 14, reactant liquor sends into dealcoholysis tower 16 with dealcoholysis tower feed pump 15.Step
3rd, reactant liquor carries out separating in dealcoholysis tower 16, wherein, control dealcoholysis tower 16 tower top temperature: 65～70 DEG C, dealcoholysis tower 16 bottom of towe
Temperature: 100～120 DEG C, dealcoholysis tower 16 overhead extraction methanol specific gravity control is at 0.792～0.796(20 DEG C) between, dealcoholysis tower 16
The extraction of tower top methanol flows into methanol storage tank 3, prepares for sodium methoxide solution, and the kettle material cooled device 17 of methanol storage tank 3 is cold
But flow into separator 18 afterwards, separator 18 is continuously separated, and the Nitroanisole after separating flows into Nitroanisole storage tank 19,
Waste water flows into waste water tank 20.
Claims (10)
1. a kind of chloronitrobenzene continuously produces the device of Nitroanisole it is characterised in that including washing water storage tank (1), washing
Water dosing pump (2), methanol storage tank (3), methanol dosing pump (4), conveying worm (5), one-level Feldalat NM meter solution prepare kettle
(6), secondary methanol sodium solution prepares kettle (7), sodium methoxide solution storage tank (8), Feldalat NM dosing pump (9), chloronitrobenzene storage tank
(10), chloronitrobenzene dosing pump (11), one-level methoxylation kettle (12), two grades of methoxylation kettles (13), three-level methoxylation kettles
(14), dealcoholysis tower dosing pump (15), dealcoholysis tower (16), cooler (17), separator (18), Nitroanisole storage tank (19), useless
Tank (20)；
Described one-level sodium methoxide solution preparation kettle (6) is identical with secondary methanol sodium solution preparation kettle (7) structure, described one-level methoxy
Base kettle (12), two grades of methoxylation kettles (13), three-level methoxylation kettle (14) structure all sames；
Described one-level sodium methoxide solution is prepared kettle (6) top and is provided with methanol charging aperture, flaky sodium hydrate input port, one-level methanol
Sodium solution is prepared kettle (6) side wall and is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export；
Described one-level methoxylation kettle (12) top is provided with Feldalat NM charging aperture, chloronitrobenzene charging aperture, one-level methoxylation kettle
(12) side wall is provided with methoxylation kettle mixed liquor import, methoxylation kettle mixture export, one-level methoxylation kettle (12) bottom
It is provided with methoxylation kettle drain；
Described separator (18) is provided with separator material inlet, light liquid outlet, heavy liquid exit；
Described washing water storage tank (1) connects with washings dosing pump (2) by pipeline, washings dosing pump (2) by pipeline and
Three-level methoxylation kettle (14) charging aperture connects, and methanol storage tank (2) is connected with methanol dosing pump (4) by pipeline, and methanol measures
Pump (4) is passed through pipeline and is connected with the methanol charging aperture of one-level sodium methoxide solution preparation kettle (6), and conveying worm (5) passes through pipeline
The flaky sodium hydrate input port preparing kettle (6) with one-level sodium methoxide solution connects, and one-level sodium methoxide solution prepares the first of kettle (6)
Sodium alkoxide mixture export passes through pipeline and secondary methanol sodium solution prepares the Feldalat NM mixed liquor inlet communication of kettle (7), two grades of first
The Feldalat NM mixture export that alcohol sodium solution prepares kettle (7) is connected with sodium methoxide solution storage tank (8) by pipeline, sodium methoxide solution
Storage tank (8) is connected with Feldalat NM dosing pump (9) by pipeline, the first of Feldalat NM dosing pump (9) and one-level methoxylation kettle (12)
Sodium alkoxide charging aperture connects, and chloronitrobenzene storage tank (10) is connected with chloronitrobenzene dosing pump (11) by pipeline, and chloronitrobenzene measures
Pump (11) is connected with the chloronitrobenzene charging aperture of one-level methoxylation (12) by pipeline, the first of one-level methoxylation kettle (12)
Epoxide kettle mixture export passes through the methoxylation kettle mixed liquor inlet communication of pipeline and two grades of methoxylation kettles (13), two grades
The methoxylation kettle mixture export of methoxylation kettle (13) passes through the methoxylation kettle of pipeline and three-level methoxylation kettle (14)
Mixed liquor inlet communication, the methoxylation kettle drain of three-level methoxylation kettle (14) passes through pipeline and dealcoholysis tower dosing pump (15)
Connection, dealcoholysis tower dosing pump (15) is connected with dealcoholysis tower (16) by pipeline, and dealcoholysis tower (16) top is passed through pipeline and store with methanol
Groove (3) connects, and dealcoholysis tower (16) bottom is connected with cooler (17) by pipeline, and cooler (17) passes through pipeline and separator (18)
Separator material inlet connection, separator (18) light liquid outlet connected with wastewater trough (20) by pipeline, separator (18)
Heavy liquid exit connected with Nitroanisole storage tank (19) by pipeline.
2. according to claim 1 chloronitrobenzene continuously produce Nitroanisole device it is characterised in that: described one-level first
Alcohol sodium solution is prepared kettle (6) and is included internal low head (22), internal straight barrel (23), upper cover (27), outer subordinate envelope (21), outer
Portion's straight barrel (24), dasher (31), shaft (30), actuating device (26), described actuating device (26) passes through support
It is fixed on upper cover (27), dasher (31) is two-layer blade, is connected with actuating device (26) by shaft (30), directly
Cylinder (23) side wall is provided with Feldalat NM mixed liquor import, Feldalat NM mixture export, in Feldalat NM mixture export side
It is provided with discharging weir (29), the open upper end of discharging weir (29), the lower end of discharging weir (29) and straight barrel inside straight barrel (23)
(23) internal connection, the upper cover (27) that described sodium methoxide solution prepares kettle (6) is provided with that flaky sodium hydrate adds mouth, methanol enters
Material mouth；
According to claim 1 chloronitrobenzene continuously produce Nitroanisole device it is characterised in that: described one-level methoxy
Base kettle (12) includes low head (33), straight barrel (35), upper cover (39), guide shell (34), agitator (43), shaft
(42), heat exchange coil (36) and actuating device (38), described actuating device (38) is fixed on upper cover (39), water conservancy diversion by support
Cylinder (34) is fixed in straight barrel (35) by support, and guide shell (34) inwall is provided with radial direction baffle plate (45), and agitator (43) leads to
Cross shaft (42) to be connected with actuating device (38), paddle device (43) is suspended in guide shell (34), straight barrel (35) with lead
It is provided with heat exchange coil (36), the side wall of straight barrel (35) is provided with methoxylation kettle mixed liquor import, methoxy between flow cartridge (34)
Base kettle mixture export, is provided with discharging weir (40), discharging weir inside the straight barrel of methoxylation kettle mixture export side
(40) opened upper end, the bottom of discharging weir (40) connects with inside straight barrel (35), described one-level methoxylation kettle (12)
Upper cover (39) is provided with sodium methoxide solution charging aperture, chloronitrobenzene charging aperture, and wherein, sodium methoxide solution charging aperture is molten with Feldalat NM
Liquid feed conduit one end connects, and the sodium methoxide solution feed conduit other end is placed in guide shell (35), chloronitrobenzene charging aperture with
Chloronitrobenzene feed conduit one end connects, and the Nitroanisole feed conduit other end is placed in guide shell (35)；
According to claim 1 chloronitrobenzene continuously produce Nitroanisole device it is characterised in that: described separator
(18) it is density contrast using two kinds of liquid, design according to law of connected vessels, the housing of separator (18) is by front side board
(48), left plate (49), right plate (52), the back side panel with radian (51), base plate (55), top board (54) composition, separator
(18) it is provided with dividing plate (50), dividing plate (50) and front side board (48), base plate (55) sealing fixation, dividing plate (50) and band radian in housing
Back side panel (51) leave gap, separator (18) enclosure interior is divided into feed zone and sub-material area by dividing plate (50), feed zone with
Sub-material area is connected by gap, is provided with mixed liquor import (47), in the front side board in sub-material area on the front side board (48) of feed zone
(48) it is provided with light liquid outlet (46) and heavy liquid exit (45), light liquid outlet (46) is higher than heavy liquid exit (45), heavy liquid exit
(45) connect with mozzle (53) sidepiece, mozzle (53) lower end connects with separator (18) housing, mozzle (53) upper end,
Lower end is all unlimited.
3. a kind of Nitroanisole producer of the device continuously producing Nitroanisole based on chloronitrobenzene described in claim 1
Method is it is characterised in that comprise the following steps:
Step 1, prepare kettle (6) in one-level sodium methoxide solution, secondary methanol sodium solution prepares compounding methanol sodium solution in kettle (7):
Prepared in kettle (6) to one-level sodium methoxide solution by conveying worm (5) and add quantitative flaky sodium hydrate, start stirring,
Then the methanol in methanol storage tank (3) puts into one-level sodium methoxide solution by dosing pump (4) and prepares in kettle (6), treats lamellar hydrogen-oxygen
After changing the whole dissolving of sodium, continuously add flaky sodium hydrate and methanol, compounding methanol sodium solution, sodium methoxide solution by setting ratio
Continuously it flow to sodium methoxide solution storage tank (8).
4. step 2, put in one-level methoxylation kettle (12), two grades of methoxylation kettles (13), three-level methoxylation kettle (14)
The methanol of kettle dischargeable capacity 70%, starts stirring, is warming up to design temperature, continuously adds sodium methoxide solution and nitro in proportion
Chlorobenzene, carries out methoxylation, when two grades of methoxylation kettles (13) have reactant liquor to flow into three-level methoxylation kettle (14), will
Washings in washing water storage tank (1) are continuously added to three-level methoxylation kettle (14) by washings dosing pump (2), three-level first
In epoxide kettle (14), reactant liquor sends into dealcoholysis tower (16) with dealcoholysis tower dosing pump (15).
5. step 3, reactant liquor carry out separating in dealcoholysis tower (16), and wherein, the extraction of dealcoholysis tower (16) tower top methanol flows into methanol
Storage tank (3), prepares for sodium methoxide solution, flows into separator after the cooled device of kettle material (17) cooling of methanol storage tank (3)
(18), separator (18) is continuously separated, and the Nitroanisole after separating flows into Nitroanisole storage tank, and waste water flows into waste water
Storage tank.
6. production method according to claim 5 is it is characterised in that in sodium methoxide solution process for preparation in step 1, adopt
Conveying worm adds flaky sodium hydrate, and piece alkali dosage passes through the motor speed control of converter adjustable screw conveyer (5)
System.
7. production method according to claim 5 it is characterised in that in step 1 chloronitrobenzene can be o-nitrochlorobenzene
Or the mixture of paranitrochlorobenzene or o-nitrochlorobenzene and paranitrochlorobenzene arbitrary proportion.
8. production method according to claim 5 is it is characterised in that in sodium methoxide solution process for preparation in step 1, methanol
Mol ratio with sodium hydroxide is: 8～15:1, and sodium methoxide solution is prepared temperature and is: 30～50 DEG C.
9. production method according to claim 5 is it is characterised in that during methoxylation in step 2, sodium methoxide solution
(in terms of sodium hydroxide) with the mol ratio of chloronitrobenzene is: 1.1～1.2:1, and reaction pressure is: 0.30～0.40mpa, reaction
Temperature is: 95～100 DEG C.
10. production method according to claim 5 it is characterised in that in step 3 dealcoholysis tower (16) tower top temperature be: 65
～70 DEG C, bottom temperature is 100～120 DEG C, and dealcoholysis tower (16) overhead extraction methanol specific gravity control is in 0.792～0.796(20
DEG C) between.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610866504.0A CN106336359A (en) | 2016-09-30 | 2016-09-30 | Device for continuously producing nitroanisole through nitrochlorobenzene and production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610866504.0A CN106336359A (en) | 2016-09-30 | 2016-09-30 | Device for continuously producing nitroanisole through nitrochlorobenzene and production method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106336359A true CN106336359A (en) | 2017-01-18 |
Family
ID=57839554
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610866504.0A Pending CN106336359A (en) | 2016-09-30 | 2016-09-30 | Device for continuously producing nitroanisole through nitrochlorobenzene and production method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106336359A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369409A (en) * | 2018-11-09 | 2019-02-22 | 宁夏华御化工有限公司 | Nitro-chlorobenzene produces interposition oil separation reutilization system and meta position oil separating method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276483A (en) * | 2011-06-30 | 2011-12-14 | 辽宁世星药化有限公司 | Production method of oamino pheylmethyl ether |
| CN102320978A (en) * | 2011-09-22 | 2012-01-18 | 江苏康恒化工有限公司 | Preparation method of anhydrous system o-nitroanisole |
| CN102580629A (en) * | 2012-03-20 | 2012-07-18 | 中国天辰工程有限公司 | Gas-liquid-liquid-solid reaction device |
| CN105566121A (en) * | 2014-10-11 | 2016-05-11 | 中国石油化工股份有限公司 | Method for reducing generation of nitrophenol in preparation process of nitroanisole |
-
2016
- 2016-09-30 CN CN201610866504.0A patent/CN106336359A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276483A (en) * | 2011-06-30 | 2011-12-14 | 辽宁世星药化有限公司 | Production method of oamino pheylmethyl ether |
| CN102320978A (en) * | 2011-09-22 | 2012-01-18 | 江苏康恒化工有限公司 | Preparation method of anhydrous system o-nitroanisole |
| CN102580629A (en) * | 2012-03-20 | 2012-07-18 | 中国天辰工程有限公司 | Gas-liquid-liquid-solid reaction device |
| CN105566121A (en) * | 2014-10-11 | 2016-05-11 | 中国石油化工股份有限公司 | Method for reducing generation of nitrophenol in preparation process of nitroanisole |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369409A (en) * | 2018-11-09 | 2019-02-22 | 宁夏华御化工有限公司 | Nitro-chlorobenzene produces interposition oil separation reutilization system and meta position oil separating method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN207221901U (en) | A kind of modified reaction kettle of the esterification | |
| CN209530732U (en) | A kind of corrosion inhibiter compounding agitator tank | |
| CN106336359A (en) | Device for continuously producing nitroanisole through nitrochlorobenzene and production method | |
| CN206512117U (en) | Nitro-chlorobenzene continuously produces the device of Nitroanisole | |
| CN203935841U (en) | A kind of efficient circulation reactor | |
| CN208320772U (en) | The automated production equipment of silicone oil | |
| CN214681746U (en) | Zinc reagent preparation facilities and reaction system | |
| CN215782906U (en) | Surface reinforcing agent preparation agitating unit | |
| CN210787321U (en) | Stirring reaction kettle | |
| CN202447063U (en) | High-efficiency reaction kettle | |
| CN106431940B (en) | Reduction with sodium bisulfide produces the device and method of aminoanisole | |
| CN209810150U (en) | Reation kettle of medical intermediate production usefulness with cooling function | |
| CN207493683U (en) | A kind of reaction kettle for being evenly heated or cooling down | |
| CN102068944B (en) | Filtration formula stirring reactor | |
| CN206328318U (en) | Reduction with sodium bisulfide produces the device of aminoanisole | |
| CN202366684U (en) | Continuous ethyl hexanoate esterification reaction kettle | |
| CN205164689U (en) | Liquid reaction device | |
| CN204911501U (en) | Stirring formula reation kettle | |
| CN205815673U (en) | Hypothermic response still | |
| CN210700113U (en) | Draw pig source reation kettle rapid heating device for heparin sodium | |
| CN105381768A (en) | Liquid reaction device | |
| CN110054380A (en) | A kind of sludge continuous low-temperature thermokalite combined pretreatment device | |
| CN215611538U (en) | Reaction kettle structure for carrying out sufficient reaction | |
| CN213557015U (en) | Chemical reaction kettle for cooling water recycling | |
| CN216605238U (en) | A reation kettle for concrete retarder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170118 |
|
| WD01 | Invention patent application deemed withdrawn after publication |