CN105601520B - A kind of nitromethane synthesis and product separator - Google Patents
A kind of nitromethane synthesis and product separator Download PDFInfo
- Publication number
- CN105601520B CN105601520B CN201610152401.8A CN201610152401A CN105601520B CN 105601520 B CN105601520 B CN 105601520B CN 201610152401 A CN201610152401 A CN 201610152401A CN 105601520 B CN105601520 B CN 105601520B
- Authority
- CN
- China
- Prior art keywords
- reactor
- steam kettle
- crude
- crude steam
- product
- 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.)
- Active
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
-
- 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
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to chemical fields, particularly disclose a kind of nitromethane synthesis and product separator.The nitromethane synthesizes and product separator, including the horizontal reactor, product separator and product purifying device being linked in sequence from front to back, the cavity of the horizontal reactor is separated into several interconnected reaction members by several flow-stopping plates, a reactor rabbling mechanism for running through each reaction member is equipped with along the axis direction of horizontal reactor in the cavity of horizontal reactor, the front end of the reactor rabbling mechanism is connected after being pierced by the head end side wall of horizontal reactor with a reactor driving mechanism.Nitromethane synthesis of the present invention and product separator, solve the problems, such as that domestic nitrite displacement method production nitromethane can only use batch production at present, after continuous reaction and distillation operation, it can preferably realize industrial-scale production, reduce production cost, production efficiency is improved, solves the problems such as environmental pollution.
Description
Technical field
The present invention relates to chemical field, more particularly to a kind of nitromethane synthesis and product separator.
Background technology
Existing nitromethane synthetic reaction is produced mostly using simple reaction kettle interval, is passed through in production process
Sodium nitrite solid is manually put into reaction kettle, sodium nitrite solid carries out anti-with dimethyl suflfate after being dissolved in reaction kettle
It should.However dimethyl suflfate can also occur hydrolytic side reactions with water, reduce the yield of reaction while reacted with sodium nitrite.
In production, in order to reduce the generation of side reaction, dimethyl suflfate is made fully to be reacted with sodium nitrite, usually by way of dropwise addition
Add in dimethyl suflfate, can only in batches, the operation of discontinuity, production efficiency is very low, and produce during expend it is more
Manpower.Secondly, dimethyl suflfate is exothermic reaction with reacting for sodium nitrite, can generate a large amount of heat in reaction process, make kettle
Interior temperature quickly increases, but traditional reaction kettle control temperature in the kettle is relatively difficult.When reaction condition control is improper, temperature is too
Low that reaction rate can be made not react even slowly very much, temperature is too high and can increase side reaction, and there are larger contingency, cause
Yield is unstable.Again, the toxic gases such as nitrous acid hydrogen methyl esters can be generated in reaction process, traditional reaction kettle can not be disposed properly
These toxic gases, the working environment of worker is poor, and there are larger security risks.
Nitromethane synthetic reaction can also generate a large amount of sodium sulphate other than generating nitromethane product.Sodium sulphate conduct
The byproduct of nitromethane production, is largely present in nitromethane waste water, has been more than the pollutant emission standard of country.Together
When, sodium sulphate is as a kind of important industrial chemicals, if not recovered with regard to direct emission, not only having polluted environment but also waste of resource.
After traditional sodium sulphate processing method is the nitromethane Waste water concentrating by sulfur acid sodium, then again by centrifuge by concentrate
In solid sodium sulfate abjection.This processing method has the following disadvantages：First, the nitromethane waste water of sulfur acid sodium is concentrated
Viscosity is very big afterwards, and the reaction kettle that while concentrating uses is spherical reaction kettle, and the opening of autoclave body bottom is smaller, leads to what is be concentrated to give
Sodium sulphate is difficult to be discharged by the opening of autoclave body bottom, is needed again into reaction kettle plus water, make sodium sulphate be diluted to paste from
Autoclave body bottom is discharged, and is re-fed into centrifuge and is dehydrated again.Secondly, sulfuric acid in the waste water after solid sodium sulfate is thrown away by centrifuge
Sodium content is still higher, even saturated solution, it is impossible to discharge or recycle immediately, it is also necessary to be further processed, work
Sequence is more complicated, reduces production efficiency, and energy consumption is larger.Again, in this processing method centrifuge operation when
Material is needed to be evenly distributed in centrifuge, if material is unevenly distributed, the operation of centrifuge leads to disequilibrium bad shocking
Centrifuge is easily damaged, and increases the repair input in later stage, and the safety of Field Force can be even threatened when serious.Finally, waste water
In can inevitably contain the harmful substances such as nitromethane, and nitromethane is readily volatilized in air, and the body of employee is caused to damage
Evil, there are some potential safety problemss.
Contain moisture in the crude product nitromethane that nitromethane synthetic reaction obtains, need to be sent to rectifying column carry out rectifying with
Improve the product purity of nitromethane.To not forming the object system of azeotrope, as long as design and suitable operation, distillate will be high-purity
The volatile components of degree, tower bottom product by be high-purity difficult volatile component.However, nitromethane in crude product nitromethane with
Water can form minimum azeotropic mixture, and when temperature is not increased to the boiling point of water or nitromethane, nitromethane is formed with water
Azeotropic mixture boils already, the mixture of water and nitromethane is made to be difficult to be efficiently separated, general rectifying can not make nitro first
Alkane obtains highly purified.The mode of existing nitromethane distillation process generally use batch fractionating, water and nitre in distillation process
The azeotropic mixture that methylmethane is formed forms liquid at the top of tower reactor after condensed device condensation, then insoluble with water using nitromethane,
The characteristics of will appear liquid level layering between the two, the water after layering is constantly discharged.With the continuous progress of distillation process, nitro
Moisture in methane is constantly reduced, and most obtains the higher nitromethane of purity at last.Traditional this distillation process consumption steam
Energy comparison is more, and distillation process is non-continuous process, increases the input of manpower.In addition, during rectifying, if
Because misoperation causes liquid in kettle to be evaporated, it will serious safety accident occurs.
Therefore, there is an urgent need for a kind of synthesis of nitromethane and product separator to solve more than technical problem.
Invention content
In order to compensate for the shortcomings of the prior art, the present invention provides a kind of reasonable design, improve the product of nitromethane
Purity simplifies the nitromethane synthesis that sodium sulphate recovery process, reaction and distillation process were carried out continuously, reduced human input
And product separator, solve problems of the prior art.
The present invention is achieved through the following technical solutions：
A kind of nitromethane synthesis and product separator, including horizontal reactor, the product being linked in sequence from front to back
Separator and product purifying device, the axis direction of the horizontal reactor housing and the angle of horizontal plane are 0-20 °, described
The cavity of horizontal reactor is separated into several interconnected reaction members by several flow-stopping plates, in horizontal reactor
In cavity a reactor rabbling mechanism for running through each reaction member, the reactor are equipped with along the axis direction of horizontal reactor
The front end of rabbling mechanism is connected after being pierced by the head end side wall of horizontal reactor with a reactor driving mechanism, horizontal reactor compared with
The reaction mixture import that reaction member of the high side roof part equipped with one and front end is interconnected, on the top of horizontal reactor
A reactor exhaust outlet and reactor content outlet port are respectively equipped on portion's side wall and bottom sidewall, after reaction mixture import
The horizontal reactor outer sheath of side is equipped with a reactor cooling body.
The product separator includes crude steam kettle, crude product receiving tank and crude product storage tank, and one is equipped in the outside of crude steam kettle
Crude steam kettle heating arrangements are equipped with a crude steam kettle stirring system in the inside of crude steam kettle, and the lower part of the crude steam kettle is reverse taper knot
Structure, the feed inlet of crude steam kettle are connected with the reaction mixture import of horizontal reactor by pipeline, are set in the bottom of crude steam kettle
Have a crude steam kettle discharge port, the top distillation mouth of crude steam kettle by pipeline successively with a crude steam kettle condenser, crude product receiving tank and
Crude product storage tank is connected, and the top gas outlet of crude product receiving tank is connected by pipeline with the inlet end of a crude product vacuum pump.
The product purifying device includes fractionating column and rectifying column, and the first charging aperture of fractionating column is stored up by pipeline and crude product
The discharge port of tank is connected, the top of the top gas outlet of fractionating column by pipeline after a fractionating column condenser with a phase separation tank
Feed inlet is connected, and the bottom discharge mouth of phase separation tank separates two-way pipeline, is directly connected all the way with the feed inlet of rectifying column, separately
It is connected after an intermediate storage tank with the feed inlet of rectifying column all the way, the top gas outlet of rectifying column is by pipeline through a rectifying column
Top feed mouth after condenser with a product receiving tank is connected, and the upper part discharge port of phase separation tank passes through pipeline and fractionating column
Second charging aperture is connected, and the bottom discharge mouth of rectifying column is connected by pipeline with the refluxing opening of fractionating column, product receiving tank
Bottom discharge mouth separate two-way pipeline, be connected all the way with the refluxing opening of rectifying column, the feed inlet of another way and a products pot
Be connected, the top gas outlet of product receiving tank and the top gas outlet of phase separation tank by pipeline and a purification vacuum pump into
Gas end is connected.
The reactor cooling body includes being set on several on the outside of horizontal reactor along horizontal reactor length direction
Reactor cooling unit, each reactor cooling unit include a reactor cooling jacket being set on the outside of horizontal reactor.
The rabbling mechanism includes the reactor agitating shaft set along the axis direction of horizontal reactor, is stirred in reactor
Axis is mixed equipped with several groups of agitating paddles, the reactor driving mechanism includes a reactor motor, the reactor agitating shaft
Front end is connected after passing through the front end side wall of horizontal reactor through a reactor speed reducer with the output shaft of reactor motor.
The flow-stopping plate is the porous plate set perpendicular to horizontal reactor axis direction, is uniformly provided on porous plate several
A aperture is sheathed on the reactor agitating shaft, and the outer ledge of porous plate is close to horizontal reactor in the middle part of porous plate
Madial wall setting.
The crude steam kettle stirring system includes the crude steam kettle agitating shaft that crude steam kettle inner cavity is set on along crude steam kettle axis direction, slightly
The top of steaming kettle agitating shaft is connected after being pierced by crude steam kettle top sidewall with crude steam kettle driving mechanism, the crude steam kettle driving mechanism packet
Include a crude steam kettle motor, the output shaft of the crude steam kettle motor after a crude steam kettle speed reducer with the front end phase of crude steam kettle agitating shaft
Even, spiral winding is formed with double ribbons on crude steam kettle agitating shaft, and the stirring sheet of a triangle is equipped in the bottom of crude steam kettle agitating shaft,
The two sides of the stirring sheet are parallel with the madial wall of crude steam kettle.
The crude steam kettle heating arrangements include being sheathed on the crude steam kettle chuck on the outside of crude steam kettle.
Double ribbons include interior ribbon and outer ribbon, the center line of interior ribbon and outer ribbon along using crude steam kettle agitating shaft as
The circular helix coiling of center line forms, and the inner side edge of the interior ribbon is fixed on crude steam kettle agitating shaft, the outer ribbon
Quantity for two, the outside that is axially and symmetrically wound on interior ribbon of the two outer ribbons along crude steam kettle agitating shaft, two outer ribbons are distinguished
It is connected by supporting rod with crude steam kettle agitating shaft, the outer side edges of the two outer ribbon and stirring sheet are close to crude steam kettle madial wall and are set
It puts.
The beneficial effects of the invention are as follows：
(1) stage of reaction：
Reaction in horizontal reactor is carried out continuously, and solves domestic nitrite displacement method production nitromethane at present
The problem of batch production can be used, after being operated using continuous reaction, can preferably realize industrial-scale production, simultaneously
Raw material availability is improved, reduces production cost, solves the problems such as environmental pollution.
(2) product separation phase：
After nitromethane and waste water in crude steam kettle are evaporated, sodium sulphate can be directly in powdered from autoclave body lower part blowing
Mouth outflow, the sodium sulphate appearance color of processing is preferable, is conducive to later sale, simplifies process, saves equipment investment, section
A large amount of manpower and materials have been saved, have been conducive to promote and apply.In distillation process, the feed liquid close to crude steam kettle agitating shaft is in interior ribbon
Under push away and moved downward under effect, a part is spilled over the ribbon face into outer ribbon, and material is made to tilt or throw upwardly along ribbon
Go out, the material risen at the top of crude steam kettle flows downward again by the promotion conducted oneself with dignity with outer ribbon, forms inside and outside, upper and lower cycle
Stream, is blended highly viscous sodium sulphate material, convective motion, is uniformly mixed material, and property is uniform, ensures that material is uniform
It is heated.
(3) product purification phase：
By negative pressure rectifying, using the methane principle different with the boiling point of water under vacuum, make the mixed of water and nitromethane
It closes object to efficiently separate, improves the product purity of nitromethane, and also reduce the usage amount of steam；Destilling tower and rectifying column
Inside there is liquid-phase reflux, avoid because misoperation causes liquid in kettle to be evaporated, ensure that safety in production；Distillation process continuously into
Row, reduces human input.
To sum up, nitromethane synthesis of the present invention and product separator solve domestic nitrite displacement method life at present
The problem of batch production can only be used by producing nitromethane, after continuous reaction and distillation operation, can preferably be realized
Industrial-scale production reduces production cost, improves production efficiency, solves the problems such as environmental pollution.
Description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is the enlarged structure schematic diagram of crude steam kettle part in Fig. 1.
In figure, 1, horizontal reactor, 2, flow-stopping plate, 3, reaction member, 4, reaction mixture import, 5, reactor exhaust
Mouthful, 6, reactor content outlet port, 7, crude steam kettle, 8, crude product receiving tank, 9, crude product storage tank, 10, crude steam kettle discharge port, 11, thick
Steam kettle condenser, 12, crude product vacuum pump, 13, fractionating column, 14, rectifying column, 15, fractionating column condenser, 16, phase separation tank, 17, in
Between storage tank, 18, rectifying column condenser, 19, product receiving tank, 20, products pot, 21, purification vacuum pump, 22, reactor cooling folder
Set, 23, reactor agitating shaft, 24, agitating paddle, 25, reactor motor, 26, reactor speed reducer, 27, crude steam kettle agitating shaft,
28th, crude steam kettle motor, 29, crude steam kettle speed reducer, 30, stirring sheet, 31, crude steam kettle chuck, 32, interior ribbon, 33, outer ribbon, 34,
Supporting rod.
Specific embodiment
In order to clarify the technical characteristics of the invention, below by specific embodiment, and its attached drawing is combined, to this hair
It is bright to be described in detail.
As shown in Fig. 1-Fig. 2, which includes the horizontal reactor 1 being linked in sequence from front to back, product separation dress
It puts and product purifying device, the axis direction of the horizontal reactor housing and the angle of horizontal plane are 0-20 °, the Horizontal counter
The cavity of device 1 is answered to be separated into several interconnected reaction members 3 by several flow-stopping plates 2, in the chamber of horizontal reactor 1
In vivo a reactor rabbling mechanism for running through each reaction member 3, the reactor are equipped with along the axis direction of horizontal reactor 1
The front end of rabbling mechanism is connected after being pierced by the head end side wall of horizontal reactor 1 with a reactor driving mechanism, in horizontal reactor 1
A higher side roof part is equipped with a reaction mixture import 4 interconnected with the reaction member 3 of front end, in horizontal reactor
A reactor exhaust outlet 5 and reactor content outlet port 6 are respectively equipped in 1 top sidewall and bottom sidewall, is mixed in reaction
1 outer sheath of horizontal reactor of 4 rear side of liquid import is equipped with a reactor cooling body.
The product separator includes crude steam kettle 7, crude product receiving tank 8 and crude product storage tank 9, is set in the outside of crude steam kettle 7
There are a crude steam kettle heating arrangements, a crude steam kettle stirring system is equipped in the inside of crude steam kettle 7, the lower part of the crude steam kettle 7 is falls
Cone structure, the feed inlet of crude steam kettle 7 is connected by pipeline with the reaction mixture import 4 of horizontal reactor 1, in crude steam kettle
7 bottom be equipped with a crude steam kettle discharge port 10, crude steam kettle 7 top distillation mouth by pipeline successively with a crude steam kettle condenser
11st, crude product receiving tank 8 is connected with crude product storage tank 9, and the top gas outlet of crude product receiving tank 8 passes through pipeline and a crude product vacuum pump 12
Inlet end be connected.
The product purifying device includes fractionating column 13 and rectifying column 14, the first charging aperture of fractionating column 13 by pipeline with
The discharge port of crude product storage tank 9 is connected, the top gas outlet of fractionating column 13 by pipeline after a fractionating column condenser 15 with one
The top feed mouth of phase separation tank 16 is connected, and the bottom discharge mouth of phase separation tank 16 separates two-way pipeline, all the way directly and rectifying column
14 feed inlet is connected, and another way is connected after an intermediate storage tank 17 with the feed inlet of rectifying column 14, the top of rectifying column 14
Portion gas outlet is connected by top feed mouth of the pipeline with a product receiving tank 19 after a rectifying column condenser 18, phase separation tank
16 upper part discharge port is connected by pipeline with the second charging aperture of fractionating column 13, and the bottom discharge mouth of rectifying column 14 passes through pipe
Road is connected with the refluxing opening of fractionating column 13, and the bottom discharge mouth of product receiving tank 19 separates two-way pipeline, all the way with rectifying column
14 refluxing opening is connected, and another way is connected with the feed inlet of a products pot 20, the top gas outlet of product receiving tank 19 with
And the top gas outlet of phase separation tank 16 is connected by pipeline with the inlet end of a purification vacuum pump 21.
The reactor cooling body includes being set on the several of 1 outside of horizontal reactor along 1 length direction of horizontal reactor
A reactor cooling unit, each reactor cooling unit include a reactor cooling folder for being set in 1 outside of horizontal reactor
Set 22.
The rabbling mechanism includes the reactor agitating shaft 23 set along the axis direction of horizontal reactor 1, is reacting
Device agitating shaft 23 is equipped with several groups of agitating paddles 24, and the reactor driving mechanism includes a reactor motor 25, the reaction
The front end of device agitating shaft 23 is passed through after the front end side wall of horizontal reactor 1 through a reactor speed reducer 26 and reactor motor 25
Output shaft is connected.
The flow-stopping plate 2 is the porous plate set perpendicular to 1 axis direction of horizontal reactor, if being uniformly provided on porous plate
An aperture is done, is sheathed on the reactor agitating shaft 23, and the outer ledge of porous plate 2 is close to Horizontal counter in the middle part of porous plate
The madial wall of device 1 is answered to set.
The crude steam kettle stirring system includes the crude steam kettle agitating shaft that 7 inner cavity of crude steam kettle is set on along 7 axis direction of crude steam kettle
27, the top of crude steam kettle agitating shaft 27 is connected after being pierced by 7 top sidewall of crude steam kettle with crude steam kettle driving mechanism, and the crude steam kettle drives
Motivation structure includes a crude steam kettle motor 28, the output shaft of the crude steam kettle motor 28 after a crude steam kettle speed reducer 29 with crude steam kettle
The front end of agitating shaft 27 is connected, and spiral winding is formed with double ribbons on crude steam kettle agitating shaft 27, in the bottom of crude steam kettle agitating shaft 27
Stirring sheet 30 equipped with a triangle, the two sides of the stirring sheet 30 are parallel with the madial wall of crude steam kettle 7.
The crude steam kettle heating arrangements include the crude steam kettle chuck 31 for being sheathed on 7 outside of crude steam kettle.
Double ribbons include interior ribbon 32 and outer ribbon 33, and the center line of interior ribbon 32 and outer ribbon 33 is along with crude steam kettle
The circular helix coiling of line forms centered on agitating shaft 27, and the inner side edge of the interior ribbon 32 is fixed on crude steam kettle agitating shaft 27
On, the quantity of the outer ribbon 33 is two, and two outer ribbons 33 are axially and symmetrically wound on interior ribbon along crude steam kettle agitating shaft 27
32 outside, two outer ribbons 33 are connected respectively by supporting rod 34 with crude steam kettle agitating shaft 27, the two outer ribbon 33 and stirring
The outer side edges of piece 30 are close to the setting of 7 madial wall of crude steam kettle.
Nitromethane synthesis of the present invention and product separator synthesize and are the step of detaching product：
(1) stage of reaction：
Dimethyl suflfate and sodium nitrite in aqueous solution mix in certain proportion from the reaction of horizontal reactor 1 respectively with flow velocity
The cavity for closing liquid import 4 into horizontal reactor 1 is reacted.Horizontal reactor 1 is designed using certain angle of inclination, and along sleeping
The axis direction of formula reactor 1 is equipped with dasher, so reaction mass is in gravity and the stirring action of dasher
Under, it reacts in flowing, reduces the back-mixing of logistics, be conducive to improve the selectivity of target product.Due to porous plate
Blocking, reaction mixture material are kept for certain residence time in each reaction member 3.After reaction carries out to a certain extent,
Reaction mixture material is discharged into crude steam kettle 7 by reactor content outlet port 6.
In reaction process, reaction mixture material needs stop 20-60 minutes in 1 cavity of horizontal reactor, can just make guarantor
Card reaction mass is fully reacted.It is described in order to control residence time of the reaction mixture material in 1 cavity of horizontal reactor
The cavity of horizontal reactor 1 is separated into several interconnected reaction members 3 by several porous plates.During production, pass through
Set 6 line valve of percent opening and trepanning mode, the rotating speed of reactor agitating shaft 23 and reactor content outlet port of porous plate
The keying of door, to control the residence time needed for reaction.
Dimethyl suflfate and sodium nitrite are reacted for exothermic reaction, temperature increase to the selectivity of target product under
Drop, in order to take reaction heat out of, horizontal reactor 1 outer sheath be equipped with cooling body, when raw material reacts, recirculated water into
Enter reactor cooling jacket 22, with reaction stream countercurrent flow, take away the heat that reaction generates.It is each by controlling during production
The temperature of each reaction member 3 of flow control of cooling unit recirculated water makes the temperature of 1 reaction mixture material of horizontal reactor
It is distributed in axial direction into ladder, improves product yield.
Reactor exhaust outlet 5 is equipped in the top sidewall of horizontal reactor 1, it is remaining after the condensed device of tail gas of discharge
Fixed gas is handled through tail gas absorber, is advantageously accounted for environmental problem and is improved the selectivity of target product.
Reaction in horizontal reactor is carried out continuously, and solves domestic nitrite displacement method production nitromethane at present
The problem of batch production can be used, after being operated using continuous reaction, can preferably realize industrial-scale production, simultaneously
Raw material availability is improved, reduces production cost, solves the problems such as environmental pollution.
(2) product separation phase：
During production, the material that the conveying of horizontal reactor 1 comes enters crude steam kettle 7, the heating of steam in crude steam kettle chuck 31
Under, heating distillation is carried out to the nitromethane waste water in crude steam kettle 7, ensures the temperature control of nitromethane waste water in distillation process
Between 80 DEG C -120 DEG C.The distillation mouth at 7 top of crude steam kettle is connected with the inlet end of crude product vacuum pump 12, the nitro first in material
Alkane and water heating are extracted out after being distilled into gaseous state by crude steam kettle distillation mouth out of crude steam kettle, are made in the condensation of crude steam kettle condenser 11
Crude product receiving tank 8 is collected into lower condensation liquefaction, condensate liquid is layered in crude product receiving tank 8, isolates crude product nitre
Methylmethane, crude product nitromethane enter nitromethane crude product storage tank 9.
After the material in crude steam kettle 7 is evaporated sodium sulphate as solid powder, solid sodium sulfate is gone out by crude steam kettle
Material mouth 10 is discharged, and realizes the separation of nitromethane and sodium sulphate and the drying of sodium sulphate.
Crude product vacuum pump 12 makes material be distilled under negative pressure state after being vacuumized to crude steam kettle 7, reduce distillation temperature
Degree, shortens distillation time, saves steam energy.After nitromethane and waste water in crude steam kettle 7 are evaporated, sodium sulphate can be with
It is directly flowed out in powdered from autoclave body lower part drain hole, the sodium sulphate appearance color of processing is preferable, is conducive to later sale.It steams
It during evaporating, pushes away under interior ribbon close to the feed liquid of agitating shaft and is moved downward under effect, a part is spilled over entering outer ribbon
Ribbon face, material is made to tilt or dish out upwardly along ribbon, rises to the material at the top of crude steam kettle 7 by dead weight and outer ribbon
It pushes and flows downward again, form inside and outside, upper and lower recycle stream, blended highly viscous sodium sulphate material, convective motion, made
Material is uniformly mixed, and property is uniform, ensures material thermally equivalent.During processing, crude steam kettle 7 uses hands-off operation, handles sulfuric acid
The toxic gas generated during sodium can be handled with centralized collection, can be realized the zero-emission of pernicious gas, avoided poison gas
Body, which is evaporate into air, pollutes production environment.The outer side edges of two outer ribbons 33 and stirring sheet 30 are close to 7 madial wall of crude steam kettle and are set
It puts, the sticky sodium sulphate got rid of in 7 madial wall of crude steam kettle can be struck off, be re-mixed with the material in crude steam kettle 7.Crude steam kettle
The solid sodium sulfate that the cone design of 7 lower parts enables the distillation in autoclave body to complete to obtain smoothly is released out of autoclave body.Nitre of the present invention
Methylmethane synthesizes and product separator simplifies process, saves equipment investment, saves a large amount of manpower and materials, be conducive to
It promotes and applies.
(3) product purification phase：
Thick nitromethane solution from crude product storage tank 9 enters fractionating column 13, and fractionating column 13 is by purifying vacuum pump 21
Vacuum action and keep -0.04 to -0.09MPa negative pressure, utilize the nitromethane original different with the boiling point of water under vacuum
Reason, the nitromethane constantly vaporization in crude product nitromethane are detached from mixture, most nitromethane that and it is a small amount of
Water is fractionated into entering the progress split-phase processing of phase separation tank 16 after 15 condensation liquefaction of tower condenser by gas outlet discharge at the top of fractionating column,
Most water stays in 13 bottom of fractionating column.
Since water is unmixing with nitromethane, so in phase separation tank 16, nitromethane can form apparent layering with water
Phenomenon, the upper strata for making phase separation tank 16 is largely water phase, and lower floor is nitromethane, and the water on upper strata is back to fractionating column through pump conveying
In 13, the nitromethane of lower floor is delivered to intermediate storage tank 17 through pump or is fed directly in rectifying column 14.In intermediate storage tank 17
Nitromethane can also be according to circumstances delivered in rectifying column 14 through pump and carry out further rectification and purification.
Rectifying column 14 also keeps negative pressure state under the vacuum action of purification vacuum pump 21, is existed using nitromethane and water
Boiling point under vacuum different principle comes out after the nitromethane vaporization in tower in material from 14 top of rectifying column, through rectifying column
Enter product receiving tank 19 after 18 condensation liquefaction of condenser, during production can according to the concentration of nitromethane in product receiving tank 19,
Nitromethane product is delivered in different products pots 20.The material of 14 bottom of rectifying column by pump be transmitted back to fractionating column 13 into
Row recycling continues to be fractionated.It purifies the fixed gas that vacuum pump 21 is sucked out and recycling is condensed by condenser, residual gas enters tail through wind turbine
The processing of aspiration tower.
More than distillation process is carried out continuously, and the nitromethane in crude product nitromethane is made constantly to be detached with water, nitromethane
The purity of product is continuously improved.
Part is not described in detail by the present invention, is the known technology of those skilled in the art of the present technique.Finally illustrate, more than it is real
Apply that example is merely illustrative of the technical solution of the present invention and unrestricted, although having been carried out specifically to the present invention with reference to preferred embodiment
It is bright, it will be understood by those of ordinary skill in the art that, technical scheme of the present invention can be modified or replaced equivalently, and
The objective and range of technical solution of the present invention are not departed from, is intended to be within the scope of the claims of the invention.
Claims (8)
1. a kind of nitromethane synthesis and product separator, it is characterized in that：Including the horizontal reacting being linked in sequence from front to back
Device, product separator and product purifying device, the axis direction of the horizontal reactor housing and the angle of horizontal plane are 0-
20 °, the cavity of the horizontal reactor is separated into several interconnected reaction members by several flow-stopping plates, horizontal
In the cavity of reactor a reactor rabbling mechanism for running through each reaction member, institute are equipped with along the axis direction of horizontal reactor
State reactor rabbling mechanism front end be pierced by the head end side wall of horizontal reactor after be connected with a reactor driving mechanism, horizontal
The reaction mixture import that reaction member of the higher side roof part of reactor equipped with one and front end is interconnected, in Horizontal counter
It answers and a reactor exhaust outlet and reactor content outlet port is respectively equipped in the top sidewall and bottom sidewall of device, mixed in reaction
Horizontal reactor outer sheath on rear side of liquid import is equipped with a reactor cooling body；The product separator include crude steam kettle,
Crude product receiving tank and crude product storage tank, a crude steam kettle heating arrangements are equipped in the outside of crude steam kettle, and one is equipped in the inside of crude steam kettle
Crude steam kettle stirring system, the lower part of the crude steam kettle is inverted pyramidal structures, and the feed inlet of crude steam kettle passes through pipeline and horizontal reacting
The reaction mixture import of device is connected, and a crude steam kettle discharge port, the top distillation mouth of crude steam kettle are equipped in the bottom of crude steam kettle
It is connected successively with a crude steam kettle condenser, crude product receiving tank and crude product storage tank by pipeline, the top gas outlet of crude product receiving tank
It is connected by pipeline with the inlet end of a crude product vacuum pump.
2. a kind of nitromethane synthesis according to claim 1 and product separator, it is characterized in that：The product purification
Device includes fractionating column and rectifying column, and the first charging aperture of fractionating column is connected by pipeline with the discharge port of crude product storage tank, point
The top gas outlet for evaporating tower is connected by pipeline after a fractionating column condenser with the top feed mouth of a phase separation tank, phase separation tank
Bottom discharge mouth separate two-way pipeline, be directly connected all the way with the feed inlet of rectifying column, another way is after an intermediate storage tank
It is connected with the feed inlet of rectifying column, the top gas outlet of rectifying column is connect by pipeline after a rectifying column condenser with a product
The top feed mouth of closed cans is connected, and the upper part discharge port of phase separation tank is connected by pipeline with the second charging aperture of fractionating column,
The bottom discharge mouth of rectifying column is connected by pipeline with the refluxing opening of fractionating column, and the bottom discharge mouth of product receiving tank separates two
Road pipeline is connected all the way with the refluxing opening of rectifying column, and another way is connected with the feed inlet of a products pot, product receiving tank
Top gas outlet and the top gas outlet of phase separation tank are connected by pipeline with the inlet end of a purification vacuum pump.
3. a kind of nitromethane synthesis according to claim 1 and product separator, it is characterized in that：The reactor is cold
But mechanism includes several reactor cooling units on the outside of horizontal reactor along horizontal reactor length direction, each anti-
Device cooling unit is answered to include a reactor cooling jacket being set on the outside of horizontal reactor.
4. a kind of nitromethane synthesis according to claim 1 and product separator, it is characterized in that：The rabbling mechanism
Include a reactor agitating shaft of the axis direction setting along horizontal reactor, several groups of stirrings are equipped on reactor agitating shaft
Paddle, the reactor driving mechanism include a reactor motor, and the front end of the reactor agitating shaft passes through horizontal reactor
It is connected after front end side wall through a reactor speed reducer with the output shaft of reactor motor.
5. a kind of nitromethane synthesis according to claim 1 and product separator, it is characterized in that：The flow-stopping plate is
Perpendicular to the porous plate of horizontal reactor axis direction setting, several apertures, the middle part of porous plate are uniformly provided on porous plate
It is sheathed on the reactor agitating shaft, and the outer ledge of porous plate is close to the madial wall setting of horizontal reactor.
6. a kind of nitromethane synthesis according to claim 1 and product separator, it is characterized in that：The crude steam kettle stirs
It mixes system to include being set on the crude steam kettle agitating shaft of crude steam kettle inner cavity along crude steam kettle axis direction, the top of crude steam kettle agitating shaft is pierced by
It is connected after crude steam kettle top sidewall with crude steam kettle driving mechanism, the crude steam kettle driving mechanism includes a crude steam kettle motor, described
The output shaft of crude steam kettle motor is connected after a crude steam kettle speed reducer with the front end of crude steam kettle agitating shaft, on crude steam kettle agitating shaft
Spiral winding is formed with double ribbons, and the stirring sheet of a triangle, the two sides of the stirring sheet are equipped in the bottom of crude steam kettle agitating shaft
It is parallel with the madial wall of crude steam kettle.
7. a kind of nitromethane synthesis according to claim 1 and product separator, it is characterized in that：The crude steam kettle adds
Heat engine structure includes being sheathed on the crude steam kettle chuck on the outside of crude steam kettle.
8. a kind of nitromethane synthesis according to claim 6 and product separator, it is characterized in that：Double ribbon packets
Include interior ribbon and outer ribbon, the center line of interior ribbon and outer ribbon along the line centered on crude steam kettle agitating shaft circular helix around
It makes, the inner side edge of the interior ribbon is fixed on crude steam kettle agitating shaft, and the quantity of the outer ribbon is two, two outer ribbons
Along the outside for being axially and symmetrically wound on interior ribbon of crude steam kettle agitating shaft, two outer ribbons are stirred respectively by supporting rod and crude steam kettle
Axis is connected, and the outer side edges of the two outer ribbon and stirring sheet are close to the setting of crude steam kettle madial wall.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610152401.8A CN105601520B (en) | 2016-03-16 | 2016-03-16 | A kind of nitromethane synthesis and product separator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610152401.8A CN105601520B (en) | 2016-03-16 | 2016-03-16 | A kind of nitromethane synthesis and product separator |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105601520A CN105601520A (en) | 2016-05-25 |
| CN105601520B true CN105601520B (en) | 2018-07-03 |
Family
ID=55981949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610152401.8A Active CN105601520B (en) | 2016-03-16 | 2016-03-16 | A kind of nitromethane synthesis and product separator |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105601520B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503568A (en) * | 2017-02-27 | 2018-09-07 | 无锡杰西医药股份有限公司 | A kind of high-purity isosulfocyanate compound preparation method suitable for industrialized production |
| CN113214086B (en) * | 2021-05-26 | 2022-09-13 | 山东中盛药化设备有限公司 | Continuous rectification and purification process of nitromethane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3725013A (en) * | 1970-11-09 | 1973-04-03 | P Konstruk Bjuro P Oboru Proiz | Multisection apparatus with conveying means for carrying out mass-exchange processes in solid-liquid systems |
| CN205420234U (en) * | 2016-03-16 | 2016-08-03 | 临沂远博化工有限公司 | Synthetic and result separator of nitromethane |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201760279U (en) * | 2010-06-28 | 2011-03-16 | 杭州原正化学工程技术装备有限公司 | Horizontal reactor |
| CN102161512B (en) * | 2011-02-25 | 2012-10-03 | 云南建水锰矿有限责任公司 | Material conveying method for horizontal reactor of potassium manganate |
-
2016
- 2016-03-16 CN CN201610152401.8A patent/CN105601520B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3725013A (en) * | 1970-11-09 | 1973-04-03 | P Konstruk Bjuro P Oboru Proiz | Multisection apparatus with conveying means for carrying out mass-exchange processes in solid-liquid systems |
| CN205420234U (en) * | 2016-03-16 | 2016-08-03 | 临沂远博化工有限公司 | Synthetic and result separator of nitromethane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105601520A (en) | 2016-05-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105418447B (en) | A kind of DMAC rectifier units and process | |
| CN207463236U (en) | A kind of heat preservation chemical reaction kettle of differential stirring | |
| CN105601520B (en) | A kind of nitromethane synthesis and product separator | |
| CN109134231A (en) | A kind of chloroacetic device and process of differential circulation continuous production | |
| CN104628589B (en) | Continuous production process and system for synthesizing N, N-dimethyl propanamide | |
| CN107721817A (en) | A kind of method and device of fixed carbon dioxide and photocatalytic reduction of carbon oxide | |
| CN212102640U (en) | System for preparing acetic anhydride by acetic acid cracking-ketene method | |
| CN205420234U (en) | Synthetic and result separator of nitromethane | |
| CN107840808A (en) | Continuous reaction rectification production cyanoacetate compound, malonate compound device and its production technology | |
| CN114570052B (en) | Method and device for continuously producing diethyl maleate | |
| CN207143010U (en) | The dehydration device of esterification products under a kind of acid condition | |
| CN106146434A (en) | A kind of preparation technology of 5 hydroxymethyl furfural | |
| CN201825893U (en) | Novel chlorthal production device | |
| CN106146441A (en) | A kind of preparation technology of furfural | |
| CN209205307U (en) | The equipment of glycerin chlorination production dichlorohydrin | |
| CN201807201U (en) | Distillation device | |
| CN205419831U (en) | Result separation and drying equipment of nitromethane building -up reactions | |
| CN208373074U (en) | A kind of neutralization reaction kettle | |
| CN208829569U (en) | It is a kind of for synthesizing the device of trifluoroethanol | |
| CN105936563A (en) | Amantadine hydrochloride sewage processing device | |
| CN101747177A (en) | Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester | |
| CN205443136U (en) | First dimension salt preparation system | |
| CN220989714U (en) | Bromine rectifying device | |
| CN110433743A (en) | The preparation facilities of perfluor isobutyl acyl fluorides | |
| CN209651904U (en) | It is used to prepare the circulator of dust technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |