CN105601520A - Device for synthesizing nitromethane and separating products - Google Patents
Device for synthesizing nitromethane and separating products Download PDFInfo
- Publication number
- CN105601520A CN105601520A CN201610152401.8A CN201610152401A CN105601520A CN 105601520 A CN105601520 A CN 105601520A CN 201610152401 A CN201610152401 A CN 201610152401A CN 105601520 A CN105601520 A CN 105601520A
- Authority
- CN
- China
- Prior art keywords
- reactor
- steam kettle
- crude
- crude steam
- nitromethane
- 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.)
- Granted
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 invention relates to the field of chemical engineering and particularly discloses a device for synthesizing nitromethane and separating products. The device comprises a horizontal reactor, a product separation device and a product purification device which are sequentially connected from front to back, wherein a cavity of the horizontal reactor is divided into a plurality of mutually communicated reaction units by virtue of a plurality of flow baffles, a reactor stirring mechanism penetrating through each reaction unit is arranged in the cavity of the horizontal reactor along the axis direction of the horizontal reactor, and the front end of the reactor stirring mechanism stretches out of the side wall of the head end of the horizontal reactor and is connected with a reactor driving mechanism. According to the device, the problem that nitromethane only can be produced in an intermittent manner in a current domestic nitrite substitution method is solved; and by virtue of continuous reaction and rectification operation, the large-scale industrial production can be well realized, the production cost is lowered, the production efficiency is improved, and a lot of problems including environmental pollution and the like are solved.
Description
Technical field
The present invention relates to chemical field, particularly a kind of nitromethane synthesizes and product separation device.
Background technology
Existing nitromethane synthetic reaction adopts simple reactor intermittently to produce mostly, production processIn by manually dropping into natrium nitrosum solid in reactor, natrium nitrosum solid in reactor, dissolve after withDimethyl suflfate reacts. But dimethyl suflfate is when reacting with natrium nitrosum, also can occur with waterHydrolytic side reactions, reduces the yield reacting. In production, in order to reduce the generation of side reaction, make sulfuric acid diformazanEster fully reacts with natrium nitrosum, conventionally adds dimethyl suflfate by the mode dripping, can only be in batches,The operation of disconnected property, production efficiency is very low, and expends more manpower in the process of producing. Secondly, sulfuric acidDimethyl ester is exothermic reaction with reacting of natrium nitrosum, in course of reaction, can produce a large amount of heat, makes temperature in stillDegree raises fast, but traditional reactor control temperature in the kettle is more difficult. When reaction condition control improper,The too low meeting of temperature does not even react very much reaction rate slowly, and temperature is too high can increase again side reaction, existsLarger contingency, causes output shakiness. Again, in course of reaction, can generate nitrous acid hydrogen methyl esters etc. poisonousGas, traditional reactor cannot properly be disposed these toxic gases, and workman's working environment is poor, existsLarger potential safety hazard.
Nitromethane synthetic reaction, except generating nitromethane product, also can produce a large amount of sodium sulphate. Sulfuric acidThe byproduct that sodium is produced as nitromethane, is present in nitromethane waste water in a large number, has exceeded national dirtDye thing discharge standard. Meanwhile, sodium sulphate is as a kind of important industrial chemicals, if without just reclaiming directlyDischarge, not only contaminated environment but also waste resource. Traditional sodium sulphate processing method is by the nitro first of contains sodium sulfateAfter alkane Waste water concentrating, and then by centrifuge, the sodium sulphate solid in concentrate is deviate from. This processing sideMethod has the following disadvantages: first, the nitromethane waste water of contains sodium sulfate viscosity after concentrated is very large, and concentratesTime the reactor that uses be spherical reactor, the opening of autoclave body bottom is less, causes the concentrated sodium sulphate obtainingBe difficult to discharge by the opening of autoclave body bottom, need again in reactor, to add water, make sodium sulphate dilution for sticking with pasteShape is discharged from autoclave body bottom, then sends into centrifuge and again dewater. Secondly, throw away sodium sulphate by centrifuge solidIn waste water after body, sodium sulphate content is still higher, is even saturated solution, can not discharge immediately or followRing utilizes, and also needs further processing, and operation more complicated, has reduced production efficiency, and energy resource consumption is larger.Again, in this processing method, centrifuge needs material to be evenly distributed in centrifuge in operation, ifMaterial skewness, the operation of centrifuge, by disequilibrium bad shocking, causes centrifuge easily to damage, and increasesThe maintenance that adds the later stage drops into, and even can threaten Field Force's safety when serious. Finally, unavoidable in waste waterCan contain the harmful substances such as nitromethane, and nitromethane easily evaporate in air, employee's health is madeBecome infringement, have certain potential safety hazard.
In the crude product nitromethane that nitromethane synthetic reaction obtains, contain moisture, need to be sent to rectifying column and carry outRectifying is to improve the product purity of nitromethane. To not forming the system of azeotrope, as long as design and operateWhen, distillate will be highly purified volatile components, tower bottom product will be highly purified difficult volatile component. SoAnd the nitromethane in crude product nitromethane and water can form minimum azeotropic mixture, be not increased to water in temperatureOr when the boiling point of nitromethane, the azeotropic mixture that nitromethane and water form seethes with excitement already, makes water and nitro firstThe mixture of alkane is difficult to effectively be separated, and it is highly purified that general rectifying cannot make nitromethane obtain. ExistingSome nitromethane distillation processes adopt the mode of batch fractionating conventionally, water and nitromethane shape in still-processThe azeotropic mixture becoming forms liquid from tower reactor top after condenser condenses, then utilizes nitromethane and water insoluble,There will be the feature of liquid level layering between the two, the water after layering is constantly discharged. Along with distillation process notDisconnected carrying out, the moisture in nitromethane constantly reduces, and obtains the most at last the nitromethane that purity is higher. TraditionThis distillation process to consume steam energy many, and still-process is non-continuous process, increased peopleThe input of power. In addition, in the process of rectifying, if because misoperation causes liquid evaporate to dryness in still, willThere is serious security incident.
Therefore, need the synthetic and product separation device of a kind of nitromethane badly and solve above technical problem.
Summary of the invention
The present invention is in order to make up the deficiencies in the prior art, provide a kind of reasonable in design, improved nitromethaneProduct purity, simplified sodium sulphate recovery process, reaction and distillation process and carried out continuously, reduced manpowerThe nitromethane dropping into synthesizes and product separation device, has solved problems of the prior art.
The present invention is achieved through the following technical solutions:
Synthetic and the product separation device of a kind of nitromethane, comprise the horizontal reactor that is linked in sequence from front to back,Separation of products device and product purifying device, the axis direction of described horizontal reactor housing and the folder of horizontal planeAngle is 0-20 °, and the cavity of described horizontal reactor is separated into several by several flow-stopping plates and is interconnectedReaction member, in the cavity of horizontal reactor, be provided with one along the axis direction of horizontal reactor and run through eachThe reactor rabbling mechanism of reaction member, the front end of described reactor rabbling mechanism passes the head of horizontal reactorAfter distolateral wall, be connected with a reactor driving mechanism, the higher side roof part of horizontal reactor be provided with one withThe reaction mixture import that the reaction member of front end is interconnected, in the top of horizontal reactor sidewall and bottomOn sidewall, be respectively equipped with a reactor exhaust outlet and reactor content and extract mouth out, at reaction mixture import rear sideHorizontal reactor outside be arranged with a reactor cooling body.
Described separation of products device comprises crude steam kettle, crude product receiving tank and crude product storage tank, in the outside of crude steam kettleBe provided with a crude steam kettle heating arrangements, be provided with a crude steam kettle stirring system, described crude steam kettle in the inner side of crude steam kettleBottom be inverted pyramidal structures, the charging aperture of crude steam kettle enters by the reaction mixture of pipeline and horizontal reactorMouth is connected, and is provided with a crude steam kettle discharging opening in the bottom of crude steam kettle, and pipe is passed through in the top distillation mouthful of crude steam kettleRoad is connected with a crude steam kettle condenser, crude product receiving tank and crude product storage tank successively, and the top of crude product receiving tank goes outGas port is connected with the inlet end of a crude product vavuum pump by pipeline.
Described product purifying device comprises fractionating column and rectifying column, the first charging aperture of fractionating column by pipeline withThe discharging opening of crude product storage tank is connected, the gas outlet, top of fractionating column by pipeline after a fractionating column condenserBe connected with its top feed mouth of a phase separation tank, the bottom discharge mouth of phase separation tank separates two-way pipeline, and a road is straightConnect with the charging aperture of rectifying column and be connected, after another Lu Jingyi intermediate storage tank, be connected with the charging aperture of rectifying column,The gas outlet, top of rectifying column by pipeline after a rectifying column condenser with its top feed of a product receiving tankMouth is connected, and the upper part discharge port of phase separation tank is connected with the second charging aperture of fractionating column by pipeline, rectifyingThe bottom discharge mouth of tower is connected with the refluxing opening of fractionating column by pipeline, the bottom discharge mouth of product receiving tankSeparate two-way pipeline, a road is connected with the refluxing opening of rectifying column, the charging aperture phase of another Lu Yuyi products potBe communicated with, the gas outlet, top of product receiving tank and the gas outlet, top of phase separation tank are purified true by pipeline andThe inlet end of empty pump is connected.
If comprising along horizontal reactor length direction, described reactor cooling body is located at horizontal reactor outsideA dry reactor cooling unit, each reactor cooling unit comprises that one is set in the anti-of horizontal reactor outsideAnswer device cooling jacket.
Described rabbling mechanism comprises the reactor shaft arranging along the axis direction of horizontal reactor, insteadAnswer device shaft to be provided with some groups of paddles, described reactor driving mechanism comprises a reactor motor, instituteThe front end of stating reactor shaft through after the front end side wall of horizontal reactor through a reactor reductor with reactThe output shaft of device motor is connected.
Described flow-stopping plate is the porous plate arranging perpendicular to horizontal reactor axis direction, on porous plate, evenly establishesHave several apertures, the middle part of porous plate is sheathed on described reactor shaft, and the outer side edges of porous plateEdge is close to the madial wall setting of horizontal reactor.
Described crude steam kettle stirring system comprises the crude steam kettle stirring of being located at crude steam kettle inner chamber along crude steam kettle axis directionAxle, the top of crude steam kettle shaft is connected with crude steam kettle driving mechanism after passing crude steam kettle top sidewall, described inCrude steam kettle driving mechanism comprises a crude steam kettle motor, and the output shaft of described crude steam kettle motor slows down through a crude steam kettleAfter machine, be connected with the front end of crude steam kettle shaft, on crude steam kettle shaft, spiral winding is shaped with two ribbons, slightlyThe bottom of steaming still shaft is provided with a leg-of-mutton stirring piece, in the dual-side of described stirring piece and crude steam kettleSidewall parallels.
Described crude steam kettle heating arrangements comprises a crude steam kettle chuck that is sheathed on crude steam kettle outside.
Described pair of ribbon comprises interior ribbon and outer ribbon, and the center line of interior ribbon and outer ribbon is along stirring with crude steam kettleMix the circular helix coiling of line centered by axle and form, the inner side edge of described interior ribbon is fixed on crude steam kettle and stirsOn axle, the quantity of described outer ribbon is two, and two outer ribbons are wound on along the axial symmetry of crude steam kettle shaftThe outside of interior ribbon, two outer ribbons are connected with crude steam kettle shaft by support bar respectively, described two outer ribbonsAnd the outer side edges of stirring piece is all close to the setting of crude steam kettle madial wall.
The invention has the beneficial effects as follows:
(1) stage of reaction:
Reaction in horizontal reactor is carried out continuously, has solved current domestic nitrite displacement method and has produced nitroMethane can only adopt a difficult problem for batch production, adopts after continuous reaction operation, can realize preferably workIndustry large-scale production has improved raw material availability simultaneously, has reduced production cost, has solved environmental pollution etc.Problems.
(2) the separation of products stage:
After nitromethane in crude steam kettle and waste water evaporate to dryness, it is Powdered from kettle that sodium sulphate can directly bePortion's drain hole flows out, and the sodium sulphate appearance color of processing is better, is conducive to later sale, has simplified operation,Save equipment investment, saved a large amount of manpower and materials, be conducive to apply. In still-process, lean onThe feed liquid of nearly crude steam kettle shaft pushes away under effect and moves downward under interior ribbon, outside a part is dished out and enteredThe ribbon face of ribbon, makes material along ribbon towards tilting or dishing out, and the material that rises to crude steam kettle top leans onThe promotion of deadweight and outer ribbon flows downward again, forms inside and outside, upper and lower circular flow, makes full-bodied sulphurAcid sodium material obtains fusion, convective motion, makes mixing of materials even, and character homogeneous ensures that material is evenly subject toHeat.
(3) product purification phase:
By negative pressure rectifying, utilize methane with water in the different principle of the boiling point under vacuum, make water and nitro firstThe mixture of alkane effectively separates, and has improved the product purity of nitromethane, and has reduced the use of steamAmount; In destilling tower and rectifying column, there is liquid-phase reflux, avoided because misoperation causes liquid evaporate to dryness in still,Ensure safety in production; Distillation process carries out continuously, has reduced human input.
To sum up, nitromethane of the present invention synthesizes and product separation device, has solved current domestic nitrite and has putThe method of changing is produced nitromethane can only adopt the difficult problem of batch production, adopt after continuous reaction and distillation operation,Can realize preferably industrial-scale production, reduce production cost, improve production efficiency, solveThe problems such as environmental pollution.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is structural representation of the present invention;
Fig. 2 is the structure for amplifying 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 outlet, 6, reactor content extracts out mouthful, 7, crude steam kettle, 8, crude product receiving tank, 9, crude productStorage tank, 10, crude steam kettle discharging opening, 11, crude steam kettle condenser, 12, crude product vavuum pump, 13, fractionating column,14, rectifying column, 15, fractionating column condenser, 16, phase separation tank, 17, intermediate storage tank, 18, rectifying column is coldCondenser, 19, product receiving tank, 20, products pot, 21, purification vavuum pump, 22, reactor cooling jacket,23, reactor shaft, 24, paddle, 25, reactor motor, 26, reactor reductor, 27,Crude steam kettle shaft, 28, crude steam kettle motor, 29, crude steam kettle reductor, 30, stirring piece, 31, slightly steamStill chuck, 32, interior ribbon, 33, outer ribbon, 34, support bar.
Detailed description of the invention
For clearly demonstrating the technical characterstic of this programme, below by detailed description of the invention, and in conjunction with its accompanying drawing,The present invention will be described in detail.
As shown in Fig. 1-Fig. 2, this embodiment comprises the horizontal reactor 1, the product that are linked in sequence from front to backProduct separator and product purifying device, the axis direction of described horizontal reactor housing and the angle of horizontal planeFor 0-20 °, the cavity of described horizontal reactor 1 is separated into several by several flow-stopping plates 2 and interconnects mutuallyLogical reaction member 3 is provided with always along the axis direction of horizontal reactor 1 in the cavity of horizontal reactor 1The reactor rabbling mechanism of wearing each reaction member 3, the front end of described reactor rabbling mechanism passes Horizontal counterAfter answering the head end sidewall of device 1, be connected with a reactor driving mechanism, on the higher side top of horizontal reactor 1Portion is provided with a reaction mixture import 4 being interconnected with reaction member 3 foremost, at horizontal reactor 1Top sidewall and bottom sidewall on be respectively equipped with a reactor exhaust outlet 5 and reactor content and extract mouthfuls 6 out,Horizontal reactor 1 outside of reaction mixture import 4 rear sides is arranged with a reactor cooling body.
Described separation of products device comprises crude steam kettle 7, crude product receiving tank 8 and crude product storage tank 9, at crude steam kettle 7Outside be provided with a crude steam kettle heating arrangements, be provided with a crude steam kettle stirring system, institute in the inner side of crude steam kettle 7The bottom of stating crude steam kettle 7 is inverted pyramidal structures, and the charging aperture of crude steam kettle 7 is by pipeline and horizontal reactor 1Reaction mixture import 4 be connected, be provided with a crude steam kettle discharging opening 10 in the bottom of crude steam kettle 7, slightly steamThe top distillation of still 7 mouthful is stored up with a crude steam kettle condenser 11, crude product receiving tank 8 and crude product successively by pipelineTank 9 is connected, and the gas outlet, top of crude product receiving tank 8 is the inlet end phase with a crude product vavuum pump 12 by pipelineBe communicated with.
Described product purifying device comprises fractionating column 13 and rectifying column 14, and the first charging aperture of fractionating column 13 is logicalPiping is connected with the discharging opening of crude product storage tank 9, the gas outlet, top of fractionating column 13 by pipeline through one pointAfter heating up in a steamer tower condenser 15, be connected with its top feed mouth of a phase separation tank 16, the bottom discharge mouth of phase separation tank 16Separate two-way pipeline, a road is directly connected with the charging aperture of rectifying column 14, another Lu Jingyi intermediate storage tank 17Be connected with the charging aperture of rectifying column 14 afterwards, the gas outlet, top of rectifying column 14 by pipeline through a rectifying columnAfter condenser 18, be connected with its top feed mouth of a product receiving tank 19, the upper part discharge port of phase separation tank 16Be connected with the second charging aperture of fractionating column 13 by pipeline, the bottom discharge mouth of rectifying column 14 passes through pipelineBe connected with the refluxing opening of fractionating column 13, the bottom discharge mouth of product receiving tank 19 separates two-way pipeline, oneRoad is connected with the refluxing opening of rectifying column 14, and the charging aperture of another Lu Yuyi products pot 20 is connected, productThe gas outlet, top of receiving tank 19 and the gas outlet, top of phase separation tank 16 are by pipeline and a purification vavuum pump21 inlet end is connected.
Described reactor cooling body comprises along horizontal reactor 1 length direction is located at horizontal reactor 1 outsideSeveral reactor cooling units, each reactor cooling unit comprises that one is set in outside horizontal reactor 1The reactor cooling jacket 22 of side.
Described rabbling mechanism comprises the reactor shaft 23 arranging along the axis direction of horizontal reactor 1,On reactor shaft 23, be provided with some groups of paddles 24, described reactor driving mechanism comprises a reactorMotor 25, the front end of described reactor shaft 23 through after the front end side wall of horizontal reactor 1 through a reactionDevice reductor 26 is connected with the output shaft of reactor motor 25.
Described flow-stopping plate 2 is the porous plate arranging perpendicular to horizontal reactor 1 axis direction, equal on porous plateEven several apertures that is provided with, the middle part of porous plate is sheathed on described reactor shaft 23, and porous plate 2Outer ledge be close to the madial wall setting of horizontal reactor 1.
Described crude steam kettle stirring system comprises the crude steam kettle of being located at crude steam kettle 7 inner chambers along crude steam kettle 7 axis directionsShaft 27, the top of crude steam kettle shaft 27 passes after crude steam kettle 7 top sidewalls and crude steam kettle driving mechanismBe connected, described crude steam kettle driving mechanism comprises a crude steam kettle motor 28, the output shaft of described crude steam kettle motor 28After a crude steam kettle reductor 29, be connected with the front end of crude steam kettle shaft 27, on crude steam kettle shaft 27Spiral winding is shaped with two ribbons, is provided with a leg-of-mutton stirring piece 30 in the bottom of crude steam kettle shaft 27, described inThe dual-side of stirring piece 30 parallels with the madial wall of crude steam kettle 7.
Described crude steam kettle heating arrangements comprises a crude steam kettle chuck 31 that is sheathed on crude steam kettle 7 outsides.
Described pair of ribbon comprises interior ribbon 32 and outer ribbon 33, the center line edge of interior ribbon 32 and outer ribbon 33Centered by crude steam kettle shaft 27, the circular helix coiling of line forms, the inner side edge of described interior ribbon 32Be fixed on crude steam kettle shaft 27, the quantity of described outer ribbon 33 is two, and two outer ribbons 33 steam along thickThe axial symmetry of still shaft 27 is wound on the outside of interior ribbon 32, and two outer ribbons 33 pass through respectively support bar34 are connected with crude steam kettle shaft 27, and the outer side edges of described two outer ribbons 33 and stirring piece 30 is all close to thick steamingStill 7 madial wall settings.
Nitromethane of the present invention is synthetic and product separation device is synthetic and step products of separated is:
(1) stage of reaction:
Dimethyl suflfate and sodium nitrite in aqueous solution in certain proportion with flow velocity respectively from horizontal reactor 1The cavity that reaction mixture import 4 enters horizontal reactor 1 reacts. Horizontal reactor 1 adopts certainAngle of inclination design, and be provided with dasher along the axis direction of horizontal reactor 1, so reaction massUnder the stirring action of gravity and dasher, react while flowing, reduce the back-mixing of logistics,Be conducive to improve the selective of target product. Due to stopping of porous plate, reactant mixture material is in each reactionUnit 3 all keeps certain time of staying. After reaction proceeds to a certain degree, reactant mixture material passes throughReactor content is extracted mouthful 6 discharges out and is entered crude steam kettle 7.
In course of reaction, reactant mixture material need to stop 20-60 minute in horizontal reactor 1 cavity,Just can make to ensure that reaction mass fully reacts. In order to control reactant mixture material in horizontal reactor 1 chamberThe time of staying in body, the cavity of described horizontal reactor 1 is separated into several phases by several porous platesIntercommunicated reaction member 3. When production, by setting the percent opening of porous plate and perforate mode, reactor stirsMix the rotating speed of axle 23 and the keying that reactor content is extracted mouthful 6 pipeline valves out, control required the stopping of reactionStay the time.
Dimethyl suflfate is exothermic reaction with reacting of natrium nitrosum, and temperature rising is selective to target productDecline to some extent, in order to take reaction heat out of, be arranged with cooling body in the outside of horizontal reactor 1, at raw materialWhile reacting, recirculated water enters reactor cooling jacket 22, and reacts logistics countercurrent flow, takes away reactionThe heat producing. When production, by controlling the each reaction member 3 of flow-control of each cooling unit recirculated waterTemperature, the temperature that makes horizontal reactor 1 reaction mixture material, axially becoming ladder to distribute, improves productYield.
On the sidewall of the top of horizontal reactor 1, be provided with reactor exhaust outlet 5, the tail gas of discharge is after condenserRemaining fixed gas is processed through tail gas absorber, is conducive to solve environmental problem and improves target productSelectively.
Reaction in horizontal reactor is carried out continuously, has solved current domestic nitrite displacement method and has produced nitroMethane can only adopt a difficult problem for batch production, adopts after continuous reaction operation, can realize preferably workIndustry large-scale production has improved raw material availability simultaneously, has reduced production cost, has solved environmental pollution etc.Problems.
(2) the separation of products stage:
When production, the material that horizontal reactor 1 transports enters crude steam kettle 7, in the interior steaming of crude steam kettle chuck 31Under the heating of vapour, the nitromethane waste water in crude steam kettle 7 is added to thermal distillation, in still-process, ensure nitreThe temperature of methylmethane waste water is controlled between 80 DEG C-120 DEG C. The distillation mouth at crude steam kettle 7 tops and crude product vacuumThe inlet end of pump 12 is connected, and after the nitromethane in material and water heating are distilled into gaseous state, distills by crude steam kettleMouth is extracted out in crude steam kettle, and under the condensation of crude steam kettle condenser 11, condensation liquefaction is collected and enters crude productReceiving tank 8, condensate liquid carries out layering in crude product receiving tank 8, isolates crude product nitromethane, crude product nitroMethane enters nitromethane crude product storage tank 9.
When the material in crude steam kettle 7 is become after pressed powder by evaporate to dryness sodium sulphate, solid sodium sulfate is passed through thickSteam still discharging opening 10 and discharge, realized nitromethane and separating of sodium sulphate and being dried of sodium sulphate.
Crude product vavuum pump 12 distills material after crude steam kettle 7 is vacuumized under negative pressure state, has reducedVapo(u)rizing temperature, has shortened distillation time, has saved steam energy. Nitromethane in crude steam kettle 7 and uselessAfter water evaporate to dryness, sodium sulphate can directly be Powdered and flow out from kettle bottom drain hole, outside the sodium sulphate of processingSight color is better, is conducive to later sale. In still-process, near the feed liquid of shaft at interior ribbonUnder push away under effect and move downward, a part is entered the ribbon face of outer ribbon by dishing out, make material along ribbon towardsTilt or dish out, the material that rises to crude steam kettle 7 tops flows downward again by the promotion of deadweight and outer ribbon,Form inside and outside, upper and lower circular flow, make full-bodied sodium sulphate material obtain fusion, convective motion, makeMixing of materials is even, and character homogeneous ensures material thermally equivalent. When processing, crude steam kettle 7 adopts closedOperation, processing the toxic gas that produces in sodium sulphate process can centralized collection processing, can realize harmful gasThe zero-emission of body, has avoided toxic gas to evaporate into and in air, has polluted production environment. Two outer ribbons 33 and stirringThe outer side edges of sheet 30 is all close to crude steam kettle 7 madial wall settings, can be by the thickness sulphur getting rid of at crude steam kettle 7 madial wallsAcid sodium strikes off, and again mixes with the material in crude steam kettle 7. The taper designs of crude steam kettle 7 bottoms makes stillDistillation in body completes the solid sodium sulfate obtaining and can in kettle, emit smoothly. Nitromethane of the present invention is syntheticAnd product separation device simplified operation, save equipment investment, save a large amount of manpower and materials, favourableIn applying.
(3) product purification phase:
Thick nitromethane solution from crude product storage tank 9 enters fractionating column 13, and fractionating column 13 is by purification vacuumThe vacuum action of pump 21 and keep-0.04 to-0.09MPa negative pressure, utilizes nitromethane and water in vacuumUnder the different principle of boiling point, nitromethane in crude product nitromethane constantly vaporization separates from mixture,That discharges most nitromethane through fractionating column condenser 15 by gas outlet, fractionating column top with a small amount of waterAfter condensation liquefaction, enter phase separation tank 16 and carry out phase-splitting processing, most water is stayed fractionating column 13 bottoms.
Due to water and nitromethane unmixing, so in phase separation tank 16, nitromethane and water can form obviouslyLamination, making the upper strata of phase separation tank 16 most of is water, lower floor is nitromethane, the water warp on upper strataPump is transmitted back to and flow in fractionating column 13, and the nitromethane of lower floor is delivered to intermediate storage tank 17 or direct through pumpBe delivered in rectifying column 14. Nitromethane in intermediate storage tank 17 also can according to circumstances, be delivered to through pumpIn rectifying column 14, carry out further rectification and purification.
Rectifying column 14 also keeps negative pressure state under the vacuum action of purification vavuum pump 21, utilizes nitro firstAlkane with water in the different principle of the boiling point under vacuum, after the nitromethane vaporization in tower in material from rectifying column 14Top out, enters product receiving tank 19 after rectifying column condenser 18 condensation liquefactions, can be according to product when productionThe concentration of product receiving tank 19 interior nitromethanes, is delivered to nitromethane product in different products pot 20.The material of rectifying column 14 bottoms is transmitted back to fractionating column 13 through pump and reclaims continuation fractionation. Purification vavuum pumpThe fixed gas of 21 sucking-offs is reclaimed by condenser condenses, and residual gas enters tail gas absorber processing through blower fan.
Above distillation process carries out continuously, the nitromethane in crude product nitromethane is separated, nitre with water is continuousThe purity of methylmethane product improves constantly.
The present invention does not describe part in detail, is those skilled in the art of the present technique's known technology. Finally explanation,Above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment to thisInvention has been described in detail, and those of ordinary skill in the art should be appreciated that can be to technology of the present inventionScheme is modified or is equal to replacement, and does not depart from aim and the scope of technical solution of the present invention, and it all shouldBe encompassed in the middle of claim scope of the present invention.
Claims (9)
1. nitromethane synthesizes and a product separation device, it is characterized in that: comprise from front to back and being linked in sequenceHorizontal reactor, separation of products device and product purifying device, the axis side of described horizontal reactor housingTo with the angle of horizontal plane be 0-20 °, the cavity of described horizontal reactor is separated into by several flow-stopping platesThe reaction member that several are interconnected, in the cavity of horizontal reactor along the axis direction of horizontal reactorBe provided with a reactor rabbling mechanism that runs through each reaction member, the front end of described reactor rabbling mechanism passesAfter the head end sidewall of horizontal reactor, be connected with a reactor driving mechanism, in the higher side of horizontal reactorTop is provided with a reaction mixture import being interconnected with reaction member foremost, at horizontal reactorOn top sidewall and bottom sidewall, be respectively equipped with a reactor exhaust outlet and reactor content and extract mouth out, in reactionThe horizontal reactor outside of mixed liquor import rear side is arranged with a reactor cooling body.
2. a kind of nitromethane according to claim 1 synthesizes and product separation device, it is characterized in that:Described separation of products device comprises crude steam kettle, crude product receiving tank and crude product storage tank, is provided with in the outside of crude steam kettleOne crude steam kettle heating arrangements, is provided with a crude steam kettle stirring system, under described crude steam kettle in the inner side of crude steam kettlePortion is inverted pyramidal structures, and the charging aperture of crude steam kettle is the reaction mixture import phase with horizontal reactor by pipelineBe communicated with, be provided with a crude steam kettle discharging opening in the bottom of crude steam kettle, the top distillation mouthful of crude steam kettle is complied with by pipelineInferiorly be connected with a crude steam kettle condenser, crude product receiving tank and crude product storage tank, the gas outlet, top of crude product receiving tankBe connected with the inlet end of a crude product vavuum pump by pipeline.
3. a kind of nitromethane according to claim 2 synthesizes and product separation device, it is characterized in that:Described product purifying device comprises fractionating column and rectifying column, and the first charging aperture of fractionating column is by pipeline and crude productThe discharging opening of storage tank is connected, the gas outlet, top of fractionating column by pipeline after a fractionating column condenser with oneIts top feed mouth of phase separation tank is connected, and the bottom discharge mouth of phase separation tank separates two-way pipeline, a road directly withThe charging aperture of rectifying column is connected, after another Lu Jingyi intermediate storage tank, is connected with the charging aperture of rectifying column, and essenceThe gas outlet, top of heating up in a steamer tower by pipeline after a rectifying column condenser with its top feed mouth of a product receiving tankBe connected, the upper part discharge port of phase separation tank is connected with the second charging aperture of fractionating column by pipeline, rectifying columnBottom discharge mouth be connected with the refluxing opening of fractionating column by pipeline, the bottom discharge mouth of product receiving tank dividesGo out two-way pipeline, a road is connected with the refluxing opening of rectifying column, and the charging aperture of another Lu Yuyi products pot is connectedLogical, the gas outlet, top of product receiving tank and the gas outlet, top of phase separation tank are by pipeline and a purification vacuumThe inlet end of pump is connected.
4. a kind of nitromethane according to claim 1 synthesizes and product separation device, it is characterized in that:Described reactor cooling body comprises along horizontal reactor length direction is located at several of horizontal reactor outsideReactor cooling unit, each reactor cooling unit comprises that one is set in the reactor in horizontal reactor outsideCooling jacket.
5. a kind of nitromethane according to claim 1 synthesizes and product separation device, it is characterized in that:Described rabbling mechanism comprises the reactor shaft arranging along the axis direction of horizontal reactor, at reactorShaft is provided with some groups of paddles, and described reactor driving mechanism comprises a reactor motor, described anti-The front end of answering device shaft through after the front end side wall of horizontal reactor through a reactor reductor and reactor electricityThe output shaft of machine is connected.
6. a kind of nitromethane according to claim 1 synthesizes and product separation device, it is characterized in that:Described flow-stopping plate is the porous plate arranging perpendicular to horizontal reactor axis direction, if be evenly provided with on porous plateA dry aperture, the middle part of porous plate is sheathed on described reactor shaft, and the outer ledge of porous plate is tightPaste the madial wall setting of horizontal reactor.
7. a kind of nitromethane according to claim 2 synthesizes and product separation device, it is characterized in that:Described crude steam kettle stirring system comprises the crude steam kettle shaft of being located at crude steam kettle inner chamber along crude steam kettle axis direction,The top of crude steam kettle shaft is connected with crude steam kettle driving mechanism after passing crude steam kettle top sidewall, described thick steamingStill driving mechanism comprises a crude steam kettle motor, and the output shaft of described crude steam kettle motor is after a crude steam kettle reductorBe connected with the front end of crude steam kettle shaft, on crude steam kettle shaft, spiral winding is shaped with two ribbons, at crude steam kettleThe bottom of shaft is provided with a leg-of-mutton stirring piece, the dual-side of described stirring piece and the madial wall of crude steam kettleParallel.
8. a kind of nitromethane according to claim 2 synthesizes and product separation device, it is characterized in that:Described crude steam kettle heating arrangements comprises a crude steam kettle chuck that is sheathed on crude steam kettle outside.
9. a kind of nitromethane according to claim 7 synthesizes and product separation device, it is characterized in that:Described pair of ribbon comprises interior ribbon and outer ribbon, and the center line edge of interior ribbon and outer ribbon is with crude steam kettle shaftCentered by the circular helix coiling of line form, the inner side edge of described interior ribbon is fixed on crude steam kettle shaft,The quantity of described outer ribbon is two, and two outer ribbons are wound on interior ribbon along the axial symmetry of crude steam kettle shaftOutside, two outer ribbons are connected with crude steam kettle shaft by support bar respectively, described two outer ribbon and stirringsThe outer side edges of sheet is all 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 true CN105601520A (en) | 2016-05-25 |
| CN105601520B 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) |
Cited By (3)
| 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 |
| CN113214086A (en) * | 2021-05-26 | 2021-08-06 | 山东中盛药化设备有限公司 | Continuous rectification and purification process of nitromethane |
| WO2024120073A1 (en) * | 2022-12-06 | 2024-06-13 | 湖北富博化工有限责任公司 | Continuous-flow synthesis method for nitromethane |
Citations (4)
| 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 |
| 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 |
| CN102161512A (en) * | 2011-02-25 | 2011-08-24 | 云南建水锰矿有限责任公司 | Material conveying method for horizontal reactor of potassium manganate |
| CN205420234U (en) * | 2016-03-16 | 2016-08-03 | 临沂远博化工有限公司 | Synthetic and result separator of nitromethane |
-
2016
- 2016-03-16 CN CN201610152401.8A patent/CN105601520B/en active Active
Patent Citations (4)
| 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 |
| 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 |
| CN102161512A (en) * | 2011-02-25 | 2011-08-24 | 云南建水锰矿有限责任公司 | Material conveying method for horizontal reactor of potassium manganate |
| CN205420234U (en) * | 2016-03-16 | 2016-08-03 | 临沂远博化工有限公司 | Synthetic and result separator of nitromethane |
Cited By (4)
| 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 |
| CN110446697A (en) * | 2017-02-27 | 2019-11-12 | 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 |
| CN113214086A (en) * | 2021-05-26 | 2021-08-06 | 山东中盛药化设备有限公司 | Continuous rectification and purification process of nitromethane |
| WO2024120073A1 (en) * | 2022-12-06 | 2024-06-13 | 湖北富博化工有限责任公司 | Continuous-flow synthesis method for nitromethane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105601520B (en) | 2018-07-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104130138B (en) | The continuous ammonification production technique of a kind of 2,4-dinitraniline | |
| CN105601520A (en) | Device for synthesizing nitromethane and separating products | |
| CN101747174A (en) | Preparation method of calcium propionate and second-effect flash distillation plant | |
| CN105771304A (en) | Double-effect countercurrent evaporation crystallization system for monosodium glutamate and working process thereof | |
| CN108129267A (en) | Low temperature Total continuity reaction system and application | |
| CN103708487B (en) | The technique of boric acid and magnesium sulfate is reclaimed from mother liquid of boric acid | |
| CN103537108B (en) | A kind of evaporation contains method and the system thereof of the ammonium sulfate of ammonium sulfite | |
| CN104109116B (en) | Method and the device thereof of one step air catalytic oxidation pyridine synthesis formic acid compounds | |
| CN106800276A (en) | Using the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid | |
| CN102275955A (en) | Method for preparing mirabilite by using sulfonated end gas absorption solution, and apparatus thereof | |
| CN103539763A (en) | Reaction separation coupling technology for continuously preparing epoxy chloropropane from dichloropropanol | |
| CN107596717B (en) | Distillation equipment for chemical production | |
| CN205420234U (en) | Synthetic and result separator of nitromethane | |
| CN104261437A (en) | Continuous potassium nitrate production system combined with liquid ammonium nitrate production | |
| CN103432974A (en) | Deaminizing and dewatering technology and special device for sodium persulfate (salt) synthetic fluid | |
| CN217473544U (en) | Potassium hydrogen peroxymonosulfate composite salt production device based on jet flow reactor | |
| CN202038873U (en) | Device adopting sulfonating tail gas absorbing liquid to prepare mirabilite | |
| CN208406934U (en) | Pseudocumene aoxidizes separator | |
| CN104147800B (en) | Two-stage methanol evaporation column and methanol evaporation technology method | |
| CN101747177A (en) | Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester | |
| CN209205307U (en) | The equipment of glycerin chlorination production dichlorohydrin | |
| CN205419831U (en) | Result separation and drying equipment of nitromethane building -up reactions | |
| CN116081886A (en) | Multistage purification treatment pool and treatment method for cellulose ether wastewater | |
| CN204685098U (en) | A kind of process units for DOTP | |
| CN220940640U (en) | Device for preparing ammonium bifluoride by AHF continuous reaction |
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 |