CN104557556B - A kind of device and process for producing isooctyl ester nitrate - Google Patents
A kind of device and process for producing isooctyl ester nitrate Download PDFInfo
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- CN104557556B CN104557556B CN201510037012.6A CN201510037012A CN104557556B CN 104557556 B CN104557556 B CN 104557556B CN 201510037012 A CN201510037012 A CN 201510037012A CN 104557556 B CN104557556 B CN 104557556B
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Abstract
The process of isooctyl ester nitrate is produced the invention discloses a kind of device for producing isooctyl ester nitrate and using the device, described device includes feed system, chilldown system, hybrid system, reaction system, reception system and circulation bath system, specifically a kind of efficiently and safely to produce the commercial plant of isooctyl ester nitrate；The problem of present invention mainly overcomes the potential safety hazard and relatively low production efficiency that prior art is present, using the attachment means of micro-mixer and the shell-and-tube reactor of alloy material, the feature that the efficient heat transfer mass transfer ability that has using the device and being easy to is directly amplified, make the conversion ratio of isooctanol up to more than 99%, the yield of isooctyl ester nitrate is up to more than 98%；Reaction serialization can be achieved with higher processing safety and reaction selectivity in the present invention, to strengthening and ensureing that the highly effective and safe of isooctyl ester nitrate produces significant.
Description
Technical field
The present invention relates to a kind of microreactor device, specifically can efficiently and safely to produce nitric acid different pungent for one kind
The microreactor device of ester and the process that isooctyl ester nitrate is produced with the device.
Background technology
Micro-reacting tcchnology originating from eighties of last century nineties, micro-reacting tcchnology be initially in the form of chip reactor,
Upper simple passage, as this chip reactor is in the extensive use of field of bioanalysis, microreactor are etched on chip
Advantage is gradually highlighted, and is gradually come to realise microreactor and is better than conventional efficient mass-and heat-transfer ability, then by micro- reaction
Device is applied to the field of chemical synthesis；Microreactor is developed into today, no longer simple to pursue the small of reaction channel, but logical
The design of structure is crossed, by the fluidic structures of macroscopic view, changes the liquid stream of liquid flow pattern formation infinitesimal yardstick, shape by reaction channel
Into efficient quickly mass-and heat-transfer.For exothermic reaction, with traditional tank reactor, reaction liberated heat can not be timely
Release, reaction temperature is unable to precise control.Therefore reaction speed is usually any limitation as with reaction scale by artificial, otherwise may
It can explode.By taking the industrial production of isooctyl ester nitrate as an example：Isooctyl ester nitrate is a kind of diesel cetane-number of function admirable
Modifier, it is possible to decrease the spontaneous combustion activation energy of diesel oil, improves flammability.The existing production technology of the product is：Using the concentrated sulfuric acid as
With nitric acid nitration reaction generation isooctyl ester nitrate occurs for catalyst, isooctanol, and reaction equation is as follows：
But the course of reaction of the product is abnormally dangerous, on the one hand because nitration reaction is strongly exothermic, the water of generation makes the concentrated sulfuric acid
It is diluted, also releases big calorimetric, once industry amplification such as more than 2000L reaction, the huge heat of generation can not turn in time
Removal is gone, and isooctyl ester nitrate continuity will be caused to decompose, or even is exploded, and limits production capacity；The traditional autoclave of another aspect
Time-consuming for dropwise addition, and product is contacted for a long time with strong acid, is substantially reduced the decomposition temperature of product, is greatly increased risk of explosion.
The content of the invention
The problem of present invention overcomes the potential safety hazard and relatively low production efficiency that prior art is present, using by a series of micro- mixed
The attachment means production isooctyl ester nitrate that the shell-and-tube reactor of clutch and alloy material is constituted, using the device have it is efficient
The feature that heat and mass ability and being easy to is directly amplified, makes the conversion ratio of isooctanol up to more than 99%, the yield of isooctyl ester nitrate
Up to more than 98%；The present invention has higher processing safety and selectivity, and reaction serialization can be achieved, to strengthening and ensureing nitre
The highly effective and safe production of the different monooctyl ester of acid is significant.Concrete technical scheme is as follows.
The application provides a kind of device for producing isooctyl ester nitrate, and described device includes feed system, chilldown system, mixing
System, reaction system, reception system and circulation bath system；The feed system includes raw material storage tank and feed pump, cleaning pump；Institute
Stating chilldown system includes micro- heat exchanger；The hybrid system includes at least one micro-mixer；The reaction system includes tubulation
Reactor；The reception system includes receiving storage tank；The raw material storage tank, feed pump, micro- heat exchanger, micro-mixer, tubulation are anti-
Answer device and receive storage tank and be connected in series；The chilldown system, hybrid system and reaction system are placed in circulation bath system；It is described micro-
Blender uses for micro-mixer A, B or C or multiple A, B, C parallel combinations.
Further, the feed system of described device includes two raw material storage tanks and two feed pumps, a cleanings
Pump；The chilldown system includes two micro- heat exchangers；The hybrid system includes micro-mixer；The reaction system includes one section
Shell-and-tube reactor；The reception system includes receiving storage tank；The raw material storage tank, feed pump, micro- heat exchanger, micro-mixer, row
Pipe reactor and reception storage tank are connected in series；The chilldown system, hybrid system and reaction system are placed in circulation bath system；Institute
Circulation bath system can also be respectively placed in by stating chilldown system, hybrid system and reaction system；The micro-mixer is micro-mixer
A, B or C or multiple A, B, C parallel combinations are used.
Further, said apparatus is applied to the process of production isooctyl ester nitrate, comprises the steps of：
1）By the nitration mixture of fuming nitric aicd and the concentrated sulfuric acid, raw material isooctanol respectively by raw material storage tank, feed pump, through micro- heat exchange
Device enters the volume flow ratio of the two entrances of micro-mixer, regulation and control nitration mixture and isooctanol, control fuming nitric aicd and isooctanol
Mol ratio is 0.95 ~ 1.5, preferably 1 ~ 1.02, and the mol ratio of the concentrated sulfuric acid and fuming nitric aicd is 0.6 ~ 2.0；
2）Two stock material liquid are mixed in micro-mixer, are exited into shell-and-tube reactor by outlet and are further reacted, anti-from tubulation
Device outlet is answered to exit into reception storage tank；
3）The product that reception storage tank is obtained separates spent acid layer, and organic layer is removed water after washing, alkali cleaning and washing again
Product isooctyl ester nitrate.
Further, above-mentioned reaction is 0 ~ 10oCarried out under the conditions of C, receive product 0 ~ 10oC conditions are carried out.There is document to grind
Study carefully report, isooctyl ester nitrate is issued to 68 in nitration mixture conditionoC can trigger continuity to decompose, and temperature rises sharply 200oMore than C, significantly
Increase risk of explosion;In addition, by experiment, it is also observed that isooctyl ester nitrate and nitration mixture are 45oDuring more than C, the rapid blackening of color,
And emerged along with smoke and gas bubble, it is easy to explode；Equally, higher reception temperature also easily triggers blast, dangerous.
Preferably, the structure of micro-mixer A described in said apparatus is：There are the flat sheet combinations of micro-structural into one by two
Individual main channel, the geometry of the passage is a kind of complicated ramp shaped structure；Fluid can constantly rise in flow process and
Decline, so as to realize the separating for several times of fluid and reconfigure；Micro-mixer A flux range is 0.5 ~ 250L/h.
Preferably, the structure of micro-mixer B described in said apparatus is：Passage and slit with shelving wall with two
Shape chiasma type passage；After liquid injects mixed cell by channel design convection current of two of the blender with shelving wall,
The tens of two kinds periodic structures for treating the flowing thin layer of mixed flow body are formed by slit-shaped chiasma type passage, layer fluid is in entrance
The vertical upward out blender in side of stream；Micro-mixer B flux range is 0.04 ~ 2.5L/h.
Preferably, the structure of micro-mixer C described in said apparatus is：Hybrid chip with series of different is tight
It is close arranged together；It is many between fluid is realized in the central area that fluid flows through different types of hybrid chip by different passages
Quick mixing can be achieved in level parcel moment diffusion；Micro-mixer C flux range is 12 ~ 30000L/h.
Preferably, the internal structure of micro- heat exchanger described in said apparatus is to be arranged by several or hundreds of micro-structural plates
Form, by high-precision laser welded seal, form micro-tubular inner chamber, heat exchange area is big.
Preferably, the shell-and-tube reactor described in said apparatus be by it is a series of can the alloy of independent assortment, enamel or not
The texture pipelines such as steel of becoming rusty are constituted.
Further, feed system described in above-mentioned device include three raw material storage tanks and four feed pumps, one it is clear
Wash storage tank；The chilldown system includes three micro- heat exchangers；The hybrid system includes at least two micro-mixers；The reaction
System includes two sections of shell-and-tube reactors；The reception system includes washing system and Distallation systm；The washing system includes two
Individual feed storage tank, three feed pumps, three separators, three reservoirs and at least two micro-mixers；The Distallation systm bag
Include a feed pump and a destilling tower；Micro- heat exchanger of the raw material storage tank of the feed system, feed pump and chilldown system, instead
Answer micro-mixer, the shell-and-tube reactor of system, the separator of washing system, reservoir, micro-mixer and Distallation systm enter
Material pump, destilling tower are connected in series；The chilldown system, hybrid system and reaction system are placed in circulation bath system；The microring array
Device uses for parallel combinations one or more kinds of in A, B or C.
Further, the feed system described in above-mentioned device include three raw material storage tanks and four feed pumps, one
Clean storage tank；The chilldown system includes three micro- heat exchangers；The hybrid system includes two micro-mixers, i.e. micro-mixer
A and B；The reaction system includes two sections of shell-and-tube reactors；The reception system includes washing system and Distallation systm；It is described to wash
Wash system including two feed storage tanks, three feed pumps, three separators, three reservoirs and two micro-mixer C, i.e. C1 and
C2；The Distallation systm includes a feed pump and a destilling tower；Raw material storage tank, feed pump and the precooling of the feed system
Micro- heat exchanger of system, the micro-mixer A or B of reaction system, shell-and-tube reactor are the separator of washing system, reservoir, micro- mixed
The feed pump of clutch C and Distallation systm, destilling tower are connected in series；The chilldown system, hybrid system and reaction system are placed in
Circulate bath system；The chilldown system, hybrid system and reaction system can also be respectively placed in circulation bath system；Knot to be produced
Cleaning solvent in beam, cleaning storage tank is squeezed into micro-reaction device the cleaning for carrying out whole system by feed pump.
When the above-mentioned device including many micro-mixers is applied into production isooctyl ester nitrate, comprise the steps of：
1）Fuming nitric aicd and the concentrated sulfuric acid are entered micro-mixer A's by raw material storage tank, feed pump, through micro- heat exchanger respectively
Two entrances, regulation and control fuming nitric aicd and the concentrated sulfuric acid volume flow ratio, control the concentrated sulfuric acid and fuming nitric aicd mol ratio be 0.6 ~
2.0, two stock material liquid are mixed in micro-mixer A, and exiting into shell-and-tube reactor by outlet further reacts, from shell-and-tube reactor
Outlet exits into micro-mixer B；
2）Raw material isooctanol enters micro-mixer B by raw material storage tank, feed pump, through micro- heat exchanger, is obtained with step 1
Nitration mixture is mixed in micro-mixer B, and exiting into shell-and-tube reactor by outlet, further reaction forms acid ester mixtures, and regulation and control are mixed
The volume flow ratio of acid and isooctanol, the mol ratio for controlling fuming nitric aicd and isooctanol is 0.95 ~ 1.5, preferably 1 ~ 1.02；Instead
It is 0 ~ 10 to answer temperatureoC；
3）Step（2）Obtain acid ester mixtures and obtain ester liquid through separator, reservoir, then micro-mixer is squeezed into by feed pump
C1 and the alkali lye mixing, washing that C1 is squeezed into by feed storage tank and feed pump, flow out alkali ester mixed liquor, then through micro-mixer C2 by water
In washing, Distallation systm product isooctyl ester nitrate is obtained through distilling column distillation；It is 0 ~ 10 to receive temperatureoC。
Specifically, said apparatus is for producing the flow of isooctyl ester nitrate：Fuming nitric aicd in feed storage tank passes through
Feed pump is squeezed into heat exchanger, is connected to micro-mixer A one of entrance by outlet after heat exchange；In feed storage tank
Sulfuric acid is squeezed into heat exchanger by feed pump, is connected to micro-mixer A another entrance by outlet after heat exchange；The two
Mixed in micro-mixer A and nitration mixture is formed by A outlet inflow shell-and-tube reactor, nitration mixture is entered micro- mixed by shell-and-tube reactor outlet
A clutch B entrance；Isooctanol in feed storage tank is squeezed into heat exchanger by feed pump, is connected after heat exchange by outlet
To micro-mixer B another entrance；It is anti-that isooctyl acid and the nitration mixture hybrid reaction in micro-mixer B flow into tubulation by B outlet
Answer further to react in device and form acid ester mixtures, acid ester mixtures enter washing system by shell-and-tube reactor outlet；Acid esters
Sedimentation separation goes out spent acid to mixture in the separator, and ester liquid then enters in reservoir, then squeezes into micro-mixer C1's through feed pump
Alkali lye in one entrance, feed storage tank is squeezed into micro-mixer C1 another entrance by feed pump, and the two is in micro-mixer C1
Middle mixing, washing, is exited into separator by outlet；Go out buck in middle alkali ester mixed liquor sedimentation separation, ester liquid then enters storage
In liquid device, then the water squeezed into through feed pump in a micro-mixer C2 entrance, feed storage tank squeezes into micro-mixer by feed pump
C2 another entrance, the two mixing, washing in micro-mixer C2, is exited into separator by outlet；It is mixed in reclaimed water ester
Close liquid sedimentation separation and go out waste water, ester liquid then enters in reservoir, then is squeezed into through feed pump in destilling tower, and moisture is distilled off, obtains
To qualified products；To be produced to terminate, the cleaning solvent in cleaning storage tank is squeezed into micro-reaction device by feed pump is entirely
The cleaning of system.
Beneficial effect：
1）Raw material potent mixing in micro-mixer, reacts the big calorimetric of release by microreactor device fast transfer to cold
In bath system, reaction reaches second level completion；Meanwhile, the big flux of micro-mixer determines that this nitration reaction can realize that industry is big
The production of scale, because the device provided by the application becomes big, directly if it need to amplify without the volume by equipment
It is that increase reactor flux change in other words arranged side by side can be achieved with；
2）React under the conditions of 0 ~ 10 DEG C and carry out it also avoid the safety risks that pyroreaction is brought；
3）When the mol ratio of nitric acid and isooctanol needed for reaction is 1 ~ 1.02, the conversion ratio of isooctanol and nitric acid is all up to
99%, yield 98%, the acid composition after reaction terminates is single sulfuric acid catalyst, has saved cost of material, has reduced nitration mixture point
From and recovery difficult.
Brief description of the drawings
Fig. 1 is the installation drawing of production isooctyl ester nitrate；
Fig. 2 is the installation drawing of production isooctyl ester nitrate；
Fig. 3 is micro-mixer A cut-away view；
Fig. 4 is micro-mixer B cut-away view；
Fig. 5 is micro-mixer C cut-away view；
In figure:1- feed systems, 2- chilldown systems, 3- hybrid systems, 4- reaction systems, 5- receives system, 6- circulation baths
System, 7- washing systems, 8- Distallation systms, 11- raw material storage tanks V1,12- raw material storage tank V2,13- raw material storage tank V3,14- charging
Pump P1,15- feed pump P2,16- feed pump P3,21- heat exchanger E1,22- heat exchanger E2,31- micro-mixer, the reaction of 41- tubulations
Device, 51- receives storage tank, 206- feed storage tanks V01,207- feed storage tank V02,208- feed storage tank V03,209- feed storage tank
V04,210- feed storage tank V05,211- cleaning storage tank V06,212- feed pump P01,213- feed pump P02,214- feed pump
P03,215- feed pump P04,216- feed pump P05,217- feed pump P06,218- feed pump P07,219- feed pump P08,
220- feed pumps P09,221- heat exchanger E01,222- heat exchanger E02,223- heat exchanger E03,224- micro-mixer A, 225- is micro-
Blender B, 226- micro-mixer C1,227- micro-mixer C2,228- shell-and-tube reactor 1,229- shell-and-tube reactors 2,230- points
From device S1,231- separators S2,232- separator S3,233- reservoir B1,234- reservoir B2,325- reservoir B3,236-
Destilling tower.
Embodiment
The present invention is further explained with reference to the accompanying drawings and examples.
As shown in figure 1, by taking the device with a blender as an example, the microreactor device for producing isooctyl ester nitrate
Connected mode is as follows：
Described device includes feed system 1, and chilldown system 2, hybrid system 3, reaction system 4 receives system 5, circulation bath
System 6, the raw material storage tank V1 of the feed system is connected to feed pump P1, then is connected to the one of micro-mixer by heat exchanger E1
Individual entrance；Raw material storage tank V2 is connected to feed pump P2, then is connected to by heat exchanger E2 another entrance of micro-mixer 31；It is micro-
The outlet of blender 31 is connected to shell-and-tube reactor 41, and shell-and-tube reactor outlet is connected in reception storage tank 51；Chilldown system 2,
Hybrid system 3 and reaction system 4 are respectively placed in circulation bath 6, temperature setting 0 ~ 10oC；Heat exchanger exit, micro-mixer outlet
Temperature monitor is set respectively with shell-and-tube reactor outlet, feed pump rear end and reception storage tank front end set pressure sensing respectively
Device.
As shown in Fig. 2 being used for producing the company of the microreactor device of isooctyl ester nitrate for many micro-mixer conjunctive uses
Connect mode：Wherein receive system and be divided into washing system 7 and Distallation systm 8 again；Fuming nitric aicd in feed storage tank V01 passes through charging
Pump P01 is squeezed into heat exchanger E01, is connected to micro-mixer A one of entrance by outlet after heat exchange；Feed storage tank
Sulfuric acid in V02 is squeezed into heat exchanger E02 by feed pump P02, and the another of micro-mixer A is connected to by outlet after heat exchange
Individual entrance；The two is mixed in micro-mixer A forms nitration mixture by A outlet inflow shell-and-tube reactor 1, and nitration mixture is by shell-and-tube reactor
1 outlet enters a micro-mixer B entrance；Isooctanol in feed storage tank V03 squeezes into heat exchanger by feed pump P03
In E03, micro-mixer B another entrance is connected to by outlet after heat exchange；Isooctyl acid and nitration mixture are mixed in micro-mixer B
Reaction is closed by further reaction forms acid ester mixtures in B outlet inflow shell-and-tube reactor 2, acid ester mixtures are reacted by tubulation
The outlet of device 2 enters washing system 7；Acid ester mixtures sedimentation separation in separator S1 goes out spent acid, and ester liquid then enters reservoir
In B1, then the alkali lye squeezed into through feed pump P06 in a micro-mixer C1 entrance, feed storage tank V04 is squeezed into by feed pump P05
Micro-mixer C1 another entrance, the two mixing, washing in micro-mixer C1, is exited into separator S2 by outlet；
The mixed liquor sedimentation separation of alkali ester goes out buck in S2, and ester liquid then enters in reservoir B2, then squeezes into micro-mixer through feed pump P07
Water in a C2 entrance, feed storage tank V05 is squeezed into micro-mixer C2 another entrance by feed pump P08, and the two is micro-
Mixing, washing in blender C2, is exited into separator S3 by outlet；Go out waste water in S3 reclaimed water ester mixed liquor sedimentation separations,
Ester liquid then enters in reservoir B3, then is squeezed into through feed pump P09 in destilling tower, and moisture is distilled off, qualified products are obtained.It is to be generated
Production terminates, and the cleaning solvent in cleaning storage tank V06 is squeezed into micro-reaction device the cleaning for carrying out whole system by feed pump P04；
In heat exchanger exit, micro-mixer outlet and shell-and-tube reactor outlet, temperature monitor, feed pump rear end and liquid storage are set respectively
Device front end sets pressure sensor respectively.
Fig. 3 is micro-mixer A internal structure schematic diagram：Micro-mixer A by two have micro-structural flat sheet combinations into
One main channel, the geometry of the passage is a kind of complicated ramp shaped structure；Fluid can constantly rise in flow process
And decline, so as to realize the separating for several times of fluid and reconfigure.
Fig. 4 is micro-mixer B internal structure schematic diagram：Micro-mixer B has two passages with shelving wall and narrow
Gap-like chiasma type passage；When liquid passes through channel design convection current injection mixed cell of two of the blender with shelving wall
Afterwards, the tens of two kinds periodic structures for treating the flowing thin layer of mixed flow body are formed by slit-shaped chiasma type passage, layer fluid exists
The upward out blender in the vertical side of entrance stream.
Fig. 5 is micro-mixer C internal structure schematic diagram：Micro-mixer C has the hybrid chip of series of different
It is arranged closely together；Between fluid being realized when the central area that fluid flows through different types of hybrid chip by different passages
Quick mixing can be achieved in multi-level parcel moment diffusion.
Embodiment 1
With Fig. 1 microreactor device, the nitration mixture of fuming nitric aicd and the concentrated sulfuric acid is added in raw material storage tank V1, and isooctanol adds
Enter into raw material storage tank V2, the volume flow ratio of regulation and control nitration mixture and isooctanol, the mol ratio for controlling fuming nitric aicd and isooctanol is
1.1, the mol ratio of the concentrated sulfuric acid and fuming nitric aicd is 1.1, is fed respectively by feed pump P1, feed pump P2, and charging overall flow rate is
20L/h, thermostated cooling bath is set to 0 ~ 10oC, two stock material liquid enter mixed are incorporated in shell-and-tube reactor of micro-mixer A and further reacted,
Reaction solution is entered in reception storage tank, and stratification, acid solution is separated, and ester layer washing, alkali cleaning and is washed to neutrality again.Product nitric acid
The purity 99.6% of different monooctyl ester, yield 98.4%.
Embodiment 2
Process is with example 1, and it is 2.0L/h only to change charging overall flow rate, uses micro-mixer B.Product isooctyl ester nitrate it is pure
Spend for 99.7%, yield 99%.
Embodiment 3
Process is with example 1, and it is 80L/h only to change charging overall flow rate, uses micro-mixer C.Product isooctyl ester nitrate it is pure
Spend for 99.2%, yield 98.6%.
Embodiment 4
Process is with example 1, and it is 0 ~ 2 to set chilldown system and the thermostated cooling bath of hybrid systemoC, sets the perseverance of reaction system
Warm cryostat is 5 ~ 10oC.The purity of product isooctyl ester nitrate is 99.7%, yield 98.7%.
Embodiment 5
With Fig. 2 microreactor device, the fuming nitric aicd in feed storage tank V01 squeezes into heat exchanger E01 by feed pump P01
In, micro-mixer A one of entrance is connected to by outlet after heat exchange；Sulfuric acid in feed storage tank V02 passes through charging
Pump P02 is squeezed into heat exchanger E02, is connected to micro-mixer A another entrance by outlet after heat exchange；The two is in microring array
Mixed in device A and the volume flow ratio that shell-and-tube reactor 1 forms nitration mixture, the regulation and control concentrated sulfuric acid and fuming nitric aicd is flowed into by A outlet, control
The mol ratio of the concentrated sulfuric acid and fuming nitric aicd processed is 1.6, and nitration mixture is exported by shell-and-tube reactor 1 to be entered one of micro-mixer B and enter
Mouthful；Charging overall flow rate is 25L/h；Isooctanol in feed storage tank V03 is squeezed into heat exchanger E03 by feed pump P03, by changing
The volume flow ratio of micro-mixer B another entrance, regulation and control nitration mixture and isooctanol is connected to after heat by outlet, smoke nitre is controlled
The mol ratio of acid and isooctanol is 1；Thermostated cooling bath is set to 0 ~ 10oC；Isooctyl acid and nitration mixture in micro-mixer B hybrid reaction by B
Outlet flow into shell-and-tube reactor 2 that further reaction forms acid ester mixtures, acid ester mixtures by shell-and-tube reactor 2 export into
Enter to washing system；Acid ester mixtures sedimentation separation in separator S1 goes out spent acid, and ester liquid then enters in reservoir B1, then through entering
The alkali lye that material pump P06 is squeezed into a micro-mixer C1 entrance, feed storage tank V04 squeezes into the another of micro-mixer C1 by feed pump
One entrance, the two mixing, washing in micro-mixer C1, is exited into separator S2 by outlet；Alkali ester is mixed in S2
Liquid sedimentation separation goes out buck, and ester liquid then enters in reservoir B2, then squeezes into through feed pump P07 a micro-mixer C2 entrance,
Water in feed storage tank V05 is squeezed into micro-mixer C2 another entrance by feed pump P08, and the two is mixed in micro-mixer C2
Washing, is exited into separator S3 by outlet；Go out waste water in S3 reclaimed water ester mixed liquor sedimentation separations, ester liquid then enters liquid storage
In device B3, then squeeze into destilling tower through feed pump P09, moisture is distilled off, the purity for obtaining product isooctyl ester nitrate is
99.8%, yield 98.8%.
The foregoing is intended to be a preferred embodiment of the present invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art in the technical scope of present disclosure, technique according to the invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (4)
1. a kind of device for producing isooctyl ester nitrate, it is characterised in that described device includes feed system, chilldown system, mixing
System, reaction system, reception system and circulation bath system；The feed system includes raw material storage tank and feed pump；The precooling
System includes micro- heat exchanger；The hybrid system includes at least one micro-mixer；The reaction system includes shell-and-tube reactor；
The reception system includes receiving storage tank；The raw material storage tank, feed pump, micro- heat exchanger, micro-mixer, shell-and-tube reactor and
Storage tank is received to be connected in series；The chilldown system, hybrid system and reaction system are placed in circulation bath system；Micro- heat exchanger
Internal structure is to be formed by several or hundreds of micro-structural plate arrangements, by laser welded seal, forms micro-tubular inner chamber, changes
Hot area is big, and the micro-mixer uses for micro-mixer A, B or C or multiple A, B, C parallel combinations, its micro-mixer A's
Structure is：By two flat sheet combinations with micro-structural into a main channel, the geometry of the passage is a kind of complicated slope
Shape structure；Fluid in flow process can continuous raising and lowering, so as to realize the separating for several times of fluid and reconfigure；Its
Micro-mixer B structure is：With two passages with shelving wall and slit-shaped chiasma type passage；When liquid passes through the mixing
After channel design convection current injection mixed cell of two of device with shelving wall, tens of are formed by slit-shaped chiasma type passage
Two kinds treat mixed flow body flowing thin layer periodic structure, layer fluid is in the upward out blender in the vertical side of entrance stream；Its is micro-
Blender C structure is：Hybrid chip with series of different is arranged closely together；When fluid is led to by different
Realize that multi-level parcel moment diffusion can be achieved quickly to mix between fluid in the central area that road flows through different types of hybrid chip
Close.
2. the device described in application claim 1 produces the process of isooctyl ester nitrate, comprise the steps of：
1）The nitration mixture of fuming nitric aicd and the concentrated sulfuric acid, raw material isooctanol are entered by raw material storage tank, feed pump, through micro- heat exchanger respectively
Enter mole of the volume flow ratio of the two entrances of micro-mixer, regulation and control nitration mixture and isooctanol, control fuming nitric aicd and isooctanol
Than for 0.95 ~ 1.5, the mol ratio of the concentrated sulfuric acid and fuming nitric aicd is 0.6 ~ 2.0；
2）Two stock material liquid are mixed in micro-mixer, are exited into shell-and-tube reactor by outlet and are further reacted, from shell-and-tube reactor
Outlet exits into reception storage tank；
3）The product that reception storage tank is obtained separates spent acid layer, and organic layer removes water to obtain product after washing, alkali cleaning and washing again
Isooctyl ester nitrate.
3. the process of production isooctyl ester nitrate according to claim 2, it is characterised in that：The reaction is 0 ~ 10oC
Under the conditions of carry out, receive product 0 ~ 10oCarried out under the conditions of C.
4. the device of production isooctyl ester nitrate according to claim 1, it is characterised in that：Described shell-and-tube reactor is served as reasons
It is a series of can the texture pipeline of the alloy of independent assortment, enamel or stainless steel constitute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN105330549A (en) * | 2015-11-20 | 2016-02-17 | 南京理工大学 | Method for preparing isooctyl nitrate in micro-channel reactor |
| CN106045860A (en) * | 2016-06-27 | 2016-10-26 | 山东益丰生化环保股份有限公司 | Novel efficient cetane number improver and preparation method thereof |
| CN106699569A (en) * | 2016-11-10 | 2017-05-24 | 庄晓东 | Continuous production process of isooctyl nitrate |
| CN107935857A (en) * | 2017-12-11 | 2018-04-20 | 中国科学院大连化学物理研究所 | A kind of production method of isooctyl ester nitrate |
| CN108147968A (en) * | 2018-01-02 | 2018-06-12 | 山东益丰生化环保股份有限公司 | A kind of continuous aftertreatment technology of isooctyl ester nitrate and equipment |
| CN109574849A (en) * | 2018-12-17 | 2019-04-05 | 山东益丰生化环保股份有限公司 | A kind of preparation method of cetane number improver |
| CN110683953B (en) * | 2019-05-15 | 2021-01-15 | 中国科学院大连化学物理研究所 | Method for continuously synthesizing isooctyl nitrate and extracting residual acid in isooctyl nitrate in microreactor |
| CN110803991A (en) * | 2019-12-03 | 2020-02-18 | 江西西林科股份有限公司 | Method for synthesizing isooctyl nitrate by micro-reaction technology |
| CN113511982B (en) * | 2020-04-10 | 2023-04-07 | 中国科学院大连化学物理研究所 | Synthetic method of hydroxyethyl hydrazine nitrate |
| CN115124426A (en) * | 2022-03-31 | 2022-09-30 | 西安万德能源化学股份有限公司 | Environment-friendly continuous production process and system for isopropyl nitrate |
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| EP0129995B2 (en) * | 1983-06-24 | 1993-09-08 | Aeci Limited | A process for the manufacture of nitric acid esters |
| US4479905A (en) * | 1983-09-19 | 1984-10-30 | Ethyl Corporation | Nitration process |
| CN1017146B (en) * | 1987-08-24 | 1992-06-24 | 西安近代化学研究所 | Process for synthesizing isooctyl nitrate |
| CN101462962B (en) * | 2007-12-19 | 2012-04-11 | 中国科学院大连化学物理研究所 | Method for synthesizing isooctyl nitrate and microchannel reactor |
| CN101698646B (en) * | 2009-11-04 | 2012-10-03 | 西安万德能源化学股份有限公司 | Continuous production technology for isooctyl nitrate |
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