CN108514854A - A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine - Google Patents
A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine Download PDFInfo
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- CN108514854A CN108514854A CN201810580481.6A CN201810580481A CN108514854A CN 108514854 A CN108514854 A CN 108514854A CN 201810580481 A CN201810580481 A CN 201810580481A CN 108514854 A CN108514854 A CN 108514854A
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- reactor
- tower body
- circulation flow
- distributor
- hexamethylene diamine
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/44—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers
- C07C209/48—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of nitriles
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- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides the circulation flow reactor that a kind of adipic dinitrile hydrogenation produces hexamethylene diamine, which is improved by the novelty to structure of reactor, is kept various composition contact fully good, is swift in response efficient, temperature gradient is small, and by-product is few, high income.Due to not setting agitating device, solves the problems, such as machine envelope leakage, and do not influence the normal maintenance and repair of equipment.This circulation flow reactor is reaction zone by internal guide shell subregion and moves hot-zone, vapor-liquid separation area, liquid circulation area, effectively overcomes and is just achieved the effect that expand and can and be evenly distributed using multiple " rising liquid section and descending liquid section ".The big problem of internal temperature gradient effectively is overcome by the setting of heat exchange coil, keeps reaction zone internal temperature gradient smaller, reaction yield improves.The present invention realizes good technique effect with innovative technological improvement, and progress that is reasonable for structure and being conducive to reaction has promotion prospect outstanding.
Description
Technical field
The present invention relates to chemical equipment technical fields, further to the gas, liquid, solid three-phase successive reaction of adipic dinitrile hydrogenation
A kind of and production, and in particular to circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine.
Background technology
Industrial adipic dinitrile hydrogenation production hexamethylene diamine has two kinds of high-pressure process and low-pressure process.
High-pressure process uses cobalt-copper catalyst, 100~135 DEG C of reaction temperature, 60~65MPa of pressure；Iron catalysis can also be used
Agent, 100~180 DEG C of reaction temperature, 30~35MPa of pressure.Reaction carries out in three-phase trickle bed reactor, the selection of hexamethylene diamine
Property about 90%~95%.
Low-pressure process uses skeleton nickel, iron-nickel or chromium-Raney nickel, reaction to be carried out in sodium hydroxide, ethanol solution.Instead
About 75 DEG C of temperature is answered, pressure 3MPa, the selectivity of hexamethylene diamine is up to 99%.
Adiponitrile catalytic hydrogenation method：NC(CH2)4CN+4H2─→H2N(CH2)6NH2For its key reaction formula.
Chinese utility model patent (publication number CN202506390U) discloses a kind of the anti-of adipic dinitrile hydrogenation preparing hexanediamine
It answers device, main innovation point to be the agitating device added, mass transport process can be strengthened, promote reaction, improve hydrogenation efficiency,
But agitating device is easily to occur revealing and operation troubles, therefore the application in big Chemical Manufacture can be subject to certain restrictions.
Separately there is Chinese utility model patent (publication number 204294211U) to disclose a kind of hexamethylene diamine reactor, mainly creates
New point is that its " rising liquid section and descending liquid section " completes the hydrogenation reaction and cycle of adiponitrile, but its multiple " rises liquid section and descending liquids
Section " can cause that each " pipeline section " interior multimedium is unevenly distributed and reaction zone temperature gradient is larger, multiple " to rise liquid section and descending liquids
Application of the section " in big Chemical Manufacture can be subject to certain restrictions.
Invention content
The present invention is directed to the technological deficiencies for the prior art, and it is anti-to provide a kind of circulation of adipic dinitrile hydrogenation production hexamethylene diamine
Device is answered, in such reactor to solve the prior art, material contact is bad, reaction efficiency is relatively low technical problem.
Another technical problem to be solved by the present invention is that such reactor of the prior art, rabbling mechanism are easy to cause object
Material leakage, and it is not easy to maintenance and repair.
The invention solves another technical problem be the prior art such reactor, internal temperature gradient is larger,
It is unfavorable for reaction controlling.
To realize that the above technical purpose, the present invention use following technical scheme：
A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine, including guide shell, Hydrogen distribution device, adiponitrile distribution
Device, heat exchange coil, discharge port, hydrogen outlet, reactor tower body, wherein guide shell are vertical to be set to inside reactor column body,
Hydrogen distribution device and adiponitrile distributor, the Hydrogen distribution device and hydrogen inlet are also respectively provided with inside reactor column body
It is connected, the adiponitrile distributor is connected with adiponitrile import, and heat exchange coil, discharge port are additionally provided with inside reactor column body
On the side wall of reactor tower body, hydrogen outlet is located at the top of reactor tower body.
Preferably, the upper end of guide shell is connected with horn mouth, the bell-mouthed wide-mouth portion is upward.On horn mouth it is big under
Small, lower part is connected with guide shell is more advantageous to the separation of vapour-liquid, and horn mouth can not also be set as reaction zone inside guide shell.
Preferably, the height and diameter of guide shell are respectively less than reactor tower body, inside reactor subregion is by guide shell
Reaction zone moves hot-zone, vapor-liquid separation area and liquid circulation area.One or more can be arranged in guide shell.
Preferably, Hydrogen distribution device and adiponitrile distributor are respectively to be used to flow with several in circle distributor the two
The hole of body distribution, both the Hydrogen distribution device and adiponitrile distributor are respectively positioned between reactor tower body and guide shell.
Preferably, adiponitrile distributor is connected with ethyl alcohol import, sodium hydroxide import simultaneously.It can be by ethyl alcohol, hydrogen-oxygen
Change sodium and accesses reactor.
Preferably, adiponitrile distributor is located at the bottom of Hydrogen distribution device.Keep fresh adiponitrile first mixed with recycle stock
It closes, is then contacted again with hydrogen.
Preferably, in annular space of the heat exchange coil between guide shell and reactor tower body, heat exchange coil and outside
Cooling desalted water pipeline is connected.Heat exchange coil comes into full contact in inside reactor and process stream, to maintain lower temperature
Gradient.It is preferably disposed in the annular space between reactor tower body and guide shell.Heat exchange coil may also set up outside reactor.
One or more snippets can be arranged in heat exchange coil.
Preferably, heat exchange coil is connected with external hot water piping.It can be used for heating or system heated before driving.
Preferably, reactor tower body is in vertical round tube shape, ratio of height to diameter is 5~50.
The present invention provides the circulation flow reactor that a kind of adipic dinitrile hydrogenation produces hexamethylene diamine, which passes through guide shell
It is reaction zone by inside reactor subregion, moves hot-zone, vapor-liquid separation area, liquid circulation area.Wherein reaction zone is by reactor tower body
Annular space subregion between guide shell forms, and three kinds of hydrogen, catalyst, adiponitrile media exist jointly herein；The bubble of hydrogen
The low density liquid of formation, and constantly rise under the stirring action of bubble, fresh hydrogen, catalyst, adiponitrile are constantly mended
It fills；Under the stirring action of hydrogen gas bubbles, boiling fluid is formed, the uniform mixing of gas, liquid, solid three-phase is improved, it is advantageous
Complete the hydrogenation reaction of adiponitrile.Moving hot-zone is determined by the position where heat exchange coil, corresponding to be set to reaction zone
It is interior, for the existing function of removing reaction heat of heat exchange coil, also play the function of dispersing liquid well.Vapor-liquid separation area by
The gas-phase space on horn mouth top forms, and the gas-liquid mixture of reaction zone carries out gas-liquid separation in horn mouth, and liquid drops to loudspeaker
Inside mouth, hydrogen-containing gas overflows liquid level, completes gas-liquid separation in the area, hydrogen-containing gas exports reactor by hydrogen outlet.Liquid
Body circulation area is the liquid phase component by isolating gas, is formed by race way guide shell is inside and outside, the hydrogen in reaction zone
Gas bubble retention loses, and liquid circulation does not just stop.
The present invention is improved by the novelty to structure of reactor, keeps various composition contact fully good, be swift in response effect
Rate is high, and temperature gradient is small, and by-product is few, high income.Due to not setting agitating device, the machine that solves the problems, such as seals leakage, and
And do not influence the normal maintenance and repair of equipment.This circulation flow reactor by internal guide shell subregion be reaction zone and move hot-zone,
Vapor-liquid separation area, liquid circulation area effectively overcome and just reach expansion energy and distribution using multiple " liter liquid section and descending liquid sections "
Even effect.The big problem of internal temperature gradient effectively is overcome by the setting of heat exchange coil, keeps reaction zone internal temperature terraced
Degree is smaller, and reaction yield improves.
Description of the drawings
Fig. 1 is the structural schematic diagram of the embodiment of the present invention 1, embodiment 2；
Fig. 2 is the structural scheme of mechanism of the embodiment of the present invention 3；
In figure：
1, reactor entirety 11, guide shell 12, horn mouth 13, Hydrogen distribution device
14, adiponitrile distributor 15, heat exchange coil 16, discharge port 17, hydrogen outlet
18, reactor tower body.
Specific implementation mode
The specific implementation mode of the present invention will be described in detail below.In order to avoid excessive unnecessary details,
It will not be described in detail in following embodiment to belonging to well known structure or function.Approximation used in following embodiment
Language can be used for quantitative expression, show to allow quantity to have certain variation in the case where not changing basic function.It is fixed except having
Adopted outer, technical and scientific term used in following embodiment has the phase being commonly understood by with those skilled in the art of the invention
Same meaning.
Embodiment 1
A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine, as shown in Figure 1, reactor includes reactor tower body
18, guide shell 11, horn mouth 12, Hydrogen distribution device 13, adiponitrile distributor 14, heat exchange coil 15, discharge port 16, hydrogen outlet
17 compositions.
The reactor 1 is tower body shape, ratio of height to diameter 5~50.
The 11 tower body shape of guide shell, ratio of height to diameter 10~50, upper part are connected with horn mouth 12.One can be arranged
Or it is multiple.It is reaction zone and shifting hot-zone, vapor-liquid separation area, liquid circulation area by reactor tower body 18 and part area
The horn mouth 12 is connected with guide shell 11, and its underpart is identical as 11 diameter of guide shell, and top expands, horn mouth
12 and the angle of guide shell 11 are 20~60 °.One or more can be set.Inside guide shell 11 as reaction zone can be with
Horn mouth 12 is not set.
The Hydrogen distribution device 13 is provided with multiple apertures, is circle distributor, is arranged in the outside of guide shell 11 or interior
Side can be equipped with the Hydrogen distribution device 13 of one or more different-diameters, be connected with hydrogen inlet.Preferred Hydrogen distribution device
13 are set in the annular space between reactor tower body 18 and guide shell 11.The 13 import unicom recycle hydrogen of Hydrogen distribution device
Gas.
The adiponitrile distributor 14 is provided with multiple apertures, is circle distributor, be arranged in the outside of guide shell 11 or
Inside, can be equipped with the adiponitrile distributor 14 of one or more different-diameters, the fresh adiponitrile of import unicom, also can be with
Ethyl alcohol is connected with sodium hydroxide import, can ethyl alcohol, sodium hydroxide be accessed reactor.Preferred adiponitrile distributor 14 is arranged
In annular space between reactor tower body 18 and guide shell 11.
The heat exchange coil 15 can be equipped with one or more snippets, can be set to inside reaction tower body or reaction tower is external
Portion can also be made in guide shell 11, be connected with external cooling desalted water, fully connect with process stream in inside reactor
It touches, while removing reaction heat, preferably maintains lower temperature gradient.Preferred heat exchange coil 15 is set to reactor column
In annular space between body 18 and guide shell 11.
The heat exchange coil 15 can be equipped with one or more snippets, can access hot water, before can be used for heating or driving
To system heat temperature raising.
A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine, is additionally provided with discharge port 16, hydrogen outlet 17.
The reaction zone is formed by the annular space subregion between reactor tower body 18 and guide shell 11, hydrogen, catalysis
Three kinds of agent, adiponitrile media existing region jointly.The low density liquid of the bubble formation of hydrogen, and in the stirring action of bubble
Lower constantly to rise, fresh hydrogen, catalyst, adiponitrile are continuously replenished.Under the stirring action of hydrogen gas bubbles, boiling is formed
Fluid improves uniform three-phase mixture, the advantageous hydrogenation reaction for completing adiponitrile.
The reaction zone can also be by inside guide shell 11, three kinds of hydrogen, catalyst, adiponitrile media are deposited jointly
Region.The low density liquid of the bubble formation of hydrogen, and constantly rise under the stirring action of bubble, fresh hydrogen,
Catalyst, adiponitrile are continuously replenished.Under the stirring action of hydrogen gas bubbles, boiling fluid is formed, gas, liquid, solid three are improved
Mutually equal mixing, the advantageous hydrogenation reaction for completing adiponitrile.
The shifting hot-zone is determined by the position where heat exchange coil 15, corresponding to be set in reaction zone, for
The existing function of removing reaction heat of heat exchange coil 15, also plays the function of dispersing liquid well.Preferably, heat exchange coil 15
It is interior to use desalted water.
The vapor-liquid separation area is made of the gas-phase space on 12 top of horn mouth, and the gas-liquid mixture of reaction zone exists
Horn mouth 12 carries out gas-liquid separation, and liquid drops to inside horn mouth 12, and hydrogen-containing gas overflows liquid level, and gas-liquid point is completed in the area
From hydrogen-containing gas exports reactor by hydrogen outlet 17.
The liquid circulation area is the real liguid by isolating gas, into inside or outside guide shell 11, until
Cycle under above.Hydrogen gas bubbles in reaction zone do not disappear, and liquid circulation does not just stop.
Embodiment 2
A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine, as shown in Figure 1, reactor whole 1 includes guide shell
11, Hydrogen distribution device 13, adiponitrile distributor 14, heat exchange coil 15, discharge port 16, hydrogen outlet 17, reactor tower body 18,
Middle guide shell 11 is vertical to be set to inside reactor tower body 18, and Hydrogen distribution is also respectively provided with inside reactor tower body 18
Device 13 and adiponitrile distributor 14, the Hydrogen distribution device 13 are connected with hydrogen inlet, the adiponitrile distributor 14 with oneself two
Nitrile import is connected, and heat exchange coil 15 is additionally provided with inside reactor tower body 18, discharge port 16 is located at the side of reactor tower body 18
On wall, hydrogen outlet 17 is located at the top of reactor tower body 18.
Wherein, the upper end of guide shell 11 is connected with horn mouth 12, and the wide-mouth portion of the horn mouth 12 is upward；Guide shell 11
Height and diameter are respectively less than reactor tower body 18, and inside reactor subregion is reaction zone, shifting hot-zone, vapor-liquid separation by guide shell 11
Area and liquid circulation area；Hydrogen distribution device 13 and adiponitrile distributor 14 are respectively to have several be used in circle distributor the two
The hole of fluid distrbution, both the Hydrogen distribution device 13 and adiponitrile distributor 14 are respectively positioned on reactor tower body 18 and guide shell
Between 11；Adiponitrile distributor 14 is connected with ethyl alcohol import, sodium hydroxide import simultaneously；Adiponitrile distributor 14 is located at hydrogen
The bottom of distributor 13；In annular space of the heat exchange coil 15 between guide shell 11 and reactor tower body, heat exchange coil 15 with it is outer
The cooling desalted water pipeline in portion is connected；Heat exchange coil 15 is connected with external hot water piping；Reactor tower body 18 is in vertical circle
Tube shape, ratio of height to diameter 5.
Embodiment 3
A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine, as shown in Fig. 2, reactor whole 1 includes guide shell
11, Hydrogen distribution device 13, adiponitrile distributor 14, heat exchange coil 15, discharge port 16, hydrogen outlet 17, reactor tower body 18,
Middle guide shell 11 is vertical to be set to inside reactor tower body 18, and Hydrogen distribution device 13 is also respectively provided with inside guide shell 11
With adiponitrile distributor 14, heat exchange coil 15 is also set to inside guide shell 11 accordingly, the Hydrogen distribution device 13 and hydrogen
Import is connected, and the adiponitrile distributor 14 is connected with adiponitrile import, and heat exchange plate is additionally provided with inside reactor tower body 18
Pipe 15, discharge port 16 are located on the side wall of reactor tower body 18, and hydrogen outlet 17 is located at the top of reactor tower body 18.Wherein,
Reactor tower body 18 is in vertical round tube shape, ratio of height to diameter 50.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention,
It is not intended to limit the invention.All all any modification, equivalent and improvement etc. done in the application range of the present invention, should all
It is included within protection scope of the present invention.
Claims (9)
1. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine, it is characterised in that including guide shell (11), Hydrogen distribution
Device (13), adiponitrile distributor (14), heat exchange coil (15), discharge port (16), hydrogen outlet (17), reactor tower body (18),
What wherein guide shell (11) was vertical is set to reactor tower body (18) inside, is also respectively provided with inside reactor tower body (18)
Hydrogen distribution device (13) and adiponitrile distributor (14), the Hydrogen distribution device (13) are connected with hydrogen inlet, the adiponitrile
Distributor (14) is connected with adiponitrile import, and heat exchange coil (15), discharge port are additionally provided with inside reactor tower body (18)
(16) it is located on the side wall of reactor tower body (18), hydrogen outlet (17) is located at the top of reactor tower body (18).
2. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that water conservancy diversion
The upper end of cylinder (11) is connected with horn mouth (12), and the wide-mouth portion of the horn mouth (12) is upward.
3. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that water conservancy diversion
The height and diameter of cylinder (11) are respectively less than reactor tower body (18), and inside reactor subregion is reaction zone, shifting by guide shell (11)
Hot-zone, vapor-liquid separation area and liquid circulation area.
4. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that hydrogen
Distributor (13) and adiponitrile distributor (14) are respectively to have several holes for fluid distrbution in circle distributor the two,
Both the Hydrogen distribution device (13) and adiponitrile distributor (14) are respectively positioned between reactor tower body (18) and guide shell (11)
Place.
5. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that oneself two
Nitrile distributor (14) while being connected with ethyl alcohol import, sodium hydroxide import.
6. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that oneself two
Nitrile distributor (14) is located at the bottom of Hydrogen distribution device (13).
7. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that heat exchange
Coil pipe (15) is located inside reactor, is preferable in the annular space between guide shell (11) and reactor tower body (18), heat exchange plate
Pipe (15) is connected with external cooling desalted water pipeline.
8. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that heat exchange
Coil pipe (15) is connected with external hot water piping.
9. a kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine according to claim 1, it is characterised in that reaction
Device tower body (18) is in vertical round tube shape, and ratio of height to diameter is 5~50.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810580481.6A CN108514854A (en) | 2018-06-07 | 2018-06-07 | A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810580481.6A CN108514854A (en) | 2018-06-07 | 2018-06-07 | A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine |
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| Publication Number | Publication Date |
|---|---|
| CN108514854A true CN108514854A (en) | 2018-09-11 |
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ID=63427211
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810580481.6A Withdrawn CN108514854A (en) | 2018-06-07 | 2018-06-07 | A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine |
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| CN (1) | CN108514854A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993370A (en) * | 2018-10-18 | 2018-12-14 | 辽宁石油化工大学 | A kind of spiral coil isothermal reactor and its application method |
| CN111790320A (en) * | 2019-04-09 | 2020-10-20 | 山西潞安矿业(集团)有限责任公司 | Slurry bed reactor and application thereof |
| CN114618394A (en) * | 2022-03-17 | 2022-06-14 | 北京道思克矿山装备技术有限公司 | Hexamethylene diamine synthesis system |
-
2018
- 2018-06-07 CN CN201810580481.6A patent/CN108514854A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993370A (en) * | 2018-10-18 | 2018-12-14 | 辽宁石油化工大学 | A kind of spiral coil isothermal reactor and its application method |
| CN108993370B (en) * | 2018-10-18 | 2021-01-12 | 辽宁石油化工大学 | Spiral coil isothermal reactor and use method thereof |
| CN111790320A (en) * | 2019-04-09 | 2020-10-20 | 山西潞安矿业(集团)有限责任公司 | Slurry bed reactor and application thereof |
| CN111790320B (en) * | 2019-04-09 | 2022-11-22 | 山西潞安矿业(集团)有限责任公司 | Slurry bed reactor and application thereof |
| CN114618394A (en) * | 2022-03-17 | 2022-06-14 | 北京道思克矿山装备技术有限公司 | Hexamethylene diamine synthesis system |
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Application publication date: 20180911 |
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