CN110090602A - A kind of hydrogenation reaction system - Google Patents
A kind of hydrogenation reaction system Download PDFInfo
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- CN110090602A CN110090602A CN201910449664.9A CN201910449664A CN110090602A CN 110090602 A CN110090602 A CN 110090602A CN 201910449664 A CN201910449664 A CN 201910449664A CN 110090602 A CN110090602 A CN 110090602A
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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
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/082—Controlling processes
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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
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/085—Feeding reactive fluids
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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
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
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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
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00212—Plates; Jackets; Cylinders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00539—Pressure
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/0061—Controlling the level
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00893—Feeding means for the reactants
- B01J2208/00911—Sparger-type feeding elements
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Abstract
The present invention relates to fine chemistry industry production technical fields, disclose a kind of hydrogenation reaction system.The hydrogenation reaction system includes: to add hydrogen kettle (1), this, which adds, is connected separately with charge pipe (21) plus hydrogen pipe (22), vacuum tube (23), nitrogen tube (30) and product withdraw pipe (29) on the autoclave body of hydrogen kettle, add to be provided on the outer wall of hydrogen kettle and add hydrogen kettle collet (3), hydrogen kettle is added to be internally provided with blender (2)；Cooling unit, the cooling unit include being arranged in add the cooling line inside hydrogen kettle and the condenser (10) added outside hydrogen kettle is arranged in, and the entrance and exit of cooling line is connected to the outlet of condenser and entrance respectively.Hydrogenation reaction system provided by the invention heat transfer is fast, temperature control is stable, hydrogen mix with material more evenly, improve conversion rate of products and purity, extend the noble metal catalyst service life, reduction noble metal catalyst loss, mitigate labor intensity of workers, reduce that energy consumption, the degree of automation be higher, high system safety.
Description
Technical field
The present invention relates to fine chemistry industry production technical fields, are used for agriculture more particularly to production such as 3,4-DCA
The hydrogenation reaction system of the intermediate of medicine, dyestuff and medicine etc..
Background technique
It needs to obtain reduzate using hydrogenation reaction in the field of fine chemical such as pesticide, dyestuff and medicine, for example, 3,
4- dichloroaniline is mainly used in terms of pesticide industry by product obtained from reacting 3,4- dichloronitrobenzene with hydrogen
In herbicides such as synthesis diuron, it is mainly used as azo dyes in terms of dye industry, synthesizing fungicide is used as in terms of medicine
Deng.
Currently, the synthetic reaction of 3,4-DCA is completed in adding hydrogen kettle, reaction process is as follows: by 3,4- dichloro
After nitrobenzene is transported to head tank metering, it is put into plus hydrogen kettle, unlatching stirring is manually added noble metal catalyst, is set using nitrogen
Change plus hydrogen kettle in air, after the completion of displacement, to adding hydrogen kettle collet to be passed through steam, steam off when material reaches 90 DEG C in kettle.
Later, from add hydrogen bottom portion hydrogen inlet be passed through hydrogen carry out hydrogenation reaction.During being passed through hydrogen, control hydrogen is added
Amount, while by cooling down to adding hydrogen kettle collet to inject cooling water, to control reaction temperature.After reaction, from adding hydrogen bottom
It is delivered to filtration system after the drain hole blowing in portion, hydride is filtered, noble metal catalyst takes out investment plus hydrogen kettle follows
Ring utilizes, and product mother liquid is delivered to refining step.
But in entire reaction process, there are the following problems:
1, during hydrogen reaction is added, by being controlled in kettle to adding hydrogen kettle collet that steam or cooling water is added
Temperature and pressure, heat transfer effect is poor, and temperature is unstable, is difficult to control, affects conversion rate of products and purity, reduce system
Safety.
2, using the method for adding hydrogen bottom portion that hydrogen is added, it is unfavorable for overhauling and operates, the Hydrogen distribution of addition is uneven,
To affect the efficiency of hydrogenation reaction, the consumption of hydrogen is increased, benefit is reduced.
3, when using hydrogen kettle bottom discharge reaction product is added, every batch of is required to be filtered reaction product, and noble metal is urged
Agent, which is taken out to put into again from filter, adds hydrogen kettle to be recycled, and increases the loss of noble metal catalyst, reduces noble metal and urge
The agent service life, to increase labor intensity of workers, can not reach closed simultaneously because the link often uses Manual material feeding
The requirement that metaplasia produces, reduces the safety of system.
Therefore, need to provide a kind of hydrogenation reaction device for being able to solve problem as described above at present.
Summary of the invention
That the object of the present invention is to provide a kind of heat transfers is fast, temperature control is stable, realize the self-loopa of heat transferring medium, is energy saving,
Hydrogen mixed with material more evenly, mass transfer is fast, reduce hydrogen consumption, improve conversion rate of products and purity, extends precious metal catalyst
The agent service life, the requirement for reaching closure production, mitigates labor intensity of workers, automation journey at the loss for reducing noble metal catalyst
Spend hydrogenation reaction device that is higher, being easy to operate and control, improve security of system.
To achieve the goals above, one aspect of the present invention provides a kind of hydrogenation reaction system, the hydrogenation reaction system packet
It includes: adding hydrogen kettle, should add and be connected separately with charge pipe plus hydrogen pipe, vacuum tube, nitrogen tube and product withdraw on the autoclave body of hydrogen kettle
It manages, is provided on described plus hydrogen kettle outer wall plus hydrogen kettle collet, described plus hydrogen kettle are internally provided with blender；Cooling unit, should
Cooling unit includes the condenser that the cooling line inside described plus hydrogen kettle is arranged in and is arranged in outside described plus hydrogen kettle, described
The entrance and exit of cooling line is connected to the outlet of the condenser and entrance respectively.
Preferably, it is additionally provided with multi-functional tube inside described plus hydrogen kettle, one end of the multi-functional tube and described plus hydrogen Guan Lian
It connects, distributor is connected on the other end, and the product withdraw pipe is connected on the multi-functional tube.
Preferably, one end for being connected with the distributor of the multi-functional tube extends to described plus hydrogen kettle bottom.
Preferably, the distributor includes a supervisor and multiple branch pipes, is provided with hydrogen discharge on each branch pipe
Mouthful.
Preferably, millipore filter is provided on the hydrogen discharge mouth.
Preferably, the hydrogen discharge mouth is arranged on the lower surface of the branch pipe.
Preferably, the cooling unit includes cooling coil, lower endless tube, upper endless tube and standpipe, the lower endless tube and institute
It states endless tube to connect with the lower end of the cooling coil and upper end respectively, multiple standpipes is connected on the upper endless tube, it is multiple
Standpipe is connected to the condenser.
Preferably, the cooling unit further includes apical ring pipe, which connects the multiple standpipe in the horizontal direction.
Preferably, the cooling unit further includes head tank, and one end of the head tank is connect with the outlet of the condenser,
The other end of the head tank is connect with the entrance of the cooling line.
Preferably, the hydrogenation reaction system further includes control unit, which can control described plus hydrogen kettle
It reaction temperature and pressure and stops in emergency.
Hydrogenation reaction system heat transfer provided by the invention is fast, temperature control is stable, realizes the self-loopa of heat transferring medium, saves energy
Source, hydrogen mixed with material more evenly, mass transfer is fast, reduce hydrogen consumption, improve conversion rate of products and purity, reducing energy consumption,
Extend the noble metal catalyst service life, the loss for reducing noble metal catalyst, the requirement for reaching closure production, mitigate worker's labour
Intensity, the degree of automation are higher, are easy to operate and control, high system safety.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural schematic diagram of hydrogenation reaction system according to the present invention；
Fig. 2 is the structural schematic diagram of hydrogenation reaction system according to the present invention plus hydrogen kettle；
Fig. 3 is the structural schematic diagram of the cooling unit of hydrogenation reaction system according to the present invention；
Fig. 4 is the structural schematic diagram of the distributor of hydrogenation reaction system according to the present invention.
Description of symbols
1 adds hydrogen kettle；2 blenders；3 add hydrogen kettle collet；4 multi-functional tubes；
5 distributors；51 supervisors；52 branch pipes；
6 millipore filters；7 hydrogen regulating valves；8 cooling medium regulating valves；
9 cooling coils；10 condensers；11 head tanks；12 lower endless tubes；
Endless tube on 13；14 apical ring pipes；15 cooling medium general pipeline；16 standpipes；
21 charge pipes；22 add hydrogen pipe；23 vacuum tubes；24 evacuated tubes；
251 into cooling water pipe；252 row's cooling water pipes；
261 steam leads；262 row's steam condensate (SC) pipes；
27 drainage conduits；28 cooling mediums enter pipe；29 product withdraw pipes；
30 nitrogen tubes；31 emergency discharge pipes
A feed opening；B adds hydrogen mouth；
C vacuum port；D evacuation port；
The steam inlet E1；E2 steam (vapor) outlet；
The cooling water inlet F1；F2 cooling water outlet；
G discharge gate；H water inlet；J product outlet；
K cooling medium outlet；L cooling medium entrance；M nitrogen mouth；N emergency discharge mouth
Specific embodiment
Hereinafter, detailed description of the preferred embodiments of the present invention is as follows referring to attached drawing.In addition, in explaining the present invention,
Judge illustrate in the case where may unnecessarily obscuring purport of the invention for relevant known function or structure, general
Omission illustrates it.
Fig. 1 is the overall structure diagram of hydrogenation reaction system according to the present invention, and Fig. 2 is according to the present invention plus hydrogen is anti-
System plus hydrogen kettle structural schematic diagram is answered, Fig. 3 is the overall structure of the cooling unit of hydrogenation reaction system according to the present invention
Schematic diagram, Fig. 4 are the structural schematic diagrams in the overlook direction of the distributor in hydrogenation reaction system according to the present invention.
A kind of hydrogenation reaction system provided by the invention includes adding hydrogen kettle 1 and cooling unit.Reduction is prepared in adding hydrogen kettle 1
Product, hydrogenation reaction are exothermic reactions, cooling unit for cooling down reactive material so that plus the temperature in hydrogen kettle 1 be maintained at anti-
Answer temperature.Add hydrogen kettle 1 and cooling unit hereinafter, will be described in detail respectively.
As depicted in figs. 1 and 2, add autoclave body of hydrogen kettle 1 itself preferably to use stainless steel, be connected separately with charge pipe on autoclave body
21, add hydrogen pipe 22, vacuum tube 23, nitrogen tube 30 and product withdraw pipe 29, and be provided with valve on each pipe, with control
Opening and closing or Auto-regulator flow.As shown in Fig. 2, plus being respectively arranged with feed opening A on the kettle cover of hydrogen kettle 1, adding hydrogen mouth B, vacuum port
C, nitrogen mouth M to be separately connected charge pipe 1 plus hydrogen pipe 22, vacuum tube 23, nitrogen tube 30, and is set on the side wall for adding hydrogen kettle 1
It is equipped with product outlet J, with connection product delivery pipe 29.It raw material and is urged by charge pipe 1 to adding to be added inside hydrogen kettle 1 as a result,
Agent is passed through hydrogen inside hydrogen kettle 1 to adding by adding hydrogen pipe 22, carries out vacuumizing place inside hydrogen kettle 1 to adding by vacuum tube 23
Reason, by nitrogen tube 30 to add be passed through inside hydrogen kettle 1 nitrogen with displaced air or to reaction liquid level pressure (part will be below
It is described in detail), product is expelled to by product withdraw pipe 29 and is added outside hydrogen kettle 1.In addition to this, on the kettle cover for adding hydrogen kettle 1
It is also provided with evacuation port D, evacuated tube 24 is connected on evacuation port D (also can be set emergency discharge pipe 31 and be used as urgent (peace
Bleed outlet N entirely)), when add situation (for example, hypertonia) is abnormal inside hydrogen kettle 1 when, can be with emergent evacuation.In addition, plus hydrogen
1 bottom of kettle is provided with discharge gate G, is connected with drainage conduit 27 on discharge gate G, by the drainage conduit 27, noble metal can be discharged and urge
Agent or material of releasing.
On this basis, add to be provided on the outer wall of hydrogen kettle 1 and add hydrogen kettle collet 3, adding hydrogen kettle collet 3 includes that setting is adding hydrogen
First opening on the top of kettle collet 3 and the second opening that the lower part for adding hydrogen kettle collet 3 is arranged in, first opening, which is used as, steams
Vapour entrance E1 and cooling water outlet F2, is connected in parallel steam lead 261 and row's cooling water pipe 252 in the first opening, and described second
Opening is used as steam (vapor) outlet E2 and cooling water inlet F1, the row's of being connected in parallel steam condensate (SC) pipe 262 and into cooling in the second opening
Water pipe 251.By adding hydrogen kettle collet 3, be passed through steam so that plus reach reaction temperature inside hydrogen kettle 1 so that reactive material is effective
It is reacted, or cooling water can be passed through, with the cooling plus hydrogen kettle 1 on the outer wall for adding hydrogen kettle 1, thus during absorbing reaction
The heat of releasing.
In addition, plus hydrogen kettle 1 be internally provided with blender 2, to be stirred to reaction mass, so that reaction mass and hydrogen
Reaction is come into full contact with, reaction efficiency and yield are improved.The blender 2 adds the driving source M outside hydrogen kettle 1 to connect with being arranged in, with
It can at the uniform velocity or speed change is stirred to react substance.In addition, blender 2 be preferably provided at aftermentioned upper endless tube 12 and lower endless tube 13 it
Between, to make reactive material and cooling line come into full contact with to exchange heat.Blender preferably uses disk turbine agitator, is revolving
The Radial Flow of high turbulence is caused when turning, stirring efficiency is higher, so that reactive material has sufficient time and cooling line
In cooling medium heat exchange.
In the present invention, in order to steadily control plus hydrogen kettle 1 in reaction temperature, hydrogenation reaction system of the invention
It further include cooling unit.The cooling unit includes that the cooling line being arranged in add inside hydrogen kettle 1 and being arranged in adds outside hydrogen kettle 1
Condenser 10, the entrance and exit of cooling line are connected to the outlet of condenser 10 and entrance respectively.In the shape for adding hydrogen kettle 1 to work
Under state, the circulating cooling substance in cooling unit.Specifically, liquid cooling medium is flowed in adding the cooling line in hydrogen kettle 1
Dynamic, in the process, liquid cooling medium can absorb the heat in hydrogenation reaction, cooling reactive material while itself gasifies,
Hydrogenation reaction is carried out in certain temperature range, the cooling medium of gasification is expelled to from the outlet of cooling line plus hydrogen
After 1 outside of kettle, exchanges heat, and be converted into liquid, can be realized with water and air in the condenser 10 being connected to cooling line
The self-loopa of heat transferring medium, it is energy saving.
In the present invention, preferably, select methanol as cooling medium.It is anti-in use of the invention plus hydrogen
System is answered to prepare in the embodiment of 3,4-DCA, the fusing point of 3, the 4- dichloronitrobenzene as raw material is 39~41
DEG C, the fusing point of 3,4-DCA is 69~71 DEG C, and the boiling point of methanol under normal pressure is 64.7 DEG C, in the reduction reaction,
Methanol can reach good cooling effect as cooling medium, methanol gasifying heat absorption.But the present invention does not limit cooling medium
Type is also possible to other cooling materials.
In the present invention, as a kind of embodiment of cooling unit, as depicted in figs. 1 and 2, cooling unit may include
Cooling coil 9, lower endless tube 12, upper endless tube 13 and standpipe 16, lower endless tube 12 and upper endless tube 13 lower end with cooling coil 9 respectively
It is connected with upper end, multiple standpipes 16 is connected on upper endless tube 13, multiple standpipe 16 is extended to by cooling medium outlet K to be added
1 outside of hydrogen kettle is simultaneously connected to condenser 10.
Cooling coil 9 is the pipeline being composed of the thin group's pipe of multiple groups, and multiple groups tubule group can be with rectangular or round uniform
Arrangement, but not limited to this, every group of tubule group includes multiple tubules.Lower endless tube 12 divides liquid cooling medium uniformly in the horizontal direction
Cloth, upper endless tube 13 collect gaseous cooling medium, balance amounts of pressurized gaseous, and standpipe 16 connects upper endless tube 13 and cooling medium general pipeline
15, as shown in Figure 1, three standpipes 16 are adding 1 parallel connection outside of hydrogen kettle to be connected to cooling medium general pipeline 15, cooling medium general pipeline 15
It is connected to condenser 10.
In the present invention, cooling coil 9 and multiple standpipes 16 are set along the vertical direction, to cool down reactant along the vertical direction
Matter, horizontally disposed upper endless tube 13, lower endless tube 12, to cool down reactive material in the horizontal direction, thereby, it is possible to comprehensive
Reactive material is cooled down, cooling line of the invention, can be with scattering device, to obtain in the case where not influencing other components
Take film-cooled heat as big as possible.
In addition, cooling unit can also include apical ring pipe 14, and the apical ring pipe 14 is along level side as shown in Figure 1, Figure 2 and shown in Fig. 4
To the multiple standpipes 16 of connection.Herein it should be noted that there are the gas phase portions on liquid phase part and liquid phase adding in hydrogen kettle 1
Point, apical ring pipe 14 is preferably disposed in gas phase portion, so as to cooling gas phase portion, and is conducive to cooling medium gaseous pressure
Balance, is conducive to cooling medium and is uniformly distributed.
Condenser 10 can be evaporative condenser, by cooling medium general pipeline 15 convey the gaseous cooling medium that comes into
Enter the tube side part of condenser 10, the shell side part of condenser 10 is passed through cooling water by water inlet H, by gaseous cooling medium
It is condensed into liquid, so that liquid cooling medium is again introduced into plus hydrogen kettle 1 carries out cooling operations.Can be set on condenser 10 by
Level sensing and water inlet switch valve etc. and carry out it is chain, to control liquid level.
In addition, the self-loopa in order to realize cooling medium, cooling unit can also include head tank 11, the head tank 11
One end is connect with the outlet of condenser 10, and the other end of head tank 11 and the entrance of cooling line connect, for example, such as Fig. 1 and Fig. 2
Shown, the entrance L of cooling line enters pipe 28 by cooling medium and connect with the other end of head tank 11, and cooling medium enters on pipe 28
It is provided with cooling medium regulating valve 8, to adjust the intake of cooling medium, cooling effect can be effectively controlled.It can on head tank 11
The temperature and pressure of the cooling medium in head tank are detected to be provided with temperature detector, pressure detector etc., and can be set
It is equipped with safety relief mouth, safety valve and emergency relief valve, so as to security control head tank 11.
In the present invention, by the cooling reactive material of cooling line, and condensing cooling medium by condenser 10 can
It is recycled.Illustrate that cooling medium (is preferably methanol in the present invention, carries out below based on methanol based on above-mentioned preferred embodiment
Illustrate, however, the present invention is not limited thereto) the course of work if, it is specific as follows: referring to FIG. 1, FIG. 2 and FIG. 4, to be entered by cooling medium
Mouth L is passed through liquid methanol to cooling line, after liquid methanol enters lower endless tube 12 and is uniformly distributed in the horizontal direction, along perpendicular
Histogram absorbs the heat of the reactive material near cooling coil 9 into each tubule for entering cooling coil 9 in the vertical direction
Amount, the liquid methanol after heat absorption, which heats up, to gasify, and gaseous methanol collects in upper endless tube 13, enters multiple standpipes 16 later and converges later
It flow in cooling medium general pipeline 15, is delivered to condenser 10 later, gaseous methanol is cold by being cooled down again after condenser 10
After congealing into liquid, liquid methanol, which enters head tank 11 and enters pipe 28 by cooling medium using potential difference, to be fed again into plus hydrogen kettle
In cooling line in 1, the one cycle of methanol is thus completed.In the process, since methanol gasifying absorbs heat, cooling line exists
Many channels are arranged on horizontal and vertical direction, compared with the previous process by adding hydrogen kettle collet 3 cooling, improve cooling
Efficiency, and by the intake of control methanol, can be more efficient and it be finely controlled cooling effect.Hydrogenation reaction of the invention
System has many advantages, such as heat transfer, and the temperature difference is small, temperature control is stable, energy saving because of the self-loopa of heat transferring medium fastly plus in hydrogen kettle.
Other than present invention advantage possessed by the above-mentioned cooling unit, also have the following advantages.
As shown in Figure 1, plus be additionally provided with multi-functional tube 4 inside hydrogen kettle 1, one end of the multi-functional tube 4 with plus hydrogen pipe 22 connect
Connect, be provided with distributor 5, millipore filter 6 on the other end, and product withdraw pipe 29 be connected to by product outlet J it is more
On function pipe 4.In fact, multi-functional tube 4 is to extend to extended segment (certainly, the multi-functional tube for adding 1 inside of hydrogen kettle plus hydrogen pipe 22
4 are also possible to be connected to the independent tubes for adding hydrogen pipe 22), why it is multi-functional tube 4 by the part names, is because in this hair
It is bright it is middle by this section of pipeline be applied not only to for hydrogen being passed through plus hydrogen kettle 1 inside, and again for discharging after the time period of the hydrogenation reaction was over
Product.Specifically, during the reaction, hydrogen is successively by adding hydrogen pipe 22, multi-functional tube 4, distributor 5 to be disposed to reactant
To participate in reaction in matter, after reaction terminates, the hydrogen regulating valve 7 for being set to and adding on hydrogen pipe 22 is closed, later from nitrogen mouth M
After nitrogen is passed through to carry out nitrogen displacement, it is passed through nitrogen binder, product is pressed into multi-functional tube from millipore filter 6, distributor 5
4, then be expelled in refining step by product withdraw pipe 29, and noble metal catalyst is then retained by millipore filter 6, is used for down
One batch reaction.
In the present invention, from adding hydrogen kettle top to be passed through hydrogen, to be conducive to overhaul and operate, and it is passed through the pipeline of hydrogen
It is used as that the channel of product is discharged again, without as in the past from adding hydrogen bottom portion that noble metal catalyst is discharged together, and it is only single
It is single to add the product withdraw pipe 29 of 1 side of hydrogen kettle to be discharged by being arranged in product, while increasing the noble metal catalyst service life, subtract
The link for having lacked Manual material feeding, greatly reduces labor intensity.And all processes can carry out in closure environment,
Improve the safety of system.
The characteristic to float in view of gas, it is preferable that one end for being provided with distributor 5 of multi-functional tube 4 extends to plus hydrogen
Hydrogen is passed through adds 1 bottom of hydrogen kettle as a result, reacted so that hydrogen comes into full contact with reactive material by the bottom of kettle 1.
As the form of distributor 5, the present invention does not do specifically limited, and the present invention provides a kind of distributor 5 of preferred form.
As shown in figure 4, distributor 5 provided by the invention includes a supervisor 51 and multiple branch pipes 52, hydrogen is provided on each branch pipe 52
Gas discharge outlet.The hydrogen discharge that the length of multiple branch pipes 52 is gradually successively decreased to both ends from center, and is arranged on each branch pipe 52
The quantity of mouth is designed according to the length of branch pipe 52.By distributor 5, hydrogen, which can be uniformly dispersed in, to be added in hydrogen kettle 1
Portion, hydrogen mix more evenly with material, and mass transfer is fast, reduce hydrogen consumption, while improving conversion rate of products and purity.
On this basis, it is preferable that hydrogen discharge mouth is arranged on the lower surface of branch pipe 52, and thus, it is possible to hydrogen is downward
Discharge, so that hydrogen be made to be contacted since the bottommost for adding hydrogen kettle 1 with reactive material as far as possible.
In addition, in order to prevent noble metal catalyst from entering multi-functional tube by hydrogen discharge mouth during product is discharged
4, it is preferable that millipore filter 6 is provided on hydrogen discharge mouth.The aperture of millipore filter 6 is according to noble metal catalyst
Partial size determines.
In addition to above structure, hydrogenation reaction system of the invention can also include control unit, which can control
Reaction temperature, the pressure etc. of system plus hydrogen kettle 1, and may be implemented to stop in emergency.Specifically, add temperature of charge in hydrogen kettle 1, pressure,
The parameters such as liquid level, added hydrogen；The operation of 2 motor of blender, electric current, fault-signal parameter；Join the aqueous position of condenser 10
Number；The various parameters such as temperature, pressure, the level parameter of head tank 11 can access control unit.For example, plus hydrogen material temperature in kettle
With cooling medium regulating valve 8 can chain control, to adjust cooling medium consumption；Hydrogen flowing quantity chain can be controlled with hydrogen regulating valve 7
System, to adjust hydrogen flowing quantity；Add 1 internal pressure of hydrogen kettle and exhaust-valve can chain control, when hypertonia in kettle, control unit
Exhaust-valve is opened in control, gas reactor is discharged.
In addition to this, for security of system, safety instrumented systems can also be arranged in hydrogenation reaction system of the invention
(SIS), logic unit entry condition is as follows:
A. plus hydrogen kettle temperature degree reaches high limit；
B. plus hydrogen kettle pressure reaches high limit；
Plus hydrogen kettle stirring motor failure c.；
D. it is manually pressed by emergency stopping system.
Above-mentioned condition occurs first, SIS logic unit starts following everything:
1. chain cutting hydrogen switch valve；
2. the chain cooling water water inlet valve and a drain valve opened plus hydrogen kettle collet is connected on pipeline, in adding hydrogen kettle collet
It is passed through cooling water；
3. chain opening emergency blow-down valve.
As a result, when emergency occurs, avoid that safety accident occurs.
In conclusion hydrogenation reaction system provided by the invention has, heat transfer is fast, temperature control is stable, realize heat transferring medium from
Circulation, energy saving, hydrogen mix with material more evenly, mass transfer is fast, reduce hydrogen consumption, raising conversion rate of products and purity,
Extend the noble metal catalyst service life, the loss for reducing noble metal catalyst, the requirement for reaching closure production, mitigate worker's labour
The advantages that intensity, the degree of automation are higher, be easy to operate and control, high system safety.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited thereto.At this
, can be with various simple variants of the technical solution of the present invention are made in the range of the technology design of invention, including each particular technique
Feature is combined in any suitable manner.In order to avoid unnecessary repetition, the present invention is to various combinations of possible ways
No further explanation will be given.But it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to the present invention
Protection scope.
Claims (10)
1. a kind of hydrogenation reaction system, which is characterized in that the hydrogenation reaction system includes:
Add hydrogen kettle (1), should plus hydrogen kettle (1) autoclave body on be connected separately with charge pipe (21), plus hydrogen pipe (22), vacuum tube (23),
Nitrogen tube (30) and product withdraw pipe (29) are provided with plus hydrogen kettle collet (3) on described plus hydrogen kettle (1) outer wall, it is described plus
Hydrogen kettle (1) is internally provided with blender (2)；
Cooling unit, the cooling unit include being arranged to add hydrogen described in described plus hydrogen kettle (1) internal cooling line and setting
The external condenser (10) of kettle (1), the entrance and exit of the cooling line respectively with the outlet of the condenser (10) and enter
Mouth connection.
2. hydrogenation reaction system according to claim 1, which is characterized in that be additionally provided with inside described plus hydrogen kettle (1) more
Function pipe (4), one end of the multi-functional tube (4) connect with described plus hydrogen pipe (22), are connected on the other end distributor (5), and
And the product withdraw pipe (29) is connected on the multi-functional tube (4).
3. hydrogenation reaction system according to claim 2, which is characterized in that being connected with for the multi-functional tube (4) is described
One end of distributor (5) extends to described plus hydrogen kettle (1) bottom.
4. hydrogenation reaction system according to claim 2, which is characterized in that the distributor (5) includes a supervisor
(51) and multiple branch pipes (52), hydrogen discharge mouth is provided on each branch pipe (52).
5. hydrogenation reaction system according to claim 4, which is characterized in that be provided with micropore mistake on the hydrogen discharge mouth
Filter (6).
6. hydrogenation reaction system according to claim 4, which is characterized in that the hydrogen discharge mouth is arranged in the branch pipe
(52) on lower surface.
7. hydrogenation reaction system as claimed in any of claims 1 to 6, which is characterized in that the cooling unit packet
Include cooling coil (9), lower endless tube (12), upper endless tube (13) and standpipe (16), the lower endless tube (12) and the upper endless tube
(13) it is connect respectively with the lower end of the cooling coil (9) and upper end, is connected with multiple standpipes (16) on the upper endless tube (13),
Multiple standpipe (16) is connected to the condenser (10).
8. hydrogenation reaction system according to claim 7, which is characterized in that the cooling unit further includes apical ring pipe
(14), which connects the multiple standpipe (16) in the horizontal direction.
9. hydrogenation reaction system according to claim 7, which is characterized in that the cooling unit further includes head tank
(11), one end of the head tank (11) is connect with the outlet of the condenser (10), the other end of the head tank (11) and institute
State the entrance connection of cooling line.
10. hydrogenation reaction system according to claim 1, which is characterized in that the hydrogenation reaction system further includes control
Unit, the control unit can control described plus hydrogen kettle (1) reaction temperature and pressure and stop in emergency.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910449664.9A CN110090602B (en) | 2019-05-28 | 2019-05-28 | Hydrogenation reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910449664.9A CN110090602B (en) | 2019-05-28 | 2019-05-28 | Hydrogenation reaction system |
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| Publication Number | Publication Date |
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| CN110090602A true CN110090602A (en) | 2019-08-06 |
| CN110090602B CN110090602B (en) | 2022-06-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910449664.9A Active CN110090602B (en) | 2019-05-28 | 2019-05-28 | Hydrogenation reaction system |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623644A (en) * | 2003-12-06 | 2005-06-08 | 杭州林达化工科技有限公司 | Process and equipment for internal heat exchanging catalytic reaction |
| CN203123948U (en) * | 2013-01-11 | 2013-08-14 | 山东富原化工有限公司 | Catalytic hydrogenation equipment with built-in filter |
| CN207970852U (en) * | 2018-01-30 | 2018-10-16 | 浙江鸿盛化工有限公司 | A kind of hydrogenation reaction kettle |
-
2019
- 2019-05-28 CN CN201910449664.9A patent/CN110090602B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623644A (en) * | 2003-12-06 | 2005-06-08 | 杭州林达化工科技有限公司 | Process and equipment for internal heat exchanging catalytic reaction |
| CN203123948U (en) * | 2013-01-11 | 2013-08-14 | 山东富原化工有限公司 | Catalytic hydrogenation equipment with built-in filter |
| CN207970852U (en) * | 2018-01-30 | 2018-10-16 | 浙江鸿盛化工有限公司 | A kind of hydrogenation reaction kettle |
Non-Patent Citations (2)
| Title |
|---|
| 全国安全生产教育培训教材编审委员会组织编写: "《加氢工艺作业》", 30 April 2013, 中国矿业大学出版社 * |
| 渠川瑾 编: "《反应釜》", 31 May 1992, 高等教育出版社 * |
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| CN110090602B (en) | 2022-06-21 |
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